Document QJo4Emj1v09V0km9DDKYrNk3v

IN THE UNITED STATES DISTRICT COURT FOR THE DISTRICT OF NEVADA NEVADA POWER COMPANY A NEVADA CORPORATION PLAINTIFF, VS MONSANTO COMPANY, A FOREIGN CORPORATION; GENERAL ELECTRIC COMPANY, A FOREIGN CORPORATION; WESTINGHOUSE ELECTRIC CORPORATION, A FOREIGN CORPORATION; AND DOES I XXV, INCLUSIVE, ' DEFENDENTS. CV-S-89-555-LDG-LRL EXHIBITS 19 - 37 TO THE DEPOSITION OF ROBERT EMMET KELLY, M.D. VOLUME I ' TAKEN ON FEBRUARY 15, 1994 MARTIN & ASSOCIATES CERTIFIED COURT REPORTERS 2200 MARKET STREET, SUITE 412 GALVESTON, TEXAS 77550 (409) 762-2222 * FAX (409) 762-8040 WATER PCB-SD0000030721 TO CHEMICAL COMPANY IT . LOOII (. ' " i i NEV 011249 WATER PCB-SD0000030722 N V 011312 WATER PCB-SD0000030723 810.92-200.08/53 MONSANTO COMPANY, ST. LOUIS, MISSOURI, U.S.A. =1 fm-- 2 co 1*1 m *4 M o(/) o lf%S33 ^3 r*3 r--3 C/3 C/3 Pv3 fS3 C4SOfe '-J oo C/3 C/5 KNGA0.|#yw, N. i. s%> f l z s;s o. St fS f -- 3* ^ 8-^. t3o a3s v< ?r |3- W | C/5 2o a ae |Isr 3 3 w o3 oo3 a" -a o2. ST O < Sf S' I' = ; ^o 'V2-->.* ^e3\\ JETS a to IS 2, 3 3* 5-^3S o ^ss-i- 5 <g` " = fo to 3. S'3- sisE? 33 o. COffQ' =--} 3 *t<o cTr* N6V 011262 WATER PCB-SD0000030724 If'E R T E E N p p o THE PROPER HANDLING OF AROCLORS AND THEIR MIXTURES IN THE ELECTRICAL INDUSTRY Monsanto Chemical Co. JCuMonsanto Organic 800 N. Div. Sales Dept. Lindbergh Blvd. St. Louis 66, Mo. DEPOSITION P. C. BENtGNUS EXHIBIT RavUaJ i January I960 NEV 007321 WATER PCB-SD0000030725 INDEX Introduction - Page 1-2 Chapter 1 Page 3-12 Page 3 Page 4 Page 12 Chapter 2 - Page 13-19 Page 13 Page 17 Chapter 3 - Page 20-21A Page 20 Page 21 Chapter 4 - Page 22-25 Page 22 Page 23 Page 25 Chapter 5 - Page 26-28 Page 26 Chapter 6 - Page 29-61 Page 29 Page 31 Page 31 Page 32 Page 38 The Proper Handling Of Aroclorr. And Their Mixtures In The Electrical Industry Procedure For Unloading Tankcars Of Aroclors And Aroclor Mixtures A) Description of the Cars B) Procedure for Unloading the Car C) Drum Packaging Storage Tanks A) Qeneral Description B) Detailed Description Gasketing and Pump Packing (A) Suggested Types Of Packing and GaBketing Materials (B) Gaskets For Askarel Capacitors and Transformers Sampling Methods A The ASTM Standard Method B Monsanto Methods (C) Drum Sampling Laboratory Analysis and Procedure (A) For Treating Aroclors and Their Mixtures with Earth Test Procedures (A) General Information (B) Detailed Instruction and Testing Methods 1. Procedure for Cleaning Electrodes 2. Dielectric Constant and Power Factor 3. Dielectric Strength WEV 007322 WATER PCB-SD0000030726 \ Page 44 Page 47 Page 49 Page 51 Page 52 Page 55 Page 59 Chapter 7 - Page 62-73 Page 64 Page 65 Page 66 Page 67 Page 68 Page 69 Page 70 Page 71 Page 72 Page 73 Chapter 8 - Page 74-76 Page 74 Page 74 Page 75 Chapter 9 - Page 77-79 Page 77 Page 77 Page 78 Page 79 4. Resistivity 5. Corrosion and Chemical Stability 6. Inorganic Chlorides 7. Acid Number 8. Moisture 9. Hydrolysis Stability Test for Aroclor 10. Thermal Stability Method for Aroclors Typical Properties Aroclor 1232 Aroclor 1242 Aroclor 1248 Aroclor 1254 Aroclor 1260 Pyranol l48l Pyranol 1488 Pyranol 1467 Pyranol 1470 Inerteen PPO Quality Requirements of Aroclors Prior to Use in the Electrical Industry Quality as Supplied to the Electrical Industry Typical Electrical Quality of Aroclors Used in the Industry Capacitor Impregnation Transformer Filling Earth Refinement of Aroclors to Arrive at the Desired Elec trical Qualities Earth Treatment in the Laboratory Preparatory to Analysis Earth Treatment by the Plant ' Manufacturing the Askarel Earth Refinement by the User Capacitor Manufacturers Transformer Manufacturers , The Effeot of Earth Refinement on Removal of Tin Tetraphenyl Scavengers from Transformer Askarel N6V 00130 WATER PCB-SD0000030727 Chapter 10 - Page 80-93 Page 80 Page 83 Contamination Avoidance of Contaminating Askarel Capacitors Avoidance of Contaminating Askarel Transformers Chapter 11 - Page 94.97 Page 94 Page 95 Chapter 12 - Page 98-100 Page 98 Page 99 Page 100 Reworking Contaminated Transformer Askarel Normal Conditions Arced Conditions Dermatology and Toxicology Skin Exposure Exposure to Vapors Vapors from a Severely Arced Askarel Transformer Attachments; Drawing No. 31-20847, The Tank Car Drawing No. 31-20848, Dome Detail Drawing No. 90-8170-5, The Horizontal Storage Tank Drawing No. D-13362, The Vertical Storage Tank Drawing No. 90-8248, The Breather Drawing No. 9C-8278, The Varec Gauge Drawing No. 90-8178, The Unloading Platform NEV 007324 WATER PCB-SD0000030728 THE PROPER HANDLING OF AROCLORS* AND THEIR MIXTURES ' IN THE ELECTRICAL INDUSTRY INTRODUCTION Monsanto's Aroclors*, especially the chlorinated biphenyls including types 12*12, 1248, 1254 and 1260, used alone or in combination with chlorinated benzenes, are commonly used die- /T lcctrlc materials of the askarel class. Askarel is a generic name referring to liquid dielectrics derived from halogenated aromatic hydrocarbons possessing excellent chemical and dielectric stability and firc-reslstance over the temperature ranges and operating conditions required of transformers and capacitors in the electrical industry. The properties of Aroclors and their mixtures, used as dielectrics are described in detail in Chapter 7 entitled, "Typical Properties". These dielectrics are manufactured under very carefully-controlled conditions in order to meet the strict and exacting electrical requirements and properties. The electrical industry's use of these fluids has been largely in accordance with the General Electric Company's patents and developments. *Aroclors - Monsanto's chlorinated biphenyls and chlorinated polyphenyls. Registered U.S. Patent Office. *F. M. Clark, "Electrical Insulation", Chem Engg. News 25. 29V'/ (1947)o -1- NEV 007325 WATER PCB-SD0000030729 I I i i ; !I l :, I 1 II .( !! ! :i I I Resulting from the wide use of these materials in the industry, trade names have been established to identify them by different manufacturers of electrical equipment. Listed alphabetically the trade names include, "Chlorextol," Allis Chalmers; ''Diaclor," Sangamo Electric; "Dykanol," Cornell Dubilier; "Elemex," Line Materials; "Hyvol," Aerovox; "Inerteen," Westlnghouse Electric; "Noflamol," Wagner Electric; and Pyranol," General Electric Company. The purpose of this bulletin is to assist the industry with the proper and safe handling of these dielectric materials in their operations. I I i I . i -' -2- ' NV 007326 WATER PCB-SD0000030730 CHAPTER 1 PROCEDURE FOR UNLOADING TANKCARS OF AROCLORS AND AROCLOR MIXTiW-g. : A. Description of the Cars , Aroclor and mixtures of Aroclors with chlorinated benzenes are shipped by Monsanto in two types of insulated tankcars- both of which are either aluminum lined or zinc-tin metallized. One type of car has heating colls inside of the tank and these are in direct contact with the product. The other, a more . widely used type of car, is a double-shell tank with heating colls between the Inner and outer shells. The steam coll connections are at the bottom of the car. Both types of tank- cars are tested for 60 pounds pressure and their steam coils are tested for 200 pounds gauge pressure. The cars are top-unloaded by displacement with dry air containing 10 mg. HrO/cu. ft. maximum. There are two or three connections on the tankcar dome depending on the type of car. Where three connections exist, . one is a two inch diameter unloading line which extends to the ' bottom of the car, the second is a one inch diameter air inlet connection and the third is a two inch diameter pressure safety vent, which Is a thin lead disc adjusted to release any pressure . in .excess of 66 pounds gauge * This safety vent is hooded for protection against dust, dirt or accidental bumping. Where only two connections exist on the dome, one Is the two inch diameter unloading line and the other is the safety vent. On these cars, it is necessary to remove the safety vent and introduce the displacement air through that connection. : .a. NEV 00732? ' WATER PCB-SD0000030731 While the tankcar drawing gives, much detail, we have been asked about the following points not given in the drawing: 1. The distance from the rail track to the top of the dome of the cars is variable. It is 13 feet and 4 inches for the 7)000 gallon cars and ranges from 11 feet to 14 feet for the 8,000 gallon cars. 2. The steam connections are located under the center of the cars.' 3. The steam pipe connection is usually a two inch pipe, but on some cars the pipe size is 1-1/4 inches. 4. American Standard taper pipe threads are used. ** -SA NE 007328 WATER PCB-SD0000030732 Drawing No. 31-20^48 shows in detail the dome of a tankcar with three connections. "A" is the two inch unloading line which`extends to a small sump at the bottom of the car. "B" is the one inch air inlet connection. "C" is the hooded safety vent. The car dome cover with fitted bolts Is shown in the center. It Is fitted with an aluminum envelope Qoetze gasket. This drawing also sh*a bottom opening in the oar. This can be opened only from the inside of the car and its purpose is for cleaning operations. It has no use at all in unloading the oar. Drawing No. 31-20847 shows the overall dimensions of the 8,000 gallon Aroclor tankcar. B. Procedure for Unloading the Cars The car should be spotted at an unloading dock similar to the one shown by Drawing No. 90-8178. The car must be level and the brakes set properly. "STOP - TANKCAR CONNECTED" signs should be placed fore and aft the car to warn switching crews. * *' * If it is ranlng or snowing or the humidity is extremely high, it is not advisable to open the car. In case the car must be sampled and opened during bad weather, a canvas canopy must be placed over the dome of the car. It la preferable to unload the oars under roof or inside the factory. Unless it Is absolutely necessary because of following described situations the dome cover should not be opened until ready for sampling. The dome cover Is sealed with a standard railroad wire and Beal, and Monsanto should be notified if this seal is found broken upon receipt of the car. WEV 00 7329 -4- WATER PCB-SD0000030733 The first step in unloading is to inspect the dome and clean around the dome cover to remove all loose dirt, water or snowWiping rags and a brush should be used to clean before the dome cover and connections are opened. Then, the screwed hood over the air-inlet valve should be removed and this valve opened fully and left open while heating the car. A Weston or metal encased thermometer should be inserted through this air-inlet valve opening and the tempera ture of the interior of the car determined. If the car temperature is below the caution temperature shown in the following Table 1, it will be necessary to take the special step of inserting a "hair-pin" heating coll through the dome of the car to preclude rupturing the tankcar seams during the heating period. TABLE I Product ASTM Pour Point C. Temperature C. Below which Caution Must Be Used in Heating Aroclor 1260 Aroclor 1254 Aroclor 1248 Aroolor 1242 Inerteen PPO Pyranol 1467 Pyranol 14J0 Pyranol 1481 + 30 + 40 + 10 + 20 -7 +5 - 19 - 10 Pre-heating is not required'' Pre-heating is not required* Pre-heating is not required* Pre-heating is not required* Except if the material has cooled below -10C. and crystals of scavenger have separated. Then, the material should be heated to 70C. (158P.) yntil complete solution has been accomplished. 5- NEV 007330 WATER PCB-SD0000030734 If the dome of the car is to be opened for the pre-heating , v* * operation, it is necessary that it be covered with a clean canvas. Extreme care must be taken to avoid getting dirt or moisture into the car. It is due to the relatively high viscosity of some of the Aroclors at low temperatures that it becomes necessary to form a column of molten material from top to bottom of the car, in the center, to prevent hydraulic pressure build-up which may rupture the tank shell if there is too rapid localized heating when employing the main steam coils. When such pre-heating is required, a satisfactory vent hole can be made by inserting a "hair-pin" coll (1/2 inch diameter brass, galvanized, or stainless steel pipe) into the open dome of the car and introducing steam through the coil until there is a column of fluid Aroclor from top to bottom. After the vent hole is melted through the material to the bottom of the car, the "hair-pin" coil should be removed and the dome cover replaced and bolted. Steam is then introduced into the main colls. It is recommended that the steam pressure be limited to 100 pounds gauge pressure, particularly when the colls are in direct contact with the Aroclor. The steam coil outlet should be trapped or throttled with a valve. It will require eight to twenty hours to bring the material to pumping temperature - depending upon weather conditions. It la essential that the air inlet valve be open during the heat ing period in order to vent the tank. c NEV 007331 WATER PCB-SD0000030735 Some calculations have been made to indioate the heat requirements for an Aroclor car. Data for an 8,000 gallon car of Aroclor 1254 are: Specific Gravity = 1.5 Specific Heat = 0.26 Btu/lb./P. Heat requirement for heating Aroclor from 30 C. (86P.) to 110C. (230F.) is: 8000 x 1.5 x 8.33 x 0.26 x (230-86) : 3,774,000 Btu. For heating from 30C. (86F.) to only 75C. (l67F.), the heat required is 2,110,000 Btu. A nine horse power boiler operating at 80 psig produces 263 lbs,/hr. of steam with no reused condensate. Returning condensate at 200F. will increase the steam output to 296 lbs./hr. at 80 psig. In the first case, heating to 110C., the over-all heat transfer co-effioient is assumed to be too low to utilize the 100% capaoity of the boiler. A value of 1500 for UA with an average h T of 133P. indicates that the useable steam is 202,000 Btu/hr. or 226 lbs./hr. steam at 80 psig. In the second ease the A T is lower and the entire output of the boiler Is useable. Tatie II sums up the approximate time calculated to heat Aroclor 1254 in an 8,000 gallon car. NEV 007332 WATER PCB-SD0000030736 TABLE II Nine HP Boiler 100# cap. (no reused condensate) 75# cap. (no reused condensate) Lbs. Steam/Hr. 263 -- 30-110C. -- 18 hrs. (86# cap) 30-756C. 9 hrs. 12 hrs. 100# oap. (condensate @ 200F.) 296 -- 8 hrs. 75# cap. (condensate @ 200P.) -- 18 hrs. 11 hrs. (76# oap) Calculations on a five horse power boiler give heating times of the following order: Five HP Boiler Lbs. Steam/Hr. 30-110C. 30-75C. 100# cap. (no reused condensate) 146 28 hrs. 16 hrs. 100# cap. (condensate <8 200F.) 164 25 hrs. 14 hrs. Aroclor oars can be heated by steam (80-100 psig) to the proper handling temperatures in a reasonable time by using a boiler source capable of producing 200,000 to 300,000 Btu/hr. The times given here are approximate and will act as a guide until experience shows the exact time for this operation. -8NEV 007333 WATER PCB-SD0000030737 1 | The proper handling temperature for the various fluids t is given in the following Table III, which indicates correspondI' i ing viscosity values: i | TABLE III Product Handling and Pumping Temperature C. Approximate Viscosity, S.U.S. Aroclor 1260 95 - 130 100 - 43 Aroclor 1254 Aroclor 1248 75 - 110 50 - 85 100 - 42 100 - 40 no>o f-no* 1242 35 - 75 100 - 40 Pyranol 1481 30 - 75 100 - 40 Pyranol 1467 20 - 55* 100 - 40 Pyranol 1470 15 - 45* 100 - 40 Inerteen PPO 20 55 100 - 40 *lf any of the scavenger is out of solution, then the material must be heated at 70 C. (158F.) until it has dissolved. Selection of pumping temperatures for any dielectric not shown on this list or which may be developed in the future should be based on a viscosity of about 100 Saybolt Universal Seconds for average pumping and about 40 S.U.S. for fast pumping. When the material has been heated to pumping temperature, a one-half inch diameter pipe "cross" arrangement containing a pressure gauge, air inlet, pressure relief valve to relieve at 30 Psig, and vent connections, should be connected to the dome air inlet pipe. Then the unloading line should be connected. Rust free and clean galvanized piping or stainless steel pipe should be used for the unloading line. NEV 00731<t WATER PCB-SD0000030738 (At this point a sample is taken as described in Chapter 4,) Dry* air is then introduced into the tankcar and pressure built up to 15 pounds gauge. The two inch valve cock on the stand pipe is opened and the discharge pipe observed to be sure the liquid is being unloaded. To protect the seams in the tankcar, the pressure must not exceed 30 pounds. The car will begin to unload at about 12 pounds pressure. When the oar is empty, the air pressure will drop off rapidly and air will blow out of the vent on the receiving tank. The air flow may be stopped at this point and the tankcar pressure released through the vent valve on the "cross" arrangement After inspecting the car to be sure that it has been completely unloaded, all connections and dome cover should be closed tightly. It is essential that the empty tankcar be sealed immediately after the car is unloaded in order to keep the car filled with dr air during return shipment. *It is essential that the displacement air used for unloading be dried thoroughly by some dehumidfying unit such as soda lime, activated alumina or similar dehydrating agent drying unit. It may be necessary to recharge the dehumidifying unit each time that a ear is unloaded. For unloading a tankcar of Aroclor within three hours, 15 standard cubic feet a minute of air at 15 pounds per square inch gauge pressure and a -100F. dew point should be supplied. If the dry air unit is to be used only for unloading tankcars, a small single tower dryer unit containing a selfcontained reactivating heater is suggested. Two manufacturers of air dryers of this type ares C. M. Kemp Mfg. Co., 405 E. Oliver Street, Baltimore 2, Maryland and Pittsburgh Lectrodryer Corporation, Foot of 32nd Street, Pittsburgh, Pennsylvania. -10- NEV 007335 WATER PCB-SD0000030739 As a final step, it is desired that a standard railroad wire seal be inserted through the slotted bolts of the car fittings. Steam should be released from the car colls and all condensate removed from the colls by blowing with air with the steam trap by-passed. All connections must be replaced as received. Adequate care should be taken in preparing and sealing the oar for return shipment. . Unloading with dry air as described is the preferred and recommended procedure because it is done with the oar dome closed which avoids contamination. Dry nitrogen may be used instead of dry air. If nitrogen ia used it is essential to notify ua (the supplier) so that we oan'take required safety precautions relative to replacing the nitrogen with air in the returned oar prior to sending our men into it for cleaning. If the oar is unloaded by pumping out of the top, whioh required opening the dome, it is most desirable that the oar be set inside of a building. If this cannot be done, then a canopy or roof should be provided over the oar dome, and the unloading should be done when the weather is dear. A dean centrifugal pump with minimum capacity of 40 gpm. 1b suggested. It will be necessary to prime the pump and only dean askarel should be used to do this. Another method for priming the pump is to use a Penberthy steam Jet, No. 22A available from Penberthy Injector Co., 1242 Holden Ave., Detroit 2, Michigan. (Further pump detail ia given on page 17) - 11 - NEV 007336 WATER PCB-SD0000030740 C. Drum Packaging Drum packaging is made with new and carefully inspected 55-gallon drums. These steel drums are lined with a specially selected baked phenolic coating. An example is NESCO No. 3 lining offered by the National Enameling and Stamping Company, Long Island, New York. Contents of the drums should not be heated by direct application of flame or strip heaters. Radiant heat from steam coils or hot air in a heated room is to be preferred. The screw plug in the drum head is fitted with a metal cap as a safe guard against tampering. The drums should be stored indoors. If outdoor storage cannot be avoided, the drums should be placed in a horizontal position and covered with a tarpaulin. nev 007337 WATER PCB-SD0000030741 CHAPTER 2 STORAGE TANKS A. General Description The storage tanks should be a minimum of 10,000 gallons and preferably 12,000 to 15,000 gallons capacity to accommodate the normal 8,000 gallon tankears. It Is preferable to locate the tanks above ground where they are easily accessible for any changes or repairs. Underground location presents difficulty In this respeot. Especially in cold climates, it is preferable to locate the tanks inside of a building. The tanks should be located conveniently with reference to the tankcar unloading facilities and the area where the dielectric is used. Although Aroclors are non-corrosive to metals, corrosion or rusting of iron and steel equipment (by oxidation) may occur resulting in contamination df the products. The resistance of Aroclors to materials of construction is given in Monsanto Teohnioal Bulletin, OP-115, entitled, "The Aroclors", Page 6. Stainless steel tanks are very satisfactory but relatively expensive. . Stainless steel pipe is relatively difficult to fabricate and it is difficult to make tight leak-proof connec tions . . Storage tanks may be of steel construction if properly metallized with zinc-tin or aluminum on the interior surfaces coming in contact with the Aroclors. -13- NEV 007338 WATER PCB-SD0000030742 The metallizing should be done according to the following procedure? 1. Clean an area of the surface by sand blasting, or a similar method to give a perfectly clean and roughened surface. The area cleaned should not be greater than can be completely metallized within a few hours after cleaning. 2. If zinc-tin metallizing is used, a ooating of zinc 0.005 inches thick should be sprayed on to the cleaned surface. This is followed immediately by a coating of tin 0.007 inches thick. 3. Aluminum metallized surfacing should be about 0.01 inch thick. The detailed procedure for metallizing and cleaning is out lined as follows: a) Sand blast, b) Coat with iron, 0.005 inches thiok. (The purpose of this coating is to provide a rougher and better bond for the finish coat of aluminum or the zinc-tin combination.) c) Apply the selected finish coat. d) Fill the tank with tap water and warm it with steam. (If an open steam line is used, do not allow the steam to impinge directly onto the metallized surface of the tank.) e) Drain the tank, f) Fill with cold water and drain, g) Wipe dry and clean with clean diaper cloth or other fabric relatively free of lint, h) Heat the tank to at least 100c. (212F.) to expell moist air. It would be benefi cial to heat the tank, allow it to cool and pull dry air through it using a dehumidfying breather in the air line, heat again etc., until the tank is full of comparatively dry air. i) Spray about 100 gallons of new, electrical grade Aroclor (not high in viscosity) or electrical grade trichlorobenzene onto the inner walls of the tank, washing the walls thoroughly (avoid breathing any fumes). J) Attach the circulating pump, the lines used, and -14- NEV 007339 WATER PCB-SD0000030743 the filter press fitted with dry paper and circulate the fluid through' the system and the tank. Install new dry filter paper several times in the press during this drying and cleaning operation. Discard the dielectric fluid used for cleaning, k) Partially fill the tank with new Aroclor dielectric and analyze it eleotrlcally and chemically to determine whether it meets specifications. If all tests are met, then fill the tank with the dielectric. The tanks should be Insulated using, preferably, glass foam beads as supplied by Dow-Corning or Libby-Owens-Ford. The suggested thickness of the glass insulation is one inch minimum to two inches maximum. The glass insulation may be covered with tar material oommonly used for weather -proofing. Another type of insulation which may be used instead of the glass is 85# Magnesia-Wool which should be covered also with the weather-proofing tar. The advantage of the glass insul ation is that it is not moisture sensitive as is the case with Magnesia-Wool. If the storage tank is located outdoors, it is best that the insulation be covered with riveted or bolted tin sheeting painted with aluminum p%lnt. This type of metal surface weathers well and is cleaned easily. All piping must be galvanized and screwed fittings must be back brazed to assure tightness. All handling'pipe lines must be traced with steam lines and insulation applied over the two lines in order to keep the handling lines and the material up to the desired pumping temperature. Usually a one-fourth inch copper steam line running parallel with the handling line will suffice. ' "15" NEV 007340 WATER PCB-SD0000030744 Under very severe conditions of low temperatures, it would be desirable to wind the steam line around the handling line about two turns to the foot. The tanks must be provided with ample pressurized heating coll surface to supply sufficient heat to the material to bring it to the proper temperature for pumping and handling as indicated in Table III. Heating coils should be either metallized steel, or preferably steel coils which have been galvanized after fabrication. It is recommended that the steam pressure on all heating colls should not exceed 100 pounds per square inch gauge; lower pressures may be used where practicable. It is essential that all steam coils be completely free from even minute leaks since this will intro duce water into the product. The steam coils may be introduced as "hair-pin" coils through a manhole at the side and bottom of the tank, or as is most often done. Inserted through the manhole at the top of the tank and then located near the bottom. External heating coils located in the Jacket of the tank may be used but this construction.is more expensive and less efficient than the internal colls. The storage tanks may be fitted with a stirrer, either through the top, side, or bottom of the tank and the propeller blade should be located near the bottom of the tank. However, insertion of a stirrer through the side offers possible source of a leak and since these materials are homogeneous, it is not essential to provide such agitation for the purpose of mixing. ' ^. NEV 007341 WATER PCB-SD0000030745 Adequate circulation can also be accomplished by using a centrifugal type pump. Gear pumps or other equipment where wear or chipping of metal parts may introduce contam ination should not be used. The pumps must be of the type designed to handle hot oil. All wetted pump parts should be either stainless steel or bronze. The centrifugal pumps must be provided with a deep stuffing box and proper packing used, as described in Chapter 3. As examples of pumps found completely satisfactory for this service, reference is made to Worthington Worthlte pumps. Blackmer pumps, Dean Bros., Peerless and Dayton Dowd Type C pumps for handling hot oil. Also, a very satisfactory arrangement for mixing or circulating and pumping the fluid from the storage tank is to use a vertical sump pump such as a Taber pump. All storage tanks must be amply provided with a dehumidifying breather such as soda lime, activated alumina, etc., units. ThiB Is essential to prevent moist air from coming in contact with the dielectric. A moisture content above 35 ppm adversely affects the electrical resistivity of these products. Provision should be made to preclude possible leakage of the drier material back into the storage tank and the drier should be inspected periodically to make sure that it is open and not plugged. B. Detailed Description Drawing No. 9C-817O shows the detailed construction of a horizontal 15,000 gallon storage tank for Aroclor and its mixtures which has been found completely satisfactory. ^ 007342 WATER PCB-SD0000030746 The various nozzles on this tank are used as follows, considering them in order from left to right on the drawings 3" nozzle Inlet for recirculation 24" nozzle For future agitator if required (not used) 3" nozzle For soda lime or calcium chloride breather connection. 36 " manhole For inspection, etc. The float guage is located in the center of this manhole. 3" nozzle 24" nozzle Not used. For future agitator if required (not used) . 3" nozzle Not used. 3" nozzle Filling inlet connection. 18" x 26" Oval nozzle For sump pump 3" nozzle For thermometer well (see detail) The two 24" nozzles were originally installed for installa tion of agitators, if required. However, it has been found unnecessary to use agitators in the storage tanks, and these nozzles could be omitted. It has been'found that circulation of the fluid by the sump pump, and into the nozzle at the opposite end of the tank, for several hours gives satisfactory blending of the tank contents. For pumping the dielectric from the storage tank, a Taber pump Company all bronze 2-1/2" x 2" vertical sump pump with monel shaft has been found to be quite satisfactory for the appli cation. -18- NEV 007343 WATER PCB-SD0000030747 The liquid level gauge used in the storage must be gas-tight. The storage tanks are equipped with Vapor Recovery Systems Co.'s "Vareo", gas-tight, automatic tank gauge as shown by drawing No. 90-8278. The storage tanks should be provided with an operating plat form suitable to the customer's conditions of operation. The dehumidifying units used as breathers on the storage tanks can be constructed as shown by Drawing No. 90-8248. The upper portion of the chamber is charged with anhydrous soda lime or another drying agent. Periodic inspection of the drying agent will show the formation of a cake of damp material on top about 1 to 1-1/2 inches deep. This cake should be removed and fresh material recharged. Any suitable construction similar to that shown on Drawing No. 90-8248 may be used for the breather units. Drawing No. D-13362 shows design detail of a 15,000 gallon vertical storage tank. The vertical type tank would seem especi ally desirable when insufficient space is available to accomodate the horizontal type tank. 19~ NEV 007344 WATER PCB-SD0000030748 CHAPTER 3 GASKETING AND PUMP PACKING Aroclors and their mixtures soften and swell natural rubber and many of the synthetic "rubber" materials. Such material not recommended for use include, Hycar P, Koroseal, Perbunan, Neoprene, etc. These materials are known sources of contamination. SUGGESTED TYPES OF PACKING AND GASKETING MATERIALS INCLUDE: 1. For Welded Flanged Pipe Connections: Garlock Packing Co., No. 901 or No. 7021, 1/8 inch asbestos fiber sheet. A ring of thin aluminum drawn tightly at the flange connections may be used satisfactorily also. 2. For Pumps: Garlock No. 234, No, 431 and Cheveron No. 7050-C are satisfactory packings. Likewise, Durametallio 's spiral asbestos fiber may be used. Johns-Manvllle and others have comparable packing materials. 3. For Valves 1 Garlock No. 117 braided packing or its equivalent is suggested. 4. Other Resistant Materials: It is indicated that duPont's Teflon, poly tetrafluoroethylene is not attacked by hot (130C.) Aroclor and is to be recom mended as a gasket material. Dow-Cornlng's Silastic, Silicone 180, is very resistant to Aroclor and Is suggested for gasket purposes. 5. In some cases cork Impregnated under pressure with Chrysler's Cycloweld 55-9 or Armstrong Cork Co.'s 1162-J and cured at 170C. may be used as a gasket material. These are baked phenolic type coatings. 6. Pipe Thread Compounds 1 When necessary to use pipe thread compounds, the following should be satisfac tory if care is taken to prevent the pipe compound from getting on the inside of the pipe. . (a) Plastio Lead Seal - manufactured by Dura- metallic Corporation ' (b) Ordinary white lead NEV 007345 -20- WATER PCB-SD0000030749 Usually It Is not necessary to use pipe thread compounds since all screwed pipe fittings should 'be sealed by back brazing. T. All new lines and fittings should be cleaned thoroughly by steaming (for two hours) and dried with air or heat. GASKETS FOR ASKAREL CAPACITORS AND TRANSFORMERS 1. For small capacitors requiring ring seals on the terminals, properly selected Silastic (silicone) tubing is cut to make the ring gasket. 2. The most effective and trouble free seal for transformer lids or covers Is to weld the cover onto the transformer shell. To remove the welded cover a weld cutting tool or bar is used. 3. Cork - Nitrile rubber composition gaskets are sometimes used to combine the desired flow limiting property of cork with the resiliency of nitrile rubber. Only fine grained cork should be used in making this composition gasket. Special gasket cementing compounds such as GE's No. 1276 or No. 880 are used to coat the gaskets to further seal them against the transformer fluid and to accomplish firm bonding to the metal surface. 4. Nitrile rubber gaskets are also used and require no adhesive to make a liquid-tight seal. Exposure of nitrile rubber gaskets to transformer askarel should be kept at a minimum and the gasket should not be compressed beyond 2/3 of the original thick ness. After long time exposure to transformer askarel fluid or its vapor, nitrile rubber is measurably deteriorated. While gaskets made of silicone or Teflon are not attacked, these materials are relatively expensive for use in large sizes. Accordingly, for the most efficient performance it is suggested that welded covers be used on askarel transformers. 5. Instruments, such as temperature gauges, etc. may be attached to the transformer using flange con nection to pipe located below the liquid level of the fluid in the transformer. Such flange con nections are usually not large in diameter. Accordingly, it seems practical to use Teflon or Silastic gaskets to make these seals, especially since it is known that askarel can migrate thru cork or composition cork gaskets used under the liquid level. 21~ NEV 007346 WATER PCB-SD0000030750 Another satisfactory approach used is to machine the flange surfaces of this type connection. - Then a Splritalllc gasket made of stainless steel ring with asbestos inter liner for resiliency can be used satisfactorily. 6. Screwed pipe fittings on askarel transformers require thorough cleaning of the threads to remove oil, grease and dirt. Then the threads are coated with a compound such as GE*s No. 880 and then tightened. ' -21A- N6V 007347 WATER PCB-SD0000030751 CHAPTER 4 SAMPLING METHODS 1.) The ASTM Standard Method for sampling electrical insulating oils is described in ASTM Designation: D923-49. This describes glass and metal thiefs for sampling drums, cans, and tankcars. A specially designed thief or bomb for sampling tankcars is described, also. A very good instrument of this type is the stainless-steel Bacon Bomb Thief with which samples of the liquid can be drawn from any level of the tankcar. The ASTM procedure describes sample containers, their cleaning and storage. Under general precautions, the ASTM mentions that, "Samples of the fluid shall not be taken until the oil is at least as warm as the surrounding air, because cold oil may condense enough moisture from a humid atmosphere to affect seriously its insulation properties. (In the case of tankcar lots, on some occasions there may be no choice, as it may be necessary to procure samples from a tankcar when the temperature is not above the surrounding air. On such occasions, the temperate of oil and air also the humidity if possible, should be noted in the report of test results.) It is undesirable to do any sampling when the relative humidity of the atmosphere exceeds 75 percent, and samples shall never be taken in the rain". -22- NEV 007340 WATER PCB-SD0000030752 Several electrical manufacturers using Aroclor dielectrics, switch the tankcars directly into the plant building or under roof before sampling and unloading. These precautions in handling are taken to avoid any contamination of the fluids which are manufactured under very strict specifications. For example, the specificatim for ionizable chlorides allows no detectable amount, (less than 0.10 parts per million). Moisture may not exceed 20 to 35 parts per million. TankcarB are cleaned and prepared under close inspection before they are filled. When filled, and analysis shows the material in the car to be satisfactory, the car is then sealed with a standard railroad wire and seal inserted through the slots of the dome fittings. Likewise, after the tankcars have been unloaded in the industry, it is requested that the dome fittings should be sealed with a railroad wire and seal. 2.) Monsanto Methods used for sampling tankcars differ somewhat from the ASTM procedure. The modified techniques are used because of their greater simplicity and they have been entirely satisfactory as employed over many years. A sample is never taken when it is raining or snowing, or when there is any chance of contaminated atmosphere moving in the direction of the car. However, in case of an emergency during inclement weather, a canopy is placed over -23- NtV 0073-.' WATER PCB-SD0000030753 the car dome before sampling. A satisfactory sample bottle is a five pint, round amber glass, packer type container fitted with a 38 millimeter Bakelite screw cap with an aluminum or tin cup liner. Bottles of this description can be purchased from the Northwestern Bottle Company, 3144 North Broadway, St. Louis, Missouri according to their No. A-7253. Only new bottles and caps are used. When a shipment of bottles is received, the bottles are capped immediately and stored in their receiving cartons. Prior to use, the exterior of the bottles is wiped with a clean cloth. The simplest sampling device used is a clean stainless steel or aluminum dipper. However, this is not' a generally preferred device because it permits sampling the car from the near surface, only. The sampling device commonly used consists of a stainless steel tube, seven feet long with one end bent into a hook, to serve as a handle and on the other end there is a stainless steel bucket with a perforated bottom. This bucket Is about 5-1/4 inches inside diameter and 6 inches deep to hold the five pint bottle. This bottle is held firmly by a stainless steel collar made to slide along the shaft of the sampling device. This collar has a clamp attachment for fixing it tightly into place where desired around the neck of the bottle. When a car is to be sampled, a new sample bottle is clamped firmly in the bucket. "2^" NE V 007350 WATER PCB-SD0000030754 All dirt Is brushed and wiped away from the car dome area using a clean rag. The car dome is opened and the cap is then removed from the sample bottle. The sampling device is inserted into the car so that the neck of the bottle is at least twelve to eighteen inches below the surface of the fluid. The sample taken is dis carded as its purpose is to rinse the bottle. A portion of the sample is used to rinse the interior of the bottle cap. This procedure is repeated until a minimum of three rinses has been made; each time the sample taken is not put back into the car. These rinses should be discarded. Then the sample is taken and the cap of the bottle is screwed down tightly. When the sample has been obtained, the car dome is replaced. immediately. The exterior of the sample bottle is wiped with a clean cloth and when returned to the laboratory it is further cleaned with a cloth dampened with pure trichlorobenzene. if the sample is to be shipped, the cap is taped with Scotch Tape. The sampling device is also cleaned with pure trichloro benzene and is stored in a dust free, air conditioned room. 3.) Drum Samplings \ glass thief, thoroughly cleaned with pure trichlorobenzene and dried is used to sample drums. -25- nev 007351 WATER PCB-SD0000030755 CHAPTER 5 . LABORATORY ANALYSIS AND PROCEDURE FOR TREATING AROCLORS AND THEIR MIXTURES WITH EARTH A sample of the Aroclor or Aroclor mixture taken from the tankcar, or drums, as described In Chapter 4, is analyzed in the laboratory to determine Its quality In accordance with the property values given in Chapter 7 For capacitor use, usually the important properties tested are resistivity, power factor, chlorides, and moisture. For transformer use dielectric strength, resistivity, moisture and chlorides are the important properties. If the sample is out of line with the shipping specifica tions, it is indicated that the sample has become contaminated. In this case, another sample is to be taken and the properties redetermined. If still out of specifications, the sample should be given treatment with earth. Treatment of the dielectric with conditioned Attapulgus earth will bring the electrical properties to the maximum attainable values. While there is complete agreement on the benefits derived from treating with conditioned earth, there is difference of opinion on details of the method, arising from factors such as the following. No doubt, there are differences in the absorbent power of various types of diatomaceous earth with respect to removing moisture, impurities and additives such as stabilizers or scavengers from the dielectric -26- NEW 007352 WATER PCB-SD0000030756 materials. The size of the earth particles, temperature and conditions of activation of the earth, the concentrations used and the temperature, the degree of agitation and time interval at which the dielectric is given earth treatment are all possible variables which are still being studied in various laboratories. The method used by Monsanto for treating the fluid with activated earth in the laboratory is: The absorbent is minus 200 mesh Attapulgus* earth acti vated Just prior to use by heating in shallow trays for four hours at 400C. (752'F.) or for at least twelve hours at 250C. (482F.). At least one quart of the dielectric sample is placed into a clean two liter Pyrex beaker or three necked flask. The beaker or flask should be cleaned Just prior to use in a manner similar to the procedure described in Chapter 6, Method No. 11,751, "Procedure for Cleaning of Electrodes, G.E. Cell and Accessories". The flask or beaker is fitted with a glass or stainless steel agitator.' Heat is applied using either a hot plate or a aias-Col mantle and is controlled by a thermostat such as a Fenwal thermo switch with a stainless steel sheath. About 0.1 to 0.2$6 of the activated earth, based on the weight of the liquid is added. *Attapulgus Division, Minerals & Chemicals Corp. of America, 210 West Washington Square, Philadelphia 5> Pennsylvania _07_ NEV 007353 WATER PCB-SD0000030757 I The more viscous dielectrics such as Aroclors 1248 and 1254 are heated at about 70* to 80*C. (158 - 176*F.) and the less viscous materials such as Aroclor 1242 and Pyranols 1481, 14671 and 1470 are heated at about 50 to 6o*c. (122 to l40F.). After heating and stirring the sample for about four hours, it is filtered using a clean Pyrex glass suction flask and a Buchner funnel fitted with a Whatman No. 1 or No. 3 filter paper. This apparatus and the bottle into which the treated sample of dielectric is transferred should have been cleaned in a manner similar to the cleaning procedure des cribed in Chapter 6. The earth treated and Mup-graded" sample is then ready for final analysis of its electrical properties. -28- NEV 007354 WATER PCB-SD0000030758 CHAPTER 6 TEST PROCEDURES A. General Information The Monsanto test methods described here with the special equipment used are some of the control tests employed to maintain the quality of Arodors for dielectric use. They are suggested as a guide for test work needed to Indicate the quality of the dielectrics used in the manufacture of electrical goods. The most significant electrical tests made on Aroclors for capacitors are: 1. Dielectric constant. 2. Power Factor. 3. Resistivity. For transformer use the most significant electrical tests of Aroclor mixtures are: 1. Dielectric Strength 2. Resistivity. Other than electrical tests, significant .measurements of quality include, moisture, chlorides, thermal and chemical stability. The following terms are defined % Dielectric Constant: The dielectric constant (sometimes called specific inductive capacity) of any substance is equal to the ratio of the capa citance of a condenser when that substance is used as the dielectri to the capacitance when there is a' vacuum between the conductors (for all practical purposes air at ordinary pressures may be used instead of a vacuum). -29- NEV 007355 WATER PCB-SD0000030759 Dielectric Strength: Dielectric strength is the rupturing strength of an insulating material when subjected to voltage stress under specific conditions and expressed in kilovolts. Breakdown varies with the shape of the electrodes and does not increase directly in proportion to the thickness of the dieleotric. Power Factor: The power factor of a dielectric is the ratio of the energy loss in the dielectric to the "apparent power" in the dielectric. Resistivity: Resistivity is electrical resistance offered to the passage of a steady current. The volume resistivity in ohms-centimeter of an oil is the ratio of the d-c potential gradient in volts per centimeter paralleling the current flow within the sample, to the current density in amperes per square centimeter at a given instant of time and under prescribed conditions, Volume resistivity is expressed in ohm-cm. ^ The analytical procedures described in detail include: 1. METHOD NO. 11,751, "PROCEDURE FOR CLEANING OF ELECTRODES, G.E. CELL AND ACCESSORIES." 2. METHOD NO. 11,608, "DIELECTRIC CONSTANT AND POWER FACTOR." 3. METHOD NO. 11,605, "DIELECTRIC STRENGTH." 4. METHOD NO. 11,607, "RESISTIVITY." 5. METHOD NO. 10,126, "CORROSION AND CHEMICAL STABILITY." 6. METHOD NO. 10,118, "INORGANIC CHLORIDES." 7. METHOD NO. 10,087, "ACID NUMBER." 8. METHOD (MODIFIED) NO. 10,620, "MOISTURE (WATER)." NEV 007356 WATER PCB-SD0000030760 9. Hydrolysis Stability Test. 10.' Thermal Stability Test. Detailed Instruction and Testing Methods. 1. METHOD NO. 11,751, "PROCEDURE FOR CLEANING OF ELEC TRODES, O.E. " Cell and Accessories. a. The Electrode Cleaning Procedure; . 1) Place the electrodes in hot electrical grade Trichlorobenzene for ten minutes. 2) Wash with unheated TCB. 3) Rinse twice with methanol and twice with tap water. 4) Place the electrodes in hot 10# Tri Sodium Phosphate solution. Soak and heat for ten minutes. 5) Wash thoroughly with tap water. CAUTION: After step 5 -- DO NOT TOUCH THE ELECTRODES WITH HANDS! ' 6) Wash with distilled water twice. 7) Dry In drying oven for at least two hours at 120C. b. The Q.E. Cell Cleaning: 1) Reclean the cell before use, when more than 8 hours have elapsed since the previous cleaning. 2) Follow the procedure for the electrodes starting at Step 4. o. Cleaning of the Accessories: 1) Apply the same cleaning procedure as given for the electrodes (Steps 1 to 7) to prepare the glass spacer and beaker for next test. 2) Clean the thermometer in the same manner as the electrodes, except for Step 7* ` 3) Place the wet thermometer (after Step 6) directly in position in the temperature Heating Unit (Modified Fisher Isotemp Oven) and allow to dry. -31- NEV 007357 WATER PCB-SD0000030761 2. METHOD NO. 11,608. "DIELECTRIC CONSTANT AND POWER FACTOR." I. -Apparatus - A. Oscilloscope; Heathklt Model 0-6. B. Constant Temperature Heating Unit; Fisher Isotemp oven. Model 13-245A, modified to include Inter wall connectors. C. A. C. Generators General Radio Type 1302-A D. Amplifier and Null Detector; General Radio type 1231-B with type 1261-A power supply. E. Capacitance Bridges General Radio Co. Capacitance Bridge type 716-C. F. Test cells: G. E. type, concentric cylinder electrodes Catalog #1,559,663. (G.E., Pittsfield. Mass. Transformer Lab.) G. Class B driver transformer: This is used for 60 cycle measurements to excite the bridge directly from the domestic power line. It has 50 volts output with a 4800 ohm resistor in service. H. Tuned Circuit Filters: General Radio Type 1231-P2 (400 and 1000 cycle) and 1231-P3 (60 cycle). These filters aid in obtaining a more accurate frequency for the measurements by removing harmonics, noise, hum, etc. ' II. Adjustment of Controls on Electrical Appartus A. On Panel No. 1 (Top Panel, Amplifier and Null Detector) a. Turn the 4-way (main power) switch on the upper right hand side to the #3 position to determine the Dielectric Constant at 1000 cycles. Turn this switch to the #2 position for measurements~a~60 cycles. b. Allow the equipment to warm up 10 minutes. c. Turn "GAIN CONTROL" to 6. d. Depress "INPUT 0.03V." button. B. On Panel No. 2 (Oscilloscope) a. Turn "INTEN." to about the 12 o'clock position. CAUTION: Do not allow a high intensity spot to remain stationary on the screen for any length of time. -32- NEV 007358 WATER PCB-SD0000030762 I i1 1 1 i i ! i ! 1 4 i i i * ! i I 111 1 .1 1 b. Using "HOR. POSITION" and "VERT. POSITION" controls center the image on the screen. . c. Adjust "FOCUS" for sharp line. d. Turn "FREQ. SELECTOR" to LOOKC. e. Turn "FREQ. VERNIER" to 80. ' f. Turn "VERTICAL GAIN" to 5. g. Turn "VERTICAL INPUT" to "10 VOLT MAX.". h. Turn "HORIZONTAL GAIN" to about 20. i. Turn "SYNCHORONIZING" to + 20. J. Turn "SYN." to "EXT. SYN." k. Turn "GEN." to "SWEEP GEN." C. On Panel No. 3 (Capacitance Bridge) a. Turn "RANGE SELECTOR" switch to "100 C" for 60 cycle measurements and to "1 KC" for 1000 cycle measurements. b. Turn "METHOD SWITCH" to direct. c. Turn "DISSIPATION FACTOR" selector switch to "0". D. On Panel No. 4 (oscillator) a. Disregard this panel for measurements at 60 cycles. b. On 1000 cycle measurements, depress the No. 10 "MULTIPLY BY" button. c. Set "FREQUENCY DIAL" to 100. d. Turn "OUTPUT" dial so that pointer is at the end of the arrow. e. Depress the "UNBAL. 5000 OHMS" button. When all of the above adjustments are made, the electrical apparatus is ready for measurement of Dielectric Constant and Power Factor. -33- NEV 007359 WATER PCB-SD0000030763 III. Determination of Constants for the Apparatus 1. Carefully assemble the cell which has been cleaned - and dried within the last 8 hours. Refer to Method No. 11,751 for the procedure to use In'clean'lng tKe cells. 2. Place the cell assembly in the Fisher oven which has been adjusted to 25C. 3. Connect the back wire inside the oven to the lead on the inner cylinder of the cell and the front wire to the lead on the outer cylinder of the cell. 4. Connect the cable from the capacitance bridge to the terminals on top of the oven so that the inner wire of the cable goes to the back terminal and the outside mesh casing of the cable (the ground) goes to the front terminal. 5. Remove the thermometer from the top of the oven before going on with the test, fill s ~TaTmporiant. 6. Make all adjustments on the electrical apparatus as directed in Paitfc I of this method. ' 7. Balance the bridge by rotating the "CAPACITANCE" and "DISSIPATION FACTOR" dials on Panel No. 3 until the wide vertical band on the oscilllscope is adjusted to a minimum width. 8. Record the sum of the readings on the "CAPACITANCE" dial and vernier and call this value A. 9. Remove the beaker containing the cell from the oven and fill it with C.P. benzene to a level 0.737 inches (ca. 3/4 inch) above the top of the concentric cylin ders of the cell. 10, Adjust the temperature of the benzene to 25C. while stirring with a thermometer. 11. Replace the cell in the oven (at 25C.) and make the same electrical connections as in Steps 3 and 4. DO NOT interchange connections. 12. Balance the bridge again as in Step 7 13. Record the sum of the readings on the "CAPACITANCE" dial and vernier and call this value B. 14. Calculate the cell constant by the following equation: Cell Constant, K - B - A (this is usually 2.27 - 1.0 around 70 mmfd.) -34- wev 007360 WATER PCB-SD0000030764 15* Remove the cell from the oven and balance the . bridge as In Step 7 with the "CAPACITANCE" and "DISSIPATION" "FACTOR" dials. 16. Record the sum of the readings on the "CAPACITANCE" dial and vernier and call this value F. (capacitance of connecting cable.) " 17. Calculate the CELL LEAD CAPACITANCE by the following equation. CELL LEAD CAPACITANCE, Q - A - F - K (this is " usually around 3 mmfd.) WHERE? A = CAPACITANCE OF ENTIRE SYSTEM IN AIR (SYSTEM CONSTANT) Q - CAPACITANCE OF THE CELL LEADS (CELL LEAD CONSTANT) F 8 CAPACITANCE OF CABLE AND WIRES WHICH CONNECT THE CELL AND CELL LEADS TO THE BRIDGE. (CONNECTOR CONSTANT) K = CAPACITANCE OF THE CELL ALONE (THE CELL CONSTANT) Tabulate the system Constant (A), the Cell Lead Constant (0), the Connector Constant (F), and the Cell Constant (K) on a piece of stiff paper and post them near the instru ment where they can be easily referred to for comparison and calculations. These constants must be checked at least once every three months and in all cases where the Dielectric Constant and/or Power Factor are out of specification. Measurement of Dielectric Constant and Power Factor on Aroolors77WranoIsT~Tnerteens, and Trl-Ttetraohloro^ ~ benzene Blends, ' A. Test Run on Cell to Determine whether It 1b Clean ancf..properly AHgneg~7~~ ! ' ... .. 1. Carefully assemble a cell which has been cleaned and dried within the past 8 hours. NOTE; Refer to method No. 11,751 for procedure to use in cleaning cells. -35- IMEV 007361 WATER PCB-SD0000030765 2. Adjust the oven control to hold at a temperature - of 100C. for all materials except Trl-Tetra Blends. If a Trl-Tetra blend Is to be tested, adjust the oven to hold a temperature of 25C. 3. Place the empty cell assembly In the oven and connect the back wire Inside the oven to the lead on the Inner cylinder of the cell, and connect the other (front) wire to the lead on the outer cylinder. 1*. Connect the cables from the capacitance bridge to the terminals on top of the oven so that the inner wire of the cable goes to the back terminal an3 the outside metal casing (ground)goes to the front terminal. 5. Allow 15 minutes for the cell to reach temperature equilibrium inside the oven. 6. Remove the thermometer from the top of the oven eTore~TaRTng"any measurements on tHe-bridgeT--' This is Important. 7. Make all the adjustments on the electrical apparatus as directed In Part I of this method, 8. Balance the bridge by rotating the "CAPACITANCE" and "DISSIPATION FACTOR" dials on Panel No. 3 until the wide vertical band on the oscilloscope screen is adjusted to a minimum width. 9. Record the sum of the readings on the "CAPACITANCE" dial and vernier and compare this value with the SYSTEM CONSTANT determined in Part II of this method. IMPORTANT: If the value obtained in Step 9 does not agree with the System Constant A (Part II) within 5 uuf, the cell must be re-cleaned, re-dried, re-assembled, and the test run for the System Constant must be repeated. NOTE: Although the above test run must be made prior to each analysis, the value obtained in Step 9 is not to be used in calculations but is to be used only as a check on the cleanliness and alignment of the cell, -36- NEV 007362 WATER PCB-SD0000030766 Procedure for Testing Materials 10. Remove the cell from the oven and fill the beaker with the material to be tested to a level 0.737 inches (ca 3/4 inch) above the cylinders of the cell. 11. Adjust the temperature of the sample to 100*0. (use hot plate) for all materials except Tri-Tetra blends. For Tri-Tetra blends, adjust the tempera ture of the sample to 25C. using an ice-water bath if necessary. NOTE: Stir sample continuously with a thermometer while adjusting the temperature. 12. Place the cell and sample in the oven and make the same connections from the cell to the bridge as in Steps 3 and 4. DO NOT interchange connec tions . 13 Allow 15 minutes for the cell to reach temperature equilibrium inside the oven. 14. Remove thermometer from the oven before taking a measurement. TKIs is Important.' ~. 15. Make the adjustment of controls on the electrical apparatus as directed in Part I of this method. 16. Balance the bridge by rotating the "CAPACITANCE" and "DISSIPATION FACTOR" dials on Panel No. 3 until the wide vertical band on the oscilloscope screen is adjusted to a minimum width. 17. Record the sum of the readings on the "CAPACITANCE" dial and vernier, and call this value X. 18. Record the sum of the readings on the "DISSIPATION FACTOR" dial and switch. Call this value D. Calculations: Dielectric Constant . X -F -0 --y-- Where: X Capacitance reading from Step 17. F Connector Constant (Determined in Part II) Q Cell Lead Constant (Determined in Part II) K e Cell Constant (Determined in Part 11) -37- NEV 007363 WATER PCB-SD0000030767 power Factor = f x D Where: " f = Test Frequency (60 cycles or 1000 cycles) f0= Frequency of "Range Selector" on Panel No.3 D = Dissipation Factor reading from Step 18. NOTE: When D (dissipation factor) is less than 0.1, the dissipation and power factors differ by less than 0.0005. Therefore, for our measure ments, power factors and dissipation factors are equal. Precision: (Reference: General Radio Manual for Model 716-C Capacitance Bridge) a. Capacitance readings are precise to + 2 mmfd. x mul tiplier reading (+ 0.2$ of full scale for each range) when the dissipation factor is less than 0.01. b. Dissipation Factor (Power Factor) readings are pre cise to + 0.0005 or + 2$ of the dial reading which ever is Targer, for values less than 0.1 for D (Dissipation Factor). 3. METHOD NO. 11,605, "DIELECTRIC STRENGTH." a. Apparatus and General Information The electrical equipment necessary to provide high voltage to permit the determination of dielectric strength of liquid dielectric at commercial power frequencies is basically quite simple. The equipment assembled in the laboratory consists of a high voltage transformer of good design and with a current capacity of 2.43 KVA and with equip ment for control of the voltage and a means of measuring the voltage and to provide safety for the operator. nem 736`' WATER PCB-SD0000030768 It is enclosed in a steel gray crackle finished cabinet measuring 42M high, 22" wide, 17" deep and set on truck casters for easy mobility. Protective equipment incorporated in this apparatus prevents the application of high voltage unless all safeguards are complied with. The door on rear of cabinet must be closed. The cover over the oil must be all the way down and the voltage control must be at 0 position. Failure to comply with these requirements will prevent any action when the red button is depressed. The test cup: Transformers, Voltmeters, and Accessories The askarel testing cup type No. 224809 supplied by General Electric Company is mounted on the top rear of the cabinet. It is protected by a heavy plastic cover, hinged at the rear for accessibility to the receptical. It is equipped with safety contactor so placed that the circuit energizing the high voltage contactor cannot be completed unless the protective cover is completely lowered and in plaoe. It is impossible for the operator or anyone else to touch the testing cup when high voltage is applied. The High Voltage Transformer manufactured by the Kelly-Koett Manufacturing Co. is of the closed core, oil immersed, shell type design. Rate @ 81,000 volt @ 40 millampers. It was recovered from a used X-ray machine purchased quite inexpensively -39- MEV 007365 WATER PCB-SD0000030769 An auto transformer- from the same X-ray machine is connected so as to limit the out-put voltage of the high voltage secondary to 50,000 volts. The primary of the auto transformer is connected to the secondary of a 2-1/2 KVA powerstat variable auto transformer supplied by the Superior Electric Company. Power to the powerstat is controlled by a 4 con tact 30 amp. solenoid circuit breaker. The voltmeter mounted on top near front edge is connected across the powerstat secondary and is calibrated to read directly in Kilovolts in the range of 0 - 50 K.V. The overload circuit breaker consists of a small relay connected between one side of the high voltage transformer secondary center tap and ground. It is adjusted to break contact on a current drain of about 50 mil Hampera. The circuit for the coil of the solenoid circuit breaker is wired through the contacts of this relay. -40- HEV 007366 WATER PCB-SD0000030770 t Safety and Operating Controls 1) Door interlock switch located on rear door 2) Test cup cover interlock switch. 3) Powerstat switch mounted on rear of unit arranged so that high voltage contactor cannot be closed unless powerstat is at zero position. 4) Main power switch on front panel. 5) Powerstat voltage control on front panel. 6) High voltage contactor push button on front panel (red). 7) Signal lamps mounted on top around voltmeter. Purpose and operation described in method of use, j b. Procedure 1) Ascertain that the temperature of the material under test is 25 ( 0.5)C. i NOTE: Testing at other temperature is likely to give `variable results which may be misleading. 2) Shake the sample container so as to thoroughly it mix the askarel before filling the test cup. J NOTE: This operation is especially important with used Aroclor as the impurities may settle to the bottom and the test may be misleading. 3) Rinse the testing cup three times with small I portions of the sample to be tested. 4) Immediately after final rinse, fill the cup to a height of not less than 20 mm. (0.787 in.) i above the top of the electrodes. i 5) Rock the cup a few times in order that any entrapped air may escape. Close cover over oil test cup. ti 6) Allow to stand 3 minutes. CAUTION: THIS IS < IMPORTANT. 7. Turn main toggle switch on front panel to "ON" (or up) position. Both green and amber pilot lights on the top at either side of the voltmeter will now glow. NEV 007367 ( -41 WATER PCB-SD0000030771 NOTE: The green signal light Is connected across the 115 volt in-put and denotes that line voltage has ' been applied to operating control circuit. Amber light is connected in series with sensitive switch located under high voltage contactors and connected to its armature. It indicates that high voltage contactor is in its rest position and away from contacts energizing auto transformer. 8) Turn voltage control (large knob on front) to extreme counter-clockwise position. 9) Depress red button on front. This energizes high voltage transformer and circuit breaker and is indicated by amber light going out and the red light directly over voltmeter will light. -- 10) Watch the voltmeter and, while holding the button "IN", turn the voltage control at such speed that will cause voltage as indicated on voltmeter to rise at a rate of 3 K.V. per second. 11) Note and Record the voltmeter reading at break down. 12) Repeat the test until two successive breakdowns occur on each of two fillings of the test cup which do not differ by more than 10$6. Report the average value of these two readings (Step 12) as the Dielectric Strength. If the limit of the instrument is reached before breakdown, report the Dielectric Strength as 50 K.V. at 25C. Cleaning of the test cup: ' . After the test is completed, drain the cup. Flush the cup with benzene. Then fill with Aroclor 1248 and let stand, until the next analysis. -42- NEV 007368 WATER PCB-SD0000030772 NOTEs An exception, when samples of oil from the plant are brought in for test, the cup must be thoroughly cleaned with benzene and carbon tetrachloride before and after running the test The electrodes: ' The testing cup has two electrodes. Both electrodes are movable and have twenty threads to the inch with index notches on both the electrodes and the lock nuts. To set the Gap: Arrange one of the electrodes and the lock nuts with the index marks in line. Move the other elec trode until it comes in firm contact with the first electrode and lock it. Now unsorew the electrode with the index marks in line (Step l) two complete turns and lock it. This will leave a gap of 0.1 inch between faces of the electrodes. Cleaning of the electrodes and the test cup free of carbon coating; The following ASTM method of cleaning shall be followed when it Is apparent from visual inspection that the electrode discs of the cup are coated with carbon. Wipe clean with dry calendered tissue paper the electrodes and the test cup. NEV 007369 WATER PCB-SD0000030773 The instrument is equipped with a 115 volt AC power supply which supplies all operating voltages for the bridge indicating circuits and in. addition supplies 500 V DC for application, to the material under test. The instrument is completely enclosed in a waxed finish shielded oak cabinet measuring 8-1/2" wide, 22-1/2" long and 8" high. Approximate weight--26 pounds. Test Electrodes: Two concentric nickel cylinders with feet, obtained from General Electric Company. The inner electrode has outside diameter of 2.8" and a height of 3.25" with area of 184 sq. cm. The outer electrode has an inside diameter of 3" and a height of 3,25" with area of 198 sq. cm. The distance between electrodes is, therefore,,0.1" or 0.254 cm. By theory, electrode constant (K) area/length is 191/0.254 or 752 where average area is 191 sq. cm. Also K - 36 x 10" x C (farads with air as dielectric) or 11.29 x C (mmfd. with air as dielectric). Glass Plate: Pyrex about 3~l/2" diameter with concentric grooves to assist in spacing electrodes. Obtained from General Electric Company. Heating Unit: Assembled in the laboratory and is the same unit -45- NEV 007371 WATER PCB-SD0000030774 described in Dielectric Constant Apparatus (see Method No. 11,608; Equipment). b. Procedure: 1) Assemble the test cell. Place the recently cleaned (within the last 8 hours--see Method No. 11,751j Step 9) electrodes in an 800 ml. beaker, . 2) Measure the capacitance of the test cell (Cg) according to Method No. 11,608 (Dielectric Constant and Power Factor measurements.) 3) Fill the cell assembly until the liquid level is 3/4 inch above the top of the electrodes. 4) Heat the assembly on the hot plate to 100 (+ 0.5)C. 5) Place the assembly inside of the testing oven. 6) Attach top lead (+) on the megohm bridge to inner electrode. 7) Attach other lead to outer electrode. 8) Throw the three switches at the top.of the megohm bridge to "ON" position. 9) Allow 10 minutes for assembly to reach temperature equilibrium inside the oven. DANGER: Make sure control knob is in "CHECK" position. Otherwise, painful shock will result if leads are touched. 10) Bring the galvanometer pointer to zero by turn ing the "ZERO ADJUST" knob in the direction in which the pointer of the galvanometer should move. 11) Turn the control knob to "CHARGE" position for 30 seconds. 12) Turn the control knob to "OPERATE" position and return the galvanometer pointer to zero by ad justment of the "MULTIPLY BY" switch and the megohm dial. 13) Read after 30 seconds. -46- N6V 007372 WATER PCB-SD0000030775 Calculation: Resistivity* - Megohm dial reading (Step 12} x "Multiply By" reading (Step 11) x capacitance of ~ cell (Step 2) in mmfd. x 11.29 x 0.001. Report the result in units of 109 ohm-cm. ^Values of resistivity are qualified by designation of temperature and voltage. These are for this test, 1008C and 500 volts DC. NOTE: It is important that the product under test, electrodes, and beaker be at uniform temperature for this determination. Temperature variations in different parts of the sample will cause the galva nometer zero to change constantly and give misleading results. CAUTION: Inasmuch as measurements must be made at a potential of 500 volts DC a shock hazard exists in the handling of this appartus. With the control knob in the charge and operate position full voltage of the bridge (500 volts) is applied to the positive and low terminals and through the test leads to the electrodes. Do not attempt to handle the electrodes of the test leads unless the control knob Is in the "CHECK" position. Possible penalty for failure to observe this precaution -- Painful Shock. 5. METHOD NO. 10,126 "CORROSION AND CHEMICAL STABILITY." a. Apparatus: G.E. Corrosion Apparatus consists of the following: 1) A Corrosion Flask - It is a 300-ml. Pyrex flask -47- NV 0073 73 WATER PCB-SD0000030776 with a ground glass 24/40 Joint equipped with - a 12-inch straight tube as an air cooled con denser. The air-condenser Is painted on the - outside with aluminum. 2) The Corrosion Apparatus: A transite box 32" long x tf" wide x 5" deep. The top of the box represents a split transite board with 5 holes cut to fit the flasks. The box is heated by two 500-watt, 15 volt G.E. Strip heaters with off-set terminals at one end (23.5" overall length). The heating length of the heating element is covered by a copper strip 19-1/2" long x 4" wide x 1/4" thick. The temperature is controlled by an automatic thermostat with temperature setting indicator. b. Procedures 1) Roll a rectangular (2" x 4") piece of aluminum foil so that it will pass through a ground glass 24/40 Joint of the corrosion test flask. CAUTION: Be careful that after rolling the specimen Hoes~not touch itself at any point. 2) Wash the aluminum foil (Step 1) scrupulously with acetone, distilled water, acetone, benzene, and chloride-free ether. 3) Then place the foil on a clean watch-glass and dry in an oven at 11078C. for 30 min. After cleaning handle the specimen with tongs or . 'forceps only. ^ "" .. 4) Weigh accurately on an analytical balance the specimen (Step 3) at room'temperature. 5) Drop the weighed aluminum foil into the chloridefree corrosion flask of the "Q.E. Corrosion Appa ratus ." Rinse out flask with sample and rinse end of condenser with sample. 6) Add 200 ml. of the product under test to the aluminum foil (Step 4 and 5). 7) Set the corrosion flask in the corrosion test appa ratus. -48- NEV 007374 WATER PCB-SD0000030777 8) Attach a 12-inch straight-tube air-cooled condenser. - the outside of which is painted with aluminum. ' - 9) Cover the exposed part of the flask with aluminum foil. 10) Heat the flask for 6 (+ 0.1) hours at 210 (+ 5)C. The temperature of the liquid in tie test flask is mea sured indirectly using a thermometer inserted through a cork stopper and into similar liquid contained in an identical flask seated adjacent to the test flask on the heating chamber. 11) At the end of the heating period, detach condenser from the flask before removing it from THenToT~pTate~ 12) Remove the flask from the hot plate and cover all of the flask with aluminum foil (when the flask is not on the hot plate.) 13) Without removing the aluminum foil covering of the flask, analyze the product (Step 6) remaining in the corrosion apparatus forj a) Appearance, Color-, and Condition. b) Inorganic (Free) Chlorides-- Apply Method No.10,118 c) Acidity (Acid Number) - Fellow Method No. 10,087 14) With a pair of clean, straight nichrome tongs, remove the aluminum foil specimen (Step 5), wash thoroughly, dry and weigh accurately on an analytical balance in the same manner as before (Steps 2, 3 and 4). Report the corrosion as loss or gain in weight to the nearest O.OOCl g. and the Chemical Stability, as indicated by the analysis of the products "After Corrosion Test", in the same way as reported for the original (as received) material. 6. METHOD NO. 10,118, "INORGANIC CHLORIDES." a. Preparation of Standards: 1) Make a primary standard of 100.0 ppm by weighing 0.1648 g. C.P. Nad into a chloride-free 1 liter volumetric flask. Dilute to the mark and mix thoroughly. Make a 10.0 ppm standard by diluting 100 ml. of the primary standard to 1 liter, and mixing well. For every 0.1 ppm standard, dilute to 10 ml. of the 10 ppm standard to one liter and -49- NEV 007375 WATER PCB-SD0000030778 mix well. A 0.1 ppm beam is considered the very faintest beam perceptible to the eye between 15.45 seconds after adding the AgNOo solution, if the beam intensity is not visible at all, or if easily visible (too strong), discard the solutions and make new standards, 2) Weigh 20.0 g. C.P. AgNOs into a chloride free dark bottle. Add 20 ml? C.P. HNO3 (chloridefree). Dilute to 200 mi, with water. 3) All solutions should be freshly prepared every two weeks and stored in glass-stoppered Pyrex bottles. '* b. Light Sources Employ the 2 battery Perilto flashlight, having a 3-4 mm. light aperture. New batteries must be used frequently in order to perceive beams properly. c. Procedures 1) Thoroughly rinse two separatory funnels with chloride-free water three or four times. Then take an aliquot from each funnel in a test tube which has been rinsed with chloride-free water. Test these aliquots for Tyndall beams by adding 3-5 drops of AgNOa and allowing 45 sec. for full beam to evolve. Absolutely no dust or chloride beam should be present. (Tf beam is present, rinse all equipment with 1:1 HNOo and repeat Step 1). " 2) When funnels are beam-free, drain out all the water except 50 ml. in one and 25 ml. in the other. Heat the water in both funnels tc boiling. (Hold stopper while heating as steam may cause- stopper to fail.) 3) Transfer 50 ml. of the sample from the sample bottle at a temperature of 95-100C. into the separatory funnel containing the 50 ml. of boiling water. (As a precautionary measure, pour some of- the sample from the sample bottle into a waste beaker before adding the 50 ml. to the funnel.) 4) Stopper the funnel and shake vigorously for at least 1 minute, venting frequently through the ' stopcock. (Care must be exercised at all times to touch neither the lower part of the funnel stem nor the ground part of the stopcock.) -50- NEV 007376 WATER PCB-SD0000030779 5) Allow the layers to separate and drain off the sample Into the second funnel containing the 25 ml. of boiling water, (as before, drain off a few ml. of the sample Into a waste beaker before draining the sample Into the second separatory funnel.) It may be necessary to heat the sample when transferring the sample to the second funnel; e.g., Aroclor 12o0. 6) Repeat step 4 and allow the layers to separate. Then drain off the sample Into a waste beaker. 7) Combine both water extracts In one funnel and shake thoroughly. 8) Take approximately a 3.0 ml. aliquot of the water extract out through the bottom of the funnel Into a 3/4" x 6" test tube. Again, first allow a few ml. to drain out before taking the aliquot. (The test tube used should be rinsed with, chloridefree water several times before using.) 9) Add approximately an equal portion of chloridefree ether. (The ether is tested by shaking a portion of it with chloride-free water and testing for Tyndall beam at the end of 45 sec. If beam is present, wash ether several times with chloridefree water until washings show no beam after adding 3-5 drops AgNO-j). 10) Shake the ether-water mixture until the emulsion in the sample disappears and the water layer is completely beam free before adding AgNOo. If emulsion is difficult to break, add sample dropwise through the ether and then shake. 11) Add 3-5 drops of 10$ AgNOj solution and test for chloride beam for 45 sec. exactly. If no beam is present at the end of 45 seconds, report as <0.1 ppm. The very faintest of beams is considered 0.1 ppm. If beam is stronger it will be necessary to compare with standards of 0.15# 0.20 up to 1.0 ppm, adding the 3-5 drops of AgNOo and comparing at the end of 45 sec. The method Is precise to the nearest 0.1 ppm. Report results to the nearest 0.1 ppm. METHOD NO. 10,087, "ACID NUMBER." a. Reagentsi 1) Nitration grade benzol. -51- 00737? WATER PCB-SD0000030780 2) Anhydrous methanol. 3) A saturated solution of phenol red (phenol sulfonphthaiein) in methanol (approx. 0.1$). 4) A 0.01 N solution of KOK in methanol. b. Procedure*. 1) Place 100 ml. of benzol, 100 ml. of methanol and 0.5 ml. (pipette) of phenol red indicator Into one of two clean dry 500 ml. Erienmeyer flasks. 2) Neutralize carefully with the 0.01 N KOH (to be first definite pink color.) 3) Pour the mixture back and forth between the two flasks several times. If the solution is still neutral, divide it equally between the two flasks, if not, repeat steps 2 and 3. 4) Weigh (+ 0.05 g.) into one of the flasks a 75.0 + 5.0 g. sample and titrate with the 0.01 N, KOH until the sample matches the blank. c. calculations: Acid No. (mg. KOH/gram sample) = ml. 0.01 N KOH x 0.56 . Sample Weight Report the results to the nearest 0.001 if they are below 0.1, otherwise to the nearest 0.01. The method is precise to + 0.002 for acid numbers below 0.01 and to + 0.01 Tn the range of 0.1 to 0.01. NOTE 1: To convert mg. KOH/gram to mg. NaOH/gram, multiply by 0.715. 8. METHOD `MODIFIED NO. 10,620, "MOISTURE (WATER)". ' a. Introductory Comments The Karl Fischer Reagent titration method used in the analytical laboratory involves use of an analyt ical balance to weigh accurately about one drop of water used in preparing the standard. Since .an analytical balance may not be available, the method has been modified and uses a purchased standard water solution as described below. Also, in the laboratory a "Dead Stop" potentiometric method for determining NEV 00737a WATER PCB-SD0000030781 the end point is often used. However, as this equipment may not be available, the procedure ' described below uses the visual indicator change < for determining the end point. bo Apparatus and Reagents: 1) Karl Fischer Burett, Automatic Pyrex No. 5750, l 25 ml. capacity. Ace Glass Company, Vineland, New Jersey. 2) Water Standard in Methanol. No. SO-W-2 {1 ml. ^ 1 mg. H2O) Fisher Scientific Company, 2.800 ( Jefferson Ave., St. Louis, Missouri. 3) Karl Fischer Reagent Solution No. SO-K-2, Fisher Scientific Company. c. Standardization of Karl Fischer Reagent l Into a 500 ml. clean, dry Erlenmeyer flask, place about 100 ml. "Anhydrous" methanol (commercially available, 99*95$). Add Karl Fischer reagent to this blank until the first color change from lemon yellow. It is not necessary to read the burette at this point. Carefully pipette 50 ml. of standard I water solution into the blanked methanol. Refill the Karl Fischer burette. Titrate the solution with gentle swirling to mix, until the same color is obtained as was obtained for the blank. Now read the burette. . ; Moisture value of K.F. reagent in terms of grams HgO per ml. - # (Moisture value of t `(Ml. Standard H2O solution) standard water so } lution in gm. per _____________ ______ ________ml. stated on lab { ml. Karl Fischer Reagent i d. Solvent Mixture: Since the solubility of the different askarels varies, the following solvent mixtures are suggested: !1 Material Anhydrous Benzene Anhydrous Methanol 1 Pyranol 1478 0 ml. 300 ml. Pyranol 1488 100 ml. 200 ml. I Pyranol 1467 100 ml. 200 ml. 1 Pyranol l48l 100 ml. 200 ml. Pyranol 1495 100 ml. 200 ml. 1 All Aroclors 110 ml. 190 ml. I Inerteen PPO 100 ml. 200 ml. -53- N6V 007379 WATER PCB-SD0000030782 e. procedure, "Visual End Point." 1) Place 100-300 ml. of dry solvent mixture (c) in a dry 500 ml. ground glass-stoppered Erle.nmeyer flask. 2) Titrate the solvent with K.P. reagent to the visual endpoint, l.e., the first change from the yellow to reddish orange that persists for 30 seconds, Refill the burette. 3) Using a beam balance, weigh to the nearest 0.1 gram by difference, a sample containing 0.03 to 0.06 grams H2O into the flask. 4) Stopper and shake until the sample Is in solution. 5) Titrate the solution with K.F. reagent to the endpoint described in Step 2. Record the volume of K.P. reagent used. Calculation; # HoO a ml. of K.P. reagent x HpO factor x 100 Sample Weight References: Mitchell, J. and Smith, D.M., Chemical Analysis, Vol. 5, Aquametry, Interscience Publishers, Inc., New York, (1948) -54- N6V 007380 WATER PCB-SD0000030783 9- 'HYDROLYSIS STABILITY TEST FOR ARC0LOR" Purpose .. To quantitatively determine the presence of unstable chlorine compounds in chlorinated biphenyls (askareis). Principle ' The method is based upon the hydrolysis of unstable chlorine compounds in as kart? Is by tn.ethar.oiic sodium hydroxide. The resulting chloride ion is determined potent ioineurioaliy by titration with silver r.Iti'ate solution in an essentially nonaqueous medium. The measured chloride icn, reported as parts per million in the askarel sample, is indicative of the relative stability of the askarsl in a dielectric system. Reagents 1. Methanol (chloride free) - 5 liters of methanol are refluxed with 0.5g Analytical Reagent Grade AgNOo for 1/2 hour. The methanol Is then distilled from the AgNCq, discarding the first 100 ml. to flush the apparatus. 90# of the charge is distilled from the flask and the contents of the flask are discarded. The methanol should be checked to assure purity by titration. The chloride ion concentration should be less than 0.01 ml. of 0.005N AgNC-j per 100 ml. of methanol. 2. Sodium Hydroxide Reagent - Analytical Reagent Grade NaOH (may be obtained from Mallinckrodt Chemical Company) Is used to prepare this reagent. A 0.1N solution is prepared by dissolving 4.0 grams of analytical reagent grade NaOH in 1 liter of chloride free methanol. 3. Sulfuric acid - Prepared by a 50:50 volumetric dilution of Analytical Reagent Grade concentrated sulfuric acid (can be obtained from Malllr.ckrodt Chemical Company) with chloride free (deionized or distilled) water. The acid is always poured into the water with constant stirring to prevent any dangerous build-up of heat. 4. 0.005N AgNO^ and G.0025N AgNOo - Prepared by dilution of an ampoule of concentrated aqueous AgNO,. Thess ampoules can be obtained from Anaehemlca Chemical Limited, Champlain, New York. This reagent may also oe prepared by dissolving 0.8495 g. of Analytical Reagent Grade AgNOo crystals (may be obtained from Mallinckrodt Chemical Company; in one liter of chloride free water containing 3.0 ml. of concentrated nitric acid. This solution should be standardized against a pure chloride standard. A sodium chloride crystal such as used in infrared spectrometer cells is a good source of pure Nad. The AgNOi solutions should be checked (at least monthly) to assure a consistent reagent. -55- NEV 007381 WATER PCB-SD0000030784 5. Acetone (chloride free) - Prepared by distillation from AgNOo as described above, for methanol and should also be checked by potentiometric titration to assure optimum purity. Normally a chloride content of less than 0.01 ml. of 0.0025N AgNOj per 100 ml. is derived by this method. 6. Benzene - Analytical Reagent Grads benzene should be used. This material is normally chloride free but should be checked by potentiometric titration to be certain. Analyti cal Reagent Grade benzene may be obtained from Mallinokrodt Chemical Co. Equipment 1. 200 ml. tall form beaker (Berzelius type). 2. Magnetic stirrer - A suitable magnetic stirrer with ring stand base can be obtained from Fisher Scientific Co. Cat. #14-511-1. This stirrer has a built-in rheostat and should be set at full speed and operated through a variac to adjust its speed. This will prevent heating of the stirrer during the stirring operation. 3. Teflon magnetic stirring bar - The bar should be cylindrical in shape and of one piece molded construction. one inch long, may be obtained from Fisher Scientific Co., Cat. #9-311-9. 4. Microburet graduated in 0.01 ml. divisions - A suitable buret may be obtained from Scientific Glass Apparatus Co., Inc. Bloomfield, New Jersey Cat. #JM-570. 5. Silver electrode - The Beckman silver billet electrode Cat #39261 is the preferred type. 6. Glass electrode - A standard glass electrode such as Beckman electrode Cat. #40498. 7. pH meter suitable for use with glass electrode - A model GS Beckman pH meter can be used. This instrument has the expanded scale and provides greatest sensitivity to incre mental emf changes. A somewhat less sensitive but, nonethe less, useable meter such as Beckman "Zeromatic" or the Leeds Northrop line operated pH meter can be used. 8. Water bath - An individual glass water bath 150mm in diameter 75mm high and containing 600 ml. of water heated to 40C. + 1C. is used. This glass water bath can be obtained from " Corning Glass Co., Corning, N.Y. Cat. #3140. 9. Usual laboratory glassware - 25 ml. pipette, buret or pipette graduated to deliver 0.5 ml., wash bottles for pure acetone methanol, water and a sturdy ringstand. -56- NEV 007382 WATER PCB-SD0000030785 Procedure for 1242 Aroclor (1499 Pyranol) 1. Twenty five grams of askarel is weighed into a tared 200 ml. beaker* to the nearest 0.01 gram on a suitable balance. 2. The' magnetic stirring bar is then added to the beaker containing the sample (without the bar touching the operators' hands), 3. Twenty five ml. 0.1N NaOH (methanolic) is added by means of a 25 ml. pipette and the beaker is covered with a watch glass. 4. The sample beaker is immersed to a depth of 1 1/4 inches in the 40 4_ 1C. water bath on a magnetic stirrer and clamped securely to a firm support. The sample is stirred at as fast a speed as possible, without pronounced splashing, for 1 houn. The water bath is not heated. No effort is made to maintain the temperature at 4oC., and it will drift toward equilibrium with room temperature. 5. After the 1 hour stir, the sample beaker is removed from the bath, 0.5 ml. of dilute sulfuric acid is added to the sample by means of a suitable pipette or buret. 125 ml. of chloride free acetone Is then added (a graduated cylinder is suitable for this purpose). 6. The sample is then titrated with 0.005N AgNOq solution using the silver-glass electrode system. Normal samples of askarel require extremely small amounts of AgNOo, for this reason the titration is run using 0.01 ml. additions and allowing sufficient time for equilibrium to be established before recording the emf change. If a change of less than Imv per 0.01 ml. addition is observed for 3 or 4 .01 ml. increments, larger additions of AgNOo may be used for instance .05 ml. until such a change isJ observed. The additions then are reduced to 0.01 ml. again to complete the titration. The endpoint normally is defined by two 50mv changes. A normal titration would yield the illowlng typical data. MV dMV* ML dML dMV/dML r-2 400 0 .06 0 392 8 .07 .01 352 8 . .08 .01 341 11 .09 .01 321 20 .10 .01 271 5.0 .11 .01 221 50 .12 .01 201 20 .13 .01 285 16 .14 .01 0 8 8 11 20 50 50 20 16 Using the GS pH meter the change is mi units and hence the meter changes observed would be 5 times this value (i.e. 25 units for 5mv). -57- NEV 0073S3 WATER PCB-SD0000030786 To calculate the change per 0.01 ml. observed, the mv change Is divided by the volume of AgNOj. By plotting dmv/dml vs. ml., the endpoint may be found to the nearest 0.001-ml. This gives a sensitivity of + O.OOTppm - to define the endpoint to + .01 ml. r.o plotting is necessary and- a sensitivity of + 3.07ppm is assumed. 7. A reagent blank is run exactly as above omitting the askarel sample. Calculations Subtract the reagent blank from the total volume of AgN03 and for the sample then: Reactive Chlorine (ppm) * Net Volume AgN03XNormality AgNO^X35.46xio3 weight : .. Procedure for 1254 and 1260 Aroclors (more viscous askarels) The procedure is followed exactly as above except that under Procedure, Step 2, 5 ml. of benzene is immediately added to the askarel sample and stirring bar. The sample is heated until it dissolves in the benzene and cooled to room temperature before proceeding to Step 3 The benzene, of course, should be Included in the reagent blank determination. Procedure for Micro Test The dechlorination test may also be run on 5 gram samples of askarels with a reduction in sensitivity. It is run exactly as the 25 gram test above except that the amount of reagents then used are 5-01 ml. NaOH (0.1N methanolic), 0.1 ml. H2SO4 for acidification, and 50 ml. of acetone to dilute the sample. 0.0025N AgN03 is used to titrate this size sample. The sensi tivity is then + 0.l8ppm rather than + O.OTppm given by the 25 g sample (without plotting the endpoint). General Comments A rapid titration can be made to the nearest 0.1 ml. using the normal potential at the equivalence point or use can be made of an automatic titrator for routine control procedures. The sensitivity in either case should be within + 0.7ppm of the value obtained by more refined techniques with 0.005N AgN03 and a 25 gram sample. The usual analytical precautions should be exercised In using this test method to prevent cross contamination from other sources of halogen in the laboratory. This means that all glassware, apparatus, and the area in wHXcE~THTs~Test is.run should be ahalytTcaTiy cl'eahT " ---- > :- -58- NEV 007384 WATER PCB-SD0000030787 10. "THERMAL STABILITY METHOD FOR AROCLORS Scope This method measures the thermal stability (chloride content) of chlorinated biphenyls used primarily as dielectrics, it is used for determining the quality of finished Aroclors. Principle Certain impurities if present in chlorinated biphenyls will break down at elevated temperatures with the liberation of HC1. The volatile HC1 is swept out of the sample with air, absorbed in water and titrated with silver nitrate solution. The results are expressed as parts per million chloride obtained during a 16 hour thermal stability test period. Reagents 1. Acetone. No special grade is required. It must contain no titratable chlorides. 2. V$> HNO3. Dilute 1 ml. concentrated HNO3 to 100 ml. 3. 0.005 NAgNOj. 0.8495g to 1000 ml. 5 ml. 0,1 NAgN03 (if available) to 100 ml. Apparatus 1. Pressure Regulator. Moore - Model 40 - 2 - 0-50" Water. Moore Products Co. H & Lycoming St., Philadelphia 24, Pennsylvania. 2. Thermoregulator. Cenco - 99015 - (Central Scientific Co.) 3. Relay. Ebert Micrelay SPST Std. Type. Ebert Electronics Corp., Queens Village, N.Y. (Any sensitive, reliable relay can be used). 4. Stirring Motor. Bodine NSI-13 B-2224 l/40 HP. 1725 R.P.M. 5. Bath Fluid. Dow Corning 550. 5 gallons 6. Leeds & Northrop ac. operated pH Meter - Cat. No. 7664 7. Silver wire electrode . 8. Mercurous Sulfate Reference Electrode. Modified L & N calomel reference electrode prepared as follows. Dismantle the internal element from the salt bridge tube of a standard L & N calomel reference electrode. Discard the saturated KC1 solution from the tube and clean out the mercurous NEV 007365 WATER PCB-SD0000030788 chloride and mercury from the internal element. Clean parts thoroughly. Add sufficient new clean mercury to the internal element to make contact with electrode wire and re-pack chamber of internal element with mercurous sulfate moistened with 0.5M potassium sulfate. Seal the chamber with non-absorbant cotton. Fill the salt bridge tube with 0.5M potassium sulfate and reassemble units. 9. Burette. 1.0 ml. microburette - Koch - Fisher Scientific Co. - 2C-110. 10. Magnetic Stirrer and glass covered stirring bar. 11. Glass Apparatus for Samples in Bath. See attached diagram. 12. capillaries. Glass capillaries approximately 0.2 mm in diameter and cut to a length that permits a flow of 45 ml. per min. of air, 13. Variac. 2 KVA. 14. Air Supply. Air under 4o lb. pressure is available in our laboratories. This air is purified by passing through a scrubber bottle containing 40^ NaOH, an empty bottle which serves as a safety, a second bottle containing cone. HpSO^ and a trap immersed in dry ice and acetone. The purified air is connected to a glass manifold having one connection for each sample. Capillaries of the appropriate length are connected between the manifold and the outlet for each sample. In this manner a constant flow of air can be obtained on all samples by applying a constant pressure to the manifold. 15. Heating Bath. A stainless steel bath constructed according to the specifications given in the attached diagram Is used. The bath is heated by applying 85 Volts to 3-500 Watt G.E. strip heaters bolted to the bottom of the bath. One 500 Watt Immersion heater is connected to the thermostat. Dow Corning 550 silicone is used as the bath liquid. The tem perature is maintained at 210 + 0.2C. The bath should be placed in hood and the tests carried out In total dark ness. Two 3 X 5" stainless steel plates not shown in the sketch are placed on top of the straightening vanes in the bottom of the bath. This provides better stirring to the ends of the bath. Twelve samples can be run in the bath at one time. . Procedure Weigh a 290 + 1 g. sample of Aroclor into the 300 ml. Erlenmeyer flask. Insert the gas inlet tube and position the flask in the 210 + 0.5C. bath. The bath fluid level should be approximately one inch below the bottom of the ground glass joint on the flask, place 10 ml. distilled water in the Volhard flask absorber and attach to the receiver tube from the Erlenmeyer flask. Connect the purified air supply from the capillary to the inlet down tube -60" NEV 007386 WATER PCB-SD0000030789 in the flask. Bubble air through the sample for 16 hours at the rate of 35 to 45 ml. per minute. (The apparatus and/or sample must be kept in the dark during the 16 hour period). Transfer the water from the absorber to a 100 ml. beaker using approximately 50 ml. acetone, and 2 drops 1% HNOo solution and titrate with 0.005N AgNO^ solution using a magnetic stirrer. The titration is stopped at 75 mv. which represents the point of maximum potential change and the titration endpoint. Silver wire and. mercurous sulfate electrodes (Ag-Hg, Hg2SC>4, 0.5M K2S04 system) are used for the titration. Calculations (Total ml. 0.005 NAgNOj used) (0.6l) = ppm chloride * 1 ml. 0.005 NAgNOg is equivalent to 0.0001773g. chloride or 0.6l ppm. Precision and Reliability The precision of the test (standard deviation) is 0.02 ppm at the 0.5 ppm chloride level and 0.06 ppm at the 2.8 ppm lev61. The method as written does not necessarily quantitatively measure the total unstable chlorides present. For screening purposes a total chloride figure is not necessary. Experience has shown that there is good correlation between the chloride figures obtained by this 16 hour thermal stability test and the quality of chlorinated biphenyls. Discussion The air supply can be checked for chloride contamination by passing the air through an empty sample flask immersed In the bath. Not more than 0.03 ml. 0.005 NAgNOg should be required to give the endpoint. The air supply can be checked for ammonia by measuring the pH of the absorber solution or titrating with 0.01N HC1. The pH should be between 6 and J. Compressed cylinder air available for breathing purposes can perhaps be used without any purification. Experience has shown that nitrogen gives low chloride figures. This indicates that air is a neces sary part of this test and that nitrogen cannot be used as a substitute. Gum rubber tubing is used in making all connections. The apparatus is cleaned with acetone. -61- NEV 007387 WATER PCB-SD0000030790 CHAPTER 7 TYPICAL PROPERTIES The 1200 series members of the Aroclor family are chlor inated biphenyls, and are made by chlorinating biphenyl to approximately the percentage of chlorine, by weight, in dicated by the last two digits of the serial number. For example, Aroclor 1254 is approximately 54# chlorine on a weight basis. Accordingly, these Aroclors are not single or simple compounds. They are a mixture of isomeric com pounds composed predominately of the chemical compound in dicated below as being their approximate equivalent: Aroclor 1242 Aroclor 1248 Aroclor 125^ Aroclor 1260 Trichlorobiphenyl Tetrachlorobiphenyl Pentachloroblphenyl Hexachlorobiphenyl . For transformer use and some capacitor- use where lower viscosity is required for better low temperature operation than offered by the above Aroclors, these products are mixed with pour point depressants, particularly trichlorobenzene resulting in various General Electric Company Pyranols described briefly as follows: Transformer Pyranol 1467* 60# of Aroclor 1260 40# of Elec. Grade Trichlorobenzene 0.125# of Tin Tetraphenyl Transformer Pyranol 1470* 45# of Aroclor 1260 55# of Elec. Grade Trichloro- Tetrachlorobenzene Mixture 0.125# of Tin Tetraphenyl % *Use of tin tetraphenyl scavenger is subject to G.E. patents and license: Royalty arrangements should be checked before using Pyranol 1467. Questions about license concerning the use of anthraquinone stabilizer for DC capacitors should be referred to Western Electric, 195 Broadway, N.Y.C. -62- 00738a WATER PCB-SD0000030791 Transformer Inerteen PPO 60# of Aroclor 1260 40# of Elec. Grade Trichlorobenzene 0.20# Phenoxypropene oxide Capacitor Pyranol 1481 75# of Aroclor 1254 25# of Elec. Grade Tri chlorobenzene Detailed properties of all of these products are given in the following property lists. -63- - NEV 007389 WATER PCB-SD0000030792 AROCLOR 1232 PROPERTY Vise. 37.8C. (ASTM D88) Specific Gravity @ 25/15.5C. (ASTM D287) Color, APHA Condition ' Clear Acidity, mg. KOH/g. Pcur Point, C. (ASTM D97) Inorganic Chlorides, ppm. Refractive Index 25C. Distillation Range (ASTM D20) Corrected for stem and barometic pressure Corrosion Water Content, ppm Resistivity 100C., 500 volts DC 0.1"gap Dielectric constant 100c. 1000 cycles (ASTM D924) Sulfates (ASTM-D117-31)* . Fixed Chlorine content (Carius)* Dielectric Strength (KV) (ASTM D877)* Hydrolysis Stability Test Chlorides, ppm. Thermal Stability Test Chlorides, ppm. TYPICAL 44 - 51 1.270 - 1.280 50 Max. 0.014 Max. -30 or lower 0.10 max. 1.6200 - 1.6220 10# - 293C. min. 50# - 310 - 320C. 90# - 360C. max. After heating with aluminum for six hours at 210C. t 10C. the aluminum must not be corroded either on visual or weight inspection and the Aroolor 1242 should meet the following specs: Color, APHA 100 max. Acidity, mg.KOH/g. 0.014 max. Inorg. Chlorides, ppm. 0.10 max. Condition Gear 35 max. 00 x 10 Ohm-cm., min. .3 - 4.5 None 31.5 - 32.5 35 min. 3.0 (tentative) max. 0.5 (tentative) max. *Not determined unless by special request. -64- 00l' WATER PCB-SD0000030793 AROCLOR 1242 PROPERTY - TYPICAL Vise. at-27.8C. (ASTM D88) Specific Gravity at 25/15oC. (ASTM D287) Color, APHA Condition Acidity, mg. KOH/g. Pour Pt., >C. (ASTM D97) Inorganic Chlorides, ppm. Refractive Index at 25 C. Distillation Range (ASTM D20) Corrected for stem and barometric pressure Corrosion 82 - 92 seconds Saybolt Univer. 1.381 - 1.392 50 max. Clear 0.01 max. -14 or lower No detectable amount 1.6240 - 1.6260 10# 325C. min. 90$ Q60i^fli'. max. After heating with aluminum for six hours at 210C + 10C, the aluminum must not be cor roded either on visual or weight inspection and the Aroclor 1242 should meet the following specs: Water Content, ppm Resistivity 100C. 500 volts DC at 0.1" gap Dielectric Constant 100C. at 1000 cycles (ASTM D924) Flash Point Cleve. Open Cup* Fire Point C.* Sulfates (ASTM-D117-31)* Fixed chlorine content (Carlus)* Specific Heat at 25C.* Evaporation at 100C for 6 hrs.* Dielectric Strength (KV) (ASTM D877)* Color, APHA 60 max. Acidity, mg.KOH/g. 0.01 max. Inorg.Chlorides,ppm no detectable ' amount Condition Clear 35 max. 500 x 109 ohm-cm., min. 4.7 - 4.9 170 - 200C. None to boiling point None ' . $43 + 0.5560 02 0.4$ max. 35 Min. Not determined unless by special request. Hydrolysis Stability Test chlorides, ppm Thermal Stability Test chlorides, ppm 1.0 (tentative) max. 0.40 (tentative) max. -65- NEV 007391 WATER PCB-SD0000030794 AROCLOR 1248 PROPERTY Vise, at 54.4C. (ASTM D-88) Spec. Gravity at 65/15.5C. (ASTM D-287) Color, APHA Condition Acidity, mg. KOH/g. Pour Point C. (ASTM D-97) Refrac. Index at 20C. Dist. Range (ASTM D-20) Water Content, ppm. Resist. 100C. 500 v D.C. at 0.1" gap Dielectric constant, 100C. 1000 cycle Dielectric Strength 25C.* Flash point, (C.O.C.)* Fixed Chlorine (Carius)* Specific heat at 25C.* Inorganic chlorides, ppm. TYPICAL 73 80, Seo. Saybold Universal 1.405 - 1.415 100 Max. Clear 0.01 max. -7 1.6285 - 1.6305 First drop 310eG, min. 1056 - 345C. Min. 90$ - 385C. Max. 35 500 x 10 Ohra-cm., min. 4.6 35 KV min. 193C. 47.5 - 48.5# 0.27 0.10 max. *Not determined unless by special request. Hydrolysis Stability Test chlorides, ppm. Thermal Stability Test chlorides, ppm. 3.0 (tentative)*max. 0.5 (tentative) max. -66- Nv 007392 WATER PCB-SD0000030795 AROCLOR 1254 PROPERTY Vise, at 98.9'C. (ASTM D88) ' Specific Gravity at 65/15*5#C. (ASTM D28?) Color, APHA Condition Acidity, mg.KOH/g. Pour Pt. *C. (ASTM D97) Inorganic Chlorides, ppm. Refractive Index at 25C. Distillation Range (ASTM D20) Corrected for stem and Barometric Pressure Corrosion TYPICAL . 44 - 48 sec. Saybolt Univer. 1.495 - 1.505 100 max. Clear 0.01 max. 7-12 No detectable amount 1.6370 - 1.6390 100 366 - 37oC. 500 371 - 383*C. 900 379 - 394*C. After heating with aluminum for 6 hours at 210*C. plus or minus 10C. the aluminum must not be corroded either on visual or weight inspection and the Aroclor 1254 should meet the following specs: Water Content, ppm. Resistivity 100C., 500 v D.C. at 0.1" gap Dielectric Constant, 100C. 1000 cycles Dielectric Strength, 25*C.* Burn Point (ASTM D92)* Sulfates (ASTM D-117-31)* Fixed Chlorine Content (Carius)* Evaporation at 100'C. for 6 hrs.* Stability* Ageing Characteristics* Specific Heat at 25*C.* Color, APHA 150 max. Acidity, mg.KOH/g. 0.01 max. Free Chlorides,ppm. . No detec table amount Condition Clear 35 max. 500 x 10^ ohm-cm., min. 4.15 - 4.35 35 KV, rain. Higher than 350*C. None 55 + 0.50 0.4jC max. There shall be no liberation of chlorine or chlorides when the material is heated at 100*C. in glass vessels in contact with air for periods of at least one month. No loss in resistivity over original value on heating in air for 96'hrs. at 100*C. 0,26 .v 1 *Not determined unless by special request. Hydrolysis Stability Test Chlorides, ppm. Thermal Stability Test Chlorides, ppm. 3.0 (tentative)max. 0.5 (tentative)max. nev 7393 WATER PCB-SD0000030796 AROCLOR 1260 PROPERTY TYPICAL Vise, at 98.9C. (ASTM D88) Specific Gravity at 90C./15.5C, (ASTM D287) Color, APHA Condition Acidity, mg.KOH/g. Pour Pt.,C.(ASTM D97) Inorganic chlorides, ppm. . Refractive Index, 25C. Distillation Range (ASTM D20) Corrected for stem and barometric pressure. Corrosion 72 - 78 Sec. Saybolt Univ. 1.555 - 1.566 150 max. Clear 0.01 max, 25 - 34 No detectable amount 1.6455 - 1.6470 10 385 - 398C. 50# 390 - 404C. 90# 400 - 420C. After heating with aluminum for 6 hrs. at 210C. + 10C. the aluminum must not be cor roded either on visual or weight inspection and the Aroclor 1260 should meet the following specs: Water content, ppm. , Resistivity,100C. 500 volts at 0.1" gap Dielectric Strength 50C.* Dielectric Strength 100C.* Dielectric Constant 100C. at 1000 cycles* Burn Pt. (ASTM D92)* Sulfates (ASTM D117-31)* Fixed chlorine content (Carius)* Evaporation at 100C. for 6 hrs.* Stability* Specific Heat at 25C.* Color, APHA 150 max. Free Chlorides,ppm. No detec table amount. Acidity,mg.KOH/g. 0.01 max. Condition Clear 35 max. 500 x 109 ohm--cm., min. 30 KV., min. 30 KV., min. 3.6 - 3.8 Higher than 350C. None 60 + 0.5# 0.2$ max. There shall be no liberation of chlorine or chlorides when the material is heated at 100C. in a glass vessel in contact with air for periods of at least one month. 0.23 *Not determined unless by special request. Hydrolysis Stability Test chlorides,ppm. Thermal Stability Test chlorides, ppm. 3.0 (tentative) max. 0.7 (tentative) max. -68- NEV 007394 WATER PCB-SD0000030797 PYRANOL 1481 PROPERTIES Viscosity at 37.8*0. Spec. Gravity at 15.5/155C. Color, APHA Condition Acidity, mg. KOH/g. Pour Pt., *C. Inorganic Chlorides, ppm. Refractive Index at 25C. Distillation Range Corrected for stem and barometric pressure. First drop 25# max. 90# Corrosion Test Change in Weight Color, APHA Acidity, after test, mg.KOH/g. Free Chlorides, ppm. Condition after test Water Content, ppm. Resistivity at 100C 500 volts, DC, 0.1"gap Dielectric Constant (100C., 1000 cycles) Hydrolysis Stability Test chlorides, ppm. Thermal Stability Test chlorides, ppm. TYPICAL . 70 - 82 sec. Saybolt Univ. 1.525 - 1.535 150 max. Clear 0.01 max. -15 or lower 0.10 max. 1.6205 - 1.6215 205C. min. Below 270C. 380 - 395C. 0.0# 200 max. 0.01 max. 0.10 max. Clear 35 max. . 100 x 109 ohm"cm1min 4.1 - 4.6 3.0 (tentative) max. 0.5 (tentative) max. -69- NEV 007395 WATER PCB-SD0000030798 PYRANOL 1488 PROPERTIES. TYPICAL Vise, at 37.8C. Spec. Grav. at 15.5/l5.5C. Color, APHA Acidity (Mg KOH/g) Water, ppm. Condition Refrac. Index at 25C. Free Chloride, ppm. Pour Point, C. Resis. at 100C., 500 v D.C. 1" gap Dielectric Strength (25C.) Corrosion: Loss of Aluminum 54-2 Sec. Saybolt Unlv. 1.560 - 1.568 150 max. .014 max. 35 max. Clear 1.6137 - 1.6147 0.10 max. ' Lower than -32C. 100 x 10^ ohm-cm min. Over 35 KV None Heating with aluminum for 6 hrs. at 200-220C. The Pyranol after heating should meet the following specs: Dielectric Constant at 1000 cycles at 100C.* Distilling Range (corrected)* 1st drop Below 270C. 90$ point Burn Point (ASTM D-92)* Fixed Chlorines* Arc Formed Gases* (Oxygen-free liquid at 25C.) Color, APHA Acidity (MgKOH/g) Free Chlorides ppm Condition 200 max. .014 max. .10 max. Clear 3.7 - 4.0 200C. min. 40$ max. 295 - 4l5C. None up to boiling point 59.1# min. Less than 1.0$ total com bustible gases including carbon monoxide, hydrogen, and volatile hydrocarbons. *Not determined unless by special request. -70- NEV 007396 WATER PCB-SD0000030799 PYRANOL 1467 PROPERTIES TYPICAL Vise, at 37.8C., (ASTM D88) Specific Gravity at 15.5/15*5C. (ASTM D-287) Color, APHA Condition Acidity, mg. KOH/g. Pour Point, C. (ASTM D-97) Inorganic Chlorides, ppm. Refractive Index at 25C. Distillation Range (ASTM D20) Corrected for stem and barometric pressure Corrosion 54+2 sec. Saybolt Univ. 1.560 - 1.568 150 max. Clear 0.01 max. -32C. or lower 0.10 max. 1.6137 - 1.6147 1st drop - 200#C. min. Below 270C. - 40# max. 907; - 395 - 415C. After heating with aluminum for 6 hrs. at 200-220C., the aluminum must not be corroded either on visual or weight in spection and the Pyranol should meet the following specs: Color, APHA Acidity, mg.KOH/g. Inorganic Chlorides PPm. Condition 200 max. 0.01 max. 5 max. Clear WaterContent, ppm. Resistivity, 100C. 500 volts, 0.1" gap Dielectric Strength, 25#C. Dielectric Constant, 100C. 1000 cycles* Tin Tetraphenyl* Burn Point, (ASTM D92)* Fixed Chlorine* Arc Formed Gases* (Oxygen Free Liquid at 25C.) 30 max. 100 x 109 ohm-cm., min. 35 KV., min. 3.7 - 4.0 0.125# + 0.01# by weight None up"*to Boiling Point 59*1# min. Less than 1.0# Total combustible gases including carbon monoxide, hydrogen and volatile hydro carbons. *Not determined unless by special request. -71- NEV 007397 WATER PCB-SD0000030800 PYRANOL 1470 PROPERTIES TYPICAL Vise, at 37.8C. (ASTM D88) Spec. Gravity at 15.5/l5.56C., (ASTM D287) Color, APHA Condition Acidity, mg. KOH/g. Pour Pt., C., (ASTM D97) Inorganic Chlorides, ppm. Refractive Index at 25C. Distillation Range (ASTM D20) Corrected for stem and barometric pressure First drop 35$ 95$ Corrosion Water Content, ppm. Resistivity, 100C., 500 v., 0.1"gap Dielectric Strength, 25C. Dielectric Constant, 100C., 1000 cycles# Tin Tetraphenyl* Burn Point, (ASTM D92)* Fixed Chlorine# Arc Formed Gases* (Oxygen Free Liquid at 25C.) Electrical Stability* 41-45 Sec. Saybolt Unlv. 1.563 - 1.571 150 max. Clear' 0.01 max. -44C., or lower 0.10 max. 1.6075 - I.6085 210C., min. 240 - 256C. 290 - 330C. 385 - 400C. 395 - 415C. After heating with aluminum for 6 hrs. at 200-220C., the aluminum must not be corroded either on visual or weight inspection and the Pyranol should meet the following specs: Color, APHA Acidity, mg.KOH/g. Inorg.Chlorides,ppm Condition 30 max. 200 max. 0.01 max. 5 max. Clear 100 x 10^ ohm-cm., min. 35 KV., min. 3.8 - 4.3 0.125$ 0.01^ by weight None up to Boiling Point 60.5 0.5 Total combustible gases in cluding carbon monoxide, hydro gen and volatile hydrocarbons. After heating for 96 hrs. at 100C. in a closed container, the resistivity should not decrease more than 10$. *Not determined unless by special request. "72- N 007398 WATER PCB-SD0000030801 INERTEEN PPO PROPERTIES Vise. @ 37.8C., (ASTM D88) Specific Gravity @ 15.5/15.5C. (ASTM D-287) Color APHA Condition Acidity, mg. KOH/g. Pour point, C. (ASTM D-97) Inorganic Chlorides, ppm. Refractive Index @ 25C. Distillation range (ASTM D20) Corrected for stem and barometic pressure Corrosion Water content, ppm. Resist., 100C. 500 Volts, 0.1" gap Dielectric Strength, 25C. Dielectric constant, 100C. 1000 cycles* Phenoxy Propene Oxide or Glycidyl Phenyl Ether Burn point, (ASTM D92)* Fixed Chlorine* Arc formed gases* (Oxygen free liquid @ 25C*) TYPICAL 54- 2 sec. Saybolt Universal 1.560 - 1.568 150 max. Clear 0.014 max. -32C. or lower 0.10 max. 1.6137 - 1.6147 First drop - 200C. min. Below 270C. - 40$ max. 90$ - 395 - 4l5C. After heating with aluminum for 6 hours at 200 - 220C. the aluminum must not be corroded either on visual or weight inspection and the askarel should meet the follow ing specs: Color, APHA 200 rr..*x. Acidity, mg.KOH/g. 0.01*! r-- Inorganic Chlorides, ppm. 2 max. Condition Clear 30 max. 100 x 10 Ohm-cm., min. 35 KV., min. 3.7 - 4.0 0.1856 - O.2256 by weight None up to boiling point 59.156 min. Less than I.O56 Total combustible gases including carbon monoxide, hydrogen and volatile hydro carbons . *Not determined unless by special request. -73- NEV 007399 WATER PCB-SD0000030802 CHAPTER 8 QUALITY REQUIREMENTS OF AROCLORS PRIOR TO USE IN THE ELECTRICAL INDUSTRY Quality as Supplied to the Electrical Industry Aroclors and their mixtures supplied to the electrical industry must meet the strict requirements specified by the Industry and given in the specifications shown in Chapter 7. The electrical qualities, such as resistivity and power factor of the materials, as supplied, are not the maximum attainable. It is impractical for the manufacturer to furnish these dielectrics to the customer at the maximum attainable qualities because even with careful packaging, sampling, shipping, and handling, these fluids may pick up traces of contaminants from "clean" tank cars, drums, pipe lines, pumps, etc. However, as supplied in accordance with the specifications, the fluids must respond readily to "up-grading" by earth treatment to arrive at the desired maximum refinement required for use by the electrical industry. Typical Electrical Quality of Aroclors Used in the Industry Capacitor Impregnation Table IV indicates the desirable minimum resistivity values of Aroclor dielectrics immediately after earth refinement by the user when ready to impregnate capacitors. These values are compared with the similar values of the material after the capacitor impregnation has been completed in a relatively clean system. -74- 007400 WATER PCB-SD0000030803 TABLE IV Dielectric Volume Resistivity Ohm-cm at 100C. and 500 volts DC. Prior to After impregnation impregnation Aroclor 1254 2.500 x 10 800 x 10 Aroclor 1242 1.500 x 10 600 x 10 Pyranol l48l 600 x 10 400 x 10 The power factor of earth refined Aroclor prior to capacitor impregnation should not exceed 0.1 percent at 100C. and 1000 cycles. Transformer Filling The minimum resistivity of transformer askarel as specified for supply to the electrical industry is 100 x 10 Ohm-cm. at 100C., 500 volts and 0.1 inch gap. While power factor is not part of the suppliers official specification, this value for freshly made transformer askarel ranges from 0.1 to 0.3 percent at 100C. and 1000 cycles. This would be approximately 0.05 percent at 20C. and 60 cycles. In order to arrive at higher and yet practical dielectric values the transformer manufacturer needs to earth refine the fluids immediately prior to using. It is reasonable to strive for a volume resistivity value around 1,500 x 10 Ohm-cm, at 100C. and power factor values of about 0.05 percent at 20C. and 60 cycles or 2 percent at 100C. and 60 cycles. -75-' NEV 007401 WATER PCB-SD0000030804 Table V compares resistivity readings with the corres ponding power factor values obtained on the given samples of typical transformer askarel. TABLE V Volume Resistivity 10e Ohm-cm. at 100C. Power Factor 60 cy. 100*0. 60 cy. 20C. 1,500 2# 0.05# 500 5* 0.1# 100 60-70 15# 20-25# 0.7# 2.0# When adequately earth refined to give a resistivity in the range of 500 to 1500 x 10 Ohm-cm. at 100C., sample of such transformer askarel taken after filling a newly constructed and relatively clean transformer should have a resistivity of at least 200 x 10 Ohm-cm. at 100C. and a corresponding power factor less than 12 percent at 100C, and 60 cycles. -76- NV 007402 WATER PCB-SD0000030805 CHAPTER 9 EARTH REFINEMENT OF AROCLORS TO ARRIVE AT THE DESIRED ELECTRICAL QUALITIES Earth Treatment In the Laboratory Preparatory to Analysis In Chapter 5 n Page 27 the laboratory procedure for preparing the test sample using 0.1 to 0.2 percent of activated earth Is given. It is also stated that the absorbent is minus 200 mesh Attapulgus earth' activated Just prior to use by heating in shallow trays for four hours at 400C. (752F.) or for at least 12 hours at 250C. (482P.) Earth Treatment by the Plant Manufacturing the Askarel Earth refinement in the plant is essentially the same as used when preparing the laboratory sample. The same amount of freshly conditioned earth (0.1 percent to 0,2 percent by weight) is added to the askarel and the mixture is agitated thoroughly and heated for about four hours. The more viscous dielectrics, such as Aroclor 1248 and Aroclor 1254 are heated at about 70 to 8oC. (158 to 176F.) and the less viscous materials such as Aroclor 1242 and Pyranols l48l, 1467 and 1470, or Inerteen PPO are heated at about 50 to 60C. (122 to l40F.) After about four hours contact the earth is removed from the dielectric fluids using a Sparkler or Sweetland or a comparable filter press, previously fitted with filter paper liners such as supplied by Carl Schleicher & Schuel Company, Inc., Keene, New Hampshire. The paper is usually 25 mils thick -77- NEV 007403 WATER PCB-SD0000030806 and must be dried at 100C. to remove moisture prior to use in the filter press. Earth Refinement by the User Capacitor Manufacturers: Capacitor manufacturers usually use the same procedure for earth refining as employed by the manufacturer of the askarels. Because this method employs loose earth which can be thoroughly mixed into the askarel, it is believed to be the most efficient and is certainly known to give very good results. However, towers (cylinders) filled with relatively coarse earth through which the dielectric fluids are pumped and recirculated have also been used by capacitor manufacturers. Transformer Manufacturers: The large manufacturers of askarel transformers usually use the same type of procedure for refinement with loose earth as employed by the manufacturer of the askarel dielectrics. Handling relatively large amounts of the askarel transformer fluid Justifies installing the tanks and filter presses required. This earth refining equipment is . usually supplemented with portable cartridge type filters or a small portable platen frame type filter press. This latter equipment is then used when newly made askarel transformers are filled with the fluid and it is necessary to clean the transformer and the fluid by draining out the fluid pumping it through the filter press or cartridges containing the earth and recirculating until the desired electrical properties are attained. Likewise, smaller manufacturers of askarel transformers can use most conveniently the portable cartridge or platen frame type filters. ,,p N6V 007404 WATER PCB-SD0000030807 t The Effect of Earth Refinement on Removal of Tin Tefcraphenyl Scavengers from the Transformer Askarel; As indicated above, normally transformer askarels respond readily to up-grading by the use of 0.1 to 0.2 percent by weight of earth based on the total weight of the fluid. However, if the fluids are unusually contaminated, larger amounts of earth are required to up-grade the dielectrics. This raises question about the selective adsorption of the scavengers by the earth treatment. It is indicated that to selectively adsorb significant amounts of the scavengers, repeated treatment with 1 percent or more of earth is required, as shown in the following table: TABLE VI REMOVAL OF TIN-TETRAPHENYL BY REPEATED TREATMENT OF ASKAREL WITH ONE PERCENT OF EARTH Sample No. Pyranol l4yo 1 Pyranol l4y0 2 Original O.II956 0.10756 Tln-tetraphenyl Content After 4 treatments After 7 treatments at 90C. at 90C. O.OI856 O.OO656 After 4 treatments After 6 treatments at 60C. at 60c. 0.02156 0.00356 -79- NEV 00 7405 WATER PCB-SD0000030808 CHAPTER 10 ... CONTAMINATION Askarels as supplied by the manufacturer respond readily to earth refining resulting in a very high order of dielectric properties. For example, it is possible to attain volume resistivity values up to 20,000 or 30,000 x 10^ Ohm-Cm. at 100C., 500 volts, 0.1 inch gap and power factor values no more than 0.05# at 100C. and 1000 cycles. Except for very special situations, it Is not practical to refine these dielectrics to this extent. In commercial use, transfer of the fluids from one clean container to another which may result in contacting traces of conducting impurities does not allow maintaining such a high order of dielectric properties. Referring to electrical values, this accounts for the more practical order of specification values as indicated in Chapter 7 and to which the electric industry has committed the supplier of the dielectrics. This also aocounts for the desirability and need of the user of askarel dielectrics to earth refine Immediately prior to use in order to arrive at the maximum and yet practical dielectric values for his given purpose. Such quality values relative to askarels for capacitors and transformer work were Indicated in the preceding Chapter 8. AVOIDANCE OF CONTAMINATING ASKAREL CAPACITORS It is necessary, practical and economical that all steps possible be taken to avoid contaminating influences in the manu facture of askarel capacitors. -80- , Mtv 001-00 WATER PCB-SD0000030809 ! Sometimes capacitor manufacturers strive to attain the very | high order of dielectric qualities possible for askarel as mentioned above. Since it is very difficult, if not almost impossible to 1 j maintain such a high order, usually capacitor manufacturers comply . with the more practical schedule attainable by normal earth refining practices as shown in Table IV Chapter 8. j Equal care must be exercised in selecting, conditioning and handling the other construction materials of the askarel capacitor. i i For example, the water used in manufacturing capacitor tissue is , either distilled or deionized. Quality control of the capacitor 1 paper requires chemical tests to characterize the fiber and its | purity. Physical and electrical tests to determine moisture and power factor are essential. Acceptable dielectric loss values of | the dry and unimpregnated paper do not suffice for Judging quality , because in some instances after impregnation with good quality ' askarel, higher dielectric losses increasing rapidly with temperature | may be obtained. The aluminum foil used must be extremely pure and free from | residual traces of rolling oils or compounds. Accordingly, the | term usually applied to the foil Is "dry" foil. Similar care and 1 purity requirements apply to the aluminum tabs used. j The paper and aluminum foil is wound to form the core in an air conditioned room and often the machine operators are required J to wear cotton gloves to prevent oil from the operators skin contaminating the cores. " ' The steel cans or turn plate capacitor cans require thorough J cleansing and degreasing with perchloroethylene of required purity and free of any objectionable stabilizing agents. Similarly, the j -81 ' NEV 007407 WATER PCB-SD0000030810 capacitor impregnating equipment and chambers must be kept clean. To facilitate maintenance of cleanliness, sometimes stainless steel construction is used. However, ordinary steel equipment is common and when "conditioned", that Is to say, coated with a thin film of clean Aroclor, this type of construction material is entirely satisfactory. To condition a new plant or clean an old one, askarel is circulated through the system, then purified by earth refining and recirculated. This process is repeated until all contaminating influences have been removed. Moisture, probably the most obvious contaminent in askarel impregnated capacitors, increases the dieleotrlc loss under AC voltage and decreases the capacitor life. Therefore, very efficient vacuum, as low as 5 or 10 microns, and heat carefully controlled up to 130C. are employed to expel the moisture from the capacitor cores prior to impregnation. Also to avoid moisture entering the askarel during storage, it is common practice to warm the dielectric in the storage tank to about 50C. in the presence of mild vacuum. Traces of any substances soluble in askarel and capable of ionization will have a marked adversed effect on the dielectric loss of the askarel or the finished capacitor. Therefore, much r care is required to avoid contamination with solder flux. For example, the use of rosin core solder is known to cause contamination. When rim sealing compounds are used in the lids of small capacitors, there must be assurance that the catalyst or other ingredients used in such materials do not cause contamination. Improperly selected pipe sealing compounds used on the threads on the fittings for sight glasses and instruments on the storage and impregnating equipment are known to have caused contamination. -82- fl nEV oo?^a WATER PCB-SD0000030811 ######* All these factors about contamination must be kept in mind when impregnating capacitors, especially by the chamber method but also by the manifold method. The moisture content of the paper used in the capacitor cores may easily introduce several gallons of water into the average impregnating chamber. This water is removed from the capacitors prior to impregnation -- usually by heating the chamber to 130C. in the presence of efficient vacuum, 100 microns or less. If the chamber is not made of the preferred materials of construction, slight corrosion (iron rusting) may occur and the film of askarel on the interior surface of the tank may become contaminated and introduce traces of impurities into the clean dielectric fluid entering the chamber for impregnating the capacitors. In fact, because of this possibility of contamination, in some operations the capacitors are conditioned and dried in a separate oven or chamber. Then when thoroughly dried, they are then transferred into a second chamber used only for impregnation. In the case of relatively large sized capacitors, such as power factor correction units, a manifold with branches may be used to handle each unit Individually rather than by the batch -- chamber method. The unimpregnated capacitors are placed into an oven and vacuum is applied to the individual units attached to the manifold. After the capacitors have been evacuated and dried> the askarel is introduced through the manifold and its branches. Care must be taken that moist air or contaminants do not collect in the branches through which the dielectric is introduced. *** -82A- NEV 007409 WATER PCB-SD0000030812 Care must be taken to avoid contamination with any kind of grease, oil, packing material and "rubber" gaskets used with the machinery, such as pumps, etc., connected with the handling and impregnating facilities. It is not practical to discuss all possible sources of contamination and it should suffice to say that the manufacturers of askarel capacitors need to and do exercise all known precautions to avoid contamination and should evaluate and life test represent ative units before supplying the finished merchandise. AVOIDANCE OF CONTAMINATING ASKAREL TRANSFORMERS Obviously, in the manufacture of askarel transformers it is impractical and impossible to employ purification or refinements as required, for example, in the production of askarel power factor correction capacitors. In a transformer, heat from the dielectric losses of "slightly" contaminated askarel is negligible compared with heat generated by the transformer core. While power factor and resistivity of the transformer fluid are important, they are not as critical as is the case when Bimilar askarels are used in capacitors. However, this does not excuse the askarel transformer manufac turer from striving to meet the practical quality requirements as given in Chapter 8. In order to meet these requirements, it is necessary to earth refine the transformer askarel immediately prior to filling the unit. After the initial fill, the fluid should be withdrawn from the transformer, circulated through an earthen filter, then pumped back into the transformer and recirculated through the filter until both the fluid and transformer are clean and show the desired power factor and resistivity values, -83- NEV 007410 WATER PCB-SD0000030813 If such normal earth refinement fails to give the desired results, it will be necessary to study the quality of the materials of construction and look for all possible sources of contamination in the transformer and handling equipment. The characteristic high dielectric strength of transformer askarel is not a good criterion of purity because with the exception of being adversely affected by moisture, it is not impaired irre spective of the contamination of soluble products which give increased power factor. F. M. Clark of General Electric Company tabulated the following values of transformer askarel selected from hundreds of askarel samples taken from commercially operating transformers to show lack of reduction of dielectric strength with marked increase of power factor values. TABLE VII DIELECTRIC STRENGTH AND POWER FACTORS OF ASKAREL IN USED TRANSFORMERS Sample Power Factor, 60 cy. at 25C., per oent Dielectric Strength at 25C. KV No. 1 0.1 38 No. 2 0.5 35 NO. 3 5 45 No. 4 15 39 No. 5 30 43 However, the need for care and proper selection of transformer construction materials is emphasized in the following tabulation which shows the marked increase of power factor resulting from contamination of the askarel with synthetic rubber materials and varnished cloth, as compared with acceptable materials of construction given in Table VIII. -84- NEV 007411 WATER PCB-SD0000030814 TABLE VIII POWER FACTOR CONTAMINATION PRODUCED BY TRANSFORMER MATERIALS AGED IN ASKAREL AT 100C. FOR 96 HOURS Material None Black varniBhed cloth Askarel Power Factor, Percent 1.0 85.0 Dielectric Strength, KV 35 42 Copper Press Board Manila Paper Phenolic resin 1.5 40 2.0 37 1.5 39 1.6 41 Shellac 6.0 36 Iron 5.0 39 Synthetic rubber 70.0 39 Contaminants which cause a high power factor will of course also impair resistivity values, The following Table IX shows the degree to which acceptable and good commonly used materials of construction lower resistivity from the original high values possessed by the askarel. TABLE IX EFFECT OF COMMONLY USED INSULATION MATERIALS ON THE RESISTIVITY OF TRANSFORMER ASKAREL Sample gir-nmr-*---nr, Volume Resistivity x__ i> 108 Ohm. -cm. a,t q10A0OC^ . 1. Freshly made askarel before heat aging 2,000 2. Same as 1, after heat aging 1,900 3. After heat aging with the following materials added a - Phenolic resin tap changer material b - Paper c - Grade A press board (tan) 1,200 750 500 NEV 0Q7A12 WATER PCB-SD0000030815 a - Grade A press board (gray) e - Grade A press board, laminated strip f - Cotton wrapping g - Glyptal 1276 cement, cured 48 hours at 110C. 500 400 300 100 The procedure used to evaluate materials of construction is simple and should be employed by all makers of askarel trans formers. One Inch square samples of the surface of the construction materials are immersed in one liter of good quality transformer askarel and heated for 96 hours at 100C. The increase in power factor and reduction of resistivity of the fluid after such exposure are compared with the values of the original fluid heated similarly but in the absence of the construction materials. The following Table X gives such a comparison and illustrates the unacceptable properties of the varnished cambric and black binding tape. TABLE X PROPERTY FRESHLY MADE TRANSFORMER ASKAREL SAME FLUID EXPOSED TO FIBER BOARD VARNISHED CAMBR! OR BLACK BINDINC TAPE PP, 100C., 1 KC Resistivity,ft100C. Ohm-cm. x ICr 0.2% 2,500 0.45* 436 3% 18 Dielectric Strength at 25C. 45 KV 45 KV 45 KV When the askarel fluid contaminated with varnished cambric or the black binding tape was treated for one hour at 75C. with one percent by weight of attapulgua earth, the power factor and resistivlt values were restored to those of the original fluid. NEV 007413 WATER PCB-SD0000030816 While there seem to be no reports of askarel transformers falling in service as a result of contamination from the use of questionable materials of construction, as discussed above, their unwise use is readily detectable and leads to embarrassing question about impairment of the transformer's life. Such a case is illustrated by an askarel transformer giving a megger reading reading as low as 3, after two years service life. The transformer had not been subjected to arcing and the dielectric strength of the askarel remained above 35 KV at 25C., or well within the specification of new askarel. Maintenance of high dielectric strength in the presence of contamination appears to account for the transformer not falling. The following Table XI compares the properties of freshly made askarel with the similar values of the fluid taken from the transformer after two years use and also with the same contaminated fluid following refinement by earth treatment. TABLE XI COMPARISON OP PROPERTIES OP CONTAMINATED TRANSFORMER ASKAREL BEFORE AND AFTER EARTH REFINEMENT PROPERTY TYPICAL OF NEW ASKAREL SAMPLE FROM TRANSFORMER USED 2 YEARS SAME SAMPLE AFTER EARTH TREATMENT 1 HOUR WITH 1# OF EART1 PF. 100C. 60'cycles * PF., 100C. 1 Kc. 1 to 2# 0.2* 150#(dissipation factor) 15# 1# 0.1# Resist. 100C. Ohm-cm. x 10 500 to 1500 ,, 6 ,, 2600 Dielectric Strength 25C. 45 Moisture ppm. 25 Acidity mg. KOH/g. 0.01 Color APHA 70 40 80 0 1000 -87- 45' 20 0.005 275 NEV 007414 WATER PCB-SD0000030817 In the above case it was determined that a varnished insula ting material used in the transformer was the source of contamination Since this continuously dissolved in the askarel, obviously, removal of the fluid, followed by earth refinement and refilling the trans former accomplished nothing. The situation pertained at the time of the initial fill persisted until the deleterious component was removed. Newly built or rebuilt transformers using acceptable materials of construction often contain undeterminable traces of impurities and "dirt" which effect power factor and resistivity, but can be removed by repeated flushing with clean askarel. The following Table XII compares the properties of the askarel sampled after the initial fill with similar values after earth refinement and "soaking'' or flushing the transformer, twice with good askarel. After the "dirt" or contamination was removed from the transformer the askarel fluid remained in good condition in the unit as shown in Table XII. TABLE XII PROPERTY SAMPLE AS RECEIVED AFTER TREATMENT Resistivity @ 100C. 30 x 10 2600 x 10 Dielectric constant @ 100C. 3.9 3.9 Power Factor @ 100C., 1000 Cycles 2* 0.27* Moisture 60 ppm. 25 ppm. Moisture solubility in askarel at 25C. is about 110 parts per million and the specification for new askarel allows a maximum of 30 parts per million of water. Essentially, moisture-free askarel was found by Clark to have a dielectric strength of 70 KV. With increased amounts of dissolved -88- NEV 007^15 WATER PCB-SD0000030818 water the dielectric strength gradually decreased and appeared to level off at a value of about 38 KV when the water content reached 80 parts per million. Water exceeding the solubility limit in askarel has a marked adverse affect on the power factor and resistivity of the dielectric fluid, which may, however, maintain its high breakdown strength even though water accumulates as a separate phase on the surface. Undissolved moisture can be removed readily from transformer askarel by warming the fluid to 70C. and blowing with dry nitrogen or by treatment with dry, conditioned earth and filtering through a press fitted with dry filter papers or through an earthen cartridge type filter. As indicated previously, moisture must be kept out of askarel transformers by using adequate gaskets, as described in Chapter 3, and preferably sealing the device with dry nitrogen over the askarel. Mineral oil is soluble in these fire-resistant transformer askarels and is regarded to be a contaminant. Petroleum hydro carbons cannot be removed from askarels and the permissable amount may not exceed 2 percent by volume lest the fire-resistant values of the askarel is impaired beyond acceptable limits. Possible contaminants in transformer manufacture include welding and solder fluxes, oils and greases, bituminous materials, pipe thread lubricants, and contamination from bushing and pot head compounds. Paint or varnish coatings must not touch the interior of the transformer shell. Adhesives or coatings applied to gaskets must not touch the interior of the transformer. nev 007416 WATER PCB-SD0000030819 All natural or synthetic rubber plastics or polymeric materials, resins, varnishes and lacquers and adhesives must be regarded as contaminants unless included In the very few acceptable classes and proved suitable by actual testing. . It is disappointing to find an askarel transformer manufacturer exercising precautions against contamination, and employing earth refinement, and yet inadvertently using a neoprene or other objectionable hose line to transfer the fluid economically!! If flexible hose needs be used, it should be a flexible stainless ' steel type or a "rubber" hose lined with Teflon. When using any of the following suggested suitable materials of construction, it is prudent to employ appropriate control evalua tion tests to be certain that the given material within a class regarded as acceptable will meet the requirements from a physical and electrical standpoint. TABLE XIII ACCEPTABLE MATERIAL FOR CONSTRUCTION OF ASKAREL TRANSFORMERS Structural Materials and Fillings Metals - Commonly used metals including steel, copper, aluminum, tin and brass are suitable if clean. Wood - Suitable if dry and free of natural gums and resins. Paper - Suitable ' Press Board - Suitable Cotton - Suitable Asbestos - Suitable Glass - Suitable Ceramics - Suitable Phenol-formaldehyde resins - Suitable if adequately cured. -90- NEV 007417 WATER PCB-SD0000030820 Melamine-formaldehyde resins - Suitable if adequately cured. Cellulose acetate - Suitable Cellulose trl-acetate - Suitable Cork - Suitable Gasketing Materials and Adhesives Metals - (As above) Teflon - Suitable Silastic (silicone) - Suitable if adequately cured. Polyurethane - Suitable if adequately cured. Cork (fine grain and bonded with phenolic resin) - Suitable, but susceptible to penetration by askarel. Nitrile rubber - Sometimes used for gaskets - but susceptible to attack by askarel. Cork Nitrile rubber - Often used Dewaxed Orange Shellac - Suitable ' Epoxy - Suitable if adequately, cured. Isocyanate - Suitable if adequately cured. Tapes and Wire Insulation Cotton - Suitable Paper - Suitable Asbestos - Suitable . Glass - Suitable Rayon - Suitable Cellulose acetate - Suitable Teflon - Suitable Silicone - Suitable -91- Ngv 007^18 WATER PCB-SD0000030821 Surface Coating for Transformer Exterior Baked Phenol-Formaldehyde - Suitable Baked Melamine-Formaldehyde - Suitable Baked Epoxies - Suitable Polyurethane Coatings - Suitable Surface Coating for Interior of Transformer Shell to Prevent Rusting In Storage 25 parts Aroclor 5460 dissolved in 75 parts lacquer thinner. ' The need for clean shop practice and avoidance of contaminating influences when building askarel transformers is emphasized by the ' following information submitted by a highly qualified manufacturer to indicate the condition of askarel sampled from normally opera ting apparatus after a number of years service. Fluid sampled from the top and bottom of at least 25 askarel transformers operatinj satisfactorily in different part of the country was analyzed, comprehensively. The following general conclusions were drawn: 1. The residual condition of the askarel samples for the most part was satisfactory, but in a few instances excessive dirt or sediment was noted. 2. Moisture content ranged from 19 to 6l parts per million with most samples between 25 and 35 ppm. This reflects a very good degree of dryness. .,3. Acidity values were all below 0.01 mg. NaOH/g which corresponds with the level of freshly made askarel. -92- NEV 007419 4 WATER PCB-SD0000030822 4. In most cases the free chlorides did not exceed 0.1 ppm., the specification limit of new askarel. The highest reading was 0.15 ppm. 5. Dielectric strength values ranged from a maximum of 46 KV to a minimum of 28 KV which values are considred satisfactory. 6. Volume resistivity at 100C. ranged from 20 to 75 x 10 Ohm-cm. which is considered to be satisfactory and may be compared with the specification for new askarel at 100 x 10 Ohm-cm., minimum. 7. Power factor values at 100eC. and 60 cycles ranged from 19 to 75 percent with most samples below 60 percent. Prom the above data considered typical and satisfactory relative to all of these askarel transformers operating in a normal manner, it is seen that under satisfactory service life the resistivity of the askarel will decrease and the power factor will increase, as indicated, from similar values of fresh askarel. These observations emphasize the need for askarel transformer makers to: 1, Earth refine the askarel immediately prior to use in order to arrive at the highest practical electrical values from the fluid. 2. Avoid construction materials which are a source of contamlnat: 3. In using acceptable and satisfactorily tested construction materials - to flush the transformer to remove traces of contaminating influences and "dirt". 93" NEV 007420 WATER PCB-SD0000030823 CHAPTER 11 REWORKING CONTAMINATED TRANSFORMER ASKAREL Normal Conditions Askarel contaminated during manufacture of the transformer or after years of normal service life should respond very readily to refinement by treatment with a few tenths of a percent of dry Fullers earth, or Attapulgus clay. This was discussed In detail In previous chapters. About askarel transformers, after years of normal service life and having continued satisfactory performance, question (difficult to answer) arises as to how high may be the power factor. Also, how low may be the volume resistivity. The case histories given in the preceding chapter seem helpful in arriving at an answer. DOble Engineering suggests to their clients that, "When used askarel is found to have a power factor of 2.0 percent or more, the cause of high power factor should be determined." (This refers to power factor measured at 20C. and 60 cycles.) Doble qualifies this suggestion stating, "If the high power factor is caused by water or other conducting matter, free chlorides or high neutralization number, the askarel is probably an operating hazard." Also, "If the high power factor is not due to these causes, it is probably not an operating hazard except that when the power factor is quite high, it may result in excessive heating of the device in which it is used." -94- NEV 007421 WATER PCB-SD0000030824 Since heat resulting from power factor increase of the askarel in most any commercial transformer is negligible compared with heat generated by the core of the transformer, this consideration does not appear important. If the suggestion were limited to a 2 percent power factor, it would appear low and probably subject to considerable objection. However, when stated as 2 percent or more, the intention and purpose of this suggestion justifies earnest consideration, although in absence of more knowledge, it appears that conclusive answer to this question is not at hand. However, it should be apparent that when the power factor of the askarel is 2, 5, or 7 percent or higher at 20C. and 60 cycles, and volume resistivity at 100C. is 20 x 10 Ohm-cm. or lower, contamination is present. As it is likely that such a condition can be rectified by simple earth treatment and filtra tion, there should be little question about desirability of doing this purification work to assure the best possible perform ance of the transformer. Arced Conditions It is fortunate that there seem to be very few cases of significantly arced transformer askarel, as it is difficult to estimate the possible success of reclaiming the fluid. Particularly, it is not easy to lower the free and also the after corrosion chloride levels within the extremely low specification limits for new askarel. -95- oo2Z WATER PCB-SD0000030825 Treatment with dry earth as usually used to refine contamina ted askarel, probably will not rectify arced askarel. Special refinement, including hydrolysis of the spent scavenger material, water extraction of excess chlorides, treatment with wet earth, special drying and finally treatment with dry earth Is required. The following example is considered typical: During routine testing of a transformer filled with askarel, a short occurred in the winding, and the arc resulted in formation of easily seen carbon particles in the fluid. The following shows the ineffectiveness of dry earth treatment and the need for wet or water treatment to reclaim a sample of this material in the laboratory. Passing the damaged fluid through filter paper failed to remove the carbon. The carbon was removed by filtering through paper fitted with a one-half inch pad of Attapulgus earth. At this stage, analysis indicated the following pertinent properties as compared with the specification limits: PROPERTIES OF TRANSFORMER ASKARELS Specification Sample Inorganic chlorides Acidity, mg. KOH/g. Moisture 0.01 ppm. max. 0.010 max. 30 ppm. max. 0.25 ppm. 0.004 75 ppm. Then 0.2 percent by weight of Attapulgus earth was added and the mixture held at 90C. and agitated for two hours and filtered. This reduced the water to 15 ppm., but the chlorides remained at 0.25 ppm. Another portion of the original sample was treated' with 0.5 percent of earth, held at 50C. and agitated for two hours and filtered. This lower temperature treatment reduced the water to only 60 ppm. and the chlorides remained at 0.25 ppm. -96- NEV 007423 WATER PCB-SD0000030826 At this stage, the electrical properties were determined and found to be well within specification limits. Property Specification Sample Resistivity @ 100C. x 10 Ohm-cm. 100 576 Power Factor @ 100C. and 1,000 Cycles ------- 0.18# Dielectric Constant @ 100C. 3-8 - 4.3 4.2 The above reclaiming tests were repeated using "wet" earth which contained 15 percent moisture. Again, the chlorides remained at the original level of 0.25 ppm., well out of specification. Then a sample of the askarel was extracted with water, using 20 percent based on the weight of the dielectric fluid. This reduced the chlorides to 0.15 ppm., and a second aqueous extrac tion uBing 10 percent of water was required to reduce the chlorides to no detectable amount. The excess moisture was then removed by blowing with dry air and finally filtering through dry earth and filter paper. Although transformer askarel is several times as expensive as mineral oil, the material is not a'high cost item. Therefore, the economies of undertaking work as described above must be weighed against the cost of new askarel. In any event a fair estimate of the reclaiming cost plus . packaging, shipment to location for the work, the cost of several analyses involved, then repackaging in new containers and cost of return freight will indicate at least 50 percent of the cost of new askarel. Accordingly, usually the most practical expedient is to purchase new askarel to replace the arced material:. -97- NEV 007424 WATER PCB-SD0000030827 CHAPTER 12 DERMATOLOGY AND TOXICOLOGY Skin Exposure Aroclors, or askarels, accidentally spilled on the skin do not cause an acute toxicity hazard, nor will they cause serious Irritation. The materials should be washed from the skin with soap and water. Prolonged skin contact should be avoided. If work clothes become impregnated with these fluids, they should be removed and washed. When sampling tank cars, canvas gloves and safety glasses, or goggles, should be worn. No special clothing is required, but the workers * garments should be laundered at least weekly and changed, if Aroclors or askarels are spilled on the clothes. If accidental burns occur from contact with hot askarels, the burn should be treated the same as any ordinary burn. Aroclor, or askarel, adhering to the burned area need not be removed Immediately unless treatment of the burn demands it in which case, soap and water, or repeated washings with a vegetable oil should be used. Accidental contact with the eyes results In painful irritation, but not permanent damage to the tissues or the sight. In event of such contact, the eyes should be flushed with a large amount of water for at least 15 minutes. The patient should then be referred to a physician who will treat with an ointment to soothe the eye. NEV 007425 WATER PCB-SD0000030828 Exposure to Vapors Vapors from hot Aroclor, or askarel, have a degree of toxicity and should not be inhaled over a prolonged period of time. Experimental work on animals indicates that the maximum safe concentrations of vapors in work rooms is in the range of 0.5 to 1.0 mg. per cubic meter of air. Harmful amounts of the materials are readily detectable by odor and irritation to the eyes. Usually, people can detect concen trations of askarels in the amount of 1.0 mg. per cubic meter of air, which is the level regarded as the safe work room limit for an 8 hour day exposure. Capacitor impregnations may be done at temperatures as high as 266P. (130C.). Following impregnation and draining the chamber, exhaust ventilation should be applied to the chamber to prevent askarel vapors entering the work room. Also, when opening a heated capacitor impregnating chamber, the workmen should wear a respirator during this short Interval of exposure. If transformer askarels are used at temperatures above 125 to 150F. to fill an open transformer, exhaust ventilation should be provided in the immediate area. The many years of satisfactory and safe use of Aroclors, or askarels, by the electrical industry for impregnating capacitors and filling transformers has demonstrated the industry's ability to handle these fluids without hazard to the workmen. It is both simple and in line with "good housekeeping" and personal cleanliness to exercise the suggested precautions in all cases -99- NEy 007426 WATER PCB-SD0000030829 Vapors from a Severely Arced Askarel Transformer Experimental data indicate that when askarel is decomposed by an electric arc, insignificant amounts of chlorine and phosgene gas are liberated. The gas is almost entirely hydrogen chloride, which is readily - detectable by its odor and its irritating characteristics in even small amounts. Thereby, adequate warning of its presence is provided and significant amounts of fumes would be likely to cause a hazard only in a closed area. Individuals would not voluntarily expose themselves to serious toxic levels of the hydrogen chloride gas fumes. -100- NV 007427 WATER_PCB-SD0000030830 W6V 0 0 7 4 2 b iI i I I IfI I i WATER PCB-SD0000030831 NEV 007429 WATER PCB-SD0000030832 WATER_PCB-SD0000030833 NEV 0 0 7 *3 1 WATER_PCB-SD0000030834 WATER PCB-SD0000030835 ; /sc#<?/s f*voc/ ff#P02-f t <i NEV 007433 WATER PCB-SD0000030836 NEV 0 0 7 4 3 4 N n 0 a\ 4acn, 1 v I Sf n\ *'b j$* h'ii I *>,<s 5 I'M j5 i S3 WATER PCB-SD0000030837 aintenance Guide 2 DEPOSITION 1 EXHIBIT | ^3 JL_5-/'JV NEV 007544 WATER_PCB-SD0000030838 ASKAREL Inspection and Maintenance Guide NEV 007545 WATER PCB-SD0000030839 TABLE OF CONTENTS SECTION A TRANSFORMER ASKAREL Page I. Introduction........................................................................................................ I II. History of Trade Name Types........................................................................... I Tabic I -- The Composition of Transformer Askarels III. Table II -- Official Transformer Askarel Shipping Specifications................... 2-3 A. General Electric Company's Transformer Pyranol A13B3B B. Westinghouse Transformer Inerteen PPO (7336-9) IV. Interchangeability and Stability......................................................................... 4 V. Directions For Handling and PersonalPrecautions............................................ 4 VI. Expected Service Life.......................................................................................... 5 VII. Dielectric Strength -- Moisture Relationship.................................................. A. Table HI -- Dielectric Strength vs. Amount of Dissolved Water in Askarel and Mineral oil B. Table IV -- Approximate Solubility of Water in Askarel and Mineral Oil. 5 VIII. Table V -- Typical Values Found in Askarel Fluid Under Various Con ditions of Use..................................................................................................... 6 IX. Check Points For Maintaining Askarel Insulation......................................... A. General Considerations B. Modern Sealing Procedures C. The Older Sealing Arrangements 9 X. Periodic Fluid Inspection.................................................................................. 11 A. Visual Inspection B. Dielectric Strength XI. Inspection Check List............................................................................... 12 XU. Contamination in Transformers...................................................................... A. Table VI -- Effect of Common Insulation Materials on Power Factor and Dielectric Strength B. Table VII -- Effect of Common Insulation Materials on VolumeResistivity 12 XIII. Refining Askarel For Re-Use........................................................................... A. Filtering Through Dry Blotter Paper To Remove Moisture and Extraneous Particles. Table VIII -- Guide to Rate of Dissolved Water Removal By Filtration. B. Earth Treatment for Maximum Improvement of Power Factor and Volume-Resistivity 1. Procedure 2. Effect of Earth on Removal of Scavengers 3. Table IX -- Approximate Relationship Between Power Factor, Volume-Resistivity and Dielectric Strength of Transformer Askarel 14 XIV. Cleaning Arced Transformers.......................................................................... 15 ' XV. Sampling ASKAREL......................................................................................... 17 NEV 007546 WATER PCB-SD0000030840 SECTION B ASKAREL FILLED SWITCHES AND TERMINAL CHAMBERS Page I. Introduction........................................................................................................ 18 II. Sources of Contamination.................................................................................. 18 III. Scaling Switches and Terminal Chambers........................................................ 19 IV. Askarcl-filled Swiiches' Maintenance................................................................ 19 SECTION C Monsanto Analytical Services on Transformer Askarel.................................. 21 Appendix A. Askarel Stability and Composition of Arc Formed Gas................................ 23 B. Solubility of Gas in Transformer Askarel......................................................... 23 C. Approximate Vapor Pressure vs. Temperature ForTransformer Askarel____ 24 D. Effect of Temperature on Dielectric Strength of Askarel................................ 24 E. Viscosity of Askarel and Mineral Oil............................................................... 24 F. Density of Transformer Askarels...................................................................... 25 G. Thermal Conductivity........................................................................................ 25 H. Heat Capacity..................................................................................................... 25 I. Coefficient of Expansion.................................................................................... 25 J. Fire-Resistance.................................................................................................... 25 K. Seals, Properties and Procurement.................................................................... 26 NEV 007347 WATER PCB-SD0000030841 SECTION A TRANSFORMER ASKAREL I. INTRODUCTION: This manual describes the operating characteristics of transformer askarel liquid insulation and how it differs from mineral oil. The information given is based on facts gathered by Monsanto over 30 years as producer of askarel, plus knowledge gained from the experience of transformer manufacturers and users. This guide is provided to outline the very simple mainte nance required for askarel fluid in "modern" transformers and to offer suggestions for the sealing and maintaining of askarel in old units. By following this guide, users will obtain maximum service from askarel insulation with a reasonable minimum of maintenance. If questions arise relating to the designing and building of transformers -- these should be referred to regular transformer suppliers. Monsanto gratefully acknowledges the assistance, guidance, and the contributions of certain data by the following: Frank M. Clark. Edward L. Raab James G. Ford ., George Shombert, Jr, General Electric General Electric Westinghouse Electric ........... Allis Chalmers II. HISTORY OF TRADE NAME TYPES "Askarel" is the generic name for non-combustible (fire-resistant) liquid insulation. In this respect, the insulation is completely different from ordinary transformer mineral oils. Transformer askarel is marketed by Monsanto. Whatever the trade marked brand, the askarel contains Monsanto's Aroclor (chlorobipheny!)... one of the best liquid insulations developed by science. This inert compound is chemically stable, fire-resistant, heat stable, non-corrosive, and has high dielectric strength under the operating conditions encountered in transformers. NEV 00754b WATER PCB-SD0000030842 Askarcl liquid insulation is made by thinning Aroclor 1260 with trichlorobenzene or tri-, tetrachlorobenzene mix. The first transformer askarel was made in 1932, in accordance with General Electric Company's patents, and was trademarked Pyranol 1488. Westinghouse, loo, offered this askarel insulation in 1936 under their trademark Inerteen. In the mid-1940's, as shown in the following table, tin tetraphenyl was added to General Electric's Pyranol to scavenge hydrogen chloride. Shortly thereafter, Westinghouse added phenoxy propene oxide to Inerteen for the same purpose. In 1963, General Electric replaced tin tetraphenyl with a diepoxide scavenger. This new formula, which replaces previous Pyranols, is called Transformer Pyranol A13B3B. Thus, today the two commercial types offormulations are General Electric's Transformer Pyranol AI3B3B type and Westinghouse Inerteen PPO (7336-9) type. The composition changes made in transformer askarel formulations arc shown in Table 1. Table I THE COMPOSITION OF TRANSFORMER ASKARELS 1488 Year Introduced....................... 1932 Ingredients! Aroclor 1260 ............................. Trichlorobenzene...................... Tetrachlorobenzene.............. Tin tetraphenyl.................... Phenoxy propene oxide........ Diepoxide.............................. 60 40 Pyranol 1467 1470 1944 1952 60 40 0.125 45 40 15 0.125 A13B3B Inerteen 1963 1936 45 60 40 40 15 0.125 Inerteen PPO (7336-9) 1945 60 40 0.20 OTHER BRAND NAMES Various electrical equipment manufacturers use other trade-marked names for askarel liquid insulation, such as Chlorextol (Allis-Chalmers); Noflamol (Wagner Electric); Saf-T-Kuhl (Kuhlman Electric). These askarel insulating liquids are one or the other of the two standard formulations. Still other manufacturers, who designate their insulation only by its generic name, askarel, assign it a number or code. By this number, Monsanto knows whether to furnish Pyranol A13B3B or Inerteen PPO (7336-9) type formulation to the user. III. OFFICIAL TRANSFORMER ASKAREL SHIPPING SPECIFICATIONS The official shipping specifications for the two modern transformer askarel formulations are shown in Table II. NEV 007549 WATER PCB-SD0000030843 OFFICIAL TRANSFORMER ASKAREL SHIPPING SPECIFICATIONS General Electric Co. 9 3 NEW 007550 WATER PCB-SD0000030844 IV. INTERCHANGEABILITY AND STABILITY A. Interchangeability: The two general types of askarel insulation shown in Table II can be either mixed or interchanged and there will be no difference in the operation of the transformer. However, askarel insulation must never be mixed with mineral oil. Over 2% mineral oil in askarel begins to lower its fire resistance. Further, materials of construction in the transformer that are compatible with askarel may not be compatible with oil and vice-versa. For example: a significant amount of askarel in a transformer built for mineral oil will attack gaskets, adhesives, core bindings, impregnating varnishes, etc. B. Stability: Askarel liquid insulation is highly pure, fire-proof liquid made under close chemical control. It does not vary in composition like the commercial range of mineral oils. Askarel does not deteriorate when exposed to air, heat, hot metal; it does not break down over long use to form conducting or corrosive chemicals; it does not oxidize or sludge. Askarel will remain perfectly stable year after year unless broken down by exposure to severe arcing. The only real "enemy" of askarel is contamination by water. Keeping askarel water-free will insure long-time service. Askarel is heavier than water. If water gets into askarel insulation, only a tiny amount (125 ppm) dissolves -- the rest floats on top. V. DIRECTIONS FOR HANDLING A. Keep Dry: In handling, storing, sampling, inspecting askarel -- and in operating askarel transformers -- take every precaution to guard the askarel insulation from exposure to high humidity and moisture contamination. Keep 5, 30, or 55 gallon drums of askarel dry; lay stored drums on their sides with the bung at the highest point from floor to keep water off the drum head (which can be sucked into the askarel by the drum "breathing"). This precaution is not necessary when drums are stored indoors, which is the preferred way of storing. B. Use Ordinary Personal Precautions: Transformer askarel has been made, handled, and used for over 30 years without causing toxic or other ill effects. It can be handled with only minor precautions. If accidentally spilled on hands, no serious skin irritation will occur. However, liquid askarel has a solvent action (similar to paint thinner) on the fats and oils of the skin and prolonged contact may lead to drying and chapping of the skin. *' NEV 007551 WATER PCB-SD0000030845 In case of contact, wash off the skin with soap and water; remove and dry clean saturated clothing. Clean up spills with rags, sawdust or absorbent clay. Eye contact may result in painful irritation but no permanent damage to tissues. If askarel gets in the eyes, flush with large amounts of water. As with all eye first-aid, refer to a physician. To relieve irritation, physicians have used a 1% Pontocaine as well as opthalmic cortisone acetate solution, or castor oil. Infrequent exposure to askarel vapors will not cause ill effects. However, prolonged exposure to high vapor concentrations should be avoided. If hot askarel must be handled in a closed or confined area, provide the area with ordinary exhaust ventilation -- or -- wear an organic cartridge respirator approved by the U. S. Bureau of Mines. VI. EXPECTED SERVICE LIFE Properly designed and installed askarel transformers will give trouble-free service for a minimum of 30 years. Since their introduction in 1932, the manufacturers report finding the over-all failure rate to be less than 0.5% for all units under test and service conditions. The Edison Electric Institute's report (1956-1958) on their member utilities publishes the failure rate for askarel transformers as 0.13 per hundred banks per year. Even the rare reports of failure are invariably found to be due to improper sealing that allows moisture to enter. VII. DIELECTRIC STRENGTH -- MOISTURE RELATIONSHIP The dielectric strength of askarel is highly sensitive to excess moisture; not sensitive to ordinary dissolved contaminants. While the dielectric strength can also be lowered by severe arcing, askarel turns noticeably black or has particles of sooty carbon floating in it if arcing has occurred. Then the transformer should be repaired and the askarel replaced. New askarel has a minimum dielectric strength of 35 K.V at 25; a maximum mois ture content of 30 ppm. If the dielectric strength is checked periodically and decreases significantly -- this indicates moisture pick-up, arcing, or both. When the dielectric strength has dropped to 26 KV or less, an analysis for water is necessary. If water is found in excess of 100 ppm at 25 C., its source should be located and corrections made. When the moisture content approaches 125 ppm (saturation level), the dielectric strength of askarel drops below the value required for efficient insulating. The moisture content should not be allowed to rise over 70 ppm; it should be held as near as possible to 30 ppm. Maintaining a low moisture level will assure high dielectric strength and top operating efficiency. Table III shows the relationship of dielectric strength vs. moisture and Table IV indicates the approximate water solubility limits in askarel and mineral oil. . . i new 007552 WATER PCB-SD0000030846 Table III RELATION OF "BREAKDOWN STRENGTH" TO AMOUNT OF DISSOLVED WATER IN ASKAREL AND MINERAL OIL Breakdown Voltage (ASTM) Water Content (PPM) Askarel Mineral Oil 0 70 KV 50 KV 20 55 39 40 47 30 60 40 26 80 38 22 110 10 5 Table IV APPROXIMATE SOLUBILITY OF WATER IN TRANSFORMER ASKAREL AND MINERAL OIL Temperature Amount of Water (PPM) Dissolved C. F. Askarel Mineral Oil --30 --20 --10 0 10 20 30 40 --22 _4 14 32 50 68 86 104 8 16 28 41 65 94 128 170 8 10 13 20 33 58 85 130 TURBIDITY . .. may be the visual sign of undissolved water, or may indicate contamination from core materials, dirt, or deteriorating construction materials. Cloudiness may also result from cold precipitation of tin telraphenyl "scavenger" that was used in the earlier Pyranols. This scavenger begins to come out of solution around I5F. above zero. To redissolve it requires heating to 150 - 200F. and agitation. High dielectric strength will quickly indicate that any turbidity present is not moisture; that the insulating efficiency of the askarel is still excellent. However, if the dielectric strength is below 26 KV, moisture should be determined, using the Karl Fischer method (ASTM D1533-60). The dielectric strength test for askarel serves primarily as an indicator for moisture. It is by far the most important maintenance test for transformer askarel. VIII. TYPICAL VALUES FOUND IN ASKAREL FLUID UNDER VARIOUS USE CONDITIONS Table V gives the entire spectrum of properties that are typical for freshly-made transformer askarel as it goes through the various normal and abnormal conditions of use. The data in Table V are in terms of only the askarelfluid and do not refer to insulation resistance or power factor measurements on the over-all transformer insulation. Several utilities studying the power factor values of the over-all transformer insulation system indicate that the unit power factor of a new askarel transformer should range from 1% to not over 5%. This would generally correspond with the askarel fluid properties as given under heading "B". 9 * NEV 007553 WATER PCB-SD0000030847 T able V '4 properly built transformer is defined as one in which the materials o f construction are chemically and electrically compatible with askarel. oa P O *0 g | 3 e .g tisll mn 8I U *n> ji5j <<s1c> g<3 oj .6 g I - J I K o -g !?1ik ill If! 8 & e.*2 w U8 a |JS Co 'Pb U 8, S|I u s As S 2 3-g Z!US > * tn !i'i'l*C0?1 1E0 f*88 I. S. >.S 'I " SJ s Co 8e Eaa 5 oa 1,* s!5 S? !j.sa a! II o ^e 1 S| ! u *1 >u >u 2 K gs* 5 ff & K . o Sa ci*OT ~1 i 5?vtsl 9 2 a 3 1 B a &fS 3 (N 2 Jl^ " ii t'&s a*? ^2 tv IN) O ss Uu J|a 7 NEV 007554 WATER PCB-SD0000030848 Starting ideally with situation "B", it is normal to expect the power factor of the fluid in a satisfactorily operating ask arc! transformer to increase as shown under heading "C". The "over-all" power factor of the transformer in normal service is expected to rise, but preferably not much beyond 5%. In (his normal situation, the moisture level of the askarel fluid and its dielectric strength will be satisfactory, as shown in heading "C". Occasionally the power factor of a non-arced, satisfactorily-operating askarel transformer is found to be relatively high, i.e., 15%. In this case, the power Jactor of the askarel fluid wilt also he high, perhaps as high as 50% at 20C. and 60 cycles. It is not good practice merely to note that high power factor of the askarel fluid is to be expected. The important step is to check dielectric strength and note whether there has been a downward trend. A downward trend in dielectric strength very likely indicates moisture entrance and should be confirmed by a Karl Fischer test for water. The importance of any abnormalities in dielectric strength and moisture content of the askarel fluid cannot be overemphasized! Where abnormal values for the dielec tric strength or moisture content occur, the power factor of the transformer can be expected to be abnormally high; the expected high power factor of the askarel fluid will induce this. The indication that a high power factor on the transformer and on the fluid is due to contamination can be verified by earth refining the askarel fluid and noting whether after refining the test results correspond with heading Assuming no mechanicul defect or arcing, if the power factor of a new askarel transformer is relatively high, the power factor of the fluid will also be high, giving the situation under heading This reflects contamination that should have been removed by the manufacturer of the transformer. In absence of mechanical defect, where there are no abnormal losses in dielectric strength, and no moisture pick-up in non-arced askarel -- the use history shows that a relatively high power factor for the askarel fluid (as compared with mineral oil) is to be expected. Normally, high power factor is due to contamination and not deterioration of the askarel operation. As shown by F. M. Clark in his book, "Insulating Materials For Design and Engineering Practice," John Wiley & Sons, N. Y., 1962 -- activated alumina can be used in the circulating system to bring the power factor down and keep it as low as possible. 9 . NEV 007555 WATER PCB-SD0000030849 IX. CHECK POINTS FOR MAINTAINING ASKAREL INSULATION A. General Considerations; Modern askarel transformers with welded construction or silicone gaskets for hand hole-cover, switch and terminal compartment covers, with properly constructed bushings require little or no maintenance. With properly con structed transformers, annual or semi-annual visual inspection and dielectric strength test of the askarel fluid should suffice for routine maintenance checking over many years of service. However, many askarel units were installed in the early 1930's -- before the development of some of the better modern gasketing materials and before improved designs were developed for sealing out moisture. Such early units should be, and can be, modernized. Leaky or deteriorated gaskets should be replaced. If the askarel has become contaminated, it should be reconditioned. At the, same time, a general clean-up of the unit and possible refinishing may be desirable. If it is not convenient to take an old transformer out of service for general repairs, leaky gaskets can be sealed temporarily by painting over the leaky area with epoxy cement. A survey of users indicates a good number of early-built askarel transformers (over 20 years old) are kept in continuous service in critical installations by the following steps (instead of modernization). The operating units are equipped with compound pressure gauges for reading pressure above and below atmospheric. Positive pressure is maintained on the shell by introducing nitrogen at 2 to 3 pounds above atomspheric. Regular workmen in the area daily record the temperature and pressure. If a sudend pressure drop is noted more nitrogen is introduced and the gaskets are checked for leaks with soap solution. Leaks are sealed by applying epoxy cement. B. Modern Sealing Procedures; Transformer purchasers should specify the following modern techniques for sealing; 1. Welding Construction: Covers, radiator connections, switch and terminal housings, instrument connections, etc. should be welded. 2. Bushing Connections: The most satisfactory bushings are the type with rolled-on flanges and two ring seals rolled into a depression in the porcelain -- scaled with silicone rubber rings held under compression. Metal-to-glass or metal-to-porcelain sealed bushings are also satisfactory. If for any reason the above type bushings cannot be used then use a por celain or glass bushing with a silicone or Viton gasket retained in a groove. The gasket can be either rectangular or circular cross section, usually (4 inch thick. 3. Small Size Connections: When not possible to weld, small size connection seals should be made with Flexitallic stainless steel rings. The surfaces must be machined and parallel. The filler between the steel laminations of the Flexitallic ring should be either silicone or Viton. ' # 9 NEW 007556 WATER PCB-SD0000030850 4. Gaskets For Hand-Hole Covers: Modern design specifies silicone gaskets. Such gaskets must be retained in a groove. The groove preferably is machined into the flange or cover. However, it can also be formed by welding concentric steel strips to the flange or the cover. Generally the gaskets should be s/l9 to V4 inch thick for covers, depending on the depth of the groove. A rectangular section is usually used. The silicone material should be Dow-Corning No. 50 Silastic or equivalent. This is a low compression set material. For best sealing 20 to 25% compres sion is recommended, with ample clearance in the groove to allow for th'.s compression. No cement is required. With reasonable care the gasket is removable without damage and is reusable. Silastic 50 is slightly swelled by askarel which contributes to the tightness of the seal. It is not deteriorated by askarel fluid or vapors. It resists weather ing and it is thermally stable and flexible at all operating temperatures. It is an excellent moisture barrier. Notes: a. Dow-Corning, Midland, Michigan will supply a list of Silastic 50 gasket fabricators to all transformer manufacturers or users. They will also furnish technical data. b. Any user of Pyranol transformers, made by General Electric Company at Rome, Ga., will receive prompt and generous help for converting to the modern silicone or Viton gaskets by contacting the General Electric Company's Service Engineering Department at Rome, Ga. See Appendix K: Seals, Properties and Procurements. C. The Older Sealing Arrangements: The older type gaskets consist of either cork or cork-nitrile rubber combinations or straight nitrile rubber. 1. Cork-Nitrile Combinations: Covers for the main tank, hand-holes, switch and terminal chambers, relief diaphrams etc. are held in place by studs welded to the flange or by bolts. The gaskets are cut with openings and placed over the bolts. Often Shellac (Westinghouse Style No. 1150419, or General Electric Company's Glyptal 1276) is used to cement the cork to the flanges. The following is recommended for scaling with (he cork -- nitrile rubber combination: Use Armstrong NC-757 cork-nitrile material or equivalent. The gasket can be cut from a single sheet or by scarfing strips of the material. A convenient method for joining strips is to make a Keystone Type joint. For this. Westinghouse, Sharon, Pa., offers their gasket cutter Style No. 328 B6I4 G0I, (about SI5). The joints should be cemented and the gasket also cemented to the flange, using one of the above cements. Excess cement should not be allowed to reach the interior of the transformer. ,.* * NEV 007557 WATER PCB-SD0000030851 After installation and bolting, the outside edge of the gasket should be coated thoroughly with epoxy cement to increase weather resistance. This epoxy cement is a paste to which a curing catalyst is added immediately before use. Typical are: a. Epoxy Patch Kit f/l-C Hysol Corporation, Olean, N. Y. b. Scotchcast Resin ff4 Minnesota Mining and Manufacturing Co. St. Paul, Minnesota c. Adhesive A-J and Activator Type B Armstrong Products Company Argonne Rd., Warsaw, Ind. d. Adhesive 9860-1, Synthetics Organic Company, Cleveland, Ohio, used with activator diethylene triamine (Carbide and Carbon Chem. Co.) 2. Straight Nitrile Rubber: When straight nitrile rubber was originally used, invariably the gasket was recessed in a groove. This was to prevent gasket flow and to protect the material against excessive compression. Although this type seal was not cemented, the nitrile rubber gasket is not reuseable. Since grooves or stops have already been provided for the nitrile rubber seal, Silastic 50 can be easily substituted and is recommended. This conforms with modern practice. X. PERIODIC FLUID INSPECTION AND WHAT CHECKPOINTS MEAN On a regular schedule -- at six, nine, or twelve month intervals -- make a simple visual inspection of your askarel insulation and run a dielectric strength check. A. Visual Inspection: Askarel is a clear, faint-yellow liquid. After long-term use this color may gradually intensify to light brown. The fluid should remain clear and free from turbidity or cloudiness. Any color change -- such as to a green, red or blue cast -- indicates extraction of impurities from the solid insulation. If a distinct foreign color pick-up is noted, check the complete range of electrical characteristics and notify the transformer maker. The electrical characteristics may be found to be unim paired. Color change alone (except for black) is not a danger signal since the contamination is not likely to impair the dielectric strength. B. Dielectric Strength: s If the dielectric strength has decreased significantly from the last inspection, or if it has gradually decreased below 26 KV range (at 25C.) -- RUN A CHECK FOR MOISTURE. Use ASTM D901, D877 (Karl Fischer Method). The dielectric strength of askarel is the major indicator to the operating efficiency of your liquid insulation and of the askarel transformer itself. Besides the "visual" inspection tests, dielectric strength is the only test necessary to run on a routine basis. Well-sealed askarel transformers have service records of 25 to 30 years on the original askarel. New askarel has a minimum dielectric strength of 35 KV at 35C., a maximum moisture content of 30 ppm. N6V 007558 WATER PCB-SD0000030852 XL INSPECTION CHECK LIST 1. If askarel is clear, even though darkened to light brown; has no sediment or turbidity; has dielectric strength over 26 KV .. . give it the inspection "OK''. 2. If askarel is clear; has foreign color of blue, green, red . .. it is "extracting color" from internal materials. This is not,of itself, an operating hazard when the dielectric strength stays over 26 KV and moisture remains low. However, this rare occur rence calls for checking into condition of the interior construction and consulting the transformer maker. 3. If askarel is clear; but dielectric strength drops to 22 or lower KV, and moisture rises over 80 ppm .. . the askarel is ready for simple "refining". If the moisture is near the saturation level (about 125 ppm), a thorough inspection should be made for water droplets in the transformer tank, and even for "globules" or water floating on the askarel surface. If found, the transformer manufacturer should be consulted for reconditioning both the transformer and the fluid. 4. If askarel is dark brown to black; if black particles of carbon are seen; and dielectric strength is low... the askarel has been broken down by arcing. It cannot be refined and should be discarded. If any of these four simple inspection tests appear out of the ordinary, or the relationship between appearance and test values is abnormal -- contact your transformer supplier for a complete analysis. Whenever a sample is to be shipped to Monsanto, please follow the directions shown under: "SAMPLING ASKAREL". . XII. CONTAMINATION IN TRANSFORMERS Unlike mineral oil which can oxidize, sludge and deteriorate -- askarel breaks down in transformer use only when strongly arced. Thus, while askarel does not decompose in normal use -- it can be contaminated more readily than the relatively non-polar mineral oil. For example the following Table VI shows how a small amount of synthetic rubber or a bit of varnished cloth markedly increases the power factor of the askarel. Please note, however, that such minor contamination has no adverse effect on the dielectric strength. As explained, moisture entrance through faulty seals seems the only contaminant in normal use that lowers the dielectric strength of transformer askarel. 12 NV 007559 WATER PCB-SD0000030853 Table VI EFFECT OF COMMON INSULATION MATERIALS ON POWER FACTOR AND DIELECTRIC STRENGTH (HEAT AGED 96 HOURS IN ASKAREL AT 1O0C.) Material Immersed None (control)......................................... .. Black varnished cloth.............................. .. Copper..................................................... .. Pressboard................................................... .. Manila paper........................................... .. Phenol formaldehyde resins.................... .. Shellac..................................................... .. Iron.......................................................... .. Synthetic rubber...................................... .. Askarel After Exposure Power Factor, Percent at 60 eye., 100C. Dielectric Strength 25C. 1.0 85.0 35 KV 42 1.5 40 2.0 37 1.5 39 1.6 4) 6.0 36 5.0 39 70.0 39 Similarly, trace contaminants from commonly used construction materials can lower the volume - resistivity of askarel, without affecting its dielectric strength. Table VII shows this. Table VII EFFECT OF COMMON INSULATION MATERIALS ON VOLUME RESISTIVITY OF ASKAREL Sample 1. New askarel before heat aging...................................... 2. New askarel after heat aging 96 hours at I00C........... 3. After heat aging with 1 sq. inch specimens of: a. Phenolic resin tap changer material........................ b. Paper............................................................................ c. Grade A press board (tan)........................................ d. Grade A press board (gray)...................................... e. Grade A press board, laminated strip..................... f. Cotton wrapping........................................................ g. Glyptal 1276 cement, cured 48 hrs. at II0*C.......... Volume Resistivity x 10* ohm-cm (at 100C., 500 Volts DC., 0.1'gap) 2,000 1,900 1,200 750 500 500 400 300 100 While trace contamination easily lowers volume resistivity from high levels, it is important as previously noted in Table V Case F, that heavy contamination (as when arced) does not lower the resistivity below the order of 10' ohm-cm. at 1006C. The different behavior of askarel vs. mineral oil in these respects can be summarized as follows: High power factor and low volume resistivity in transformer mineral oils are commonly regarded as "danger signals" that the oil has deteriorated and broken down chemically. This is NOT TRUE of askarel liquid insulation, unless the dielectric strength is low. U NEV 007560 WATER PCB-SD0000030854 XIII. REFINING ASKAREL FOR 1E-USE A. Filtering Through Dry Blotter Paper to Remove Moisture and Extraneous Partciles: Most operators prefer portable refining apparatus, such as a plate press filled . with a dolly, (available from Sparkler, Mundelein, III., Westinghouse Main tenance and Repair Dept., Chicago, or General Electric Co., Pittsfield, Mass.); or the earthen cartridge filter type, (available from Industrial Filter Corp., Lebanon, Ind.). Filter paper liners for the plate press are available from Carl Schleicher and Schuell Company, Keane, New Hampshire and manufacturers of filter presses listed above. The filter paper must be dried immediately before use. For best results, spread the paper for maximum surface exposure in a hot air circulating oven and heat it for 4 to 6 hours at I ICC. If possible do not take the transformer out of service until ready to filter the fluid. This will keep the transformer coils relatively hot and dry. Processing the fluid should start immediately after de-energizing the unit. Circulate the askarel hot (but not over 55-60C.) through the filter fitted with the dry paper liners. After filtration the dielectric strength of the askarel should be 35 KV minimum. 1, Precautions: Filtering should not be done when the relative humidity exceeds 75%. 2. Any flexible hoses and gaskets on the refining equipment should be lined with or made of materials that will not be softened by contact with askarel fluid. (Silicone or Teflon-lined, or flexible metal materials are suitable.) Table VIII GUIDE TO RATE OF DISSOLVED WATER REMOVAL BV FILTERING ASKAREL THROUGH A PAPER PRESS Pae Through Paper Prew 01 2 3 4 3 6 Water In Aikarel PPM IIS 35 22 18 12 1to0 KEV 007561 WATER_PCB-SD0000030855 B. Earth Treatment for Maximum Improvement of Power Factor and VolumeResistivity: 1. Procedure: (The askarel liquid should be relatively dry prior to the following earth filtration.) Use finely divided Attapulgus clay or Fuller's earth (dried and activated by healing for 12 hours at 300-350F. immediately prior to use) as a coating on the filter paper surface. The amount of earth used should be 0.1 to 0.2 per cent by weight on the weight of the askarel to be treated. (Askarel weighs about 13 pounds per gallon). To deposit the earth evenly, stir one-third of the earth with a small portion of askarel in a clean container. Pump the mixture through the filter and follow with two more one-third portions. Then circulate askarel taken from near the top of the transformer, pass it hot (not over 55-60C.) through the earth coated filter and feed back through the bottom transformer outlet. Continue circulation until the fluid is clear and test shows that the electrical properties are fully restored. 2. Effect of Earth on Removal of Scavengers: Only slight and insignificant loss (by selective absorption) of tinletraphenyl and epoxides occurs when askarel is refined by treatment with 0.1 to 0.2 per cent by weight of earth. To remove significant amounts of the scavengers requires repetitious treatment with much larger amounts of earth. 3. Table IX -- Approximate Relationship Between Power Factor, Volume Resistivity and Dielectric Strength of Transformer Askarel: Power Factor (60 eye.) I00C. 25C. 2% 5% 15% 20-25% 40-50% 0.05% 0.1% 0.7% 2.0% -- Volume Resistivity x 10 ohm-cm. (at 100C., 500 Volts DC., 0,1' gap) 1500 500 100 60-70 25 Dielectric Strength 25C., 0.1' gap 35 KV 35 35 35 35 If it is desired (although these factors are not generally considered important for askarel transformers), to keep the power factor as low as possible and the resistivity as high as possible, hang a container of anhydrous alumina or activated clay in the circulating system of the transformer. XIV. CLEANING ARCED TRANSFORMERS If a unit has arced so that the askarel is no longer fit for use, a thorough cleaning of the unit is necessary before refilling with new askarel insulation and returning it to service*. Follow this procedure: . 15 NEV 007&62 WATER PCB-SD0000030856 A. Drain out all dark, carbon-contaminated askarel. (Discard by dumping or burying where it will not contaminate a water supply.) B. Carefully brush carbon deposits from internal parts and insulation, using a soft bristle brush making sure that insulation is not damaged. C. Flush thoroughly using new askarel (not an oil, not a cleaning solvent). D. Flush a second time with fresh askarel; drain; then fill to the proper level with new askarel. E. Energize transformer to warm the fluid for 24 to 48 hours; then circulate the askarel through a filter, returning it to the unit filtered and ready for use. This assumes that the cause of arcing has been established and corrections made. When severe arcing occurs, major repairs are usually necessary and the unit rebuilt. This procedure can be applied for flushing out repaired units. NEV 007563 WATER PCB-SD0000030857 XV. SAMPLING ASKAREL Take a sample as close to the top of the liquid surface as possible. (Many large askarel transformers have a built-in sampling tube near the surface for convenient sampling). Then, to make sure that your SAMPLE truly represents your askarel insulation, take another sample from the bottom. If additional sampling tube connections are contrived on the valves for easier sampling, make the tubes of clean glass, stainless steel, aluminum or tin for rigid types; and silicone or Teflon tubing for flexible types. Use NEW containers for the askarel sample. A new and thoroughly pre-dried smallmouth quart glass bottle fitted with a Bakelite screw cap fitted with an aluminum or (in bottle cap liner is recommended for "quick on-the-site testing." (If complete analysis is to be made, a 5-pint size sample is required). Be sure that the new bottle does not stand open to collect dust or moisture. Rinse the sample bottle and cap lining two or three times with askarel from the transformer; then fill it. If the sample will be tested promptly, a clear glass bottle can be used. If sample is to be stored indefinitely, use an amber glass bottle or wrap clear glass with aluminum foil. A. Select a dry day. Do not sample insulation on a warm, moist day when humidity exceeds 75%, and ... B. Make sure that the askarel is at least as warm as the surrounding air. (Cold liquids can condense moisture from humid air.) C. When sampling askarel from transformers, it is best to take the sample when the unit is warm and operating at average or maximum load. Especially as a check on moisture (as reflected by a dielectric strength test), sampling the warm askarel more truly represents its condition during operation. Experience shows that water will migrate from a transformer's solid insulation to the askarel liquid and vice versa, depending on temperature. Therefore, when the transformer is hot, the moisture is most likely to be found in the liquid. This accounts largely for periodic variations in dielectric strength. For example: a relatively high dielectric strength may be found during winter months and a relatively low dielectric strength during the summer months on samples taken from the same unit. 17 NEV 0075t><t WATER PCB-SD0000030858 SECTION B ASKAREL FILLED SWITCHES AND TERMINAL CHAMBERS 1. INTRODUCTION: High voltage leads are usually connected to askaret or mineral oil-filled network transformers and power centers through terminal chambers and switches. In some cases terminal chambers are not used, and the high voltage leads are connected directly to the switch terminals. They may be filled with either askarel or mineral oil. Switches are usually rotary or drum type fitted with a revolving block and porcelain unit as the principal element arranged for three-phase service. (A cutaway view of a typical terminal chamber-switch combination is shown for reference.) Askarel transformers with attached switches have been in use for about 30 years. When they were first introduced, the availability of insulating and gasketing materials was rather limited and even the best materials at the lime had no service history. As a result, inadequate gasketing materials such as cork, nitrile rubber, and nitrile rubbcr-and-cork particles were used. While satisfactory for a limited period of time, these materials cannot be depended on for the expected long life of the equipment. The terminal chamber is usually above or below the switch compartment and separated by a steel wall through which the bushings are inserted. When bushings are properly selected and correctly installed, there is no leakage from one compart ment to the other. With poor bushing seals, and the terminal chamber above the switch, potting compounds or cable oil can seep into the askarel. When the terminal chamber is below the switch, askarel can drain into the terminal chamber. 11. SOURCES OF CONTAMINATION There are three possible sources of contamination for askarel in switches and terminal chambers; they rank in this order of frequency: (1) water entering through poor gaskets; (2) decomposition products from arcing when switch is used to break magnetizing current; (3) entrance of pothead or cable compounds through leaky bushing seals. Unlike an askarel transformer where the amount of contaminant is likely to be very small (probably only trace amounts) in relation to the volume of askarel fluid -- in switches or terminal chambers with faulty seals, the amount of contamination can be relatively large. *' NEV 007565 WATER PCB-SD0000030859 Experience has shown that, based on the number of installed askarel-switch units, the percentage of failures is extremely small. When investigated, it has been found that most failures originate in the switch chamber. Water is the chief source of contamination. However, heavy contamination of askarel with petrolatum and asphalt material, due to leakage, have caused a few failures. Petrolatum is used frequently for filling terminal chambers. When either cable oil or petrolatum seeps into askarel, no great harm results. The fire resistance will be somewhat decreased and power factor of the askarel will increase with an accom panying drop in resistivity. While highly undesirable, it is doubtful that failure of the unit results. Where asphaltic compounds are used in place of petrolatum, the danger is increased somewhat because asphaltic contamination may cause exces sively high dielectric losses in the askarel. When the terminal chamber is below the switch chamber, the potting compound can be contaminated by askarel if the bushing seals are leaky. This is undesirable because the askarel will increase the power factor and conductivity of the potting compound or cable oil and develop heat from dielectric loss. If this mixture is drawn into the cable insulation, a cable failure is likely. This again emphasizes the impor tance of tight bushing assemblies. III, SEALING SWITCHES AND TERMINAL CHAMBERS Proper bushing construction, use of Silastic seals and welding wherever possible is highly desirable (as covered in Section A). Where an elastomeric seal is to be used in contact with both askarel and petroleum oil, DuPont's Viton is suggested. For new equipment the user should specify these modern sealing arrangements to keep out contaminants and minimize maintenance. IV. MAINTENANCE FOR ASKAREL FILLED SWITCHES A. Switches used for grounding after power source has been de-energized will not undergo arcing. B. Switches interrupting magnetizing current will be subject to arcing; the amount of decomposition will depend on power interrupted, time and frequency of oper ation. As a general rule, the liquid should be checked after 5 to 10 operations. NEV 007566 19 WATER PCB-SD0000030860 1. On newly installed switches, check the askarel at 3,6 and 12 month intervals; if found satisfactory, check once annually thereafter. With proper attention to the gasketing of covers and bushings, experience will probably indicate that less frequent inspection is warranted. 2. Check askarel for: a. Dielectric strength (ASTM D877): It should be 26 KV minimum. If dielectric strength is low, confirm presence of water by Karl Fischer method ASTM D-1533. Filter to remove moisture. Dielectric strength should then be 30 KV minimum. b. Presence of carbon from arcing; Fluid should be relatively free of carbon. If badly arced and very black, replace fluid. If only minute amounts of carbon are present, filtration is recommended. Check power factor of liquid (should not be over 5% at 25C. and 60 cycles). Flush out switch chamber with several gallons of fresh askarel before refilling. 3. If there is discoloration, high power factor, detectable change in specific gravity or refractive index, or if fluid flashes below 250F., there is a possibility of seepage of potting compound into the switch compartment. In this case, correct any leaky bushing seals with proper replacements and fill with new askarel. 4. If terminal chamber is below switch, check potting compound for presence of askarel (can usually be detected by odor or by an increase in specific gravity). If askarel is present, correct any leaky bushing seals with proper replacements, and renew compounds. 5. Examine cover gaskets visually. Deterioration can be detected by swelling and cracking of the exposed edge. In cases of severe deterioration, liquid seepage is usually present. 6. Check for leakage at packing gland of switching shaft. If leaking, repack with a Silastic ring type gasket. # 20 NV 007567 WATER PCB-SD0000030861 SECTION C ANALYTICAL SERVICES ON TRANSFORMER ASKAREL AVAILABLE FROM MONSANTO Transformer users not wishing to make their own fluid analyses can obtain the service from Monsanto. Simply contact Monsanto and specify what analyses are wanted. You will be sent the proper-sized sample container filled with fresh askarel. When you receive this, empty it and carefully take your sample (following the procedure for sampling in this guide). Send the container to Monsanto's laboratory. Charges listed include sample container, shipping, handling and laboratory costs. Types of Analyses Available Analysis I) ROUTINE MAINTENANCE CHECK Total Charge: $20.00 To determine the general condition of the fluid and find whether further analysis is neces sary. (one-quart sample required) Properties Tested Color and Condition Dielectric Strength Moisture ' You will be notified of the results of this test. If further testing is indicated, and you want a complete analysis, you will be sent a five-pint sample container. This sample will be used for the following series of tests: Analysis 2) COMPLETE ANALYSIS Total Charge: $50.00 (a) To determine the extent of fluid contamination, (b) earth refinement to determine what degree of restoration of electrical and insulating properties is possible, (c) check test to see how the fluid re ponded to earth treatment. a) Complete Analysis: to determine the extent of contamination Properties Tested Color and Condition Specific Gravity Refractive Index Water Free Chlorides Acidity Dielectric Strength Power Factor, Dielectric Constant, and Resistivity NEV 007566 WATER_PCB-SD0000030862 b) Earth Refinement Response: Consists of treatment for 2.5 hours at 50-60C. with 0.1 to 0.2 percent by weight of properly conditioned Attapulgus clay and then filtration through dry filter paper. c) Analysis After Laboratory Earth Refinement: Properties Tested Refractive Index Water Free Chlorides Acidity Dielectric Strength Power Factor, Dielectric Constant, and Resistivity You will be notified of the results of this test series on your sample. Then aftei refining your entire transformer fluid fill you can check on the results by requesting the following analysis: Analysis 3) ANALYSIS AFTER EARTH REFINEMENT Total Charge: $30.00 (This charge will not apply when analyses I and 2 have already been made.) To determine whether the entire lot of the askarel fill responded to the same extent as the laboratory sample, (five-pint sample required) Properties Tested Color and Condition Refractive Index Water Free Chlorides Acidity Dielectric Strength Power Factor, Dielectric Constant, and Resistivity To arrange for the tests described above write to the following address: Paul G. Benignus Monsanto Chemical Company 800 North Lindbergh Blvd. St. Louis 66, Missouri Samples to be tested should be clearly marked for identification and sent directly to: Monsanto Chemical Company W. G. Krummrich Laboratory Monsanto, Illinois Attention: R. Kuster # 22 NEV 007569 WATER PCB-SD0000030863 APPENDIX APPENDIX A -- Askarel Stability and Composition of Arc Formed Gas: Askarel insulation is one of the most inert, chemically-stable heat resistant, non corrosive liquids known. It will not break down, oxidize or sludge when exposed to air and high temperatures, 150C. or even somewhat higher. Arcing, however, will break down the compound to liberate some hydrogen chloride and small amounts of carbon. APPROXIMATE COMPOSITION ARC FORMED GAS FROM TRANSFORMER ASKAREL Cas carbon monoxide......................... carbon dioxide.............................. oxygen........................................... inerl gases..................................... hydrogen chloride........................ (note the absence of phosgene) Amount 0.3 per cent 0.3 0.6 1.5 97.3 This arc-formed gas is non-flammable and non-combustible. These requirements must be met in accordance with the Underwriters' Laboratory for permission to use the term askarel. Mineral oil evolves combustible hydrogen and hydrocarbon gases. For all practical purposes, the amount of gas liberated from mineral oil or askarel under a given set of conditions is about 100 cubic centimeters per kilowatt-second. APPENDIX B Carbon dioxide............... Air.................................... Nitrogen.......................... Hydrogen chloride1 .... I) In absence of scavenger SOLUBILITY OF GAS IN TRANSFORMER ASKAREL Percent of Gai By Volume Corrected to: 25C. 760 mm 2sc. lore. 0C. 760 mm isc. iorc. 71% 47% -- -- 5.7 4.9 5.8 5.0 6.0 4.8 5.5 4.4 37.8 50.9 ---- 23 NEV 007570 WATER PCB-SD0000030864 APPENDIX C APPROXIMATE VAPOR PRESSURE VI. TEMPERATURE FOR TRANSFORMER ASKAREL Temperature 'C 40 60 80 100 120 140 Inerteen PPO, 7336-9 I mm Hg. 5 9 30 60 90 Transformer Pyranol A13B3B 0.9 mm Hg. 3.5 8.3 18 32 53 APPENDIX D EFFECT OF TEMPERATURE ON DIELECTRIC STRENGTH OF ASKAREL Temperature C. --60 --40 --20 0 20 40 60 80 Dielectric Strength 67 KV 63 57 35 50 30 48 45 APPENDIX E COMPARISON QF THE APPROXIMATE VISCOSITY IN SAYBOLT UNIVERSAL SECONDS OF TRANSFORMER ASKARELS AND MINERAL OIL Temp. C. --20 0 20 40 60 80 100 Transformer Pyranol AI3B3B 1,000 100 70 45 39 34 30 10-C Mineral Oil 1,000 ISO 85 49 40 34 30 Inerteen PPO, 7336-9 2,800 195 85 50 40 36 33 : 24 new 007571 WATER PCB-SD0000030865 APPENDIX F THE DENSITY OF INERTEEN PPO 7336-9 AND TRANSFORMER PYRANOL AI3B3B Tlmperature *C. Approx. Denlily gm /cc. Inerteen PPO, 7336-9 Transformer Pyranol AI3B3B 0 1.374 1.577 20- 1.552 1.555 40 1.529 1.332 60 1.507 1.510 80 1.485 1.488 APPENDIX G The thermal conductivity values of transformer Pyranol A13B3B at 27C. and 58C. are 26.2 and 23.8 x 10-5 calories centimeters'1, degrees centrigrade'1, second-1, respectively. Or, approximately 0.06 BTU per (hr.) (sq. ft.) (F.) per foot. This same approximation applies to Inerteen PPO (7336-9). APPENDIX H Heat Capacity Over the temperature range or 25 to 125C. the specific heat of transformer askarel is close to 0.30 calories per gram per degree. APPENDIX I Coefficient of Expansion The average coefficient of expansion of transformer askarel over the temperature range 20 to 100C. is 0.0007 cc/cc/C. One gallon would increase to 1.056 gallons on heating from 20 to 100C. APPENDIX J Fire-Resistance To use the generic name "askarel," the fluids must be approved by the Underwriters' Laboratories as possessing adequate fire-resistance and freedom from forming explosive gases when arced. These liquids do not have a burn point (ASTM D92-33) (Cleveland open cup method) up to about 205C., at which temperatures they begin to boil. The significance of this is that they do not burn or support combustion under conditions encountered in transformer operation. Thus the danger of secondary explosion (or fire) is eliminated. 25 NV 007572 WATER PCB-SD0000030866 APPENDIX K Seals, Properties and Procurement Dow Corning Corporation, Midland, Michigan with District's at Atlanta, Boston, Chicago, Cleveland, Dallas, Los Angeles, New York City, Washington, D, C. and Toronto has available Bulletin 09-019, August 1962 entitled ''Silastic Design Data". This lists the gasket fabricators throughout the country from whom the "Silastic SO" gasketing can be purchased in sheet, extrusions or molded shapes. Generally Silastic 50 sheet goods are stocked by local die cutters, hence, could be generally purchased locally. Usually, small quantities of gaskets are die cut. If larger quantities are needed, tools are made of the same type used to cut other elastomers. Where the gasket is extruded for fitting Into a machined groove or between gasket stops, Dow-Coming advises use of a scarved joint. This joint is then cemented using Dow Coming's Silastic 140 (clear) or their RTV 731 (white) materials, which air cure. Dow Corning points out that the local "rubber" fabricators purchase the Silastic 50 in billet form. This is worked on a roll mill in preparation for sheeting or extrusion. Then to obtain the desired physical properties the fabricator must oven cure the Silastic 50 for 24 hours at 480F. SPECIFICATIONS* Color............................................ White Specific Gravity at 77F............. 1.20 * 0.02 ASTM D676 -- Hardness, Shore A. Scale.......... 43 to 60 ASTM D412 -- Tensile Strength, psi. min.......................... 800 ASTM D4I2 -- Elongation, percent, min............................230 ASTM D39S -- Compression Set after 22 hours at 300F., percent, max.............................. 30 All physical properties measured on 0.075 inch thick samples molded 5 minutes at 240F., and oven cured 24 hours at 480F. General Electric Company, Redmond Circle, Rome, Ga., uses silicone or DuPont's Viton wherever it is not possible or desirable to weld. For some small seals, where good matching surfaces are provided, Flexitallic stainless steel rings are used. By contacting the Engineering Services Department of General Electric Company, Redmond Circle, Rome, Ga., users of Pyranol transformers made prior to develop ment of these modern seals will obtain prompt assistance for conversion. Users of askarel transformers made by other manufacturers should contact the original transformer manufacturer, or Monsanto for assistance in converting to these modern seals. 00 75 73 26 WATER PCB-SD0000030867 00**1* WATER PCB-SD0000030868 NOTES nev 0075 75 WATER PCB-SD0000030869 MONSANTO FUNCTIONAL FLUIDS DIPT. too N. LINDBERGH BLVD. ST. LOUIS, MISSOURI UtM The information herein regarding obtaining optimum results from askarel fluids in your transformer hu been accumulated by Monsanto for over 30 years from the experience of makers and users of askarel transformers and it is believed will be helpful. Nothing herein shall be construed as applying to other than askarel insulation. Data and maintenance suggestions herein do not apply to the other components of the transformer. All operating end maintenance suggestions recommended by the manufacturer of the transformer should also be carefully followed. Because these maintenance directions apply only to the askarel insulation, Monsanto disclaims any liability for damage to property or injury to persons arising from transformer operation. ' NEV 007576 U'ho U % A WATER_PCB-SD0000030870 u u booi up, Hwart Borgni - 00 MP. Bill Maddox - NY HP* Fi 8tum - HI Munb 8# 196I MP. J. 0. Sullivan 0. 1, Linok Company Clifton# Man Jintj . Daar Mr. Sullivant Mp Howard Borgan of our co*miv haa aaknd that m lami1 your roquoat for oral toxioity information oiKAroolor produota va havo aeuta owl data on Aroolor HWIftd Aroolor 125% TMH data ara 4.15 nl/kg fop Aroolop 1242 and 3.10 nlA* fop Aroclor 1254# both in rata. Z do not hava oteoni oral toxioity infemotion on thaaa produota ainea we do not on*Mop than aa advlaabla for uaa In food produota The raally elgnlfleant problea in handling Arcelor* ooaeo fro* tha possibility of demtltls through rapaatad akin oontaot and tha poaalhility of apa* tamlo effaota through ropaatsd Inhalation of vapopa In axOOSSlVO OMOntMtiOM. . Aa you probably know# tha Anarloan Confaranoa of Oovarnaantp.l Induatrial Hyglanlsta haa aatabllahad a Hyglsnlo Standard or Msxlaaaa Allowable Concentration (MAC) for an eigfrt<hotir working day for two of tha Aroolor produota. Thaaa data ara for Aroolor 1242*1 Milligram par cubic meter and for Aroolor 1254# 0.5 milllgran par oubio natar. Wa suggest to milMm who handle these produota that oars be takan to avoid axtanaive to the unprotected skin and to axoaaaivo vapor* Monsanto ond ita Mleam haw handled many millions of pound* of thaaa produota with m difficulty# topping thaaa simple handling praoautiora to wind. If wo p bo of further halp# plaaaa lot ua toon. Siurtly# jr<* RBXipjk R, Basnet Raiily; m. d. Mdloal Direotor NEV 161141 WATER PCB-SD0000030871 EXHIBIT 6D Monsanto Chemical Company St. Loots 4. Missorax ^Lu-Uk*^ ' July 25, 1956 ' Mr* Ho W. Speicher, Administrator Industrial Hygiene . Westlnghouse Electric Corporation East Pittsburgh* Pennsylvania . .. Dear Mr. Speicher: ' " ' Thank you for your letter of July -19' requesting toxicity Infor mation on several of our Aroclors 'and atmospheric sampling methods. ' I an sending under separate cover two detailed reports published by personnel at the Kettering Laboratories .entitled* "The Toxicity of tee Vapors of Aroclors 1242 and 1254." 'Tie data contained herein were condensed and presented by Dr, Tireon at the AIEA meting to Philadelphia this year. - It was published to the form presented to the June* 1956 Issue of the "AIHA Quarterly*" a copy of which I am sure you oust have. I am asMng Dr. Treon, by a copy of this letter* to send you a reprint of his publication If such Is available at the present time. ot* You will note that Dr. Treen has proposed that the hygienic stan dard for Aroclor 1242 be tentatively established at 2 milligrams per cubic meter and that the standard for 1254 be estSBXBBga^at ^ISjCpCSEPamTB^ cubic meter. I am sorry thai t we d`o not `have xL However, we have so particular '<* ^reason to expect that a sr jj.enj:..chlorinated .biphenyl offers' ^-'any greater hazard than a per cent chlorinated' biphenyl. "L/^You will note further that Dr.-Trtoo'a work discusses a modified jwJ; Willson hydrocarbon apparatus' used to the sampling of his test V atmospheres. In a limited mount of sailing to our own plants we have used the Willson equipment as shipped to us. I have en closed a description of the operating procedure prepared by one of our research groups which s .%ooewhat more detailed than that provided with the instrument ;' . You have.previously seen our complete reports on the decomposition of Prdraql when allowed to drip or flow onto-'a: heated natal Inconel surfaceThe- data to'those reports have convinced us that there la no greater'acute hazard should Pydraul accidentally contact metals at the temperatures investigated than there would be with other industrial hydraulic fluids.' I do not have any data, to .support ar.y conclusions as to what might occur If the Fydraul were to be used NPC00035799 WATER PCB-SD0000030872 Mr* 1* . SpeIcher, Administrator -- Page 2 -- July 25, 1956 as a hydraulic fluid In malting massea ltm_. die.cast Inga. We do have a report that one plantmanoling large quantities of molten ma^eatom purposely sprayed Pydraul into the molten material primarily to aee if there would be a great deal of spattering of the maj^esium The co^any reported to us that their testa convinced them that Pydraul could be used Whether or not they are using Pydraul, .1 cannot aasr, t I note in rereading your letter that I have hot answered your question relative to akin effects following Aroclor contact. ' Vfc recommend that repeated and prolonged akin contact with any or-zne Aroclors ee avoided-. we nave patch tasted several or ' them with"Efegatlv* faults, to addition, .reported eases of |akin irritation have been surprisingly few to view of the heavy f tonnage quantities of Aroclor manufactured 'and handled in the last twenty years We believe, however, '-that care to handling and good personal hygiene is necessary to avoid irritation As with manyr chlorinated hydrocarbons,'-emposure to 'sufficient quantities over a long enough period of time cbuld conceivably 'result in`chloraene*-' to this respect, however, the Aroclors are nojcjshl. j^'jpMO^chloranenegsns,: such as chlorinated naphtha lenes!! To our knowledge, there have never oeen ahy"cases bf" chloracn* in the electrical to*astry8s use of these products, If I can be of any further assistance, please let me know. Very truly yours. Elmer P. Wheeler Mr. Paul 0. Benlgsus Monsanto` NPC00035800 WATER PCB-SD0000030873 -A BOG Paul Benignus-GO Oatsbar m 1959 m.. lift Hr. 1 MUlrnr fpalahar Adalnlatratar# toAntriml Hyglana lloatrla Corporation lut ttttaburgh, fannarlvaala laar Wilbur i Viank you for yew lattar of 0tobr 21 Inquiring about the aafo uaa of t*4hlriipb*fiyl and a nlxturs of 4cp triahloro- banaaoa and 60)1 . Va narkat trlahlorodlshanyl /<JItIqc 1242*0 Xha acnblna- tlan of haxaahlarodlpnaagrl trla|ilp<6tnana ! known n^ap**'- oonblnatlan la our fha phyalaal and ahaadaal proportion of tha Aroalnra nantlanad aro tuna an tha tabla an pogsa % and 5 of tha anoloaod Aroalar bullatln# inaloaad alao la a mprlnt MMtei tha roaulta of ahronla toxleity atudlaa with AralmnQMtm and 12$4, tha following acaoMnta ananarlng your quoatlona aarlally ara Iwi cn Infamotion Mitain4 in thaaa bullatlna. X toallava prolig*4 and rapaatad *Jdn aantaat with my af tha Aroalora ohould ba avoldad for two raasana. In tha r&rat plaao# tha lata nhlarlnatad product* art llfulda and art mm1 lant aolvsnta f? oils and fats in tha tMn m wU aa othar organia material*. taaandljrf it ia poaalbla that prslanaad or rapaatad akin omlMt aould load to ahlamaa* Z know of only tm mm% whom auth agporlonaa ban 4rtlop4 during tha long hlatovy of production and uaa of tha ArMlon to ana aaaa* an Aralar vaa btlng tn#4 m a boat tranafar aadlun In a gyatan that aUMii vpr to aaaapa ahan tha natar&al was haatad to 600% Aavaral worliifttj davalopod "blaakfeoadg" ahiah warn found fey ft InAntrial phyalalan tout which In his wrd* vara aa in* lgnlflaant that tha mu wars not mm of than dot would a gansral praatitionar notlaa than* ffcla Indlaatsa ta na hanarar* 1 DEPOSITION II EXHIBIT 1 a-ir-'H NEV 006347 WATER PCB-SD0000030874 Up. S, Wilbur Spelohar--Page 2~October S3, 1959 that sufficient exposure, *i#ther by inhalation of vapor* or akin sontaet, an result in Mormon# which 1 think we oust assume could be an indication of more serious systemic Injury if the mpmum was allowed to oontlnue. A fond case of BUd hloraonc about which we have any knowledge resulted from dipping their hands In the - liquid Aroolor as if it were mineral oil or vegetable oil. In addition, their clothing sooner or later became Impregnated with the material and thus exposure was magnified. leu asked at what temperature local exhaust ventilation should be provided. Although the distillation range for Aroelor 1242 la 325-360OC. and 385-420<>C. for Aroelor 1200, I feel that good praetloe diotatea that local exhaust ventilation be provided when any of the Aroelora are heated above 1507. in open tanka or In any ay*ten* where the material la not In a completely aneloced system (vapor-proof tanka, kettles, pumps, piping, etc.), This may be ultra conservative because as the distil lation ranges and vapor pressure curves (page 12 of the Aroelor bulletin) lndleate, the loss of vapor* at 1507. should not be significant except in any work area where general ventilation or air ohanges do not exist. Your next question related again to possible skin and systemic effects and I believe It is answered above. In connection with the 40^ trichlorobenzene-6o Aroelor 1260 combination, 1 believe the thoughts expressed above also apply. X understand that the trichlorobenzene which Is used Is a mixture of the 1,2,3-# l#2,4-# and 1,3,5-lsomers which will begin to distill at 205C* Again, I believe this indicates a low vapor pressur* for tha solvent st room temperatures. The only reference wa have to trlohlorobensens toxiolty Is con tained in the Public Health Service Publication No. 414 entitled "the Halogenated Toxloity and potential Bangera" by Dr. W. F von Oettingen, 0.8. Oovernment Printing Office, 1955 (paxes 297-S9&)* Dp. von Oettingen rafara to some wo* dona in 1937 whioh indicated that the triahlorobenaana m lass tootle than nmo or dlehlorobensene. in my opinion, a reasonable MAC for tliia material would be 100 pavta per million Bio eneloeed publication on tha toxicity of Aroelor 1242 and 1254 suggests an MAC for 1242 of 2 milligrams per cubic meter which is twice that rtoenMended by tha AC01H for a chlorinated di phenyl of unstated ehloriM content to the ease of 1854, tt publication suggests that the MAO of 1 milligram per cubic meter "ree amended tentatively for safe indutrial praetloe by tha Anariaan Cenfaranae of Governmental Znduatrial Hygienists* ie reasonable to the ether hand, reference to Henry *syth*s Cummlnas Memerlal iMtw* of 1956 in whloh he dlseueead ito Mai* for the then existing -hyiitnie tandards" indloates that 006348 WATER PCB-SD0000030875 Hr. Vilbar feolahor--ft 3--0tb#r 83# W9 . that NlkOs of 1 a^faua* for Aroolor 1248 and 0*3 a^um* far Aroalor X894 aro boto roallatlo* Xa tho abaoaao of aiqr aturonla toalolty data on Imiw I860* aa auggaat an NM) 9t 0*5 Ba/tua, tho mm m 1a tho aaaa of 1834 X tow toiaa la oao plant ahora thaao aatorlala war uaod for #apItr aM tranaforaara* tho aara and luMUng and tha prmt^lma of oxbauat vontllatlon mm not in aooordanoo with tho thoughts upftiMd abovo* Tha only roportod dlfflaultF m aona mU4 ayo lirltatlan vban Imprecation aablaata iten tho itaaa vara tjoatod to 110-ltDC. roloaaod of trihlvo* baaaano uni tho Aroolor into tho vnan tho tabtooi ten loaod* Xtt ay Bind# Nb aablnata iNuU ho vontUabod to tte voooro ratbor than Um than to to nlnati into tho X tow boon told that roar aonpoaor to* had aona 80-83 raara1 nu.uo's-U/u-uo with tha produota dlaouaaod atow* Xt wa iuuiiMI Uul Rr Jhaaa 1 Ford* msuiiif C tranafonaar aanuftaturlns onalnotrint at jots1 Bmrm Fiant would to A i >00000 of laferaa%lm rocaxnlna ooparlonoo with Saortoon FFO. dlallarly# Mr# l, X ttorburar of rour BlooBlngton Indiana Float to* boon *alAi#4 vith tho uao of Awiw 1248 Fovhapa jm hava al- raoAr dlaauaaod potential m9mf with thaao gantloMn if m, X *M to lateraatod In laaminc of tholr paantloal ox- ,,;;j0 *lth feu.-; produatO. X Mute to {':: you to FAttaburgh naxt dlnoavaly* With iNlNUNI 8 Murnr F ttwolar Militant BdraOtOT Nteloal. Popartaant NV 006349 WATER PCB-SD0000030876 bcci Paul Benlgnus April 26, 1966 Mr Alvin V. Crow Qumrierman Maintenance Public Works Department U* S* Naval Station Kodiak* Alaska Dear Mr Crow: Your letter of April 15th ha* been referred to me for repljr. t 1 have enclosed a booklet which describes fire resistant transformer fluids which have the generic name "Askarel." You will note on page 2 and page 3 of the enclosed Askarel Qulde that there are several commercial or trademark types of formulations, sane of which are described in tables 1 and 2. Chemically these transformer fluids are mixtures of chlorinated diphenyl and trichloro anchor tetrachlorobenaene. The history of the manufacturing* handling and uae of these products dates back approximately 30 years* In that time there have been no cases of serious Illness or toxic effects when simple precautions to avoid exposures have been followed. In the case of chlorinated diphenyls, a Hygienic Guide haa been published by the American Industrial Hygiene Association for the materials containing 420 and 540 chlorine* The diphenyl in Askarel is diphenyl chlorinated to 600. The toxicity characteristics then are believed to be similar to the 5^0 chlorinated material* The trnwd {m differentiated from toxicity) le less in handling thenSDSTmaterlal since it Is less volatile than the materials with lower degrees of chlorination* The vapors from transformer Askarel are somewhat toxic and should not be breathed continuously over a prolonged period of time* With the fluid at room temperature m would expect that there would be some odor of the fluid* The level or concentration which la barely detectable by smell should not be hasardous. to the other Mod, if the fluid la heated and vapors which are liberated are allowed to socumulate in an (i DEPOSITION I EXHIBIT 1 sn I NEV 161229 WATER PCB-SD0000030877 HP* Mvte V. CrflW April 25, 1966 taga a unventlisted rota* or srea* Wm concentration oouM beoams significant. M gmmmla paapla em dataat a emmlnfelon An Urn anount of 0.5 to 1.0 ng par cubic mstar of air which Is ragardad m tha aafb vortooi llait for an 8-bow daily axpoaura (5 days a waak* naak in M waak out). Tmtlomr Aakaral aaeldantally apUlad on tha skin d@n not prasant an aouta tooclolty tmsard nor will it mum mrlom irritation It should ba mov<S Aron tha Mon by wmshlns with soup and wilts1, however, btciust stptaM and prolonged wpotur* nay laad to drying and chapping of ths skill baoauaa of tha "solvant mtimn of tha fluid -- which Bight ba compared to the drying of the akin fron using paint woOTir or many othar solvents in a caralass fashion Vapor* rltM4 in high concentration* whan tha fluid is hsatad will eausa aya irritation. It ia pointed out on paga 5 of the anolossd Askarel Quid# that typical opthalaio solutions or olntasnts for raliaving pain in tha ayaa may ha uaad affear flushing tha ayaa with larga aaounta of water. Long rang# aeoumulatlva affscta froa exposure to Askaral fluids mild not be mooted unloss workntn mm exposed to high levels of vapors s number of hours a diy, day in and diy out or allowed the naterlal to reaaln on the skin for prolonged period* of feiaa and at frequent and rapaatad intarvals. Excessive vapor lnhallatlon or akin eenfeaat eu load to an offoot on fell livor as is the ease with many chlorinafciid hydrocarbon* * Ms hmv* novor haard of snob effoota in workers installing* repairing or servicing ferdnsfornew, however. If exhaust vantilatlon osnnot ba provided to ranova tha vapor* ralaasad by leaks, tha workm should ba provided with respiratory protootlon equipment if repairs and ervlelng ara required in an araa share tha vapors am Irritating fete eyes and nose or throat. If I oa ba of any fuvthar aaaiatanoa* plaasa do not haaitata to lat m taov Very truly yours. Re mm% Kelly, M.D. ftedieal Dims few Enel. Askarel booklet Hygienic Guide "Chlorodiphenyls NEV 161230 WATER PCB-SD0000030878 ^v. rU- tur o o HYGIENIC GUIDE SERIES Chlorodiphenyls (Containing 42% and 54% Chlorine) o /w\ <w ( i AtlOClAflOM O o o o o o (x + y 3 or 5) Cly Significant Physical Propartial1 The chlorodiphenyl* are light straw-colored mobile (42r* chlorinated I and viacous (S4Tc chlorinated) liquid* vuth typical chlorinated aromatic odors. These compound* are chlorinated to specific weight* of chlorine. Chlorodiphenyl (42d>) contains 42.0 = 0.5 chlorine, an amount corresponding to three chlorine atoms in unassisned position*. Chlorodiphenyl (54<T i contain* 54.3 7t chlorine corresponding to five chlorine atoms in unassigned positions. Both compound** are insoluble in water, but soluble in bentene, kerosene, acetone, amyl alcohol, ether andE- chlorofomt. - Chlorodiphenyl (42%) Chlorodiphenyl (54%) Molecular weight: 247.53 126.45 r Flash point (Cleveland O. C.): Distillation range: 176 -180 C (319' 356* F) 325*-366*C None ity.m'c. Specific gravity: 1.381-1.392 (25715.3*C) 1.495-1.505 (65715.3`C) Vapor pressure: 0*C 0.001 tnm 0.00006 tnm 25*C 0.006 mm (est) 0.00054 mm (wt / 150*C 4,3 nm 1.4 nun 200 C 29.0 mm 9.0 mm At 25*C and 760 tnm Hg: Saturated air contains 0.060 mg/liter 0.009 mg/Iiter ! mg/liter = 98.8 ppm 74.9 ppm 1 ppa = 0.010 mg/liter 0.013 mg/liter 1. Hygienic Standards A. Recommended maximal atmospheric concentrations (8 hours): One milli gram chlorrtdiphcnyl (42fr) per cubic meter of air and 0.5 milligram chloro diphenyl (54f,r I per cubic rtetCT of air.1 This is based on the results of The Caeiaiitu* with# M iektwwbdft tbs pf^parati* W it* nadicM informxtinn wciim ml tk Gxid* b* tlx Ic(iu!(fLsl HtfKM sad ciiiieji TaairelocT Citt of I. M. A., Mtd to ackuoolrdn W tb oviuaoc* of Efaer P. Wb*Wr and Jack T. Garrett ta lb of tba Guide. chronic animal inhalation studies.1 B. Short exposure tolerance : Ten mg of a diphenyl of unspecified chlorine content per cubic meter of air has been reported as unbearably irritating.4 C. Atmospheric concentration immedi ately hazardous to life: Not known for man. irritation of the eyes, nose and throat a: levels which have not caused acute illness preclude the likeli hood of voluntary exposure to immedi ately hazardous concenu ations. ADM 005640 WATER PCB-SD0000030879 Jinuary.prbruary, 1965 II. Totie Properties . A. Inhalation: Experiments with ehloro- dipltenvl (42% chlorine! wxre run at concentrations of 8.6 fit;/liter and at . 6.83 pg/litcr of air. Cats. mice, rabbits and rats were unalTertcd by the higher level while guinea pigs showed poor growth after seventeen 7-hour/day ex posures over 24 days. Eightv-four 7hour/day exposures at the tower con centration had essentially no effect on similar species of animals.1 In the case of chlorodiphenyl (54% chlorine! eightv-three 7-hour/day ex posures over 121 days to a concentra tion of 5.4 ng/liter resulted in injury to liver cells and increased liver weights in rats. At a concentration of 1.5 ^g/Iiter for one hundred and fifty 7-hour/day exposures over 213 days, the rats showed distinct microscopic changes in the liver.' The literature contains many refer ences to the potential toxic effects of chlorinated diphenyls in man and ani mals. The early work included investi gations of chlorinated naphthalenes, chlorinated diphenyls, chlorinated diphenyl oxide and various mixtures of these. An early report indicated serious toxic effects from chlorodiphenyl chlori nated to the extent of 65%.' A later report by the principal author properly identified the earlier sample as a mix ture of chlorinated diphenyl and chlori nated diphenyl benzene.* However, only a few authors of subsequent papers, bul letins or textbooks have noted this cor rection and the original data are cited repeatedly as relating to chlorinated diphenyl alone. B. Skin contact: Both compounds are readily absorbed through the clipped, intact skin of rabbits. The minimum lethal dose when tlse undiluted mate rials were applied to the covered clipped, intact skin of rabbits for 24 hours was approximately 1.0 gm/kg for the 42% chlorinated and 1.5 gm/kg for the 54% chlorinated.' Local .xtion on the skin is similar to that of common organic solvents where contact leads to removal of natural fats and oils with subsequent drying and cracking of the skin. ' Human cases of cltloracnc have not been reported from the use of these two specific chlorodiphenyl*. The potential undoubtedly exists because of cases which were reported from the use of chlorodiphenyl with a higher chlorine content and from mixtures with other chlorinated aromatic compounds.* *-* C. Eve contact: The liquid products and their vapors are moderately irritating to eye tissues. ' D. Ingestion: The acute oral toxicities of the undiluted compounds arc not great as evidenced by oral LDw`s in rats of approximately 8.65 gm (7.61 to 9.78 gm! per kilogram for the 42% chlori nated and 11.9 gm (10.48 to 13.45 em' per kilogram for the 54% chlorinated.' Central atrophy of the liver appears to be the chief toxic effect. III. Industrial Hygiene Practice A. Industrial uses: The chlorodiphenvls are used as dielectrics for condensers.^ capacitors and transformers, plasticizers:. in synthetic resins, in emulsion adhes- ' iv, as nonflammable hydraulic fluids and as transfer media. * B. Evalvation or exposures: ' 1. Air sampling and analysis: a. Direct field methods: None b. Laboratory methods: . (1) Collect in secondary butyl alcohol in fritted bubbler or two large impingers in series; concentrate sample and complete analysis by one of various methods for chlo rinated hydrocarbons.* (2) Sample air through combuition furnace, collect chloride ion from decom posed chlorodiphenyl in suitable alkaline solution and determine chloride ion con centration.' C. Hazards and their recommended control: 1. Inhalation: Absorption is chiefly by inlialation. Concentrations in the workroom atmosphere should be maintained below the recommended levels. Where the chlorinated diphenyls are used at room tempera- ( c c c c o o ADM 00 5 8A 1 WATER PCB-SD0000030880 o o o o o o o o o Janua ry-Fcb ruary, 1965 . turn, the hazard of inhalation is considered slight or absent. When these . materials are subjected to elevated temperatures, the process either should be completely enclosed or other adequate mechanical ex haust ventilation must be provided to reduce concentrations to safe levels. In heat transfer media appli cations, the system must be designed and constructed so that it is leak proof. Special gasket materials and pump seals are available to present leakage. The reservoir tank should be airtight except for a vent to the outdoors. In tire event of spills or leaks of hot fluids, use chemical cartridge respirators or eas masks approved by the U. S. Bureau of Mines for protection against organic vapors. These will preside good protection up to the concentrations shown on the approval labels and the odor will give ample warning if it comes through the device. 2. Skin contact: Operations and handl ing procedures should be such as to avoid the possibility of prolonged or repeated skin contact. Contaminated clothing must be laundered before reuse. 3. Eye contact: Eye protection should be used where there is a possibility* of liquid splashes. 4. Ingestion: Ingestion of these mate rials is not a problem in industry. 5. Fire and explosion: The chlorodiphenyls are fire-resistant or essenti ally nonflammable liquids. When exposed to flame or hot surfaces they may decompose to form CO, GOg, HC1, phenolic and aldehydes depending on the temperature, avail ability of oxygen, area of the heated surface, rate of application of the liquid to the surface and other variable*. IV. Medical Information A. Emergency treatsient: Skin surfaces exposed to chlorodiphenyls should be thoroughly washed with soap and water at once. If clothing has been contami nated it should be removed promptly. If exposure to a high vapor concen tration occurs, as in the case of spills at elevated temperatures, the patient should be moved from exposure and kept at rest until seen by a physician. Oxygen should be administered if breathing is difficult. Eyes contaminated with chlorodiphenyl should be irrigated with water for at least 15 minutes and the patient should be seen by a physician. Depend ing on the amount of inflammation and pain present, drugs like Cortispoiin1 ointment and topical Pontocainc15 mav be indicated. B. Special procedures: Persons who are regularly or rr|>vaicdly exposed to chlorodiphenyls should be examined periodi cally to detect early evidence of skin irritation and /'or liver damage. Persons with known liver disease should not be exposed to repeated contact with the chlorodiphenyls. V. RefertncM 1. Monsanto Company, Organic Chemi cals Division: Tech. Bulletin # PL-386, Aroclor Plasticizers (Dec. I960). ' 2. American Conference of Governmental Industrial Hygienists: Threshold Limit Values for 1964. .4.W.4 Arch. Environ. Health 9: 545 (1964>. 3. Treon, J. F., F. P. Cleveland. J. Cappel, and R. W. Atchley: The Toxicity of the Vapors of Aroclor 1242 and Aroclor 1254. Amer. Ini. Hvg. Assoc. Quart. 17: m (1956N. ` 4. Elkins, H. B.: The Chemistry of Indus trial Toxicology. John WUev and Sons, Inc., New York (19591. ' 5. Drinker. C. K., M. F. Warren, and G. A. Bennet: The Problem of Possible Systemic Effects from Certain Chlori nated Hydrocarbons. /. Ind. Hvg. Tox icol. 19: 283 (19371. ' 6. Drinker, C. K.: Further Observations on the Possible Systemic Toxicity of Certain of the Chlorinated Hydrocar bons. /. Ind. Hyg. Toxicol. 21: 155 (1939). _ 7. Wheeler, E. P.: Personal Communica tion, Monsanto Company, St. I^suis, Missouri 63166. 8. Greenburg, L., M. R. Mayen, and A. R. Smith: The Systemic Effects Result ing from Exposure to Certain Chlori nated Hydrocarbons. J. Ind. Hyg. Toxicol. 21: 29 (1939). . O 6 WATER PCB-SD0000030881 HYGIENIC GUIDES COMMITTEE C. P. CxiHSTit, Chaitmm N. E. Bolton' E. E. Campiell |. W. Clayton H. B. Elkin* P. D. Halley Mark Hrre J. A. Houohtox D. R. McFee J. M. McNciney, Ja. J. E. PeteesonJ. B. OuSMNIPfKI E. A. PrtTtEi U. C. PoEEAMt R- L. Raleick W. L Sutton R. C. Wand* G. L Wilson Hygienic Guide sheets may be obtained from the American industrial kyoiene assocla- tion. 14125 Prevoit. Detroit 27. Michigan, at 25 cents each for two-page reprint!: JO cents each for four-page reprinu. All orders for lets than 12.00 must be prepaid. Discount of 2054 on orders of five or more Guides: 4054 discount on orders of 100 or mere Guides. Special looseleaf binders for the Guides may also be ordered from the Association office (or $1.25 each. ( c c c o o o 4DM nn^Rti WATER_PCB-SD0000030882 Monsanto MontiMo C<n,.ny 00 N. Stlouii. MJ.io.H Ml# Phono; 0(4) 6B4-K>00 TOXICITY AND SAFE HANDLING OP ASKAREL On the basis of animal toxicity studies, the Askarels may be considered only slightly toxic from the stand point of accidental ingestion or a single accidental massive skin exposure. Similarly, single exposures to high concentrations of vapors (when heated suffi ciently to volatilize) or high concentrations of decom position products (if the fluid is accidentally discharged into the fire chamber) are not serious hazards because the irritating character of such concentrations preclude voluntary exposure. Repeated or prolonged skin exposure should be avoided since the Askarel fluids act as solvents for fats and oils of the skin. Removal of these natural, protective barriers can lead to drying and chapping such as oocurs with exposures to paint thlnners* More Important, the fluid may be absorbed if It Is allowed to remain on the unbroken skin. For these reasons, we recommend that the skin be washed with soap and water if there Is con tact. A skin burn resulting from accidental contact with hot fluid should be treated in the normal manner for any thermal burn due to hot oils. Because of low vapor pressure, there if no significant vapor inhalation hazard when an Askarel fluid is at room temperature. For example, there is no vapor exposure problem while transferring the fluid from its shipping container to the using equipment. On the other hand, .the vapors emitted by Askarels heated to elevated tem peratures are injurious on prolonged or repeated expo sure. The "Threshold Limit Value" or atmospheric vapor concentration which cannot be safely exceeded (on a daily basis) la 0.5 - 1.0 milligrams of Askarel vapor per cubio meter of air In the workroom. March 4, 1971 R. Emmet Kelly, M. D. Medical Director WATER_PCB-SD0000030883 Monsanto EUROPE 8.A. PROM : ^ Brussels, Belgium tMAMk 4 LOCATION* DATE ; February 22, 1967 SUBJECT : RFFERENCE : TO : DW Dr. R. Emmet Kelly St. Louis CC : J.R. Buchanan, St Louis J.E. Filer, Brussels D.V. Hardy, MCL Eugene Wilde, St Louis Dear Dr. Kelly, I should like to refer to your letter dated the 10th of February and our telephone discussion of yesterday's date. I enclose a copy of Sttren Jensen's original paper' which in fact was presented in English - Dr. Jensen apologises for the typing etc. but this copy is taken from his original paper which has not yet been re-typed and tidied up. I asked our agent in Sweden to dig out the various pieces of information that you required and I attach a copy of his reply dated February 17th which I think fully covers the point raised in your letter. If there areany small points outstanding, please let me know and I will try to get you further information. I am sending the only copy of Mr. Jensen's paper to you and therefore if any of the other recipients of this letter needs to have access, they can take a copy from yourself. I would however emphasize the post script on page 3 of Ola Palm's letter in which he states Mr. Jensen has consented to send us the full copy of his paper on the understanding that this is used only internally within the Monsanto organization. 1 DEPOSITION | EXHIBIT | 3a 1 NEV 023647 M-3 WATER PCB-SD0000030884 Q f CfUsu, . ^ ! I l Mr Chairman, ladle and go)"ntil<eCnen, In honor to our Brlttieh boot X will try to hold thlo lecture In Sngllob. ' ii tho tltlo of thlo lecture etateo, X an today going to toll about tho dlooorory of sobo hitherto unobserved ohlorlnatod hydrocarbons haring up to eight ohlorlno In the Molooulo and found In residue aaa- lycle. She ehonlool nano of polychlorinated blfonylo ( In tho following oailed BOB), So got familiar with PCS X will ot&rt with tbo choclotry and -tozlcologl. Chonlatry Sh 5.U V V Sho naln oharaotoriotlo of PCB It 1. Thefr Tory high otablllty. i.o an ozeaple thoy oon bo bollod with nltrln aold without being destroyed. 2. Thoy are hardly notabollood In llring orgenlan. J* if noro than 4 ohlorlno are pro^aent they are non Inflcmablo. It le clear that those throe ohoraoterlatloa dote It easy to understand that when they havo entered the living organlen. the will hare a low pereletonoe . But it Is difficult to explain how they find their way Into the living organics. One thing aeons to be dear, they don't oobo froa agricultural uoa, but froa a teohnlcal one and Boat probable It ftomoe to the nature via waetoe that are tried to bo burnt up, beoauoe then we have thou at once In tho air, beoaust of their non lnflaaabillty. .gozloolo,d A NEV 106549 The PCB woro introduced in 1929 and ae early 1936 Jonee and Aldon reported that 23 out of 24 non employed in nanufacturlng of PCB cuffcrod fron an neno fora oraptlon of tho akin, lone did not nppoer until 6 to 8 monthe after tho material wae firot uood. In 1937 Drinker roportod that rate oxpoetd to ohlorlnatod biphenyle In concentration of approxlaately 1 ng/n^* for 16 hours a day for 6 wooke ohov/dd damage of tho livor. i After that tine the allowed ooneontratlon of PCB in air lo 0,5 ag/t^. , (Por PDt tho eoae value le 0.9 - 1 Bg/m*). Tho naao authore flniohcd ' tholr experinenta In 1938, and related that thooo oonpounde have an Injourlouo offoot, nonlfoetod solely In tho liver. Ohlorlnatod bipohnyio! ^ appeared to bo tho noot lnjourioue ohlorlnatod oonpounde of all tested, ( * WATER PCB-SD0000030885 o o 2. \ t Orenburg, Mayor ond Smith 1939 reported that PCB and polychlorinated naphtoloaos arc blamed for the death of three young workers,. and that" pregnant women and person* who hav* at any tine had any liver dlocaooo aro particularly suspeotible. ' ftdal, Haller and Benton gave 1942 animals PCB including odminiotrotion ! j j j I by inhalation, ingootlon and akin aboorbtlon. ilietologioal examination or tho viscera ehowed important toxic afreet only in the ok in and llvor, and the dogenoratlon effects in the liver aro eeacntially the ooae whatever woe the method for the administration. Paribok (1955/ found as an occupational poison in th# eloctrioal industry, mixed tetra and ponta cbloroblphenyl oaueoa follieulitie, comedo, pyodermia and othar skin affeotione, and that lte principal toxio affeot is fatty degeneration of tbs llvor. Miller (1944) injected 69 g BCB (4 and 5 chlorine) aubcontancouely in 52 gulnoa pigs. Eight to ton days after injection, fat droplets trero noted in the liver eelle, and after 16 dayo they were present in moderu.c or very large numbers. Babbits end rats were also teste*d. in this inrvootl- gstion, as well as the PCB was adminlstated both continouely, subcontlaously or ingested in tho food. In "the feeding experiment 6 guinea pigs received 2 doses of 69 mg of tho chlorinated biphenyl 1 week apart. Death occurred in 11 to 29 dayo. finally Mo Baughlln 1964 reported a method to teot the chemical toxicity and teratogonio effaot by injection into the yolk aac of fertile egge ; ' j : j I j J ! j i : | prior to Incubation. PCB was found between the eight compounds among 100 tested having the highest order of toxicity. Ho hatch was found st a level of 25 mg p egg. At a level of 10 mg per egg, one chick hatched | j j out of 20 Injected eggs, but died 2 days later. Some embryos which wore j examined after they died, ohowed weak deformities (ofton a short upper brak); and growth retardation. Dead aeetate resulted aa an example in no hatch . < t a lavol of 1 ag per egg. Autopsy of ths dead aabyos hove showed exton ! aivo brain damage. Uercurio chloride showed no hatch even at a level of ; 0,5 mg per egg. As ths analytical chemistry is a pronounoad service science I have boon in contact with many solantiats from other fields during tho work with residue analysis, and X have always found this contact very stimulating for my own work. This oo-opcratlon often demands that we are talking the same scientific language. Because of this need 1 will today try to give a looture in low level analytical ohomiotry for biologioto, illustrated by tho residue analyolo of polychlorinated biphenyls. The lecture will be divided in the following throe eub-divioionsi . -------- ---------- ------- NEV 106550 WATER PCB-SD0000030886 o o3 1. Chemistry of FOB and their toxicology. 2. Analytical Method a for residue analysis end proof of etructuroo. 5. Behaviour of BOB in nature, differenciee in metabolising rato of the FOB components, potenoatlon in an ecological oerie, con centration levels and exonplea of aample* which have been provod to oon- . tain FCB. A sesidue analysis can be dlvidod ini ' 1 Extraction of the pesticides from the biological material, * followed by a careful oleanlng-up to take away lnterforring substances, moat often fata. t 2. Identification onolyels by mean of gas chromatography. Thln- ,, layer ohronatography and maas spectrometry. J. Quantitative analyeia. , . At on ecological laboratory in Biksmusdet in Stockholm 1-2 g of a sample is out out of the biological material and transferred into a welgbod and carefully cleaned test tube, and stored at -20 until analysis. Smaller samples hav# been used, min. 5 mg of body fat, and with dry materials such as hair, featbsrs, pins needles 100 mg are sufficient to reach the desired 10 nj/g level in residue analysis. In oases of water proofs 1 1. is used for reaching the 10 pg/g. level. B.l(homog) In order to facilitate complete extraction of the fatty materials from the biological sample, the doulbe amount of finely powdered anhydrous magnesium sulphate is added to the sampling tube, and the whole is homo genised with an lnsertable homogeniser. The resulting powder le transferred into a apodal Soxhlet oxtractor. After 4 hours of extraction the solvent is svsporatsd, leaving the fat in a small weighed test tube at the bottom *Sox.-tubs) of the extractor. This fat is dissolved in methylene chloride in such a .way that 100 ul (o,1 ml) contain 20 mg of fat. The 100 ul solution is now transferred to a little object glass, 3x7 cm, covered with a sllieagel layer 1 ma thick, in order to form a line 0,7 cm from one end of the slide. Inserting this thin-layer plate into a vessel the bottom of which le eovtred by a few mm of methylene Chloride, tho advent will be sucked up in the dry layer of eillcagel, and at least reach the upper end of the plate. The fact is that the fat bee a grantor affinity to the powder on the plate than the chlorinated hydrocarbon have. - and we get a separation. The fat being more polar than tho chlorinated hydrocarbons will never go longor than 2 cm before thi NEV 106551 WATER PCB-SD0000030887 * o' o 4* \ f BwraiotJ tuba 5 6 ge eolvont roachos the upper part of the glass. Tho front of the fat eppoara q.uite visible agai.net a lamp, and with tho aid of a rasor blade tho sone above the fat la transferred to the elution tuba and tha chlorlnatad biooldoe absorbed on the ponder ean non be luted by one Bl of ether. Tho conoentratlon la auffiolant for detootioh of the chlorinated hydrocarbons down to the 10""*^ g level. Tho next atop in tho analytical procedure cencerne the f.aparatt.v.i At tii* different chlorlnatod hydrocarbonu that the one.pi % */ Bnttor of foot) this ie a troubleoone task. It ie easy to estimate vhtt lo not pro sent, but more difficult to aay exactly one la prsaent. Tt cuffor from tha negative demonstration, aa will be ehown lator. At first a few worda about the separation of the oonpononte proaont In the aaapla and their visualisation. The separation la accompliehod by mm of a gas chromatograph fitted to a detector that transfers lta Inpulee to a recorder. The ayeten la shortly dosoribsdt A spirally fernod glaaa tube with an Innor diameter of 2 aa and about 2 a In length la filled up by a support, covered with an thin layer of an oil. The tube la heated In tha chromatograph to about 200. Through the tube a otream of nitrogen eontlnoualy follows. Whan about 10 ul (l/lOO of 1 Bl) of the purified sample la Injected Into tha tube, the components of tbs aaapla will be evaporieed and go forward through the column with the gas atreaa. Aa tha constituents have different affinity to tha column filling thoy dll pase tha column with different apeod and It will tako different tine for then to roach tho detoctor at tho other end of the glaea tuba. If the temperature and tha nitrogen flow nro held constant thia time, tho retention time, haa a spoelflcvalue for a certain compound. This is true, but unfortunately It is also a fact that two componenta ocn have tha aamo retention time. This la one of the bigger problems In gaa ohromatographio analysis of unknown samples, as will aoon be obvious. * To make it possible to ostlmato tho ratontlon time it la naoaaaary to Visualise tho chlorlnatod hydrocarbons. Tor that purpoao Bore or loss paoiflo deteetora are uaad. Tho dotootor most often uaod in postieldo amalyaia is tha so eailed oloctron capture detector, which can detect down to one ploogram ( g of llndon). Unfortunately thia detector ie not specific for chlorine, bu givea answer also for oxygonoontaining compounda. The response hers la muo^i lowor but can be eountorbalancod if the concen tration of tho oxygon containing la much higher. The principle for tho oloctron capture dotootor lb shortly* At the end of tho gao chromatographic tube is plaood a little tub con taining a foil mad# of titanium tritldo. This la ap-radiant. The p- NEV 106552 WATER PCB-SD0000030888 o o5 particles aro Mooting with the nitrogen molecules coming iron the column, then we get 4 -- " * Mg. Over the dctoctor we hove m tension of 90 volt and by mean of the electrons wo will got constant electrical eurront over the detector. This standing current, le transferred to a on-nY recordor as a oonotant baseline, then now a chlorinated hydrocarbon leaveo the column this compound hoc a high affinity to the oloetrono and this means that the amount of olootrons will diminish, and they will diminish proportionally to the amount of ohlorine. Tho electrical current will also diminish and this is noted as a peak on the recorder. Tho area of the peak will be proportional to the amount of substance in the sample. By mean of a standard injection it is now possible to compare the reten- tlon time and the area of an unknown component with the retention tine and area of the known standard. As said before this detector is not speci fic for ohlrine but anyhow very useful, because of its high sensitivity. The eyetem described has, as w* have seen, two disadvantages: t. Two different compounde oen have the name retention time and bo detected ae one peak. 2, A regietrated peak does not need to be chlorinated , becauoo the detector is not specific. If the sample is injected In two different columns with different chemical properties we have increased the chance for a good separation. I S' two compounds have the same retention time on one column they may not have it on another. When a result seemo doubtful, - if the compound being responsible for a certain peak contains chlorine or not - it le possible to eoneentrate the sample and analyse it on a less sensitive detector such as the nlcroclouaetrle one, which is specific for ohlorine. The compound ia burned in a furnace and teh generated chlorine titrated directly. ' As is seen from the two last mentioned possibilities it is anyhow poooible ,to get a rather high degree of certainty in residue analysis, but it is rather tlme-consumelng work.When using this method just described, we very Often found that many chromatograms from residua analysis of most oarefully purified samples still contain a large number of peaks. Uspy of these have retention times that do not agree with any known chlorinated pesticides, or their metabolites. This chromatogram eon serve ae an example. It was obtained by reddue analysis of a eea-eagle found dead in the archipelago of Stockholm. In the range of the known peaks, there are eo many unidentified that there elco must be an obvious risk of the .. known peaks to be covered by unknown nor.. If this remark io found true, the reported reoulto of many previous quan- NEV 106553 WATER PCB-SD0000030889 6 oo titablve analyais must be brought into question. In the procent investi gation it le shown that moot of the unknown peak of chromatograms at residue analysis of chlorinated peetioidos or# due to polychlorinated biphenyls. I will show s chromatogram of human fat analysed on a ao colled Sk 96 column| the moat often used type in pesticide analyses. Early retention time a woro in agreoaont with DI), DPTop and PPTpp. Hoxt elide ohowo tho same sample analyeod on a QK-1 column. Now the former 2 PBX peoko havo divided into 4 peaks,and two of them are still in agreement with Dyjpp ' and op.t the two new were unknown. logically, these unknown components were at first thought to be metabolites of tho insecticides. Against that spoke that nelgther treatment nor . concentrated sulfuric aold in other. This treatment made It rather euro that the compounds did not contain osygen. In Sweden residues of organic mo* eury have been investigated rather intensively in the Swedish fauna. As these compounds give very high responses to the electron capture detec tor it woe also Investigated if the unknown peoko could hove a mercuric origin. It was found that tho water-ecological series.had .high residues of both meroury (Weotermaxk.Johnelo) and the unknown ones, when the o&ae indivi duals wore analysed. Anyhow, the pheasant suffering moot from mercury poisoning only contained low levels of electron capturing compounds and these belonged to the normal insecticides. Therefore the unknown could hardly be mercu rials or metabolites of then. As the eagle aample giving the chromatogram shorn in fig. 10. could be aetlmoted to contain KPT and DDE up to 13 g/kg in extractable fat, the amount of unknown compounds also were suggested to be in the same range, and tehn sufficiently high to do a run on the combined gas chromatograph mass spectrometer. If this oould be dons successfully it would be possible ' to get very important informations about the chemical nature of the unknown, for ex. the molekular weight numbers of chlorine etc. This method is up to now the method giving the highest degree of certainty in the low level analytical chemistry, amounte of 100 ng substance being enough. As this method for identification of totally unknown residues surely will be very important in the future (when f,ex. a biologist has found that fishes in a river die) it mayb$oasible by mean of this method to find out exactly what compoundo are responsible for the death. For this reason, I will go into cone details with this method. In tho actual case we took the extract from 20 mg eagle and concentrated NEV 106554 WATER PCB-SD0000030890 < I It as aueh as possible and Bade an injection on the gas chromatograph I eoabinod with the mass apectroneter* The result was the chromatogram j shown on tho next slide* Every timo the recordor showed that a compound | is loaving the column, the sffluont is lod to the mass spsctromotor. Mon j just a fow words about the boss apse. i ! Tho Boleoules leaving the column are bonded with electrons at Z. t/o have ! now got tho molocule positive charged, but with tho some mass as before. ; This M4 la aeoolerated in a vacuum sad will tbon get a kinetic snorgi. . . where la the spood. Noxt eomos the mognstlc field that . I tries to bead the direction of the molecule. This will be big for a small soleoule and less for i ; If ws have a slove in the other end we con directly read the molecular weight. Added to this parent molecule M4 we will aloo get addition in ; formations, because of tho fact that U+ may not be etbble, a part of 1 ! , them will be broken down before they reach tho sieve in the other end. ! F,"* M DDT U WS - OCIj ' Mass spectrograms from ths different unknown peaks in the eagle sample ao j shown. The mass numbers equal to the molecular weights of the unkuowno , could be read to 426,392, 358, 324. Astonishingly, ths molecular diffeI rencea were constantly 34 mass units. This difference shows a fomilcrity : in origin of the unknown. How the fact ia that chlorine exelsts ea a j mixture of two isotopes with atom weights 35 and 37 in proportion 75 25. If , ( the moleouls has one chlorine, this will give two moleoule peaks, one for . Cl., and one for 01-,,. If there are two chlorine we have the possibility f // P I : of one with only Olj^, one with both C1^ and 37 and one with 2 Cl^ and ! therefore i NEV 106555 WATER_PCB-SD0000030891 e oo Tho rotation of tho ponko found on tho different mono opec woro: Molecular weight 324 358 392 426 Ohlorino eontont 5 . -6 .. 7. _ 8 An explanation of the familiarity of the compounds can be giron if one substance la built from the former by substituting a hydrogen with ohlorino IK H* 01, 801 HC1 u\ 34 Then it la possibla to calculate tho molecular weight of the parent hydrocarbon PHC. Mpjjp m M - x + X Mjj , where U la tho aoleoulor weight of the oonponont having x ohlorino atoms. P.ex. for m 426 and 8 Cl we will get K?He . 426 - 280 + 8 * 154 and equal with tho other molokyla. The aoat probable formula with carbon and hydrogen giving this molecular weight is C^2 H,0 and this can only be satlofled when the paront-hydro- carboa la biphenyl, and the unknown being polychlorinated biphenyls. This explanation was later fully verified by injection of a synthetic PBC on the mass spec. furthermore extensive gas ehromatographio investigations proved that the TOO standard gave peaks with the oame retention time as the unknown peaks from the sea eagle. With the method just described 2 suppose that we have a new possibility to atudy the residues in the air because the pine needles can allweys bo . We have had great difficult; in quantifying the PCB, but when getting a little more time it will be possible. We have done a few calculations on a few apeolee, and I suppose they are right within a factor 2. We have found the residue to be from It baa been my statement here to-day to present this method for studies of defiling of the nature, and with this method a new typo of defiling agents baa been found to be present in nature, and a few experiment have shown where'they may be found. How this method la going to be uood in the first hadn to aatiBato how the situation is in nature as a whole, and in the other hand to find tho leaks throug which they find its way to nature. 8oea maybe are present here today to get news about the leaks, and to then I want to ony come back in a year. NEV 106556 WATER PCB-SD0000030892 9. OO 80 much I think Z ean soy again that the FOB hardly can como from agriculture. As support for this suggeotion 1 con say that we have found PCB in oaglo foathcro iron Bikomueoot from 19441 where hardly any ehlorinstod posticides were used in sgrloultrue. On moro thing that 1 find important to soy is that in contrast to the mercury problcn this dooo not aoom to bo a pur Swedish problem. I have Just studied ehronatograno tokon from tendon air, and they cloorly oontoin PCB, and dr. Boldon bao told mo that ho alao find them in hie fiohsomploa. But finally in waiting at moro results I-ishould liko to pointH$@ morething. It is provod that x>c: oomos to nsturo, wo dont bnow how whero they ars usod, but they are vory pereistant to ohemicale and to fire. I think the poison Jury should try to state that a oontent of POB eholl always be found in an open declara tion. NEV 106557 WATER PCB-SD0000030893 WATER PCB-SD0000030894 o%a# % 6 VQ>, % < % $ tv *M V V) *) <5 V N N X, ? is Mn 2o o NEV 106559 WATER PCB-SD0000030895 WATER PCB-SD0000030896 Curve I *Q Curve 2 Curve 3 Curve * %N > *^ S %% *H \ % NEV 106561 WATER PCB-SD0000030897 WATER PCB-SD0000030898 lo I? k %1 $ x> $ n CMtlui d i 5 --C-tww &- & S * * e> t >o * <f NEV 106563 J/VVOA//7 WATER_PCB-SD0000030899 o 'o / NEV 106564 4;) WATER PCB-SD0000030900 WATER PCB-SD0000030901 WATER PCB-SD0000030902 NEW 1 0 6 5 6 8 WATER PCB-SD0000030903 ! % & NEV 106569 WATER PCB-SD0000030904 o s y t-'vyJo/? *is *\ j \ =5 k / J V It IN i\l ] $ $ S & 8 O* $ ft . ' * * ^TO ^Ofc WATER PCB-SD0000030905 NEV 106571 WATER PCB-SD0000030906 i o 6 ii i ^ "g 5> $ i ;l - S i S <T g' NEV 106572 WATER PCB-SD0000030907 oo { NEV 106573 WATER PCB-SD0000030908 o e^. o 3 | o < Vi* X ft 5$ ** ft t I i i iI II NEV 106574 \ WATER PCB-SD0000030909 Monsanto ......,*-6 f E, E, Wheeler - St, Louis 4 September 11* 1968 rp CCl Dr. H. E. Kelly Pr..^.Scott Tucker proposed Protocols for ^?gbl.pry^rox 1 c 1 ty Hr. R. "KelTerl Studies at Industrial lo-Test Lab. c'i*c*cr . .. ^Mr'ii'^Cummlng Pa ton -- TO : Dr. W. R. Richard. Attached Is a copy of a letter from Industrial Bio-Test and proposed protocols for Aroclor toxicity studies. This arrives Just as I am leaving for two weeks. I will take this material with me and if possible send you my comments before the end of next week. If it appears desirable to have a session with Dr. Kelly and Bill Hunt to discuss this matter before I return* I am sure Dr. Kelly will be happy to see you. ' EPW:cjs Wheeler , 72 30 ** o tv . (1 DEPOSITION I 1 sr NEV 167288 WATER PCB-SD0000030910 SududhMl DIO -TEST XoiQiaj&ueh Snc. 1610 FRONTAGE ROAD NORTHBROOK* ILLINOIS 60062 aria coat nt mr^HONt m-ioio September 9, 1968 Mr. Elmer P, Wheeler Monsanto Company 800 N. Lindbergh Blvd. * " St* Louie* Missouri 68166 1 1* * Dear Mr. Wheeler: ' .* . . * t. I am submitting a collection of protocols for studies with Aroclors,. * The studies proposed, with prices, are as follows: z 1 %t S ` X. Rat Tissue Study a Aroolor 1 2 levels . Aroclor XI 2 levels Aroclor HI 2 levels Toxa'phene 2 levels ' Controls Total ' * $2,700 Additional reference materials could be Included for $600 per material (2 levels). This price is exclusive of analyses. If you choose for us to do all or part of the analytical work, we could work on a cost plus basis or we could pro vide ybu with'a quotation after we have run through the method. We found no really useful information In our scan of the literature on the metabolism of chlorinated pesticides, I feel that we can get much informa tion from analysis for tissue residues and from study of urine and feces collected from treated animals. It Is not possible to quote for such studies In the absence of fore-knowledge of findings. This could be set up on a cost plus basis with provision to review after the expenditure of a defined sum. One should be able to at least define the problem on a budget of $5,000. NEV 162002 WATER PCB-SD0000030911 Mr. Elmer P, Wheeler September 9 1968 Page 2 - %. n. Chicken Toxicitv. Reproduction and Meat and Egg Residue Study Three Aroclors with common controls Exclusive of`aitn*?al*ytical costs $15,000 m. Mallard Duck Study-- Three Aroclors .with common controls^ _ Exclusive of. analytical jsosts IV. 3-Generation Reproduction Study in Rats Three Aroclors with common controls 0 V. 2-Year Chronic Toxicity Study in Rats Three Aroclors with common controls VI. 2-Year Chronic Toxicity Study in Dogs Throe Aroclors with common controls $5,000 . ' % $35,ooo '; * V 4a' \** * "4 ' - I'. $57,500. ' ` ' *4 v .f -r' $85,000 ' vii. Subacute Fish Toxicity Study e We have not done such a study but we have built one apparatus which allows investigation of as many as five concentrations of one material plus controls simultaneously for extended periods of time, starting with fingeriings and continuing through a reproduction cycle it this is desired. ' '. If one wanted only to measure the accumulation of test materials over a 90-day period, the cost,' using 5 concentrations * would be ap .. proxlmately $1,500 p6r species for one material, exclusive of analyses. Extending the study through a reproduction cycle would cost an addition . al $3,500. . In any of those studies, material (urine, feces or tissues) could be retained for analysis to determine species differences relative to accumulation and metabolism. . '' NEV 162003 WATER PCB-SD0000030912 o M r. Elmer P. Wheeler o September 9 1968 Page 3 The cumulative cost of the defined studies, exclusive of analytical costs and fish studies, amounts to $200,200. ' As Dr: Calandra has told you,' billings could be arranged to accommodate to your budgetary needs. ------------- .Your comments on this program will be welcome and-should further per-r son^l discussions seem desirable, we will be glad to meet with you either here or in St, DouisJ . ** . Sincerely yours, P4^.t.n Otis E, Fancher, Ph. D. Director It *M - -r OEFsBMS enc* * % . NEV 16200% WATER PCB-SD0000030913 9*idu4bioJ' BIO - TEST Ja&(HaUJue4>, Snc. 1810 FRONTAGE ROAD . .NORTHBROOK, ILLINOIS 60062 . AM A COOK Hi ' mtAMONl 1TI-I010 . PROTOCOLS FOR . MONSANTO COMPANY '* ` AROCLOR STUDIES ' NEW 1%34?2 WATER PCB-SD0000030914 $ndnlUial BlO-1 E S T ItoteUvud-, Site. PROTOCOL. FOR , MONSANTO COMPANY . , A TISSUE`RESIDUE STUDY IN ALBINO RATS '. . WITH AROCLORS 1. Outline of Experiment . A. Type and Length: Tissue Residue Study; duration 30 days B, Animal Species Tested; Male Albino Rats (approximately 100 g) C. Organization of Groups; '' Group Number of Animals Male Female Dietary Concentration in ppm Control ` 1 n 15 15 ' 15 . ' ; '1515 . 15 . None . . . Low.dose level ' High dose level D. Test Material Administration . ' ' Diets will be prepared fresh weekly by mixing the calculated quantity of test material with a standard pulverized rat ration. Food will be allowed ad libitum. : . .II. II. Parameters to be Studied ` ' - '. . A. Feed Consumption ' ' ' Feed consumption will be determined weekly for each animal. Reactions . ' ' . Observations for untoward behavioral reactions will be made. '. NEV 143473 t WATER PCB-SD0000030915 B 1 O - T E S T " ImaioAM, Hhc. 2 C; Gross Pathology ' . Upon sacrifice, organs and tissues will be examined grossly for pathologic alterations. _ # *o ' _' . HI. Sample Collection At the end of 30 days all animals will be sacrificed and samples of muscle, fat, liver and kidney will bet taken from each animal, Samples of each tissue from each animal will be frozen and will either be shipped to Monsanto for analysis or analyses will be done by Bio-Test. OEFiDMS 9-9-68 NEV 14347% WATER PCB-SD0000030916 SnduiUial BI0-1EST *-/io^aioAicS, Pttc, PROTOCOL, FOR . MONSANTO COMPANY * ' CHICKEN TOXICITY, REPRODUCTION AND RESIDUE STUDY ON AROGLOR . s'. The object of the study will be to investigate the general toxic effects of the test material on young adult male and female chickens with special emphasis upon hatchability of eggs and viability of offspring. In addition, ' samples of meat and eggs will be analysed for test material residues (either by Monsanto or by Bio-Test). . Sixteen male and 80 female 12-week old white Leghorn chickens will be selected'for the study. These animals will be equally-divided into one control and three test groups. The three test groups will correspond to graded dietary levels of the test material. Dosing will begin immediately and will continue through the egg collection period. . . The chickens in the control and test groups will be weighed weekly and observations for mortality, reactions and general food disappearance . will be made periodically during the study. ' _ As each group begins laying (at 17 to .18 weeks of age), the eggs will . be collected daily and egg weights recorded. When the egg weights are consistently between 50 and 60 grams, and at least 20 per cent of the hens are laying, the daily egg production will be collected and placed in an ' incubator tray. Egg collection will be continued for 28 days from collection NEV 143475 " ' .' WATER PCB-SD0000030917 B I o - T E S Y tMaiMiai, Sue, 2 Day One or until at least 100 eggs per group are available for hatching. 0 During the storage period (not to exceed live days lor any group ol eggs), the eggs will be turned twice daily. The eggs will be placed in an incubator maintained at 99 to 100F with a wet bulb reading of 85F. The egg production lor an additional week will be collected lor analysis. Total egg production and egg weights will be recorded. At the end of the egg collection period, one-half of the chickens in each group will be sacrificed, defeathered and quick-frozen. The car casses and the eggs retained for analysis will be shipped to Monsanto or will be retained for analysis at Bio-Test. . The remaining chickens will be placed on a 30-day recovery regimen during which time the test material will be removed from the test diets. Eggs will be collected once each week. At the end of this period, the re maining chickens will be sacrificed and handled in the same manner as those at the end of the test feeding period. The carcasses and eggs will again be ` retained for analysis. ' .1 The chicks from the first generation will be observed for 30 days post-hatching. . . ` * ; RJPsDMS O 9-9-68 NEV 1*3*76 WATER PCB-SD0000030918 $tid<t4hial B 1 0 - T E S 1 ktaknloi., 9nc, PROTOCOL FOR MONSANTO COMPANY .DUCK TOXICITY AND.RESIDUE STUDY ' ON AROCLOR The object of the study will be to investigate the general toxic effects of the test material on young adult male and female mallard ducks and to' determine residue levels in specific organs and whole carcass. Twenty male and twenty female young adult mallard ducks will be selected for the study. These animals will be equally divided into one control and three test groups. The three test group's will correspond to graded dietary levels of the test material. ' * ' The ducks in the control and test groups will be weighed weekly and observations for mortality, reactions and general food disappearance will be made periodically during the study. At the end of a 30-day feeding period, one-half of the animals in each group will be sacrificed, defeathered and subjected to a gross pathological . examination. The liver, kidneys and samples of skeletal muscle and fat will be removed from each bird and packaged separately, These tissues will be quick-frozen and retained for analysis for the test material The remaining ducks will be placed on a 30-day recovery regimen during which time the test material will be removed from!the test diets. NEV 143477 WATER PCB-SD0000030919 SndiuUial B i O - i E S T Site. 2 At the end of thi6 period, the remaining ducks will be sacrificed and . handled in the same manner as those at the end of the test feeding period. i ; .. . # RJP:DMS. 9-9-68 NEV 143478 WATER PCB-SD0000030920  Jiiduikial B 1 O - 1 ESI J<~ 'vtatoAioi, fac. O PROTOCOL FOR MONSANTO COMPANY THREE -GENERATION REPRODUCTION STUDY ' OF AROCLOR ' IN ALBINO RATS . I. General ' _ A three-generation reproduction study will be conducted with Sprague-Dawley derived albino rats. A total of 96 weanlings (32 males and 64 females) will be equally subdivided into three test groups and one control group. The three test groups will correspond to the feeding of three graded dietary levels of the test material, . ; II. o II. First Generation . '' . A. Parental Animals ' ` . 1. Diets and Feeding All diets will be prepared in the'central diet room of the laboratories. The basic ration with which all diets are prepared is a standard, pulverized rat stock diet*. The diets for any given test group will be prepared by adding a calculated weight of the test material to a pre-weighed portion of the stock diet. ' . The amount of food allotted per week to each rat is to be sufficient for ad libitum feeding. However, checks will be made daily to ensure that the food jars are not empty. . NEV 143479 9 * Purina Ral Chow, Ra.lslon Purina Company, f*i,, jUmt.*, MJnsonvi, WATER PCB-SD0000030921 hiduikial B I 0 T S I laUtatMUl. Shc. 2 2. Dody Weights and Weight Gains . . The body weight of each rat in every group will be deter- ,4 i * ' ' . ' mined and recorded initially, and weekly thereafter until the animals . ;' are 100 days old, ' '' ' 3, Mortality, Reactions and General Observations ' Mortality and abnormal behavioral reactions will be recorded daily. The animals also will be observed for fertility, length i '. - * * . . ,. of gestation and lactation performance, '. 4, Mating Procedure When the animals reach 100 days of age, each male will ' be randomly mated with two females from the same group. After suc cessful copulation, determined by the presence of a copulation plug or blood in the vagina, the male will be removed from the females and returned to his original cage. Any male failing to copulate within two cstrus cycles of the female will be replaced by another male of the same group. However, no more than two males will be used per female during a given breeding cycle. Records will be kept of the number of successful 6 . : ' copulations observed, the number of estrus cycles required to obtain a ; ' mating, and the number of resulting pregnancies. These data will be !j:- utiliz-cd to calculate mating and fertility indices. . The Fla litters obtained will be weaned at 21 days post- t . partum. The females will then be given a 10-day rest period and again ! ' ' mated, the above procedure being repeated to obtain Fib weanlings. i. ' ' .. ^ '' NEV 1*3480 WATER PCB-SD0000030922 UndnlOual B 1 0 T E 5 T lalmafatiei; Sue. 3 5. Pathologic Studies . . After the second litter has been weaned (following approx imately 33 weeks on test), 8 male and 8 female animals from each group will be sacrificed and gross pathologic observations will be made. Organ weights will be taken on the liver, kidneys, spleen, gonads, heart, brain and any organs which appear abnormal. A complete set of tissues will .f be removed and fixed in a ten per cent formalin solution. In addition, microscopic examinations will be conducted upon five males and five females from both the control and the high test groups. If abnormalities are noted, the affected organs of the lower test group animals will also be examined. . % NEV 1A3*81 WATER PCB-SD0000030923 HtuliiiOual B I 0 T ' S T JaUtafoiiei, Sue 4 O o o The following tis sue s and organa will fee examined: Tissues and Organs Examined Grossly Tissues and Organs . Examined Microscopically Heart Trachea ' Lungs Liver Pancreas Esophagus Stomach Intestinal tract Spleen Lymph nodes Kidneys Urinary bladder Testes Ovaries Prostate Seminal vesicles Uterus Pituitary gland , Adrenal glands Salivary glands Thyroid glands Skeletal muscle Bone Peripheral nerve Eyes Brain Thymus . Optic nerves Aorta ' Spinal cord Heart (right and left ventricles) Trachea Lungs . Liver '` Pancreas Esophagus ` Stomach (cardiac, fundic and pyloric regions) \' . Small intestine (duodenum, *' jejunum and ileum) . Caecum . Colon ' Spleen Lymph node (cervical and mesenteric) Kidney ^ ^ . Urinary Bladder ` Testis ' Ovary ' .- . Prostate Seminal vesicles '. Uterus . Pituitary gland Adrenal gland Salivary gland (submaxillary) Thyroid gland Parathyroid gland Bone marrow (sternum and femur) ' Peripheral nerve (sciatic) Brain (cerebrum, cerebellum and pons) . Spinal cord (three levels) ' Post-mortem animals will be examined in the same manner but organ weights will not be recorded, . *. Throughout gross and microscopic examination, particular % : * attention will be paid to the reproductive organs. .. . ' NEV 143482 WATER PCB-SD0000030924 StuLiiixial B I 0 * T S T Ja&mUu'ed, Sfx. ' ' . ' 5 B. Progeny . .' ' . . 1. Body Weight Data ' ./ . , ' Pups will be weighed at weaning. ... a. , 2. Mortality, Reactions and General Observations `` All pups will be examined for physical abnormalities at ; birth and the number of viable and stillborn members of each litter recorded. Records of survival at periodic intervals during the lacta. #* . tion period will be maintained and a final examination for physical abnormalities will be made at the weaning of each litter. ' ' 3. Survival Data . Survival indices will b.e calculated for various points during the lactation period. On the fifth day of lactation, litters of greater than 10 pups will be reduced to that number. 4. Pathologic Studies . A gross internal pathologic examination will be made upon any pup appearing abnormal. No such examinations wiil be made upon progeny which appear normal. ,. . & % ' ' ' e * III. Second and Third Generations _ . The procedures followed for the second and third generations will . be identical to those described for the first generation except that the _ parental animals for the F2 generation in each group will be selected from Fib weanlings of that group. Parents for the F3 generation will be selected from F2b litters. . ; ' . ' . . NEV 143483 WATER PCB-SD0000030925 Suduil'ual B 1 O - T E S T lalmatcydai, htc. 6 In addition, ten male and ten female pups from the F3b litters of each test group and the control group will be sacrificed at weaning (21 days post-partum) and subjected to complete gross and microscopic . . 4 examination. ' ' * IV. Reports . A complete formal report will be submitted upon completion of each generation. # * ' MLK:PSH 9-5-68 NEV 1*3*84 WATER PCB-SD0000030926 SiidirtUioi B I O - T E S T / 'oictiviiei, Site. PROTOCOL FOR MONSANTO COMPANY I TWO-YEAR CHRONIC ORAL TOXICITY OF ' AROGLOR ; IN ALBINO RATS 1,, Outline of Investigation '. A. Type and Length: Two-Year Chronic Oral Toxicity B, Animal Species Tested: Charles River Strain Albino Rats G,, Organisation: .. Group Control Test I Test II Test III Number of Animals Male Female * Dietary Level of ' Test Material .. . (ppm) 30 . 30 . . ..None Administered 30 30 . Low Level ' 30 30 ' Middle Level 30 30 High Level D. Means of Administration: Voluntary oral Ingestion; ad libitum feeding of diets containing various levels of test material, JL Parameters To Be Investigated A. Body Weights NEV 143485 A)J animals will be weighed weekly during the first three months oi the study and monthly for the remainder of the two-year test period. . WATER PCB-SD0000030927 SttdtiiiAial B I 0 - Y E $ T lal&ialotiti. Sue. 2 B. Food Consumption ' ' .' Weekly food consumption will be recorded for the first three months of the investigation. Thereafter, monthly spot checks will be . made. .. ' ' ' C. Mortality and Reactions ' Checks for mortality and untoward behavioral reactions will be conducted daily. . D. Hematologic Studies, Clinical Blood Chemistry Studies and ' Urine Analyses . The studies listed below will be conducted on five rats of each 6ex from the Control Group and Test Group III at the beginning of the study and after 3, 6, 9, 12, 18 and 24 months of feeding: ' 1. Hematology: Hematocrit value, hemoglobin concentration, erythrocyte count and total and differential leukocyte counts. 2. Clinical Blood Chemistry: Blood urea nitrogen concentration ,. (BUN), serum alkaline phosphatase activity (SAP), blood glucose concentration and serum glutamic - pyruvic trans ' aminase activity (SGPT). ' 3. Urine Analyses: Albumin concentration, glucose concentra- _ . tion, microscopic elements examination, pH determination and specific gravity, _. . The above listed studies will be conducted on animals in the . lower dose groups if significant findings appear among high dose animals. * , * " NEV 1*3*86 WATER PCB-SD0000030928 Stxbdkid B I 0 T E 5 T lakteiortei, Stic. 3 E. Pathologic Studies ' 1. Gross '. Complete gross autopsies will be conducted upon all post mortem animals unless precluded by post-mortem autolysis, all animals sacrificed in extremis, five males and live females from each group sacrificed after three months of testing and upon all animals surviving 24 months of testing. At the time of each autopsy, representative tissues * and organs will be taken.and fixed in 10 per cent formalin solution. Absolute organ weights will be recorded and organ - body ' weight ratios and organ - brain weight ratios will be calculated and sub jected to statistical analysis, viz. Analysis of Variance and/or MtM-tests, The following organs will be included: liver, kidneys, s pie on, gonads, heart, brain and any other organ appearing abnormal upon gross examina tion. 2. Microscopic Microscopic examinations will be conducted upon tissues and organs taken from selected animals sacrificed in extremis, and five males and five females from the control and highest dietary dose groups sacrificed after three months and 24 months of testing. The tissues and organs to be examined will include: heart, liver, lung, pancreas, stom ach (cardia, fundus and pylorus), small intestine (duodenum, jejunum and ileum), caecum, colon, .spleen, lymph node, kidney, urinary bladder, testes, ovary, prostate, uterus, pituitary gland, adrenal gland, salivary .. . . '* ' . '' . .1 v NEV 1434B7 . ^' r WATER PCB-SD0000030929 Ditdiiikicl B I 0 - T E 5 T lal&iaiyilci, Snc, 4 gland (submaxillary), thyroid gland, parathyroid gland, skeletal muscle, bone marrow, peripheral nerve, trachea, spinal cord, eye, optic nerve and brain (cerebrum, cerebellum and pons). Any significant tissue or organ changes at the high dose level would also be examined at the lower levels. F. Reports . . . Interim status reports will be submitted after 3, 12 and 18 . .months of testing. These reports will contain pertinent data collected to that date. . . . At the conclusion of the study, three copies of a final formal . report will be submitted, ' ' . MLKrPSB 9- 5-6B ' NEV 1*3488 WATER PCB-SD0000030930  : ..frJidiAial B i O - T E S T Jalu*iat>tic4, Sac. / PROTOCOL FOR MO N SAN% TO COMPANY TWO-YEAR CHRONIC ORAL TOXICITY ' OF ' AROCLOR IN BEAOLE DOGS I,. Outline of Experiment .' ' _. A. Type and Length; Two-Year Chronic Oral Toxicity . ' ! B. Animal Species Tested: Pure-Bred Beagle Dogs 0` . C. Test Material: Aroclor *. ' . . D. Organization; Three Test Groups and One Control Group 1. Number of Dogs/Group; Eight (four males and four females) 2. Dose Levels: Control Group - None . Test Group I - Low level .. Test Group II - Middle level ' Test Group HI > High level 3,, Means of Administration: Voluntary oral Ingestion; ad libitum . ; ' feeding of test material In diet. i R, Parameters To Be Investigated ..... . . . . A. Body Weights ' * ' - . . All animals will be weighed weekly. . ' .; B. Food Consumption Weekly food consumption will be recorded. C. Mortality and Reactions Mortality and untoward behavioral reactions will be recorded dally. ' NEV 143489 WATER PCB-SD0000030931 4 * fridulitial B I O - T E S T . Maiydai-, Sac. D. Hematologic Studies, Blood Chemistry Studies and Urine Analyses The studies listed below will be conducted upon all dogs prior to the inception of the test, after lr 3, 6, 12 and 18 months of testing and i * ' . just prior to its conclusion. . 1. Hematology: Hematocrit, hemoglobin, erythrocyte count,' . and both total and differential leukocyte counts. * 2. Blood Chemistry; Blood urea nitrogen, blood glucose, serum alkaline phosphatase, serum glutamic-pyruvic transaminase . and serum glutamic -oxalacetic transaminase. . 3. Urine Analyses: Albumin, glutose, pH, microscopic elements ' and specific gravity. ' . 'I ... O E, Pathologic Studies . 1. Gross Pathologic Studies . ,' Complete gross autopsies will be conducted upon animals sacrificed in extremis and upon all post-mortem animals during the inves tigation. At the conclusion of the 24-month study, mil surviving dogs will be sacrificed and examined. At the time of each sacrifice, a complete set of tissues will be removed from each dog and preserved In ten per cent formalin solution for histopatholcjgic examination. Also at the time of each sacrifice, the weight of the jliver, kidneys, spleen, gonads, thyroid, adrenals, pituitary and heart will be recorded. ' 2. Histopathologic Studies _ NEV 143490 I. Histopathologic examinations will be conducted on tissues . . i. . ' ' taken from animals sacrificedj.nlaxtr emls, from post-mortem animals WATER PCB-SD0000030932 1 *< ' frubuteal BSO-TEST . Site. i and from all animals sacrificed after 24 months of feeding. The tissues to be included in the examinations are as follows: lung, heart, liver, pancreas, mesenteric lymph node, stomach (cardia, fundus and pylorus), ' small intestine (duodenum, jejunum and ileum), colon, caecum, kidney, adrenal gland, urinary bladder, testes, ovaries, prostate, thyroid gland, submaxillary salivary gland, parathyroid gland, uterus, brain (cerebrum, . cerebellum and pons), bone and bone marrow (femur), and skeletal muscle (gastrocnemius). * * . ' . F. Reports . * Interim status reports will be submitted after 3, 12 and 18 months of testing. These reports will contain pertinent data collected.to that date. O . At the conclusion of the study, three copies of a final formal report will be submitted, .. / O MLKsPSH 9-5-68 NEV 143491 WATER PCB-SD0000030933 December 20, 1968 Dr. Jooeph C. Celandra Industrial Dio-Test Laboratories* l((o. 1810 Frontage Road ' Northbrook* Illinois 60062 Pear joe i rrgz This letter authorizes the initiation of two of the proposed Aroolor studies as followst Project Ho. BTL Aroolor X-Fowl - Gross Toxicity la - Aroolor 1242 lb - Aroolor 1254 Ic - Aroolor 1260 Id - Aroolor 5460 ie - Toxaphene If - DOT Ig - Chlorinated naphthalene The protocol for these etudles le to be eonsletent with our discussions when you were In 8t. Louis and 1 would appreciate receiving a note from you outlining what you plan to do with an approximate cost. Project No. PTL - Aroolor XX - 30 Day Rat Tissue Study lla - Aroolor 1242 IZb - Aroolor 1254 XXo Aroolor I860 Xld - Aroolor 5460 Zle - Toxaphene Ilf - DOT . XXg - Chlorinated naphthalene . DEPOSITION EXHIBIT 35* N6V 008162 WATER_PCB-SD0000030934 Dr. Joseph C. Calandra -2- December 20, I960 These studies aro to be carried out ta proposed in your protocol aubmittcd with the letter of Dr. Fancher dated September 9, 1968. That letter Indicates a eoet of $2,700 for three of the Aroclors, Toxaphene and controls. Further it indicates that additional materials could be Included for $600 per material. Since we are adding additional Aroclor, DDT and chlorinated naphthalene X assume that the rat tissue study will cost approximately 1*4,500. We arc obtaining samples of several chlorinated naphthalenes and will provide you the material to be investigated. Do you have a readily available source of DDT or shall I get this for you through our Agricultural Chemical Group! I have enclosed s copy of my summary of our meeting when you were down here (as you and I discussed it). There Is also a copy of Dill Richard's version* 1 hope you hove licked the flu bug and will have s happy holiday. Elnoerely, Elmer F. Vheoler Manager, Environmental Health EFWtcJs Enclosure cci V. ft. Richard ft. E. Keller/flcott Tucker< C. Faton w. Ku Johnson ft* So KellyA* H. Hunt NEV 008163 WATER PCB-SD0000030935 April 8, 1970 Herbert BlUMnthal Ph.D. Chief, Petitions Review Branch Bureau of Foods# Pesticides and Product Safety U. S Food and Drug Administration 200 C Street, Southwest Washington, D* C. 20204 Dear Herbi Confirming our telephone oonversetlon 1 have enclosed Xerox ooples of the status report* for tha ehronle toxicity studies for our Aroolors at Industrial Bio Test, Inc* Specifically, three of our polychlorinated Biphenyls are under Investigation* Thess are Aroolors 1242 (bbiipphheennyyll chlorinated chlorinated to to the the extent extent of of 42J<)# 5V' # 1254 end 1260 biphenyl chlorinated to the extent of 60* Studies Include two year oral administration to rats, two year oral feeding to dogs and a three generation rat reproduction study* As indicated in the enclosures, the levels of admin istration are 1, 10 and 100 ppm for each of the com pounds* Further# the status reports for the ehronle dog studies represent data at ths ehd of nine months* The enclosed copies on the rat studies show data at the end of six months administration* As ws mentioned on ths telephone# we added 30Q rats to the ehronle studies after the original two year projsot had gottan underway to allow a sufficient number of animals for sacrifices at three# six and twelve months* Hlatopfcthology ha* bean completed on ths sserifloed animal* and Dr. Calandra has reported verbally that thers ars no positive pathological findings* Dr* Herbert B lumentha1 April 8, 1970 rage Tw The rat reproduction stadias are into tha saoood gener ation* At this point Dr* Calandra has Indicated that thora definitely has been no affaot with any of tha compounds at tha 10 ppm dietary level* There is some equivocal posalbla affaot in tha animals at tha 100 ppm laval with Arcelor 125^ If you havs any spaciflc questions sftar reviewing tha enclosed status summaries, please faal free to call Dr* Calandra or Dr Fancher directly* Beat personal regards* Sincerely, ft Etamet Kelly, K* D* Medical Director REKlJu c.o. Dr. Joseph C. Calandra Dr* Otla 2* Fancher b.c, W. B. Papageorge 0. W. Ingle Enclosure* NEV 000630 WATER PCB-SD0000030937 Monsanto 00 H ' Mltfltl ! am: omi M-tooo THREE-OEHERATION REPRODUCTION SWOT IN AIBZNO RATS WITH: AROCLOR 1242 AROCLOR 1254 AROCLOR 1260 RESULTS OP TOE FIRST OQIEMTION September 4, 1970 Submitted by: R. Emmet Kelly, M. D. Medical Director NPC00009503 *4 ' WATER PCB-SD0000030938 [a f f UH**<* I _ } ' | ; ' SruBu&trj&l BIO -TEST JtGhmhwA. Snc. 1010 montage road NORTHBROOK, ILLINOIS *0063 .** . ' '. . . REPORTTO . MONSANTO COMPANY THREE-GENERATION REPRODUCTION STUDY IN ALBINO RATS - AROCLOR 1242 RESULTS OF THE FIRST GENERATION SEPTEMBER 4, 1970 IBT NO. P8797 . 3 / ~J>C009504 WATER PCB-SD0000030939 z i SmUaiVuci BIO -TEST XaimahukA, 3m. 1010 9RONTACE ROAD NORTHOROOK. ILLINOIS 00062 September 4, 1970 l ! Mr. Elmer Wheeler Monsanto Company Medical Department 100 N. Lindbergh Boulevard St. Louis, Missouri 63166 Dear Mr. Wheelers Re: IBT No. P7297 - Three-Generation Reproduction . Study in Albino Rats - Aroclor 1242 We are submitting herewith our laboratory report dated September 4, 1970, prepared in connection with the above study. This report presents the results of the first generation. Very truly yours. -- JCC/kJl ' J. C. Calandra President 9* ' NPC00009505 WATER PCB-SD0000030940 fjit-Jjl D I O T E S T Smc. REPORT TO MONSANTO COMPANY THREE-GENERATION REPRODUCTION STUDY . IN ALBINO RATS - AROCLOR 1242 ' RESULTS OF THE FIRST GENERATION SEPTEMBER 4. 1970 1. Outline ef Study 1BT NO. P7297 ' ' A. Type and Length; Three gene ration reproduction study B. Animal Specie* Taated: Cher lea River albino rate C. Material Teated: Aroclor 1242, Lot No. AK-255 . D. Starting Data: May 1, 1969 E. Statua of this Report; Completion of the fir at generation (Fo parents - Fla and Fib progeny) F. Organisation- A atructural outline of the experiment la given in Table 1. NPC00009506 -v: WATER_PCB-SD0000030941 J BIO-TEST JaUtoktit*. Jnc. 2 Croon C T-I T-11 T-II1 TABLE 1 ' TEST MATERIALS Aroclor 1242 Outline of Experiment Fo Generation Dietary Level (ppm) None Number of Animals Male Female 8U 1 8 It 10 8 It 100 8 16 G. Mum of AdmlnUtratlon: Voluntary oral Ingestion. ^00009507 WATER_PCB-SD0000030942 yj OlO'TEST JmLmLtMti, Sue. 3 jL Summary The first generation of a thrce-genorallon reproduction study of Aroclor 1241, Lot No. AK-255, at dietary levels of 1, 10 and 100 parts per million has been completed. The following data were obtained during the first gene ration: . A. Progeny (Fla and Fib) The numbers of pups delivered and weaned by treated females were generally as large or larger than those from the control group. The survival indices of progeny from treated females were higher than the indices for controls. The lactation indices of the T-UI group, but not the T-I or T-U groups, were slightly lower than these indices for the control group. All progeny body weights were normal and there were no unusual reactions noted among any offspring- fi. Parental Animals (Po) The body weights of the treated males and females were nor mal and compared favorably with those of the controls. One T-ni male died during the pre-mating period;-one T-I female died while lactating (or her second litter; one control female died during parturition of her first litter. NPC00009508 WATER_PCB-SD0000030943 \ S BIO*TEST %* 4 Tk. d.u obtained frfr P*"1*1**1* . tbe.e animala revealed no .ipr, between ...t and .. control rats. Organ weight dat studies confirmed the absence o . -.hr results of the histopathologic * .. oaihologic changes which could ? be related to the ingestion of p Matin, indie... l.r.ili: -W. .[ pro,nancy and parturition for treated anir*- `v*re normal cod compared favorably to those of control an1-*-** Respects *. submitted, 1NDUSTR- * B10-TEST LABORATORJES, INC. ,, Report prepared bv: -o, , \/\ ^ e vl, \/a--/w f -- 1 1~ JsmeiTv rnup !.* * *'7 . Rat Toxi. * Department * . leport approved by: M. L. K>- ''rcr* Piy' Manago. ..-Ecology OJ; O-tHisrE'a. x f' ,_`c_r* spht.< Dn.* September 4. If70 r>.Ajl:psh NPC00009509. WATER PCB-SD0000030944 jlO*TIST $m, 32 4. Reactions '^ No untoward behavioral roaetloni wore observed among . tr test or control progeny. / NPC00009S10 WATER_PCB-SD0000030945 a * ,, Sttduibicl BIO -TEST JPcJ&iatiHjut&, Snc. 1010 MONTAGe ROAD NORTHBROOK, Ill'NOlS MOM **CA C*C ill mtMMC REPORT TO MONSANTO COMPANY THREE-GENERATION REPRODUCTION STUDY IN ALBINO RATS - AROCLOR 1214 RESULTS OF THE FIRST GENERATION SEPTEMBER 4, 1970 ' 1BT NO. P7297 NPC00009511 WATER PCB-SD0000030946 i SniuiOual DIO -TEST Jk&oiatatieA, Snc. MIO PRONTAOC ROAD ' NORTHBROOK. ULINOIS 6006S September 4, IfTO Ur. Elmer Wheeler *^n*anto Company -died Department ; N\ Lindbergh Doulevard . Louis, Missouri 63166 . . Ivsr Mr. Wheeler: Re: IDT No. P7297 * Three-Generation Reproduction Study in Albino Rats - Aroctor i2S4 We are submitting herewith our laboratory report dated `.ember 4, 1970, prepared in connection with the above study. This report presents the results of the first generation. . Very truly youre, `j ------ <-_____ . ' :c/kji J. C. Calandra President ! , 'l upC00009512 WATER PCB-SD0000030947 510 T E S T ImowlMA'J, Jttc. REPORT TO ' MONSANTO COMPANY THREE-GENERATION REPRODUCTION STUDY IN ALBINO RATS - AROCLOR .1114 . RESULTS OF THE FIRST GENERATION Outline of Study SEPTEMBER 4, If 70 1BT NO. P7297 A. Type and Length: Three-gen*ration reproduction study B. Animal Specie* Tested: Charlec River albino rata C. Material Teated: Aroclor 1214, Lot No. AK-38 D. Starting Date; May 8, 1969 E. Statua of thla Report: Completion of the first generation (Fo parents - Fla and Fib progeny) F. Organisation; A etructural outline of the experiment ia given . In Table 1. NPC00009513 i WATER PCB-SD0000030948 UlQ-TEST JaUuiltUci, Site. 2 roup I 11 III TABLE 1 TEST MATEIUAL: Aroclcr 12S4 Outline of Experiment Fo Generation Dietary Level (PPm) None 9 1 Number of Animals Male Female 8 16 8 16 10 8 16 ' 100 8 16 G. Mean* of Administration: Voluntary oral Ingestion* WC00009514 WATER_PCB-SD0000030949 A ;jmJ BIO-TEST JeUifn*iei, foe. ^ < | u. Summary 4> . . The first generation of a thrco-gc: eratlon tcproduction study of Aroclor 1254. Lot No. AK-5B, at dietary loveia of 1, ig Joo ppm ] hu been completed. The following data were obtained during the t first generation: | A. Progeny ' ' '' j The dau from progeny of females fed cither 1 or 10 ppm ' were norma) In all reapeeta. Although no adverse finding a were noted in Ute first litter of females fed 100 ppm. the number of pupa delivered and weaned for the second Utter was significantly lower than normal. The survival of pupa that were delivered was alao significantly luwr than normal In view of these findings, the females fed 100 ppm wrrt? rammed for a third Utter. The data from this litter substantiated thu findings noted : the second Utter. ' * ' 1 B. Parental Animals * Females fed 100 ppm gained slightly less weight that did alrole. Males fed 100 ppm and all raU fed etU*r f t,r ffj ^ iMbltcd weight gains which were not different iron, wte were no deaths which could be related to l)t Aroclor and no unusual behavioral reactions were n>>*-*i. , Cross pathologic examinations revealed # " Vl between test and control rata. tlUkr NPC00009515 . __ WATER_PCB- j,,fiST &k. 4 Statistical .-nalv vt- upon organ weight data revealed several .mi difference .. Significantly higher liver to body weight ratios ,-r.**rded for all rata .tod 160 ppm, however the absolute weights . >.!(;nificantly higher o.ily in males. Males fed 1 or 10 ppm exhlfen;ntficsntly lower liver weights and liver to body weight ratios. .rvation of thyroid weights was noted for both males and females : :o ppm. Histopathologic examination of tissues and organs revealed .di'.is in three of five males. No other significant differences noted between test and control animals. The mating index for the third litters of rats fed 100 ppm was . low and, in the second matings of these animals, three females rbed their litters. All other mating indices, fertility indices, r.ces of pregnancy and parturition and mean gestation times were Respectfully submitted, INDUSTRIAL BIO-TEST LABORATORIES, INC. .U. Plank Croup Leader Rat Toxicity Department i approved by; M. I.. Kcphng.-Y. Pl^liT hi.A|:cr, Toxicology NPC00009516 WATER PCB-SD0000030951 010 * T E S T /Wn*% A*. SI 4. Reactions No untoward behavioral reactions were observed among ithcr lest or control progeny. NPC00009S17 .4, WATER PCB-SD0000030952 9ruSjusOuaL DIO TEST JaJUtal&tkA. 3nc. 1RI0 FRONT ACC ROAD. NORTHBROOK. ILLINOIS 600A2 ; i i t i REPORT TO MONSANTO COMPANY THREE -GENERATION REPRODUCTION STUDY IN ALBINO RATS - AROCLOR 1260 RESULTS OF THE FIRST GENERATION SEPTEMBER 4, 1970 . IBT NO. P7297 ' .' ! I ! ' *i ! I I NPC00009S18 i 1! I : I WATER_PCB-SD0000030953 Sn&Mikk-I BIO -T1ST Jtaho'itJbfueA. Snc. IBtO FRONTAGC ROAD NORTHBROOK. IUINOIS *0062 September 4, 1970 I Inter Wheeler nto Company 1 Department Lindbergh Boulevard ais, Missouri 63166 ir. Wheeler: . Re: 1BT No. P7297 - Three*Gene ration Reproduction Study in Albino Rata - Arcelor 1160 We are submitting herewith our laboratory report dated ber 4, 1970, prepared in connection with the above study. Thia report preaenta the reaulta of the first generation. Very truly yours, ^ 7t*~ * - , < . J. C. Calandra President ' NPC00009519 i i t : WATER PCB-SD0000030954 I O T E S T jlui+\af*Uiii, %*e. i i i REPORT TO MONSANTO COMPANY THREE-GENERATION REPRODUCTION STUDY IN ALBINO RATS - AROCLOR 1260 RESULTS OF THE FIRST GENERATION SEPTEMBER 4, 1970 IBT NO. P7297 Outline of Stu<?y A. Tyoc and Length: Three-gene ration reproduction study D. Animal Species Tested: Charles River albino rats . Materia! Tested: Aroclor 1260, Lot No. AK-3 3. Starting Date: May 8, 1969 '- Slalui of This Report: Completion of the first gene ration |F parents - Fla and FIb progeny) * Organisation: A structural outline of the experiment is given in Table I. 4i !i I ii i i I iI NPC00009520 ! i WATER PCB-SD0000030955 D-TE ST .fee. 2 TABLE l . TEST MATERIAL: Aroclor 1260 Outline of Experiment fo Generation Dietary Level (ppm) None 1 10 100 Number of Animal* Male Female 8 16 8 16 8 16 8 16 *' ! of Admlntatmtion: Voluntary oral ingeition. ti I ! \ HPC00009521 WATER OT ES T St6. 3 Summary The results of the first generation of a three-gone ration reprodue- tudy conducted on albino rats fed Aroclor 1260, Lot No. AK-3, at ry levels of 1, 10 and 100 parts per million are presented below. \. Progeny (Fla and Fib) . The number of pups delivered and weaned by treated femalasi 'sscntielly the same as controls. In the second (Fib) litters, s fed 100 ppm delivered slightly more stillborn pups than did ols. Survival indices of progeny from treated females were not ent from the control indices. The body weights of the weanlings treated females were normal, and there were no unusual reactions among any offspring. . Parental Animals (Po) The body weights of the males and females receiving Aroclor m their diet were about the same as those of the controls. One 1 female died while giving birth during her first pregnancy, were no untoward behavioral reactions noted. " Cross autopsy conducted upon males and females in all groups *d no observable changes between test and control rats. The weights and ratios of males fed 1 or 10 ppm we re lower than con- while the liver weight* and ratios of males fed 100 ppm were tt than controls. Histopathologic examinations revealed no NPC00009522 0 | O I E S T Jayiei%iaS, }ttc. 4 .angcs in the tissues and organs which could be attributed to the Inges,n of Aroclnr 1260. The mating indices for both litters of rats fed 100 ppm we re rcr than control. However, the index for the second (Fib) litter is thin the normal range of the rat strain used. All other mating indices, rtility indices, incidences of pregnancy and parturition and gestation net lor treated animals compared favorably to the controls. Respectfully submitted. INDUSTRIAL BIO-TEST LABORATORIES, INC. port prepared by: vCV'V JayiTds B. Plank Croup Leader Rat Toxicity Department port approved by: M. L. Keplintfcr. P&D. Manager, Toxicology .DL.^ .?rwwv.gjq.,h..J Otis E. Fanchcr, Ph. D. Scientific Director I \ 9 i I ii i ! I I I i icinlicr 4, 1970 i;pih MPC00009S23 WATER PCB-SD0000030958  TEST JulexatMieU Sue. 11 3* Reac1 tio""nl,nas" '* ft No untoword behavioral reactions were noted among the ai animals in any group. " ? Autopsy Findings a. Cross Autopsy Findings At the time of sacrifice, gross autopsy revealed no cnees between test and control animals. b. Organ Weights and Ratios Mean organ weights, organ to body weight ratios and . to brain weight ratios are assembled in Tables VI through XJH. ! NPC00009524 I "f.. WATER_PCB-SD0000030959 tu~l OiO-TEST JuSjisilnh't, Xtc. 32 4. Reaction! No untoward behavioral reactions were observed among either test or cost.' progeny. NPCOOOO9525 WATER PCB-SD0000030960 $ StidtatwU BI O -TEST XalyyujJ&wzb, Snc. 1810 FRONTAGE ROAD NORTHBROOK. ILLINOIS 60062 November 12, 1971 ) o Mr. Elmer P. Wheeler Monsanto Company 800 North Lindbergh Boulevard St. Louis, Missouri 63166 Dear Mr. Wheelers Re: IBT No. B7298 - Two-Year Chronic Oral Toxicity Study with Aroclor 1260 in Albino Rats We are submitting herewith our laboratory report dated November 12, 1971, prepared in connection with the above study. Very truly yours, JCC/kjl J. C. Calandra ` President i DEPOSITION EXHIBIT 35 NEV 009990 WATER PCB-SD0000030961 , project m. ' REPORT. pILE / ~ct SttSuASual BIO -TEST 1810 FRONTAGE ROAD NORTHBROOK. ILLINOIS 60062 Stic. REPORT TO ` MONSANTO COMPANY . TWO-YEAR CHRONIC ORAL TOXICITY WITH AROCLOR 1260 . ->< r' IN ALBINO RATS > NOVEMBER 12,? 1971 V. 'i ; IBT NO. B7298 ' m \ 0Q9991 WATER PCB-SD0000030962 fruLtihud. B l O - T E S T JeAnoMm, Sne. REPORT TO . MONSANTO COMPANY TWO-YEAR CHRONIC ORAL TOXICITY WITH AROCLOR 1260 IN ALBINO RATS NOVEMBER 12, 1971 IBT NO. B7298 1, Introduction At the request of Monsanto Company, a two-year chronic oral toxicity study was conducted using albino rats to determine the potential toxicity of Aroclor 1260, Lot No. AK-3. The following report presents the results of this investigation. NEV 009992 WATER_PCB-SD0000030963 * hvLulbual B I O - T E S T /at&iakUU, $nc. 2 O II, Summary A two-year chronic toxicity study was conducted using albino rats led diets containing 1 (T-I), 10 (T-II), or 100 (T-III) ppm Aroclor 1260. Food consumption and body weight gains were not altered at any level of Aroclor 1260 fed. The number of animals dying and the time at which the deaths occurred did not vary among the test and control groups. Hematological and clinical blood chemistry studies conducted after 3, 6, 9, 12, 18, or 24 months did not reveal any affects related to Aroclor 1260. Urine analyses failed to reveal any differences between test and control animals. At sacrifice after 3, 6, or 12 months on test organ weights, organ to body weight and organ to brain weight ratios disclosed several randomly . occurring intergroup differences. The lack of any consistent dose related response and the absence of any deleterious histopathologic change confirm that these differences were not related to the ingestion of Aroclor 1260. At the final sacrifice after 24 months on test, the liver weights and liver to body weight or brain weight ratios were significantly elevated in the rats from the T-III group. Histologic examination of the livers * # from the T-IU group revealed several animals with vacuolar change. This lesion is morphologically indicative of fatty degeneration. Specific fat stains confirmed the presence of fat in these vacuoles. Focal hypertrophy and focal hyperplasia were also found in the livers from animals fed Aroclor 1260. NEV 009993 WATER PCB-SD0000030964 2. uluiiual B 1 O - 1 E S T laUmUiiei, 2nc. 3 Hyperplasia of the urinary bladder was found in an animal from the control group but not in any of the test animals. The incidences and types of all tumors were about the same in all groups, including the control group, and are considered normal for rats of this age. ' Respectfully submitted, . INDUSTRIAL BIO-TEST LABORATORIES, INC. by: Report prepared . ^VwAlx Philip Smith, B. S. Assistant Toxicologist Rat Toxicity Report approved by: Q Jambs B. Plank Settlor Group Leader Rat Toxicity Paul L. Weight, Pn. D. Section Head, Toxicology Manager, Toxicology November 12, 1971 lamssjn NEV 009994 WATER PCB-SD0000030965 4' I' Q Q B I O - 1 1 S T laj&urivtiei. $ne. 4 HI. Procedure 4 A. Experimental Animals The animals employed in the test were Charles River strain* albino rats. Four hundred rats (200 males and 200 females) were selected for the experiment, ear-punched with the animal number assigned and housed individually in standard wire-bottomed steel rat cages. Each cage bore a color-coded card identifying the rat with re spect to project number, dose level assignment, individual animal number and sex. B. Organization of Groups A structural outline of the experiment is given in Table I. TABLE I ,, TEST MATERIAL: Aroclor 1260 Two-Year Chronic Oral Toxicity Study - Albino Rats ' Outline of Experiment Group Number of Animals Male Female Dietary Level . . (PPm> __ ....... - . Control 50 50 None Administered T-I so 50 ` * ' 1 T-ll 50 50 . 10 T-III SO 50 100 Charles River Breeding Laboratories, North Wilmington, Mass. NEV 009995 WATER PCB-SD0000030966 2rJiiu*l B I O - T E 5 T XalmatmUS; Ptte. 5 o I I ! i C. Diets, Feeding and Food Consumption . All diets were prepared in the central diet room of this laboratory. The basic ration from which all diets were constructed was a standard, pulverized stock rat ration*. The diet for any given test group was prepared by blending the calculated amount of Aroclor 1260 with a pre-weighed portion of the stock ration in a Hobart mixer. . . Fresh diets were prepared each week and every rat was offered an amount of food sufficient for ad libitum feeding. . Food consumption was recorded for five rats of each sex in every group weekly for the first three months and monthly for the next nine months. Thereafter, periodic spot checks were made. D. Body Weights and Weight Gains Initially, the body weight of each rat in every group was deter mined and recorded. Thereafter, individual weighings were made weekly for the first 13 weeks and monthly thereafter until the conclusion of the investigation. _____ ' - ' E. Mortality and Reactions " _ ____ __ ' ` ____ __ ;.. . " .. Checks for mortality and abnormal behavioral reactions were .made daily throughout the investigation. ; F. Hematologic Studies and Urine Analyses 1' Blood studies, including determinations of hemoglobin concentra tions, hemotocrit value, erythrocyte count and both total and differential * Purina Rat Chow, Ralston Purina Co., St. Louis, Mo. NEV 009996 WATER PCB-SD0000030967  Sn&altial B ! O - I E 8 T JaSmaimied, 9ne, i' 6 O leukocyte counts, were conducted upon five males and five females from both the control and 100 ppm groups. . Urine analyses for the presence of glucose, albumin, micro scopic elements, and determinations of pH and specific gravity were con ducted upon urine samples at the same time intervals and from the same animals as those employed for the blood studies. These, studies were conducted after 3, 6, 9, 12, 18, and 24 months of feeding. G. Clinical Blood Chemistry Studies Determinations of blood urea nitrogen concentration (BUN), serum alkaline phosphatase activity (SAP), fasted blood glucose .concen tration and serum glutamic-pyruvic transaminase activity (SGPT) were conducted after 3, 6, 9, 12, 18, and 24 months of feeding upon the same rats as were the routine blood studies. '' H. Pathologic Studies When an animal succumbed during the test period, a gross autopsy was performed. In those cases when postmortem autolysis was not ad- vanced, representative tissues were taken and preserved in ten percent formalin solution for possible future histopathologic study. After 3, 6, and 12 months of testing, five animals of each sex from each group were sacrificed and subjected to complete gross pathologic examinations. i NEV 009997 WATER PCB-SD0000030968 BI O-TE S T Dmc. 7 Absolute organ weights were recorded and organ to body weight and organ to brain weight ratios computed. The following organs were included: liver, kidneys, spleen, gonads, heart and brain. These data were then subjected to statistical analysis. An Analysis of Variance was conducted first and significant effects disclosed by that treatment were further studied by "t"-tests. Complete microscopic examinations were conducted upon the tissues and organs from all control and 100 ppm group rats sacrificed after 3, 6, or 1Z months of testing. The following tissues and organs were included in the examinations: heart, trachea, lungs, liver, pancreas, esophagus, stomach, small intestine (duodenum, jejunum and ileum), caecum, colon, spleen, lymph nodes, kidneys, urinary bladder, gonads, prostate gland, seminal vesicles, uterus, pituitary gland, adrenal glands, salivary glands, thyroid gland, parathyroid glands, skeletal muscle, .. sternum, bone, peripheral nerve, spinal cord and brain (cerebrum, ' * cerebellum and pons). . The aforementioned tissues were prepared and stained with Hematoxylin-Eosin stain. . '` ` . After two years of feeding, all surviving animals were sacrificed and subjected to complete gross pathologic examination. Hie absolute weights of the liver, kidneys, spleen, gonads, heart and brain were recorded immediately after sacrifice. NEV 009998 WATER PCB-SD0000030969 ' SiuLdbual B I O - T E S T lalniafoiiai.. Hue. 8 Microscopic examinations were conducted upon tissues and organs from selected animals dying during the experiment and upon all animals from the final sacrifice. i, Tissues and organs examined were the same as those previously mentioned. 1. Tumor Incidence and Classification A tabulation of the incidence of tumor formation in each group was made at the conclusion of the investigation. In addition, tumor data for individual animals including location, weight, size and pathologic classification were recorded. 9 NEV 009999 WATER PCB-SD0000030970 Stuktikial B ! O - T E S T JaktaltMUl, Due. 9 O IV. Results A. Body Weights and Weight Gains .' The male and female body weight data are assembled In Table II. The data in this table also include the 3, 12 and 24 month total weight 9 gains. There were no significant effects due to ingestion of the compound Q 4 NEW 010000 WATER PCB-SD0000030971 ' JHUA4) tAUM- O sO nelt (o4 o3 a a .**^*<**- 4J M 4J Sk g H v o O' H a o >4 0) 6 ri H M if in rO -* fw ns in m tn *-i eo ns if m m * if nO *4* n --< m4 4f 00 f- 00 ow O' 00 "< 60 00 00 oo O 00 >4 M 't ns ns m ns SM S'- o vO O' O' n- o' tn m h- 00 sO m oo r Hf M 4* ns if nj r\j #&>* ^4 O' 00 <-4if* Cs'-j ^ t4 n- m if ns f*. 0s v nM< ns Of-' ^m 'if ns a*<t 3 so *4 MdH) m 4) 1 > * o H 2 o** TJ * g * &9> m * X o*4 o *"* -d* 0 O sO O' 'f n- if nS 00 44 J3 "5 s6 jt p6 a> in 0 vD 0 ,w' m m M* o ns n f M O' m O vO if M 4 @s m mm cn ^ r- in n nj <N 4* %0 4j n nj o nm n if ns co n ^ P.J aj to M 'O ^ ns *o -- ^ fvJ if 'O O' in cn ns m n- m n ns _j _4 %o ^ n ns ^=4 c^4 1 00 if f4 00 ^ ^1 c iji pa i 60 rn < if ns n ^ V U* ns oo O V0 4f ns nl '(f wm n csj ns i if m ns oo 'iOf nns- <"> n> m i if ns S', m m vo ^ ns in ns ns vO Tf ea 00 O' m *o ns m n t~ us n ns p o sO 4f rn pa *8 m ft w*4 O"4' S2 h* nn ns cn ns n ns n nj ns m nifs _O*' O O' m o w 4f O' ns -i . ns i-i f- 00 n^si ww-4 -* t# o nns -< ns n Oc^l' 'O-l O f'ns ^4 n O f ns - n >*0 *n 'O n vo n vo o Wn4 me**i n m n n n <rn H .< .4 .. . I 8 w %04 "t)# o vs M 8 a b -n Ik <--Oi $4 u e a ou *4 < A 2 Ui , p4 NM c ro^ SN S fa o #=# Sh o o NEV 010001 WATER PCB-SD0000030972 I C ontrol 100 00 V in m <NJ v n sO ^ m rsl sO fM c- m in S'O0 m (TV ess -- o o O' t- to O' O' O' fsO to O' ea O BO (s. to |s. to V ts- to 0 09 m 09 sO A 00 n- 03 V s0 to US <-I to m sO CA Is, r- o '* to cV t" S0 ro to n sO to sO CO oo so r- sO - fM 00 't* vO m f\S O' m sO n n o sO to to eo fA if, SO to om in ?n s> in fM (A esl sO to 00 f0 fM fA sS ro sO O M* sO to to sO to rsi sO to to to O' to m to o -* fM so n ~t 1-4 00 VO m ca fs. o ~f %o to . m M sO fM m fA 00 T|* (s. IT* tA *- tfi --< in to o fs eo o mm - to o to H m n (s. (S, o w to sO sO AS o m n m ns mO %n n 60 IS. O' O' fM S0 -- Os mM S0 * O' O' * fM oa O' ns n fM fa 2 fa 2 fa 2 fa . - ,* ' NEV 010002 o ^"3 WATER PCB-SD0000030973 *fos0S IV ^8oo*4 M OC < a a$ 3 (4 B < s H w B _ J3 *d* , 5 *5 * yo^_,S *g 2 OOm' i-n-j<i rAmS4 m CmO APmHS .Wiiff 0mo0 PoH 3 " IM Arft --tinni 'imOf m ams *iinof mi0f0 -t ( <^0 itnn M %iC-Oo vtiOnf inx S'- i0iff0 %otnoo vtmn PfP*HH. t0^A40 MM 4J ta>-i mmo r<~-t mmO mpH n<4s< r- m i'rIf-f fmo- Mf4 O6in"' pimnn) ttn-n im-f< ten^. mtn tttnn" omo QfM rtmo- mhif- irtnn- tOmn' pH O t- mm iron- <t^o- **`?f*0e2L #--r** *UCi rO?' vtO- tfmOn vMt0- PifH 0 ft" ipnH 'toO'* -rif*- *o0 vtt>O-- mm""t ihtf-- 'O ^ 0ro~0 mo vOO' tinn gfn*mQ v!O*-' toon vtS*'*- miiff \i^o tr^^n- h<*f mtn %&*o4 *0a00- --00t soooo tinfn vr~f*i OTstj<t' in A. TpTHff m4 rOm' \'iO0f irOO- <'iO0f vO oMo fsS ff- "tf *'0f I^f - r iaof* t>A^S m<4< n %o in etno tn WrAS vM^O -At*Ji- o tOn' tPn4 *<<ht< i0 f* 0otn0 mK> *o4 jS ) ^^ M M *3irl! $* D *mMo C o U S f*t Sfct H O^=4 100 4 NEV 010003 WATER PCB-SD0000030974 $nduibual B 1 O - I E S T JaiotativueS, $ne. 13 B. Food Consumption The data obtained from the food consumption measurements conducted during the first 12 months of feeding are summarized in Table III. These data revealed no significant difference between test and control rats. The periodic checks conducted during the remainder of the investigation also revealed no outstanding differences between test and control animals. . NEW 010004 WATER PCB-SD0000030975 ../ i Jt- d* B I O - T E S T JaJuHaimded, 9*$^, s* o 1 .U8 cSj 1m & u (&ft M(h*- ^o t t < Qnc O au ,-v. w I, y pm- 'mO ipn- n n m m I I < *s0 I IQ a Jr ao W 4 B 4p3* I m < H H f-rht! O (coA 0 ooa 1 (*4> }oHt fA ~l O' 9-4 mpH pO' "4 fTM4 o pa pa mH O' vO 00 r4 fsj 41 p- to O' O' O' P- ^-4 Os_4' mpH GO 9-4 re*f4 O' **4 O' ^=4 't ^4 *l sO OH' pH O' o CpHO mfH 9-4 o O' f"4 mpH to "^*f4 TpHO pH ipnH to O' OpH' pa pH OpH' ipnH N0 60 41 pm '9=4 O' tf m M v*OH pH pa TmO ^=4 4pH< pa m mpH N o f--4 0 PO' m pH 00 0% OpH' to 4 p4H* pa t*- tpoH o N0 O"4' mM S^ wra co o pa ra o o pa TppOHa 'O o O<*4' OpH' fTM4 esj tan> ^0 pfO-- to tpoH TppHHO fopH NfO0 o O' f-4 fs*li 1-4 O m PTpOH pH pH o pa vo9--04 OoM' OIP'H*' rf=H 9IA-4 TO TpOH PopH ipHn pH spOOH' O' tpHo pH t~ mpH O' INS #TM4 PHpH4* M r*4 ppHa (N 9*4 in %o mM fA ISI o tPoH 5 pH "ptnH* 0pH0 pH ** #=4 ppHa o tn m0N <* to O' t~ ,CpH-O* in O' n0 4* ^4 O' 0N f4 . 2 fa 2 fa . Sfa 2 fa VT. > PtfK lE 04a2 <8* a oc u oo 14 NEV 010005 WATER PCB-SD0000030976 Srululi'ual BIO-TEST Xa&tMio'Uoi-, Hhc. 15 st*O- ^M 'O oq m--* 'wCM eo M^ 5 (M O 2 <i a . 4 .u8 o H < *0 w5 (4 <4 Q * C0 fl 1 1 > 9 V 1 i2 SH H| O 0 u H1 w B H H (4 Jl" fM fw oo cm ># CcMn *o>0m--*> Ow Oeo' o --> tC"M- fMO* Mso* Om' Weo Om*' O' o e 'O 6N0 NIA vtofi vO 60 visOj Mm* m4 <-* W t- --< M Ifl O' eft 'ON 'O PO -4**too ttoo O' o r*C-- O' M* 'O ^ eo tf fM OM' \CoO foO' ^^ 00 "m*< m 'O 'O *n O' <* eo m 00 M* 00 ^ o h- 60 Ml O' ^ oo in oo_ <t*oo O-t' wto or- n cm f* Nh --a *--i hh *0 09 O' ^ sO 00 O' m1 'O P'1 w^ O' 'mO w9 S f*c S Im Sm S fn *8 S > " ail ^ uJ^ .J2J *?2 oh (oJ O o*- o NEV 010006 WATER PCB-SD0000030977 $*tduil>Ual B I O - T E S T jtali&*ai&/Ue, Hue, 16 C, Mortality and Reactions A frequency distribution of natural deaths occurring during the investigation appears in Table IV, No untoward behavioral reactions were noted among any of the animals employed in the investigation, ' 4 NEV 010007 WATER PCB-SD0000030978 $' 0 1 O T E S f JZal&iaU'u&i, $*tc. eQdVo* men mm m tn mcn %m% mm mm H$o mfM ^n S M - " r- fM fM^ ffMn mNm*I n*i wn o hj* m * B 0r--maoHI m t O' ve h in o oo m 'Ot- *d eo 5 sOi r- in r^n f- oo m -- m m m <n 1 c!J> <2 duVo u dv B I um M o I m "< >-i m m cn mo o V4 to OI' oo - oo om *o oo oo -ho om t Im oo oo -ho --h o S tom 2 to 2 to In 2 v *o s s dv0M B 1s I 5u .us 17 Qs * NEV 010008 WATER PCB-SD0000030979 jttdudUial B I O T E S T Ja&o^aUUei, Pnc. 18 D. Hematologic and Clinical Blood Chemistry Studio8 Mean male and female hematologic and clinical blood chemistry data are summarized in Tables V through IX. Values for all parameters investigated were within the normal range for the albino rat. No significant differences between test and control values were observed. NEV 010009 WATER PCB-SD0000030980 9*vLuihiaL B i O * T E S T JahyuU&ud, $ne. 19 . * NEV 010010 WATER PCB-SD0000030981 Dn-Lubual B I O * T E S T labmUuM, 9nc. 20 rv4t 4 l NEV 010011 WATER PCB-SD0000030982 \ Snduilwd B 1 W I fe 1 XaJt&iatvuei, 'Jttc. o } TABLE V ll erenti cnphoc Month ? IM N9 n 4Co-9e ' . 4-tn0* <4J ^49 m TO oe Mo M*OM' 4M0e ^9---1 H 2 *S Oft cg <~m TOe foSt o9=4 4I<MM XO- "gHg0s$V*5*p* O' i TTOO*9i TOH 0"n0*e O' sa 5 VU4 1) 4^0 9 *$ T#9""O49f ' one*l ooTMO4 dV u 0 ' o T"O4 TwOH9 40 40 0-4s9 t'-9 A 4f0c $ s4> 4J 2 o 03 U 50oXy <M 4m*9 . TO 4%>009 409 4m CIHO toO^9' M9 ro- <39 9r>-9 4mO06 Jr*at.. M- eo 6t-9 o0O09' 'Nt9 NM9 r- u 3 *t JH C. S -) 6O*0 4tmo9 n to mX 44m00e %%o09 00 imn o4co9 n aM0 ooAo ' eo 0in0 o rOJ' Sex 2 U* 2^ o 3^ *2 -* 4ovaB 9'oM=4 o0 U o ro*i Cl * & NEV 010012 WATER PCB-SD0000030983 T A B L E V H continued 24 0.2 0.2 0.2 Sndtuhial BIO-TEST Sue. M't ^0 o f--91 * m 00 oo 9 0 e9t 04 8*0 0*1 0*1 M -3 j- f--M< g f I N .5 O o is* O' H 9 94 lw 5^ 5 o .9 %oo 3 MVo. o a O o >us o wB iS <4 > -k o N CO He tn 4 o eM9 S' a u 9 1 bo 2 H ptf W H JorJt He O V a m M 9 o r>3 0o O 6 #*=# 9 o . o *rmt >* o o O' e oe o o o oe eo - 00 9 e 0 * 0 0 * * o 0d o e 9 o * 0 9 * 'O 0 s fa Sex SI E JI3.8, 0 &eo O e 2 fa o 22 NEV 010013 WATER PCB-SD0000030984 $*tduiU*al BIO-TEST lal&iai&Ual' Pm. o o oo 23 9 3 2 Ui 2h NEV 010014 u WATER PCB-SD0000030985 Ptulnihial B I O * T E S T jSa&&U3U>iMi, Pho, 6A -* aV6O0 _CO 'Si _ 60 g g g 12 - ?s Mm tr> * \ M <0 n r- ^ 24 $ n e*oo n wXv 2 fo o ft oc u n O' n *>s 2h o o NEV 010015 WATER PCB-SD0000030986 indnUMal BIU I fc S I ate\al*Uei, !/hc. n M * 9 f*M< PM ra 0 0 o. fM v=4 fa * m ea fM *^04 99 0 w 4 f- tn 0^ foM 4 f*j. O' e f0 *n M #TM4 in fM 'O o. O' 40 fM 6 e- h eo 0 ' CM 4 00 *=f 0=4 fM fM =4 %eoo O' to M oo o en fMa O' O' O' oH 0fo0 *n - eOo' O' -4 $4 0000 fOM' mm--9 00 *o O' 00 If% 4 -4 * m fM s H #4 % m *4 m <*0 *$ H "4 Wo fM m =^ m4 m r~ a -3 4 H s Ua $v t4> ea o oC U 3 o -o - 25 NEV 010016 WATER PCB-SD0000030987 SnJudhdai B I O - 1 fc S i lamaUMcS, yc. 26 E. Urine Analyses Mean male and female urine analyses data are summarized in Tables X through XII. Determinations for glucose concentration were negative for all rats at every interval of examination. No' differences were noted between the urine from control and test animals at the intervals of examination. NEV 010017 WATER PCB-SD0000030988 PudtuUial BIO-TEST 2ahyiait>>ue4.. 9no. AS as m fM <* 0< I OAoS < o w *(0 X W oH m mv fTM*4 H4 V 3 u .kg 0a 6 J }Ht 1 ts a ce *0 a a * a tn fl aa AS c c oo a a ca aa AS a c aa aa a oO c a aa n c a 6 2 Ik V) ou oe O 00 2 ik o o 27 4 010018 WATER PCB-SD0000030989 jnduU'ual B I O T E S T Ja&tvuiU'Uci, $ne. 28 O 4* to TO to TO t*- TO TO TO ToO M0 7J o X W *4 r- TO a ^ O' to r*- 5 6 to t- I t- 00 s0 wB u aftt .d2 > * 0 1 > 4aX)t 9 4) 2 =4 fsl + H$ *r-4t ^ t) fi u .M9 & >> m2 9) ia o m a 12z2 b 8 0 o ** e o IOm>uO4 fs^5c ^ z 2 4 to z z r- rTO TO . C- TO C- 44 ** z +8 zz zz zz 4 n z z z z ^a*c4 Ui UiO Sex 100 54) 9v Ea o 2 8) h 4) SLg 1 rp-t o z iH 4) tt e=4*4) & 4) U n 4*44 II 0u o2 a>H 4o=4 oM tn 2 ii *5 U 6 it SU 2 4J ^*4 f\s m ++ NEV 010019 WATER PCB-SD0000030990 'Jtiduitoial iHW> I C3 1 x&MViauvue*, jne. e>*J C~n1 o m\ o o m *v ^ Oo B OW 3 5 el 3 sa 1 w a iuH? 1 f'nVnftHGK HI pf'Hlj 5 I h MD 0Ma u Vi 2 {* 1 o* fO o <# oeNo fv| rPN-j o pj o I a.. si m tr> u V tO (\) oo wOh en . O' o>n* m ron 4M O' fM - O 90 tn M o Moo eac 0 0*=! MO' Po'4 o e* *0 tOM O-l K 4 S C*4 o 5 ^V6Q,J O co O oo NEV 010020 WATER PCB-SD0000030991 PnJuliwd B 1 O - T E S T lalmatMMi, Sne, 30 F. Pathologic Studies Three-Month Sacrifice a. Gross Pathologic Findings No outstanding differences were noted between test and control rats upon gross pathological examination. b. Organ Weight and Organ to Body and Organ to Brain Weight Ratio Data The results of the statistical analyses conducted on absolute organ weights, organ to body weight and organ to brain weight ratios are summarized in Tables XIII through XVIII. Significant differences between a test group and the control group are designated by asterisks following the test values. Organ weights, organ to body weight and organ to brain weight ratios disclosed several randomly occurring intergroup differences. The lack of any consistent dose related response and the absence of any deleterious histopathologic change confirm that these differences were not related to the ingestion of Aroclor 1260. . NEV 010021 WATER PCB-SD0000030992  ffuLtiliUd B I O I E 5 I lohyiabyuu, Sne, 31 :'! i O 0 oo ft NEV 010022 WATER PCB-SD0000030993 S ta tis tic a lly s ig n ific a n t difference at the 99 p e rc e n t confidence le v e l. yaduilual D I v l c <* I j.awvwmet, jne. fc X O W a H <4 a'V. *> v aa tbo s o tn n - s O' A & u V n) aj n u <4 *2 OT [J 4J e 4mS o s i VPt fl X rttoot H 5 4>> W as fvl f\J VO SO m 6 0 e NN ff) r- o o<t*tn . <o ^ o't 4 o-4 Oo NEV 010023 WATER PCB-SD0000030994 Sndu-ihial B 1 O I E 5 I J'abQ-xato'uoi, $nc. 0 a 90 ct4 0 *<3 AS 0 N pH m O' 43 E m 9 fM cn \S 99e e=4 V Si O 0 O O O" <s4 A t) pH pvj pH pH f4 pH m rt 0e (0 s 0 0 O 0 to t* 0 33 TEST M A T E R IA L: A r o c lo r 1260 amv 00 t- <0 fvS tr> m n < m Am B 9 0 0 9 O 0 e*a 0 M & h o V a 'SrOO- < e-pe eo 6tm04 e- NfcV 010024 WATER PCB-SD0000030995  ^uUUVUal D I %J I C9 I xatmaume*, yna. 34 WATER PCB-SD0000030996 WATER PCB-SD0000030997 B1O-T EST Uno, ^m 4<WH3D> vp^*TMd* v > ^=Vr4t 6 V fa JT-* to 6- r t(Mo mon CNS n n SU a*rt Ls W j o m v s 00 f tn lfAsi * m *A A & & 4) o V a O CHJ ei rut T3 W C3 <4 4463J0 Co V > *V b9o 6 0 Q V 1 a 4J a43 bao 6K0* ihV \pomj v o M tvO o M 6m- O fn O' A 6 o i o o .a O 60 O U fM o o O 0s 09 o m g e en m "t oooo s es m u O 6 w -1 fM O' O09' 4630 g U< IT h m r- IA i o o M o 9 iM o 36 TABLE X V III NEV 010027 WATER PCB-SD0000030998 Pnduihud BI O T E S T jtol&uU&iici, 9*tc. 37 c. Histopathologic Findings Histopathologic examination of tissues and organs taken from all animals from both the control and 100 ppm groups was conducted. Tables XIX and XX list all histopathologic changes noted. All of the lesions noted in the microscopic examina tion of tissues were those of spontaneous disease and are not unusual for the albino rat. The most frequent findings were lesions in the trachea and lung9, indicating chronic murine pneumonia. These oc curred in the control as well as the rats fed Aroclor 1260. i NEV 010026 WATER PCB-SD0000030999 StulMtMal UIW* I I JlalKnalvticl, 'Jne. 38 O TABLE XIX TEST MATERIAL: Aroclor 1260 Two-Year Chronic Oral Toxicity Study - Albino Rats Histopathologic Changes ' Three-Month Sacrifice Group: Control Number of Animals Organ Examined Findings 5 Males Trachea Lung Urinary bladder Tracheitis Chronic respiratory disease Hyperplasia 5 Females Lung Chronic respiratory disease Ave rage Incidence Grade 1 1.0 1 3 1 1.0 1.0 1.0 All other tissues and organs were normal histologically. Grading System 0.5 = minimal 1.0 = slight 2.0 = mild 3.0 = moderate 4.0 = severe 5.0 = extreme . ' . ' i . NEV 010029 WATER PCB-SD0000031000 " PttJttihiol B i O - I t b I laimaUMU, Vhc. 39 TABLE XX TEST MATERIALS Aroclor 1260 Two-Year Chronic Oral Toxicity Study - Albino Rats Histopathologic Changes ' Three-Month Sacrifice Group: 100 ppm ' Number of Animals Organ Examined Findings 5 Males Trachea Lung Tracheitis Chronic respiratory disease 5 Females Trachea Lung Kidney Tracheitis ' Chronic respiratory disease Focal lymphoid infiltration Average Incidence Grade 4 1.0 2 1.0 3 2 - 1 1.0 1.0 1.0 All other tissues and organs were normal histologically. Grading System 0.5 = minimal 1.0* slight 2.0 = mild 3.0 = moderate 4.0 = severe 5.0 = extreme O NEV 010030 WATER PCB-SD0000031001 gndiOUial tt @ U I t y i XoSo4am40i, Unc. 40 9 l I iI i O 2. Six-Month Sacrifice a. Gross Pathologic Findings No outstanding differences were noted between test and control animals. * b. Organ Weight and Organ to Body and Organ to Brain Weight Ratio Data ' The results of the statistical analyses conducted on absolute organ weights, organ to body weight and organ to brain weight ratios are summarized in Tables XXI through XXVI. Organ weights, organ to body weight and organ to brain weight ratios disclosed several randomly occurring intergroup differences. The lack of any consistent dose related response and the absentee of any deleterious histopathologic change confirm that these differences were not related to the ingestion of Aroclor 1260. NEV 010031 ! WATER PCB-SD0000031002 * S ta tis tic a lly s ig n ific a n t d iffe re n c e a t the 95 p e rc e n t confidence le v e l. * * S ta tis tic a lly s ig n ific a n t difference a t the 99 p e rce n t confidence le v e l. D 1 U I t i I Jtab&natvueA, 9mc. O o S %o ^-} 2 .a m o w m g bo 7<boJ W H W >s I w 73 xo H fdH 5 o *a ohb ft o a Its o 9 X6H0 V f6sl0 U a o 4 sI JwJ V B > 9V s e-i w bt> .fc *4 <eM B6 u ; oi* ft a1 a*00 a flgit rV co r o r0=*# 4 erbpt 0> a tbt s O * * W A o * m m5 a p< 3 26 MtJ 0 e 0 m # e *> tn n o SS * tOJ wM _ wv * # 0* h- O' * tn * O' * 9 a 0 0 e 0 M 2 ^i fM tn 0* ob V *# a in XM SV o in V lb s 60 Mb O * * ee * o Wd M 41 S %oo r>l ft b . Ob oo c - o o <4M *ou ^^ o u Q NEV 010032 WATER PCB-SD0000031003 $tidjtiVual B I O T E S T * S ta tis tic a lly s ig n ific a n t d iffe re n c e a t the 95 p e rc e n t co n fid e n ce le v e l. Unc, o9 & 4J. X 3 ^ g *A*>* *CVmM ^\*4> inM .^M (M 4 tin 8M14 ii s <IM..m-* .m<O--.l'. .O<--' O o ^2 P4 ** e Sal ?> oo S0 WM _ Cno 3125 a*4 s 0 * * *o*tA*** .CVA.OO* .fAlo* Ao*..fo- .r- .mtn V x46>*0 i>2fi mh *55 M$sAi w m Ov 3 2 OtN*-.' mj.(>sj .tmnn .mpan , 9 * A* O^ tfAOe* 00*0%n n O0%' 41 > O ao . <M < E Att e2 oO g w c*J o u *4 -* ** .2 ** Q< NEV 010033 WATER PCB-SD0000031004 ^ I * I b # JQUi. -a^ S ta tis tic a lly s ig n ific a n t d iffe re n ce at the 95 percent confidence le v e l. V OM o *4 fr V<4 z^ Q wO ` HbhOUo < EffC>t],| C o O o o # nev 010034 WATER PCB-SD0000031005 * S ta tis tic a lly s ig n ific a n t d iffe re n c e a t the 95 p e rc e n t confidence le v e l. I. io M W i 49 @ 4.feMM e?FU*. * wO' or o tn fNSOS o o oNorO>9 & rofo'-e o 4 m4 m'N4f 4*1 t|'-*4 c*. r~9 Or-' tO-' w A MO0 \J Aj o oe ooo Omn4' o NNOOnd o o MNO9 o NN0OO0d o NooO4' # 4 enOOo' o * o or- oooo mm % ftMn4 N#AO* in *A>4 rt 44 osfts* GO 445* o4-4 oco--1 U NEV 010035 \ WATER PCB-SD0000031006 * * S ta tis tic a lly s ig n ific a n t d iffe re n ce a t the 99 p e rce n t confidence level. ynditiVuM BIU teal xam%awm4>, yme. O 5 I @0 cn C0 ? 55 6 n in o eo r* o o o c in o ^h |s^ tiO ! a t> smh s rw <O' o 0*0* O' f4r-1 5O Im 4) CSS r r i eo o r- o so * K O A 6 to 0 fsj n n OO o s a, 1./ m u fl 3 <4 P$ V o u euP4 V 0A H <4 6 44&VHSAs * oc 2 u 1 3W) is w 4 fl <5 * Vt 3 a > CM eo C0 eo m 00 CO oo X fsj CM M css 0 oe o O o o S #0 p, O <$ m v a mo t-si| m o <o o N ft g 2 t> & w> I oI* V *3 m n*o S 45 H3 3 CaM . <oM to< Ba *<4 rOo2-t wQ, *ohO* 8 o --o wev 010036 WATER PCB-SD0000031007 O 5 6 I o mB * c ToJ H fj 6 4>f e i ;' / TEST M A T E R IA L: A ro c lo r 1260 * S ta tis tic a lly sig n ifica n t d iffe re n ce at the 95 percent confidence level. NEV 010037 WATER PCB-SD0000031008 ; V Stuinit'ual B I O - T E S T laimaU'Ued., 9nc. 47 O c. Histopathologic Findings ' Histopathologic examination of tissues and organs taken from all animals from both the control and 100 ppm groups was conducted. * Tables XXVII and XXVIII list all histopathologic changes noted. All of the lesions noted in the microscopic examination of tissues were those of spontaneous disease and are not unusual for the albino rat. The most frequent findings were lesions in the trachea and lungs, indicating chronic murine pneumonia. These occurred in the control as well as the rats fed Aroclor 1260. 4 o NEV 01003a WATER PCB-SD0000031009 Sfjulkld B I O - T E S I laUtaiMded, 'Jne. 48 TABLE XXVII TEST MATERIAL: Arcelor 1260 Two-Year Chronic Oral Toxicity Study - Albino Rats Histopathologic Changes Six-Month Sacrifice '' Group: Control Number of Animals Organ Examined Findings Average Incidence Grade 5 Males Trachea Lung Liver Skeletal muscle Tracheitis Focal tracheitis Focal pneumonitis Hyperemia Focal pericholangitis Focal inflammation 2 2 1 2 1 1 1.5 1.0 0.5 1.0 1.0 1.0 5 Females Trachea Lung Liver Kidney Focal tracheitis Hyperemia Hyperemia Pericholangitis Focal inflammation 1 . 1.0 2 2.5 1 1.0 1 0.5 I 1.0 All other tissues and organs were normal histologically. Grading System 0.5 minimal . 1.0 * slight r~ ' 2.0' mild '. 3.0 * moderate 4.0 = severe 5.0 * extreme O NEV 010039 WATER PCB-SD0000031010 o i ^/ * t - J xaw-vmvuc*. j/hc. TABLE XXVIII TEST MATERIAL: Aroclor 1260 Two-Year Chronic Oral Toxicity Study - Albino Rats Histopathologic Changes Six-Month Sacrifice ' Group: 100 ppm . Number of Animals Organ Examined Findings Ave rage Incidence Grade 5 Males Trachea Lung Liver Tracheitis Focal tracheitis Focal pneumonitis Hyperemia Hyperemia Focal pericholangitis 2 1 4 4 1 1. 2.0 0.5 1.0 1.5 1.0 0.5 5 Females Trachea Lung Liver Kidney Focal tracheitis Focal pneumonitis Hyperemia Hyperemia Focal pericholangitis Focal nephritis 2 0. 5 2 ' 1.0 1 3.0 2 1.5 1 0.5 3 0.5 All other tissues and organs were normal histologically. Grading System 0.5 = minimal 1.0 = slight 2.0 = mild 3.0 = moderate 4.0= severe 5.0 = extreme NEV 0100*0 WATER PCB-SD0000031011 * $ndu.lUiai B I O - T E S T JtotmaknM, Unc. 50 3. Twelve-Month Sacrifice ' * Gross Pathologic Findings Gross pathologic findings among test animals were not significantly different from those noted in control animals. b. Organ Weight and Ratio Data The mean organ weight and ratio data collected at the twelve month sacrifice are presented in Tables XXIX through XXXIV. % Statistically significant differences are designated by asterisks following the test group value. ' Organ weights, organ to body weight and organ to brain weight ratios disclosed several randomly occurring intergroup differences. The lack of any consistent dose related response and the absence of any deleterious histopathologic change confirm that these differences were not related to the ingestion of Aroclor 1260. " O NV 010041 WATER PCB-SD0000031012 o I I o o3 ts3 a <4 2 vQ o w H o Ra a 9 H oc (4 Pi JS IoX <d H c o 3 4J Ies V u <5- * a* C sou U osi at c (4 w h * (4 JfHt) <5 O VM m*4 4* cd *c i be4o M fh--9 v e*- m '*c<o4e P* fsl m y 5*4 ^ "tS .gw u t e5 IV ) dtv W> s 00 o O' CO 0 o m 0 O I - -5 3M) ^ EV ra tnn o in 46A*9 n O' p- tn `J bo ti |4 V 2v-* bo m # 9 t> O' O' o o s 9 260 bO g l p m P* fst N tn 4* o ft) a A6B *4 g V >n m f*- t fO - *9 * M g- fes 0m * ov 2a M IM *4 O oM CO SO * 4r=t5 ; te) P O u c o u -- oo ft) f>t) ft) --Va fuet) Vuc V ft) *0 "O ej 6C oo uo ft) 0o ho oh f0t)4 If)t. m^ O' O' ft) ft) 55 .iJ 4- n) <4 o> o> C0ft) CV U .ft) ft) S3 d *0 9o 9o %4 *e=4 oe4 4 6 S) 4 44@tu4d43 i4Hutid4t 4p4i 4e4a) 4(44 <4 WW ## <8> NEV 010042 WATER PCB-SD0000031013 * * S ta tis tic a lly s ig n ific a n t d iffe re n ce at the 99 p e rce n t confidence le v e l. ymaunuoi. di w a %. j a S<IC. O i4 4J u> tOo' to O' TO XtHo 47 * to S <4 i 9 V47) a 2 Or-' vO o fSQ| fSV-40 tt*oo 0 M 2 (2 o 5so JS=o4 < e * to *e*4 oe4 X o H rt O u #u U3 9{=5 ort W 5 C 0 2 1 > 41 4eJl 9) JS A o 2 m 1 *> n 4= w _ *3 0g S tofe ^o o o 4* .d 4) 9 4) 2 o tr 47 *o=4 c (t4o o7. oo to "CNCOJ* w 0n <to3 'irt u2 O fi 9 of^e 'O 0 frTMS* O m fM 0 TtoO O0 VotO0 0 ttOrooe tmro-9 V 7 uc0V tpi S ou +e* Vuh oao 4w5 <4 bfi uw U 4(V7 , in O' m v<4 # * um\ 0 rt#oQ too 7 X oo > H MtHo 47 n fM M M v Vc V S3 to o$4 m 4) o to* O o *3 2 m u sm d 4^ 90 Et&=t3 47 47 *i e si 4* to O 0>4 c0 u * o u 4# V) WATER_PCB-SD0000031014 S ta tis tic a lly s ig n ific a n t d iffe re n ce at the 95 p e rce n t confidence le v e l. I I JS 3 i UI Vi (v4 0 <M4 a W oI (4 *0 9 9s <J o 4e4 l * (4 fl fe4O Vi W O NEV 010044 WATER PCB-SD0000031015 * S ta tis tic a lly s ig n ific a n t d iffe re n c e a t the 95 p e rc e n t c o n fid e n c e le v e l * * S ta tis tic a lly s ig n ific a n t d iffe re n ce at the 99 p e rce n t confidence le v e l SitUiOfiau v/ i & i i ts&ueMptests*iH'-S, o 3 *> 05 rt 43 fHei) E* U V * "m S> d0C0 M Si > il 8 *3 oM h 2 * M rm- tn oo 0 oo f- nj p=4 d* r*. eo AS in in 0 0 o O' 09 wW 0e 0*0 =4 H *>. o o 2 V> *n r- m Jf &v 4od=H9 | > o 05 *3 ft 43 c .b*Oi 4> V 60 ht tf\J O m fM o o O' 0 *n Al o o o s ao : > o o 0 wfeO a44603*0)0 2 o d O 8mv> O s j Rtrafyt U o 0) V T3O s *0 O' m IA IA q@ O 00 tm CO O' A 0 g fbeO w o fl t) "0 eA O M p4 w m H *4 M 43 60 dc t> 0 Q o # Ik e sd 60 a ob iSwtI d< CO tn c=d m *> *3 e 0 0 2 tn tn * <* > O 7fr E& fa p(1 w + b c 0 u ^4 ' d o m*4 V 5 WATER_PCB-SD0000031016  o xs <4 --i J4t3e=43O <4 0u *o O9 m m vs ovo tt to a4 s > n ?n ra o O' m s v0O0 to 2 o o a0 < 1 m f- *-t r- o a WAa* aFu4 2 a e\oj on on ^n JWa) ^ H c tul o 9 *3HKo A a 0c 21 tf 9 J4Ct>4!0 V.<-> soC14 is*) * fee 4 u rt av > *4 nofl to *n <--3 A O' VO f*- o8MU o8? 2 \80 o M9 O fM9 o 049 O UJO o u urt fVJ or v-o w Ho* -* m r- vo O' *A vSO 4 o o o NEV 010046 WATER PCB-SD0000031017 duiliial B S O - T E S 1 $ttc. 56 TE S T M A T E R IA L : A ro c lo r 1260 t NfcV 0i00<%? WATER PCB-SD0000031018 c. Histopathologic Findings Histopathologic examination of tissues taken from each rat sacrificed from the control and 100 ppm groups after twelve months of testing was conducted. Tables XXXV and XXXVI list all hisopathologic changes noted. ' All of the lesions noted in the microscopic examination of tissues were those of spontaneous disease and are not unusual for the albino rat. The most frequent findings were lesions in the trachea and lungs, indicating chronic murine pneumonia. These occurred in the control' as well as the rats fed Aroclor 1260. 4 NEV 01004b WATER PCB-SD0000031019 90 9 TABLE XXXV TEST MATERIAL! Aroclor 1260 Two-Year Chronic Oral Toxicity Study - Albino Rats Histopathologic Changes Twelve-Month Sacrifice Group: Control Number of Animals 5 Males 5 Females Organ Examined Trachea Lung Urinary Bladder Trachea Lung Colon Findings Incidence Average Grade Tracheitis Chronic respiratory disease Calculus l 2 1 1.0 1.0 1.0 Tracheitis Chronic respiratory disease Parasites 1 0 1 1. 1.0 1.0 1.0 - All other tissues and organs were normal histologically. Grading System 0.5 * minimal 1.0 slight 2.0 mild 3.0 * moderate 4.0 > severe 5.0 extreme NEV 010049 WATER PCB-SD0000031020 Sndidbdai 8 I O T E 8 I laUrnUum, 'Jhc. sv TABLE XXXVI TEST MATERIAL? Aroclor 1260 Two-Year Chronic Oral Toxicity Study - Albino Rats Histopathologic Changes Twelve-Month Sacrifice Group: 100 ppm Number of Animals 5 Males 5 Females Organ Examined Trachea Lung Kidney Liver Trachea Lung Findings Incidence Average Grade Tracheitis Chronic respiratory disease Focal lymphoid infiltration Vacuolar change of random cells 1 3 1 1 1.0 1.0 1.0 1.0 Tracheitis Chronic respiratory disease 1' 1 1.0 ' 1.0 All other tissues and organ* were normal histologically. Grading System 0,5= minimal 1.0s slight 2.0 mild 3.0 * moderate 4.0 s severe 5.0 extreme . - O NEV 010050 WATER PCB-SD0000031021 Jndullual B I O - T E S T JafotaUttei, 9mc. 60 4. Final Sacrifice a. Gross Pathologic Findings Gross pathologic findings among test animals were not significantly different from those noted in control animals. b. Organ Weight and Ratio Data . Hie mean organ weight and ratio data collected at the final sacrifice are presented in Tables XXXVII through XLII. Statistically significant differences are designated by asterisks following the test group value. Absolute liver weights and liver to body weight or liver to brain weight ratios were significantly elevated in those rats fed 100 ppm Aroclor 1260. Other organ weights, organ to body weight and organ to brain weight ratios disclosed several randomly occurring intergroup differences. The lack of any consistent dose related response and the absence of any - deleterious histopathologic change confirm that these differences were not related to the ingestion of Aroclor 1260 . NEV 010051 WATER PCB-SD0000031022 DtululVUal B I O - T E S I Jai&mUtuS, Pne. m <4 o4 J*oO*o m M E .40 IM %o 60 %PO'DS' o o 1 ^ (3 o r2Nt ^w60 "fi t <WM4 ^ts)| <4 O2 n O' opa * O O' f~l 61 & 43 O n (4 v->4> (0 m o mn o* pa *4* 4J E m n n 5 t* o 5a * S w5 H 5 a f) v o 43 > 40V Is rt _ 2 J6H30 o XuM oH> aXui <4 w (4 .IV5i M a a <mH4 O md Pm <u *3i t O DO w c<640 VV) fl) 52 n o 0 to t^. er^ol * r* 'Oe 'I* ue e*0a o<&M4o >4 *1 o >*) n 'O *# (4 84> 0a m 'O o e M Am h 0 M54 w60 6 v <4 2 oMl rfa'l r*J #* O' Ora' 8 h o a* M So ~ 2 o o U eV-4 i-->S Vco oc **>Vft tJfVpt# (ouS uCoS 44 *J aa V t> uO 0 VuV aa n O' O' O' 0V 55 44 44 <4 <4 0V 0o (t3t aV AX> JX> ^aes*4 a40 s s<&d uu a*t a*4 0Cn=0! nC6f0 x s. <O4 O4 am#N am wa wa . NEV 010052 WATER PCB-SD0000031023 UI w ,,A (MH/ytldiUA U&, Om d M O' O N afsoj O' r- ** x E * B-4fl fej .5 " 2 *> o O' O' o otos --Vrti M (ft \8 n o tn o d* 0 o 2OoO OJ O *5 TO <^5 2 . 48 L ^ pd o * 7fJt w5 o U 9o *o o H *dH 4J fjoHfio V o ts 0c * oo M O O 4 tf V |M 1 o o a *> *4"4> * TO M TO (4 co < < Ci E J4iOVSsJ4O ' tofl V fc. av u s u V ft m .s c c D 0=V4 a > -oo r 00 w rct es 60 u O w f--vrt4 2 O 00 --< o TO r. o +4 tn -4 o m o TO n IA O' e- f- 0 a o o o o H crt *w no w 4t-t4) *-s e-i O' o e-a eOo' O 2 J? >0. o n n o -* o o U NEV 010053 WATER PCB-SD0000031024 om tf m m f6 o Ce*O-a r- o o to O' *A o Jr63a0 6 t> o Q o o m S> Cm Mm oc d 6N0 m Wi>>H !A Q 2 =# * "n03 to to >e* my 010054 WATER PCB-SD0000031025  jeuU4ii/iud4s u i w * ;O I. J ii i i <d*U44-. oH 4c*efM2Ht)a ft) 13 (0f"t 6V f- o fc frs*-* r- o OS 6O0 oo <t< sr0- o .S " i3 w "e <mu4 V4>) o V0 rt eo e 0s 60 s* eo eo o O' 9 o 2o o o o bt> eo eo 0S O' fs* eo eo 0} fS| fsj fsj 6 6 9 oOO O I # * w 9* er-oHt Os fSJ 9 o 9 tn M fM e m #*=9 9 s O o o 5 TABLE X LI ; ; ! ) > il m a) 4 ' i4> Q o u c o o o _0 e v M e * 8 sa 6Ha0 X a (4 u a w 1? < NtV Q10055 WATER PCB-SD0000031026 SiuLtUiuil B I O * T E S T $nc. w E , Q 8 S60 in!3 ^6 ho fi> m in mm<*a 2 m 5 S rt (n I 8 ^ 'S M *C3 3.3-2rt & SS \J * vO m * m m 0H Tf V0 d w o .s oo 3s s sO tt A X a %o --i * . U o S*N I *8 o. w 0 rt Ir u *o V 1 S. S H5 O 0u) f4 ort W r** .S d 40 0 d rt 43 ?* X *- *8^ W OJ "5? V ns vO en o f\J o* m s* rn # # in m Cee'On o $ *e8o l o^ I S U* U o J? g ^ n M n u 0 0 wNa ccs g5 m nw O O 4 V m * s0 in t* O' O' O' O' 1 o v Ss M Su m4, --t 0*h0 m* 2 a i nS ns ni ns 66 o h Ji ^ > tol c o U oo -* o NEV 010056 WATER PCB-SD0000031027 SnJult'ual B I O - T E S T lalmat&tici, Sac. 67 c. Histopathologic Findings Histopathologic examination of tissues and organs taken from all animals sacrificed after 24 months on test was conducted. Tables XLIIl through XLVI list all histopathologic changes noted.* Table XLVII contains the results of the histopathologic examination of the urinary bladders. Significant liver injury was found in animals fed 100 ppm Aroclor 1260 (T-III). The compound associated lesions consisted of vacuolar change, focal hypertrophy and focal hyperplasia. In addition, there were lesions of inflammation, necrosis, fibrosis and minor degeneration in this group which, although seen in the controls and lower test groups, were more severe and frequent in the T-III group. The vacuolar change was not seen in the control animals but was observed occasionally in livers from T-I (1 ppm) and T-II (10 ppm) _ animals. It was frequent in the T-III animals. This lesion is morphologically indicative of fatty degeneration. Formalin-frozen sections of livers from ^ represenative animals which displayed vacuolar changes were stained with ' Oil Red 0 to reveal the presence of fat. The vacuolar lesion in the cytoplasm of these cells was positively identified as fat. The hypertrophic change found in the liver was focal and often limited to the central lobular area where groups of cells were swollen to two or three times their normal size with clear pink homogenous cytoplasm. The hyperplasia was associated with the same cells and appeared to be an ' NfcV 010057 WATER PCB-SD0000031028 $*uLtiU*al B I O - T E S T lalMat&'Uci., $nc, 68 extension of the hypertrophic lesion. The hyperplastic cells were also usually hypertrophic. The most severe examples of hyperplasia appeared as nodular growths with limited compression of the surrounding normal hepatic tissue. * The minor lesions of degeneration, hepatitis, ductule cell proliferation, necrosis and focal lymphoid infiltration seen in the control animals and the T-I and T-Il groups are lesions of spontaneous disease and are not related to the Aroclor 1260. This level of liver disease is not unusual in old animals. Hyperplasia of the urinary bladder was found in an animal from the control group. This finding was not present in any of the rats fed Aroclor 1260. All of the other lesions in other tissues found in these animals are related to spontaneous disease and they are not unusual for old rats. Donovan E. Gordon, D. V. M. , Ph. D. Diplomat, American College of Veterinary Pathologists NEV 010056 WATER PCB-SD0000031029 . jew*. OV & o f5| t> ^ <$ oooooooooooooooo 4) o e > 3 (nO'HNH(n(OMNHHrttHN u a 4> n b m (d B a a g-s 2 s s 3X S fl o a M 60 O o W 6-1 3 id ri .s g4 ^ * m o g u * ft g *< o *41 0H1 g m .s *e .s H (4 oU fi 3 o o H V N id es O X' o< Co iLd *Idi *wfHt NVfi Vo UH 4^2 *O* .ONflorud pIuj U l*< Q 4f0=H*4) mw ^ *5 w fed N o3 ao 43 v ua 41 <ud mH 6 ts s, 4M3 "" ft^ -h curt .y p S oM w 43 _ O H ft g *4r3t 6 6 id U <d ft t) m i"s 0H1 frj-s u 43 ft ft xx O oWH> 4.Hr3t C id ,2 ' rt -l iud o H a U* id v 4CjJ 4o3 oa tpj, id id C > o k p .5 s 6 s Xs 5m 10 <0 ft H .9 4U #X mw 0) V d #4 NEV 010059 WATER PCB-SD0000031030 PhJUuVuoI BIO-TEST Xa&o'uiio'uci. Stic. 70 o ert*n v tj UV t*o4 OOOOOOIAOOOO oooo ooo * e fv| ==4 p=4 pM S* fH O *"4 |S| "4 ** e=4 --< 'tuc*s> u 5 e* ^ ^ 0< I %o < favj N o X *g m 64>0 u o -H w oH 6 V u ah-t o i? g x 60 y O o H O$ o *3 5 G0 d to o< *onH* .s fn a (4 o a N av >1* o a V V) .r i |9 8. SITJ 4> cr> 3 g XUMo3 3 *d O du o tK B *d IS .g V) fhHlj -2'g4 d H f~ $a4 .<2M y o $w H 1 *r O ei > M v V^ 73 yy 6S5S M a y n 3 o u g d 3 30Z> **nrfH*tt ctor *3 6C t-o. *.a <14 Co Q* 5 <fMl) *3 d cu G o y j ao<a n m'rt O b V **tH3o o 6 y a { % OG d a Zp4J ^ N * it is 4> fr c 6. d-- V to jz o o u ox aa, o uj d *to4 *G2 <0 d 7l3-l* CQ m t d u 6S0 (Pd O G ^ *u O>4 & oA H^U a d uf=< to o <0 u 1( it i oc 7J V fi E 'S o ym a *H ww I rt a tl 13 60 0 <4 (i44 Ga .5>- SHJ4 |ii| o oS-52 m (CTl UC | E : ii . 02 o { fSJ r g V4 o 4M> C--4 <MH |5 u rt E V Ui NEV 010060 n ytt3oo to E- M cH '. V X4J o E' ii a mc < o WATER_PCB-SD0000031031 ">(5i Sg r OOOOOOOOOOOOOOO o c V *D f\| --J TABLE X LIV Sem inal V e sicle o f>3 Uo m W> m o(4 m *2 89 fl 60 0 1 4* w x S a a O m S* H c* e* Twa3& rKt U O X <4 ou w **4 -! 4* o * coH Xo 1-1 (4 UH n -) O X. ho 4<4* fes m a'-g CH O 0> ft) n tai M ^(g4 O |V4 J! JS m '2n B fH u <4 o 43 8o 0 6 O h h ffi V J<4J Iys! *nH as aw rt TO0 H u^ u o^ ga *J o*1 4K3 3O C U < ffi d *(34 n2 4h*** dmSi 4H3 " - a*0 eN ,2 4 3 u *2 eco cou .32 O rC UUH nhU uco cco Jrj o) J 2E6 Sr1 e<4 ert ft S 5 (4 W crtdt. h(4 'S<M4 Mdp (.s5! IH J4 0 <4 1 ! Si! 5 $ C 43 X f> u d A L^2h 3 ou 0. 4 0 2 3B !< w rt 2 NEV 010061 WATER PCB-SD0000031032 2>*S 2 2 oo OOOOOOiAOOOO O r Pd d eH P"4 fv| **H PH V V *000 fsl f\J cn ^ eH TM3 M pH p=H eH f\| TA B LE X L IV continued A c a n th o s is n4m> 5 6 4U) --OMuHl *H o Wid o tg *3 id .a *mo0*4 (n aa a g 0 <4 dm > n fi4 c SHo ' a I if h^ u n f> W *uHo **uH0 m0 jg<nO4 2S oX oX ux 4oJ 8 6 tMHd _W <od <ud ,2 ,2 OO m *XH3 > *o 8 fO *2 "b 43 '2 o o u o <d 5 fiJS 8 UUHUJn ao id id cS 2 .ort *u-ah 43 V *tt-*4 4&3 41 iod to, mo60 O S' d >>..t2s Sid -*u 43 w o id * 60 id o rt J2 >U TeJ p(-4H O TM* iGd 4PO) O 69 8 t N 3g -S s h *4 a mu Id 2 NEV 010062 WATER PCB-SD0000031033 %-v 2t 4 ooooooooooo UC Vo *0 ff) 'iji O' K> -l m .0 * .s 9u(4 O s<4 r* ov4 tg-<) w dhO^(4T >mdmoH Cwn> K <2*4 ^((fX-X>l X C JtUhVcCrAttM M*4W46HCiu34>0 ROw64)0 UUhco X (4 (U0a4 oo> m r-t cum aC>M *oac=>t .-6crU<t0 H ir ,Cl '2*d(oo4 2 \aoMOd 60 Oao fotf c IgaVV. wOw *a 6^ 2 mo 13 6o Ui NEV 010063 s9 a*(yeo4-*o V *> .45aK-> Vm vH ii it (0 o o .4 <4? in (4 Bo rMt 2a 'oo B& I H * 'iOHrMt o <m o <n o 8 m V gm u V o i ii tn o 3 oft - WATER PCB-SD0000031034 0tAs, n r ooooooooooo ooo o> ct) *0 n e ^ TEST M A T E R IA L : A ro c lo r 1260 m vw> c a a8 g& o60 o 0 4 W .d.l 1 grS &o to (5 Ml TBrJ* to w <4 'eU#o=4 M *nVH0 <ou4 >s >> oM - (4 u2 *xJ 8V)i UqH J#yC UcH XhO J(h34 XN OHU *u J(Ud4 60 atV4 y<t*4 ca j 8 >o #4 (A I o S eTM3 rj Ss 4 *2 t. e o ^ 2 -S ha 6 <c 4 4) u Sui m a(44> h(N4 ^C3 m V S5 j n $E 2 13 t>- V (4 BV to NEV 01006^ WATER_PCB-SD0000031035 HtuLuUiaL B 1 O T E S T XaluHaivuci, Due. > <D n i opHoe"H *ooC^ oH o*HoH ofSj oP"H oeHosHo*-4 75 T A B LE X L V continued o rOcfo<) soO 6hO *o3 *> V 60 s Vu pMooVHH y W 3 s. rt .5 o 8 aa, o a *4 o f) V tT +> s S. MU C n ao fa X>S5Is<(OOf8nd42f>i hpMHHwmM&3O&iU*jM=&ronyocu*t( f,SIyuH2uqyWH*ttj <oA+orMw^ay.'/ S*iSo^0oawcEyH>.i3X?4'4^y0:ae3otj*3?h->.2*^i2-h(0-j1 u3odw**o h3..U2mmomy2221J^^tw3o3*Uwwycoto m h y > fvt y c 4y3 fgt S >> p ,t{ S l^-g y 2^ w* wa-4 j3K y y fa NEV 010065 Sk a fyt I $ t4 60 O p4=o-H* H y It it oo 43 m O c y rhVt y * 46*VJ> 1 St oo o OM cp0H ^4 en cV M3 ft O m y J3 H X y C t/ pH * w o H ii tn o o# -- WATER PCB-SD0000031036 0v Sf-O 2g 1 OOOOOOOOOO OOOOOO fM "* ** ** eH H em osiderosis Focal lym phoid in filtra tio n C alcified concretions in pelvis c> *e 0e'rtNHrtNHNNN|v,HH u 2 5 o .9 s T3 5 w J feO B 06 6 U (X *4 X W o *4 BH Pi H u 1 H u3 O u 3 0woH g d -04 m p*4 B d CU S 0 (X o o o Vi O u0 & V n SmMl .s Ui n rt 43 V w1-4 o M S. 0 *o nl .a 0O O0 ^ -JJ (X 0 4) U 00 .6 a *JJ <w2 Oe ' fVii 4) 'JrvJt 0 43 BO nl & 45 8 080 cO nuo M 0 *433 - 0 3 o .2 0 <8*5 o oa rj rt s w -a II a o b0 6h a 11--4 0 u o 02 BO CC O 4) g s 0 "v"4 6U huo H 0t> o9 ft *VV S p le e n K idney W oo c u 0 > i3 fed 0 4) *H 0 2 o NEV 010066 WATER PCB-SD0000031037 9 V *4**^ m& O ct9<Ajn 77 w <M4 o V . -5 O O O oo o oooooo Vo cv on=* ewa *M e-4 ff| 4 43 #hm mm T A B L E X L V I continued t*>>o 9 43 u 0 fVo-ot u hH O n) W -* <d aa. o-4 aa rad .s O M w 1 +oH*i 8 o 4 * V JH I 0 m w> C U .8 LJ "=i 3 3-i33 &SS *a S 5 o c oe 3 . >* *> i,,*d 32 *23 8 8 6 g . W O >* *4 3# D K h ftiH < 0 e *-s imd (o4 ot o o4 a rt ur ua o a 0 a id ssII a JoH3 id 6 0 o 3o T5 id OOW> 4 *. J fMt iUd nOfi &5 0>4 Om 5; d IE f0"4) s *3 g NEV 010067 in WATER PCB-SD0000031038 bo o S2 1 ooooo tsm4 m=4 *=4 IfM oooooooo A ll other tissues and organs w ere n o rm a l h isto lo g ica lly. S3 2 uo 'O ss so3 w5 wV> 60 o <H a 04 H6oo0 Vul Wrt o o .atS la 4rWWoaJt 6 a Vu "d0O> IA fM *0 CO h H H H H nH) fl) Pm a g *No H sy Vr0<)i JC * B .3 o gOa, j* r^oHaH 9 6.2 H .2 8 rt UVp4 J22 o> ua T3 a 2 x 2 U g wH 8 3 I0m bcHd CH 2g. sg |2 *3(*i B E a h c<}3 c z -a ioyd O 4mS X>Is u #iHd 'o , VH) ow VVcvi ogVyl W & rat HpHa *fal1) >Oo* rTyo{O y 3** H -eo 8 iad *o Sj .*3 x** w w `r* "aCyH vWHi J^aG S* y C S3. 04 ^ ^ saH Zw, Vidi fi Vto a Vi OSsV oo o8^. hUO2 u K O S O H 2 U 2C o 0%) V .a I1 >couu w S V>0>l 3 ff *t0f4)) BV h m 1 IT? 82 e X j rt 5 fl D 3 t! l & * 8 2 | o V><l Md (S NEV 010068 WATER PCB-SD0000031039  Mrt ) *<VMo4 O *PmucVuo"l --* C^| I *5 TABLE X LV II o 4<> S o <NmX->i ^ < n x 0 *3 o * tBo rt .5 sV y *oa vo H erh*Ht MV 60 OrTt o .a o c o fy6o=*0 6 -s M >* 5 4roa=f V H W t*- oe-i vM a IOA V) S &rt m VJ- v '0O MC l W& 5^ 60 5a ft W H gy uV rt .9 V rat w upi o ft 0V I.9 Ve no eo 5a 430y> 1 o Va Hi ri 60 a o> rt .9 $v ou a o ft a -H T* r* ^ o'# 8 2ft 2 ft 2 ft 2 ft to ? Sm O O a *- aa H C. i t_j m< mi o Hw I a| ,o H3 H N PI NV 010069 WATER PCB-SD0000031040 . 2na44it'%4tH U.U4t&iaUM4e4, jnc. G. Detailed Description of Tumor Findings Tumor data for individual animals including location, weight and pathologic classification are presented in Tables XLVIII through LI. None of these tumors could be related to the ingestion of Aroclor i 1260 and are considered normal for a random population of rats this age. f 1 O A i t 1 NEW 010070 WATER PCB-SD0000031041 30 uO cO w4"l M M r* aB M M uA Nxf W M IMxf <4 (4 (4 a(4 Pi I o--OsIj 3 ma SR ?S yo 2 w u a o Ho a OM 4oJ4 o0 U eo<M-44 u O oc V Pu O %oa vnv oa 3cJ4* a *(-D4t u *8V<Oa044 xjMH> I(4T 8 n) oB aUH u(u4 s E .8 .V2V<O0044 4*2ORo<M34 vi <4 8 Bo<mU4 du B S 4 2 < 22 EoCv(oR4 a*4 * <4 E B<4 a M 'eB W^ 1 ra j\j KK H s| KX oo n <n XX t N ra XX f>3 f4 Q <M4 V * a a b r- CO O' O' O 2 "t* m wj cn (4 s<4 ofl o4 -EOc<Ov4 rftr B . H E <4 ft 2 4* KK gB3 K >< n n M o Oo' o mCO o cn oe XautI E eSO < <VM4 8 ft mR S iO8 <; O S*o8 MPi av E * !3 c v E 3 S T.OEo3 < e="4 R ** es J*OS0) vu < Co Booa < Ro E *> < O NEV 010071 3 g g-g w 3a afNij ft vD f*t r-t ft 1 00|* ft 9 o in ft t ` fMn ' f0t4 \cs ft ft 1 4* 'O1 vD vD WATER_PCB-SD0000031042 M ^aw g o M (M N N tf* M fM (MM sH e4 s R Tv3 V |-S <4 2 0 0A I o W%a n fS| 0 I 8 8 51 a* 1o' O rt S o U A e(4 o R v * O 3 o &5 w UO I os 5 X ua ow p 9 H o H *3 O oM o 0 4o3 Li O fr, *a 0C NH RO SA w KX t <f) 8 sO XX lf P4 K. n -* K n oo JJ t0o Up \u <4 0 1 *(M) w iS I toors0 N 1 *0oD0 Mtoo~. 1 "I O' tC-O*l8 moootf0 a t; 3 is 3(4 s a G0 $*8 q >, 0N R0 R0 B 8 n < 4 E E 4* 3-8 .-8 3 a3 3 a fr <4 o 8 3 6 O NEV 010072 Sg ws u 55 s1 U1i O' #r\-i \r. mi ,% U10i :* ^tn Uii U1i Uii #m*# fcm=M--4 WATER PCB-SD0000031043 ! O dw sH -4* "<NtJ fSj f'tMf* fM *. M a m m a ry fib ro a d e n o m a w oa o 3x 5x 2 s I i mm d iT *3 wB U.94 I*rt ou a a o H *ruHt 0 o0 uo V XpJ< U t0 0c <0 Oa u <v4 I od (U6 tt(do4* Vc 2B W& X m X 0* A60 pfe MP l oo oe O' K tn K !t*n 00 0N 5 U *8 & S 4 1d B B a B4 is tl o A < K( 1 a *M> *o0 3 jdM 4= u g a 8 5 (4 ^a 33 I$ to 2 9 .0 Abdomen s *g W ft, 9 ft4 i u* I (m 1 fc* 1 S T) m 63 *o o 5d 4 (4 f\S O fM N p*4 M fM M Ui t fM M NEV 010073 WATER PCB-SD0000031044 <^#$4441 o'i 5 od s do y H fM of od 3 OS rut a I *H (90) <* 6 f 1w w ft Ou 1 H aW t-SJ o u ft O V N W **4 X eo K *0 o U HaV JHD e o E S 2, voD9 * ^ IA sn M ^ X *0 fa eo 49 <4 sroc *aov4 o>4 Sc ^ .2 >i4N g: 2 1 ffi Eo t^Qj oSoa(4 v y Xy ,1 .fi w d $ c NX .fM <* fM cn1 u0 -At fM SM NEV 010074 WATER PCB-SD0000031045 u 0 v-/ " L. S 1 /(WWM, ?HC. J3O*s s O0 mv H pm rvj ^ ro M cm . ea rma OPo4J *0u0n-M a< Wa H< S e; w H Hw W H B 3 3(2 VOi ! ft oo O b0 HJHfjt g01 a 00 Vrut 3to <to4 u S> E ^.H rMt , *M sa 8 dwVMO0 & ^oi mtnn ione Vi V> 4Oa urt > <; 2 sh b e t0 0 # M* * vO eo O' fM ' fM fM fM (M r O 01 NfcV 010075 WATER PCB-SD0000031046 "t * fvl iM M f\*t *0 I JJ Po y a W 1 5 H 34 I 3 Wn fI m &HU O 1 H H -* o oIn oa y 02 il O yw QV u<t>4 !*1 4 E 1 <4 <4 sOu <4 6o aV<d4 Sirt H8 PaV< gg V *V0 *<f0M9t4 *fo(U94t as iTdO |TMfO( | 'OPV|4 Dw ffwCM48tL. 'a* ! 0B*4 43 u n (4 (4 ss 6o(4 v6 \ KX 0 fs| KK 41 ^ n K X w O o o M Vo0 p .ae>** 6* 5 2 6 a B 8 3 1 aV 3 2 S foi 3 4 eOM moI -U-* n en Hp4I U"4*i n NEV 010076 WATER PCB-SD0000031047 .. .. .. - { t). . t Si P. Wheeler - St. Louis October 21, 1968 Polychlorinated Biphenyls In the Environment . .* * . W. R. Richard . WHICH R. E. Kelly^M. r `-Kei FviCELL C. Payton - CPAYT H. Bergen - HBERO W. K. Johnson - WJOHN S Attached is a Xerox copy of a technical paper which Scott Tucker and X picked up in Washington recently. This was provided ub by Donald A. Spencer of the National Agricultural Chemicals Association. Mr. Spencer requested that the paper be held "confidential" until such time as it may be published. Spencer indicated that if this paper were distributed one of his principal "sources" would refuse to give him prepublica tion information in the future. . Rlsebrough1s presentation (the attached) was made at a meeting of 20 to 30 toxicologists held at the University of Rochester in June. The meeting was billed as "The First Annual Conference on Toxicologyf"and was underwritten presumably by the AEC which has had contracts at Rochester for many years. Attendance was by invitation only. The meeting dealt "exclusively" with pesticides with about . one-third of the papers relating to mercury. As far as Spencer knows the papers, including the attached, will undoubtedly be printed as proceedings ,of the conference although X suspect individual authors were given permission to publish elsewhere. In a few words, Rlsebrough has found PCBs along with chlorinated pesticides in a number of species of fish and birds along the California coast as well as in waters off Baja. California and Central America. Be further reports PCB in fish from the Channel Islands and Puget Sound. No PCB was detected in the liver of tuna taken in the Galapagos Archipelago. 'Scott Tucker is going to scrutinize the analytical aspects and particularly the validity of some of the assumptions made by the author. cs Attachment Elmer P. Wheeler. 5 DEPOSITION EXHIBIT 36 Nev 022116 WATER PCB-SD0000031048 MINUTES OF MEETING OF THE CORPORATE DEVELOPMENT COMMITTEE ' . November 17, 1969 . Present: Messrs. * E. J. Bock, Chairman H . H . Bible . ' . J. R. c k . . ' ' J L. Gi ) 1 is E.-J. Putzell . C . H. Sommer . *1 N. Ehlers, Secretary ORGANIC DIVISION, LAW AND MEDICAL DEPARTMENTS -- REPORT ON POLY CHLORINATED BIPHENYLS Present: Messrs. C. J. Smith, J. Mason, T. K. Smith, H. S. Bergen, J. E. SprInggate, R. E . Kelly, E. P. Wheeler, Rodney Harris, Jr., D. W. Miller, W. C. Robinson Monsanto1s worldwide Aroclor business_amounts to 104 M Ibs./yr., 70M used in functional fluids and 31* M in plasticizers. This represents $22 M in sales. Products range from monoch1orobipheny1 WATER PCB-SD0000031049 78. to decachlorobiphenyl , terpheny1s , and chlorinated terpheny1$. Production locations are a t Annis ton, Alabama, Sauget, Illinois Newport, U.K. and Yokkaichi , Japan. . ' Environmental Aspects - E. P. Wheeler The 5 and 6 chlorinated biphenyls (Aroc1 or 12 5^ and 1 260) have been found a t 1imited 1 oca tions in water , in birds and some forms of aquatic life. Recent indications are that such biphenyls may affect reproduct 1 on of fowl life and may be toxic to shrimp. These products are not toxic from the acute standpoint to man or fish but there is some evidence of ecological buildup in certain water deposits, in fish and ultimately in bird life. - Aroc1ors 1248 and 1ower in number are believed to be biodegradable but this has not been cone 1 usive1y es tab 11 shed as yet. p Plan of Action - H. S. Bergen and J. E. Springgate The availability of alternate products to satisfy customer requirements was reviewed. Main problems are that no replacement product is available for capacitors and replacement products for other uses pose a pollution problem. In plasticizer uses , evidence Is not ava i 1ab1e as to whether Aroc1 ors escape from end products, either through leeching or by dispersal in burning. . t. . .* \ The .recommended plan of action Is to establ1sh a tailored program for each business -group' and each customer market situation to assure that the 1 os s of PCB' s in the environment, if any, is minimal. NEV 1.76945 ** WATER PCB-SD0000031050 73. I. Appoint a Project Manager - responsible for the overall management of the Aroc1 or pollution problem. He would be assisted by a Task Force from members of each business group plus Medical, Law, Engineering and Manufacturing. 2.. Notify all Aroc1 or customers of PCB problem. 3. Reduce and effectively contro1 PCB effluents from Monsanto plants. ' k. Educate customers on need to reduce and effectively control PCB effluents at their plants. 5 Develop and implement new packaging systems for Aroc1 or 1 25V 1260. . 6. Introduce to market, replacement products for Aroc1 or 125V1260. 7. Continue and expand biodegradation test program with Aroc1 or series , particularly 12V, 12k8 and 125k. 8 . Continue toxicolog1ca1 test program. 9. Accelerate present analytical test program. 10. Determine feasibility and cos t of eliminating 5/6 Cl in Aroc1 ors 12k2 and 12k8. 2 1 1 . Study incineration products. -1 12. Develop business plan to offer: - Mon s an to fluid Reclamation and Recovery with Enviro Chem. (Reclamation already under-way a t Findett.) Cost of this program is estimated at approximate 1y $k00M SARE and $700M capital to change equipment. ' Conclusions: In light of the recent and developing ev i dence of a possible threat to certaIn species of bird and aquatic life, we should plan to discontinue the manufacture, of Aroc1ors 125k and 1260. The Division is instructed to develop a program to discontinue these products and report this to the Committee. The status of Aroc1 or 12k2 should continue to be tested to determine whether it cont ribu tes to this problem. Other products which might be involved should also be examined. (Excerpt to Messrs. H. L. Mlnckler, Rodney Harris, Jr., R. E. Kelly, T. K. Smith.) ' NEV 176946 WATER PCB-SD0000031051 X PCB PRESENTATION TO v/V^ CORPORATE DEVELOPMENT COMMITTEE I. INTRODUCTION t *.. <ire hare today to acquaint you with the PCB (Aroclor) | pollution problem and to secure your guidance and approval | on a recommended plan of action, v tI . # . . . Certain PCB's have recently been identified by various f *' scientists along with DDT in fish, birds, and other wildlife. j.'rom the standpoint of reproduction, the PCB's are highly i !I toxic to birds. In a few moments, Elmer Wheeler will describe I i the problem in detail. I Our objective is to describe for you the basic problems, ` l the is;sues Involved, review alternative courses of action, and suggest an action plan program for your approval. T'iiir. is a serious matter, not only from the pollution viewpoint, but also because of the $? Mi worldwide customer business involved with resultant gi-oos profits of $10 75 and a not investment of approximately $9 15. In addition, there could be possible adverse legal and public relations problems leveled against Monsanto. Our Agenda will be as follov.-s: V* A* NEV 176947 0****" asap*,. .. ,, < WATER PCB-SD0000031052 -2- PCB AGENDA REVIEW I. INTRODUCTION ' II. THE PROBLEM - DEVELOPMENTS INCRIMINATING PCB's - COMPLEXITY OF IDENTIFICATION - NATURE OF - SERIOUSNESS III. LAW DEPARTMENT VIEWPOINT AND RECOMMENDATIONS IV. EFFECT ON MONSANTO AND ALTERNATIVES V. FUNCTIONAL FLUID BUSINESS GROUP DISCUSSION - MARKETS, USES - SOURCES OF POLLUTION - CUSTOMER EFFECT VI. PLASTICIZER BUSINESS GROUP DISCUSSION - MARKETS, USES - SOURCES OF POLLUTION VII. RECOMMENDED ACTION PLAN * VIII. SUMMARY NEV 176948 C `{f- WATER PCB-SD0000031053 3- By 'fay of introduction, the Organic Division and the Medical Department has been actively engaged for the last 18 months in developing facts and knowledge on this subject by personal visits to Universities and Industrial test laboratories, other worldwide producers, and other industrial collaborators, as well .is keeping abreast of all literature and news sources on the subject as well as funding a toxicological and analytical test program In excess of $100 M. We established an Ad Hoc Committee of both Business Groups and Medical which recently issued a report - much of which will be discussed today. We have learned a lot, but there is much yet to learn as you will hear. What arc TCP's? They arc polychlorinated biphenyls - better known to us as Aroclors. The next slide will quickly re familiarize you with our Arocldr business. ,wnj*7r.wi<n' NEV l?6949 it - ...... WATER PCB-SD0000031054 MONSANTO WORLDWIDE AROCLOR BUSINESS pounds/year sales/year 104 H $22 H (70 M in Functional Fluids 34 M in Plasticizers) t ($l6 M in Functional Fluids $ 6 M in Plasticizers) GROSS PROFIT/YKAR $10.0 TI ($7.5 M in Functional Fluids . $2.5 M In Plasticizers) gross investment $13 M ($8.8 M net investment) ROI ' WORLDWIDE M/I MONSANTO PRODUCTION LOCATIONS: 10.5$ 62$ USA (2 plants, Anniston, Alabama Sauget, Illinois) UK (Newport) JAPAN (Yokkaiehl) ' OTHER PRODUCERS: Bayer, Prodelec, Caffaro, Flick, Kanegahuchi, and several Eastern European producers (all ex-USA) , t\ t' \ NEV 176950 WATER PCB-SD0000031055 I 5- THE AROCLOR PRODUCT LINE CHEMICAL NAME TRADE NAME MONOCl ILOROBiriIENYL AROCLOR 1221 DICHLOROB1PH ENYL AROCLOR 1232 TRICHLOROBI PHENYL AROCLOR 1242 TETRACHLOROBIPHENYL AROCLOR 12*48 PENTACHLOROBIPHENYL AROCLOR 1254 H EX ACHLOROBIPHENYL AROCLOR 1260 HEPTACHLOROBIP1IENYL AROCLOR 1262 OCTACHLOROBIPHENYL AROCLOR 1268 DECACHLOROBIPIIENYL AROCLOR 1270 TERPHENYLS SANTOWAX CHLORINATED TERPHENYL AROCLOR 5460 NATURE OP MATERIAL THIN LIQUID OILY LIQUID HEAVY MOLAS . THICK TAR V> SOLID V SOLID' N6V 176951 WATER PCB-SD0000031056 Theie are theoretically 210 different isomers of chlorinated biphenyls. ' Monsanto entered the Aroclor market in 1930 by acquiring Swan Chemical Company. The first load of Aroclor went out of Anniston, Alabama to General Electric in 1931. Since then, the market has grown to one of Monsanto's most profitable franchises. This franchise is now being threatened *by 1 c "''"I < ,L'1" A recently found pollution problems which Elmer V/heeler will now discuss. '. II, The Problem (Wheeler) - see attached Appendix A III, Law Department Viewpoint and Hecommendations (French) Effect on Monsanto and Our Alternative Courses of Action As discussed, Aroclors 125^ and 1260 -- the 5 and 6 Cl ringed biphenyls are the ones most seriously involved in the pollution problem. Both Plasticizers and Fluids Groups are involved as shown: NEV 176952 WATER PCB-SD0000031057 t AROCLOR SALES (M POUNDS) AROCLOR 1234 AROCLOR 1260 & ABOVE FLUIDS 1.45 3.7 5.15 PLASTICIZERS 5.4 UL 7.1 TOTAL 6.85 5.4 12.23 I It ' I N6V W"3 WATER PCB-SD0000031058 We considered 4 alternative courses or action; (Slide) Alternative 1: Do nothing was considered unacceptable from a legal, moral ad customer , public relations & company policy viewpoint. This is also the quickest route to being forced out of business. Alternative 2: Go out of total Aroclor business was considered unacceptable from a Divisional viewpoint, but from a Corporate viewpoint may be necessary. Only-you-can-make-1hat-de ci-s io n. All Aroclor products are not serious pollutants - many deg rack; there is too much customer/market need and selfishly too much Monsanto profit to go out. To go out would require a write off of Aroclor net Investment of $7 M (10//share) or if biphenyl included $8.8 H (12^/share). In addition, Inventory disposition, continuing cost of utilitiv.-s, and back-up capital and serious manpower & resources reallocation at Anniston. Alternative 3: Go out of Aroclor 1254 and 1260. This was seriously considered and may eventually occur by our actions and customer actions, nevertheless, we feel that segments of this business are defensible or arc so "confined" in use that specific plans of action are called for this portion. Our reasons for eliminating this alternative will become clearer as we outline our action plans. WATER_PCB-SD0000031059 ALTERNATIVE COURSES OP ACTION 1. DO NOTHING - JUST REACT TO LEGISLATION AND EMOTION. 2. GO OUT OP TOTAL AROCLOR BUSINESS. 3. GO OUT OP AROCLOR 1254 AND 1260 PRODUCTION 4. DEVELOP SPECIFIC ACTION PLANS "TAILORED" TO EACH BUSINESS GROUP AND EACH CUSTOMER/MARKET SITUATION TO "CLEAN UP" THE MESS. / NEV H6955 S WATER PCB-SD0000031060 Alternative *1: Develop specific action plans .tailored to each Business Group and each customer/market situation, - was the alternative selected at this point of time and based on our knowledge from a Divisional viewpoint as making Monsanto act in the most positive, responsible way to society and our customers, as well as our interests. ' However, because of the magnitude and seriousness of this problem and its total implications for Corp'oratd Monsanto, 11 ( . .. .. i <' /'/ - '': ' '' v * **`A; " ^he fina^ decision on this matter must be made by-the CDC. Functional Fluids Business Group Discussion: Aroclors are'used widely in 3 of our ^ market areas in the Fluids Group: NEV 17^956 WATER PCB-SD0000031061 FLUIDS USE OF AROCLCRS BY MARKET AREA ol & col s MARKET AREA AROCLOR PRODUCT INDUSTRIAL HEAT TRANSFER ELECTRICAL TOTAL 1242 1248 121>4 . 1260 & Above 4.1 1.2 0.6 5.9 1.1 36 41.2 1.0 - 2.2 0.1 0.8 0.9 - 3.5 4.1 2.2 . 40.3 40.4 NEV i7C>9&7 s WATER PCB-SD0000031062 SOURCES OP FLUIDS POLLUTION APPLICATION INDUSTRIAL FLUIDS DIELECTRICS HEAT TRANSFER PRODUCING PLANTS ' INTENSITY OF POLLUTION CREATEST (DIRECT) (INDIRECT CONTAINED) (INDIRECT CONTAINED) LEAST (DIRECT) N6V 17695a s WATER PCB-SD0000031063 -1^- ' FLUIDS CUSTOMER ALTERNATIVES AREA OF APPLICATION Industrial Fluids Transformer Capacitors Heat Transfer PRODUCT OF CHOICE CUSTOMER OPTIONS Pydraul 312/F-9/ Customer could get along A-200/Phosphate Esters/ without us, but Pydraul Water Glycol 312 favored. H?0 Glycol has some pollution problem Phosphate ester route ok at present. Alr/Oil/Aroclor/Gas Could drop Aroclor at sacrifice of safety, cost or size of equipment or noise level. Aroclors No immediate replacement available. Longer term oil at expense of size and cost of efficiency and redesign of equipment. Thermlnol Oil/Dow therm/T66 . T55 T?7 TQ8 No option for FR liquid market. Other system possibility. Liquid systems favored. T66 and T55 increasing rapidly in use. Oil also a pollution problem. nev ITO'59 WATER PCB-SD0000031064 Customer Choices &; Alternatives & Penalties: Summarizing, some of our customers have no immediate alternative, some could change only at sacrifices of safety, or cost or various technical factors. Only in the Industrial field could the customer make an immediate conversion. . PCB Threat to Functional Fluids Business and Profit: NEV 176960 WATER PCB-SD0000031065 FLUIDS BUSINESS THREATENED (1970 BUDGET) PROBLEM Confined to A-1254/ 1260 only. Spreads to A-1242 and 1248 First to: a) Industrial Fluids Then to: b) Dielectric Fluids Then to: c) Beat Transfer SALES $ 3.0 M GROSS PROFIT $1.38 M " $ 4.0 M $1.6 M $ 8.0 M $3.8 M $ 1.0 M $16.0 M $ .6 T\ $7.36 m 7W 'y. 7/ NEV 176961 WATER PCB-SD0000031066 PLASTICIZERS (TORLD-UIDE) i.A>/ SJ'J/s.Sj ECLLAMS POUaDS *\ o L \y o> Va (D ca 0 V* A X alt. /.rcolors c? O 0 ,*i 3'voO K $ 2.5 K AROCLCR 1254/1260 Ti P $1.? K () 9.5 :? V 20/i; $0.8 7 (32/) NEV 176962 WATER PCB-SD0000031067 -16- COMT'i: V;TS; IXiSTTi'CT.TOrcS li'HCM P.P. . 1. Targe number of direct U.S. customers - 570. 2. Customers are small: 23 direct customers - 4?$* A-1254/1260 sales, 3 50;* domestic A-12J4/1260 sales through distributors - difficult to police. NEV 176963 WATER PCB-SD0000031068 n K'.-VAK?;TS ' j 959 SALES MAJOR AROCLOR TS2D : : Cvrbonloss Carbon Paper 8.B 'M lb. . Aroclor 1242 ; Kot Kelt Adhesives 5.7 K lb. Aroclor 5450 : Sv;ii.!:.'dnu Pool Paints 1.7 7i lb. Aroclor 12-11V''" Aroclor 5450) Protective Coatings 5.3 M lb. Aroclor IZy.V' Aroclor 5J.o:) i il.uloior. C'r.c-sives 1.5 xT lb. Aroclor 125-0 / Arocioc 12o0 Soelante ; 3.0 w lb. Aroclor 1254) Aroclor ai; Modi1 cr..t eor. 2.0 K lb. Aroclor Aroclor rio. .-ir. / ^ *< Kir. col la .oour : 5.0 Vi lb. Aroclor i?- ij'./. Aroclor ) ^ * CO!-'.:-;' lao: 1. 1OV: stajor cur; to;..or (85/^ of A roclor i2-1:2 cola). ; ; . 1;v - of dc:ne..t Ac .'.roclors sol C! *>4. NEV 176964 I WATER PCB-SD0000031069 POSSIBLE CCXTAXUATION SOURCES (PLASTICIZERS) MARKET APPLICATION SOURCE Costings Marine Paints) Leaching Later tame ) , linings ) ' Coatings Sv;ir;i^lns Pool Leaching- Paints . Carbonless - Vaporization Carbon Paper . V/zix Mo dil'i cation - Vaporization Itsulsior. Adhesives Contact v.'ith product via packaging. In cineration. Lot Molt Adhesive- Contract with product via packaging. In cineration. ' Sealark s Automotive Long-term. lc-aching (41 ll') 'i lv* * C \*0.1 cu.?.x, r.orw'-^.ncs IS h-l25L'r /1260 USED? Yes Yes go Yes Yes No Ur.iko Cluicis, Arcelor plasticizers are cosv.bin.a. in .0 plastics ut; -roauoo t.10 Pinal product - therefore, Par 1 'so . Pi lOi.io r.vch as wastes fror. our manufacturing plant , >..r-,-jc:isr3 pl,. :to ..no iT.ci leasing of drums com-non to both groxm ; or px-otoctivo coatings are not considered a h.'..,h ;J o % f* '.roclr -- processing or 'v.u NEV 176965 WATER PCB-SD0000031070 II PLASTICIZER EUSIR/.SS T!IRISATEt.'KD PRO v*>y* 1. Confined to A-lRl>-:/i260 typo only. SOI' to ail chlon > .ted bl phony.* 0..*U 0 S,;.. to a n .W. V**,*/..- - * id at"J. ch.V) .toir b W<a ^ a >t S. 0 i j SALES R"T.:IKRL--:$4.3 :`>2.0 0.0 a.P. RETAINED (LOST) $1.7 Ti (-$0.8 1) $0.6 K (-$1.9 E) 0.0 (~$2.p h) sord on prospects s#v .... .<5. r 4 r. (/J. 8.'. sen ;olor- 1262/4463 fhich are very 000 to A-1234/i-^O and these have boon included va A-1234/1260. NEV 176966 WATER PCB-SD0000031071 RECOMMENDED ACTION PLAN THE JOINT ACTION PLAN DEVELOPED BY THE FUNCTIONAL FLUIDS AND PLASTICIZER BUSINESS CROUPS, AND THE MEDICAL AND LAW DEPARTMENTS IS AS FOLLOWS: . 1. Appoint a Project Manager - responsible for the overall management of the Aroclor pollution problem. He would be assisted by a Task Force from members of each Business Group plus Medical, Law, Engineering and Manufacturing. 2. Notify all Aroclor customers of PCB problem and relabel containers - within 60 days, 3. Clean up Monsanto plants* effluents within 12 months. 4. Develop and implement new packaging systems for Aroclor 1254/1260 - within 6 months. 5. Educate customers on need for clean-up at their plants - within 4 months. 6. Introduct to market, replacement products for 'Aroclor 1254/1260 - beginning l/l/'fO (Fluids), 4/1/70 (Plasticizers). NEV 176967 WATER PCB-SD0000031072 RECOMMENDED ACTION PLAN Continue and expand biodegratation test program with Aroclor series, particularly 1242, 1248 and 1254. Continue toxicological test program. Accelerate present analytical test program. Determine feasibility and cost of eliminating 5/6 Cl2 in Aroclors 1242 and 1248. (3/70) Study incineration products. (3/70) Develop business plan to offer: Monsanto Fluid Reclamation and Recovery with Enviro Chem (4/70). (Reclamation already underway at Findett.) I NEV 176968 WATER PCB-SD0000031073 WHAT rXCLP WE EXPECT FROM THIS PROGRAM? Through. this action program* Monsanto would expect to: P.^-tain or convert a good portion of our business and profits: PHVBLJ5MS ' a. Confined to A-125V 1260. b, Spreads to A-1248 and 1242. CONVERT on RETAIN $20.3 M $10 H $M SALES OUT OF PRESENT $22 1 $22 M ODDS OF SUCCESS 70% 60# 2, n further valuable knowledge and time to: a. Learn more facts. . b. Protect our position. c. Make further decisions regarding our program. d. Contribute to overall pollution knowledge. 3, Clean-up the major contributing PCS pollution factors. 4, Minimize customer complaints and hardships. NEV 176969 WATER PCB-SD0000031074 The Program Would: 1. Cost some money. Esfc. SAKE - $*100-500 M Est. Capital - $700 M $1.1 1 - 1.2 W ' 2. Expose us to continued adverse publicity and possible law suits. ,, < 3. Cause some customer discontent - but much less than an abrupt termination of production. NEV 176970 WATER PCB-SD0000031075 SUMMARY In summary, the PCB pollution problem is a very serious one. It Is a worldwide ecological problem. At present the most serious offenders are the 5 and 6 chlorine containing products (Aroclors 1254 and 1260). There are some Indications other members are biodegradable to varying degrees. Currently, much l scientific testing is underway and more information will be forthcoming. Monsanto must act in a positive cooperative fashion. A plan of action has been discussed which we feel Indicates responsible action. Our stakes are large and because of the many possible effects on the Corporation - your guidance and approval of the suggested action program is requested. Thank you for your consideration. May we answer any questions? NEV 176971 WATER PCB-SD0000031076 V. GENTLEMEN: -. MY PARTICIPATION IN THIS PRESENTATION WILL BE A BRIEF REVIEW OF THE DEVELOPMENTS WHICH INCRIMINATE THE POLY CHLORINATED BIPHENYLS INCLUDING OUR AROCLORS AS NEARLY ik'! ronmental CON TAW NA STATES; OEPIETION IN POPULATION OF THIS SPECIES IN CALIFORNIA; AND THE REPORTED EFFECT ON THE BROWN PELICAN IN CALIFORNIA. 3) PCB'S ARE PARTICULARLY TOXIC TO SHRIMP. AT PENSACOLA, THERE WAS A LOSS OF 1 TO 3 GALLONS PER DAY OF AROCLOR 1254 INTO THE ESCAMBIA RIVER FROM OUR NYLON PLANT. THE RESULTANT CONCENTRATIONS OF PCB ONE-OUARTER MILE BELOW THE PLANT WERE ABOVE THE LEVELS NEEDED TO KILL JUVENILE SHRIMP IN LABORATORY TESTS. 4) THERE ARE STILL MANY UNKNOWNS BUT SPECULATION AS TO THE ROLE OF PCB'S IS RAMPANT. ' ALTHOUGH SOME. OF THE REPORTS OF ANALYTICAL IDENTIFICATION Ai*7 ARE* NOT -CERTAIN. THE MEDICAL DEPARTMENT--AFTER 18 MONTHS OF INVESTIGATION IN CONJUNCTION WITH THE ORGANIC DIVISION--IS CERTAIN THAT THE PCB'S CAN BE RESPONSIBLE FOR ECOLOGICAL DAMAGE. THERE IS NO SCIENTIFIC CONSENSUS AS TO THE DEGREE OF PCB INVOLVEMENT BUT THESE COMPOUNDS CANNOT ESCAPE A SIGNIFICANT SHARE OF THE BLAME FOR DAMAGE. NEV 176972 WATER PCB-SD0000031077 SPECULATION IS LEADING TO CONCERN WHICH MAY GROW TO ALARM. .. THE MEDICAL DEPARTMENT BELIEVES THAT THE MYRIAD OF INVESTIGATORS PRESENTLY WORKING ON PCB'S IN GOVERNMENT AND UNIVERSITY LABORATORIES IS CERTAIN TO PROMOTE A MORE PROMINENT ROLE FOR PCB DAMAGE , LEADING AT BEST TO EXTREMELY DAMAGING PUBLICITY AND, AT WORST, LEADING TO COMPLETE BANNING OF THESE PRODUCTS. NEV 176973 WATER_PCB-SD0000031078 i iitftJtmkjtL' CERTAINLY ALL OF YOU ARE AWARE OF THE PRESENT CONCERN ABOUT THE RESIDUES OF DDT, ITS METABOLITES AND OTHER CHLORINATED HYDROCARBON PESTICIDES THROUGHOUT THE WORLD. SINCE WORLD WAR II AND IN THE LAST DECADE IN PARTICULAR, .THERE HAS BEEN A SAMPLING NETWORK WHICH HAS IDENTIFIED DDT AND ITS METABOLITES IN PRACTICALLY EVERY LIVING ORGANISM-AN-D-IN THE AIR, WATER AND SOIL ACROSS THE FACE / OF THE GLOBE. IT WOULD NOT BE UNEXPECTED TO FIND THAT EACH OF US IN THIS ROOM HAS 5 TO 10 ppm OF DDT IN OUR FATTY TISSUES. 0 AS ANALYTICAL TECHNIQUES HAVE IMPROVED AND INCLUDED VERY SENSITIVE GAS CHROMATOGRAPHY METHODS, INTERFERING SUBSTANCES HAVE APPEARED WHICH RAISE QUESTIONS AS TO THE VALIDITY OF PRESENT AND EARLIER DETERMINATIONS OF DDT MATERIALS. ' THIS DIAGRAM INDICATES THE GAS CHROMATOGRAMS OF SEVERAL OF OUR AROCLORS. AT THE BOTTOM THE PEAKS FOR VARIOUS HYDROCARBON PESTICIDES ARE SHOWN. IT IS OBVIOUS THAT SOME OF THE PREDOMINANT PEAKS IN THE AROCLORS FALL IN THE SAME POSITION IN TERMS OF RETENTION TIME AS DOT . ' NEV 176974 WATER_PCB-SD0000031079 AND ITS METABOLITES. PLEASE NOTICE THAT THIS IS PARTICULARLY TRUE FOR AROCLORS 1254 AND 1260 ANO IT IS THESE TWO PARTICULAR POLYCHLORINATED BIPHENYLS, WHETHER MANUFACTURED BY MONSANTO OR OUR COMPETITORS, THAT ARE THE PRODUCTS WHICH ARE MOST CONSISTENTLY IDENTIFIED ( PENTA JPO'-OeTA' CHLORO). LET ME EMPHASIZE THIS POINT BECAUSE IT HAS A PARTICULAR BEARING ON THE FUTURE MANUFACTURE, SALES AND USE OF THE WHOLE PRODUCT LINE. . WHERE HAVE THE PCB'S BEEN FOUND? THIS NEXT TRANSPARENCY INDICATES LOCATIONS WHERE THESE MATERIALS HAVE BEEN REPORTED. THE AMOUNTS FOUND VARY FROM PARTS PER TRILLION IN SOME WATER SAMPLES TO HUNDREDS OF PARTS PER MILLION IN FISH AND SOME FISH-EATING BIRDS. LET ME DIGRESS A MOMENT TO EQUATE THESE UNITS OF PPM, PPB AND PPT TO SOMETHING THAT WE ALL RECOGNIZE (SHOW TRANSPARENCY ON COMPARISON OF PPM TO FIFTHS). . RETURNING TO THE REPORTED FINDINGS OF THE PCB'S, THE VALUES THAT HAVE BEEN REPORTED IN SWEDEN VARY FROM 10 PPB IN FISH, BIRDS AND-EGGS TO 20,000 ppm IN ONE OR TWO SINGLE SPECIMENS. IN THE LATTER CASE, THESE HAVE BEEN DEAD BIRDS AND THERE IS SOME QUESTION AS TO THE VALIDITY OF THE RESULTS. IN REGARD TO CHILDREN"$ HAIR, DR. JENSEN HAS POINTED OUT THAT HIS FIVE MONTH OLD CHILD HAD MORE PCB'S IN THE HAIR THAN HIS THREE AND SIX YEAR OLD CHILDREN AND HE POSTULATED THAT THIS WAS DUE TO THE PCB BEING IN MOTHER'S MILK. THE SAME LEVELSOF PCB'S HAVE BEEN FOUND IN FISH, BIRDS, AND EGGS IN NEV 176975 WATER_PCB-SD0000031080 -3- 6REAT BRITAIN AND THE NETHERLANDS. IN THE UNITED STATES AS WE HAVE INDICATED, THE FCB'S HAVE BEEN FOUND IN IN-LAND WATERS. THIS IS QUITE DIFFERENT UP TO THIS POINT AS REGARDS THEIR DISTRIBUTION IN GREAT BRITAIN, IN THE NETHERLANDS AND IN THE SCANOANAVIAN COUNTRIES. l/pERHAPS I SHOULD REMIND YOU THAT MONSANTO IS THE SOLE PRODUCER AND SUPPLIER OF POLYCHLORINATED BIPHENYLS IN THE.UNITED STATES AND GREAT BRITAIN. THIS IS IMPORTANT SINCE ANY PUBLIC OR GOVERNMENTAL AGENCY ACTIVITY WHICH MAY LEAD TO THE RESTRICTION OF USE OF POLYCHLORINATED BIPHENYLS MAKES MONSANTO PARTICULARLY VULNERABLE FROM A PUBLIC RELATIONS STANDPOINT IN THE UNITED STATES, GREAT BRITAIN AND PROBABLY CANADA. IN TERMS OF TOXIC OR HARMFUL EFFECTS FROM THE PRESENCE OF PCB'S, WE CAN MAKES THESE STATEMENTS SUPPORTED BY A GROWING AMOUNT OF TOXICOLOGICAL RESEARCH DATA: 1. THE AROCLOR'S ARE NOT HIGHLY TOXIC FROM AN ACUTE STANDPOINT TO MAN, ANIMALS, BIRDS OR FISH. FOR ' EXAMPLE. THEY ARE NOT NEARLY AS TOXIC AS DDT AND CERTAINLY MUCH' LESS TOXIC THAN DIELDRIN AND AIDRIN. .. 2. FROM A CHRONIC TOXICITY STANDPOINT, THE PCB'S MAY BE CONSIDERED "MODERATELY TOXIC" TO MAN, ANIMALS AND FISH. FROM THE STANDPOINT OF REPRODUCTION, THE PCB'S ARE HIGHLY TOXIC TO BIRDS, THIS CON CLUSION IS BASED ON ON-GOING RESEARCH AT OUR . CONSULTING LABORATORY IN CHICAGO WHERE WHITE LEGHORN CHICKENS--A RELATIVELY RESISTANT MEMBER OF THE BIRD SPECIES--ARE LAYING EGGS AFTER BEING ' NEV I7b97b WATER_PCB-SD0000031081 < . -4- FED A DIET OF 10 PPM WHICH FAIL TO HATCH. AT TOO PPM THE EGGS HAVE GREATLY REDUCEO EGG SHELL THICKNESS AS WELL. IN THE AQUATIC ENVIRONMENT, SHRIMP APPEAR TO BE PARTICULARLY SENSITIVE TO THE PCB'S. IN A TEST CONDUCTED AT THE BUREAU OF COMMERCIAL FISHERIES LABORATORY, GULFSTREAM, FLORIDA, 5 PPB CAUSED THE DEATH OF 18 OUT OF 25 JUVENILE SHRIMP IN 18 DAYS. ALTHOUGH AT THIS POINT THE PCB'S ARE NOT BEING TOUTED AS SERIOUS TOXICANTS, THERE HAVE BEEN COMMENTS IN EACH OF THE PUBLICATIONS WHICH HAVE APPEARED WHICH HAVE IMPLIED-IF NOT STATED DIRECTLY--THAT THESE MATERIALS ARE "HIGHLY TOXIC". THE FUTURE OF THESE MATERIALS IS THREATENED MORE BY THE POTENTIAL EFFECT ON SOME FORMS OF WILDLIFE RATHER THAN POTENTIAL TOXIC EFFECTS AS WE USUALLY THINK OF THEM IN RELATION TO HUMAN OR ANIMAL FOOOS. IN THE ENVIRONMENT WE ARE FACED WITH THIS CYCLE--FISH IN WATER CONTAINING PPB OF PCB CONCENTRATE THE MATERIAL TO PPM. THE SWEDES SAY THAT LARGER FISH EATING SUCH SMALLER ONES SHOW A HO FOLD INCREASE IN THE AMOUNT OF PCB IN THEIR TISSUES. BIRDS THEN EATING THESE FISH SHOW 100 FOLD CONCENTRATION OF PCB FROM THAT IN THE FISH WHICH THEY HAVE EATEN. IT IS POSTULATED AS IN THE CASE OF DOT THAT THIS CONCENTRATION LEADS TO EGGS WITH LITTLE OR NOT SHELL THICKNESS AND WITH DECREASED OR NO REPRODUCTION. NEV i7o<*77 WATER_PCB-SD0000031082 -5- HOW DO THE PCB'S GET INTO THE ENVIRONMENT? OUR EFFORTS TO DATE HAVE NOT SEEN COMPLETELY SUCCESSFUL IN PIN-POINTING SOURCES OF THE PCB'S. AS MR. BERGEN AND MR. SPRINGATE WILL-DISCUSS SHORTLY, HE DO HAVE SOME IDEAS CONCERNING SPECIFIC PRODUCT USES. WE CAN, HOWEVER, MENTION THREE INSTANCES WHICH WILL GIVE SOME IMPRESSION AS TO SOURCES SUCH AS OUR MANUFACTURING PLANTS, A MONSANTO "CUSTOMER"PLANT, AND EARLY RESULTS OF WIDE-SPREAD SAMPLING IN LAKE MICHIGAN (SHOW TRANS PARENCY OF SEVERN RIVER, PENSACOLA AND LAKE MICHIGAN). THIS IS AN INDICATION OF THE PCB CONCENTRATION IN MUD NEAR THE OUTFALL OF OUR NEWPORT PLANT. YOU WILL NOTE THE SCALE IN MILES AT THE BOTTOM AND THE DISTRIBUTION OF PCB ALONG THE ESTUARY OF THE SEVERN RIVER. SIMILAR FINDINGS COULD BE SHOWN FOR THE STREAMS BELOW OUR ANNISTON AND KRUMMRICH PLANTS. AN INDICATION OF "CUSTOMER" USAGE AS A SOURCE IS INDICATED IN THIS SLIDE. THIS IS A MONSANTO CUSTOMER PLANT WHERE THE PENSACOLA INSTALLATION WAS USING FIRE RESISTANT AIR COMPRESSOR LUBRICANT CONTAINING AROCLOR 1254. IT HAS REPORTED THAT ONE-FOURTH'MILE BELOH OUR PLANT OUTFALL, 40 PPB OF PCB HAS PRESENT. AT THE BRIDGE AT HIGHWAY 90, 0.5 PPB WAS REPORTED. THE STATE AND UNIVERSITY IN DOING FURTHER SAMPLING REACHED IN BEHIND THE SKIMMERS ON THE OUTFALL OF OUR PLANT AND FOUND PPB. N6V 176978 WATER_PCB-SD0000031083 .. . -6- AS A FURTHER EXAMPLE OF THE POSSIBLE SOURCES FROM OUR CUSTOMER PLANTS, THISTRANSPARENCY SHOWS EARLY REPORTS OF SAMPLES FROM LAKE MICHIGAN. WATER SAMPLES HAVE SHOWN PARTS PER TRILLION TO PARTS PER BILLION OF THE HIGHER CHLORINATED BIPHENYLS. WHEN WE BROUGHT THIS BACK TO OUR MARKETING GROUPS, THEY QUICKLY POINTED OUT THAT ONE COULD ALMOST PIN-POINT OUR CUSTOMER USAGE ALONG THE SHORES OF LAKE MICHIGAN. THESE THREE INSTANCES REFLECT WHAT MIGHT BE TERMED DIRECT CONTAMINATION. AS YOU WILL HEAR, THE POSSIBLE SOURCES OF INDIRECT CONTAMINATION MIGHT BE RELATED TO EVERY SINGLE USE OF OUR PRODUCTS WHETHER THE USES BE IN ELECTRICAL APPLICATIONS, OTHER INDUSTRIAL FLUIDS, OR PLASTICIZER USAGE . THE SCIENTISTS WHO HAVE PUBLISHED THEIR FINDING OF THE PCB'S IN NATURE HAVE IN EVERY INSTANCE MENTIONED THE POSSIBLE SOURCES AS THE LIOUID MATERIALS AS INDUSTRIAL ' POLLUTANTS AND THE PLASTICIZER USES WHERE IN THE MANUFACTURE OF A PLASTIC MATERIAL SOME VAPORS ARE LOST TO THE ATMOSPHERE AND ULTIMATELY END UP IN THE OCEAN AS CHEMICAL FALL-OUT. HAVE THE HONOR IF IT BE SUCH OF NAVJNjSjMIS QUOTED IN THIS NEW BOOK ON CHEMICAL FALL-OUT. ' *hW HAVE POSTULATED ALSO THAT SINCE THE PCB'S ARE VIRTUALLY INDESTRUCTIBLE, EVERY POUND EVER MANUFACTURED ULTIMATELY HAS ESCAPED INTO THE ENVIRONMENT AND REMAINS THERE. AS FAR AS FUTURE ACTION IS CONCERNED, THE MEDICAL DEPARTMENT PROPOSES TO CONTINUE A PROGRAM, AND I MIGHT ADD--AN EXPANDED NEV 176979 WATER_PCB-SD0000031084 -7PROGRAM--WHICH WE HOPE WILL PERMIT THE CONTINUED USE OF AROCLORS 1254 AND 1260 IN THOSE APPLICATIONS WHERE ESCAPE' INTO THE ENVIRONMENT CAN BE POLICED AND PREVENTED. SECONDLY, WE HOPE TO DEVELOP DATA THAT WILL SHOW THAT THE LOWER CHLORINATED BIPHENYLS, THAT IS--AROCLOR 1242 AND THOSE LOWER IN CHLORINATION, ARE DEGRADED IN THE ENVIRONMENT AND THUS DO NOT PRESENT A THREAT TO WILDLIFE. THERE IS SOME INDICATION FROM WORK UNDERWAY IN RUABON THAT AROCLOR 1242 WILL INDEED DEGRADE BIOLOGICALLY. THERE IS A PUBLISHED REPORT FROM THE UNIVERSITY OF UTRECHT WHERE 1242 FED TO QUAIL SHOWED VIRTUALLY COMPLETE DEGRADATION. AS I HAVE MENTIONED EARLIER, EXCEPT FOR ONE OR TWO INSTANCES AROCLOR 1242 HAS NOT BEEN IDENTIFIED ALONG WITH THE PESTICIDE RESIDUES. THIS IN ITSELF SUGGESTS THAT THIS MATERIAL IS DEGRADED. WE WOULD HOPE THEN THAT OUR EFFORTS WILL PROTECT THE CONTINUED SALE AND USE OF AROCLORS 1242, WHICH AS MR. BERGEN AND MR. SPRINGATE WILL INDICATE; MAKES UP A MAJOR PORTION OF OUR AROCLOR BUSINESS. WE WOULD BE LESS THAN HONEST HOWEVER, IF WE DID NOT POINT OUT THAT THE SCIENTIFIC DATA TO BE DEVELOPED FROM OUR OWN RESEARCH AS WELL AS BY ANY NUMBER OF THE 50 GOVERNMENTAL OR UNIVERSITY LABORATORIES THAT HAVE REQUESTED SAMPLES OF AROCLORS MAY NOT BE FAVORABLE REGARDING AROCLOR 1 ^. IN SUMMARY, THE MEDICAL DEPARTMENT FEELS THAT LONG-RANGE^ THERE MAY BE LESS THAN A 50* CHANCE OF SUCCESS IN PROTECTING N6V 176980 WATER_PCB-SD0000031085 -8- THE MARKETS FOR THE POLYCHLORINATED BIPHENYLS. WE FEEL THE ODDS DEPEND ON AT* LEAST FIVE FACTORS BEYOND OUR CONTROL: 1. WE MAY FIND THAT THE PREVENTION OF ESCAPE OF THESE MATERIALS TO THE ENVIRONMENT IS IMPOSSIBLE-- EXCEPT IN VERY LIMITED APPLICATIONS. 2. ALTHOUGH, AS I HAVE INDICATED EARLIER, THERE IS SOME EVIDENCE THAT THE LOWER CHLORINATED MATERIALS SUCH AS AROCLOR 1242 ARE BIODEGRADABLE, FURTHER RESERACH SPONSORED BY MONSANTO OR OTHERS, MAY PROVE THAT THIS IS NOT THE CASE. 3. WE CANNOT CONTROL THE EFFORTS OF THE CHLORINATED PESTICIDE MANUFACTURES WHO--IN DEFENSE OF THEIR PRODUCTS, DDT AND THE OTHERS--HAVE BEGUN TO EMPHASIZE IN GOVERNMENT HEARINGS AND SCIENTIFIC SEMINARS IHAT THE PAST AND CURRENT RESIDUE ANALYSIS MAY BE UNDULY ALARMING BECAUSE OF THE PCB INTERFERENCE. 4. IT WILL BE DIFFICULT -- IF NOT 1MPOSSIBLE--TO COUNTERACT THE EFFORTS OF OUR COMPETITORS IN THE FUNCTIONAL FLUID APPLICATIONS WHO HAVE BEGUN TO BROADCAST THE POTENTIAL PCB PROBLEM--NOT ONLY TO OUR CUSTOMERS BUT TO REGULATORY AGENCIES SUCH AS THE MICHIGAN DEPT. OF NATURAL RESOURCES, AND 5. WE MAY FINO IT IMPOSSIBLE TO COUNTERACT THE EFFORTS OF THOSE SCIENTISTS AND PSEUDO-SCIENTISTS NOW INVOLVED IN THE U. S. AND EUROPEAN WILDLIFE CONSERVATION EFFORT WHO--TO PUT IT MILDLY--DO NOT ALWAYS REACT RESPONSIBY. ' \' NEV 176981 WATER_PCB-SD0000031086 6 HAVE AROC AS YOU CAN IMAGINE, ME IN THE MEDICAL DEPARTMENT HAVE BEEN CONCERNED DURING THESE MANY MONTHS ABOUT THE POSSIBILITY OF LEGAL AND FINANCIAL LIABILITY WHICH. MAY FACE MONSANTO IN THIS SITUATION. `^BWrpRENCH IS NEXT ON THE PROGRAM TO DISCUSS THIS ASPECT Of THE PROBLEM. NEV 176982 WATER_PCB-SD0000031087 i1s 1) THE 5 AND 6 CHLORINATED BIPHENYLS--OUR AROCLORS 1254 AND 1260--ARE PRESENT IN THE ENVIRONMENT, IN BIRDS, FISH, AND OTHER AOUATIC LIFE. , ' * 2) THESE, IN PART OR SOLELY, ARE AFFECTING REPRODUCTION OF SOME SPECIES OF BIRDS. 3) PCB'S ARE PARTICULARLY TOXIC TO SHRIMP. 4) THERE ARE STILL MANY UNKNOWNS BUT SPECULATION AS TO THE ROLE OF PCB'S IS RAMPANT. * 5) SPECULATION IS LEADING TO CONCERN WHICH MAY GROW TO ALARM. NEV 176983 WATER PCB-SD0000031088 j i:,ona `jn,v.*ui'.?.ol;'/.ao |] fii* ` ` * ' ' ' ' *" Analjlit of Ctclot racldut*. Chron.A - purified eagle extreot* ChronB. - purified eagle extreot at above after nitration* Chron. C.-polychlorinated biphenyl olutlon a. Coluan 6 % Q? 1 EC-deteotor WATER_PCB-SD0000031089 1 PART PER MILLION --- 1 DROP IN 90 FIFTHS 1 PART PER BILLION --- 1 DROP IN 90,000 FIFTHS OR --- 1 OUNCE IN 1,000 TANK CARS NEV 176985 WATER PCB-SD0000031090 NEV 176986 WATER PCB-SD0000031091 ffa r u 'S *n WATER PCB-SD0000031092 345 1 INDEX 2 3 THE WITNESS: ROBERT EMMET KELLY, M.D . VOLUME III 4 5 EXAMINATION: PAGE 6 By Mr. Kim (Continued) .............. 349 7 8 KELLY EXHIBITS: 9 Exhibit No. 38 ......................................................... 350 "Report of Dr. Frederick B. Flinn 10 of Patch Tests Made on Material Received from Swann Research, Inc., 11 Dated May 25, 1954 12 Exhibit No. 39 .......................................... ............... 375 "Medical Research Project No. 13 MR-4 6, The Toxicity and Potential Dangers of Inerteen," Submitted by 14 W. F. von Oettingen, M.D., Ph.D. 15 Exhibit No. 4 0 .......................................................... 378 "The Toxicology of Inerteen and 16 Related Substances Including a Method of Analysis for Halogenated 17 Hydrocarbons in the Air," by A. J. Fleming, M.D. 18 Exhibit No. 41 .......................................................... 378 19 "The Effect of Inerteen and Several Related Substances Upon the White 20 Rat," W. T. Read, Jr., M.D. 21 Exhibit No . 42 ................ .............................. .. 4 33 Letter Dated February 14, 1950, 22 to Dr. Louis W. Spolyar from R. Emmet Kelly, M.D. 23 Exhibit No. 4 3 ....................... 438 24 State of Indiana, State Board of Health, Letter Dated February 28, 25 1950, to Dr. R. Emmet Kelly from L. W. Spolyar, M.D. Martin & Associates ( 409 ) 762-2222 WATER PCB-SD0000031093 346 1 Index (Continued) 2 3 KELLY EXHIBITS: PAGE 4 Exhibit No . 4 4 .................................. .................. * 465 Memorandum Dated December 12, 1966, 5 to Mr. D. Wood from R. Emmet Kelly, M. D. 6 Exhibit No* 4 5 468 Memorandum Dated December 1, 1966, to G. R. Buchanan from D. Wood e Exhibit No . 4 6 ............................... .......................... 480 9 Monsanto Memorandum Dated January 12, 1967, to P. G. Benignus 10 et al, from D. V. N. Hardy 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 Martin & Associates ( 409 ) 762-2222 WATER PCB-SD0000031094 493 1 INDEX 2 3 THE WITNESS: ROBERT EMMET KELLY, M. VOLUME IV 4 5 EXAMINATION: 6 ? By Mr. Kim (Continued) PAGE 496 8 KELLY EXHIBITS: 9 Exhibit No. 4 7 .......................................................... 497 Monsanto Memorandum Dated 10 January 26 , 19 6 7 , to G. R. Buchanan from D. Wood 11 Exhibit No. 4 8 .......................................................... 500 12 Memorandum Dated February 13, 1967, to R. Emmet Kelly, M.D., from Gene 13 Wilde 14 Exhibit No . 4 9 ............................ ................. .. 589 Monsanto Memorandum Dated June 12, 15 1956, to Dr. R. Emmet Kelly from Elmer P. Wheeler 16 Exhibit No. 50 .......................................................... 589 17 Monsanto Memorandum Dated June 12, 1956, to Dr. R. Emmet Kelly from 18 Elmer P. Wheeler 19 20 21 22 23 24 25 Martin & Associates ( 409 ) 762-2222 WATER PCB-SD0000031095 / 8 19M Don or io Hama: a# ninr ov mwe *an m ow iubhiiil mwiB nai wrM miiM, m. fha *)Mt A thla iatoatlcatloa na to Aotoadaa vbttktar Mt tto wliu okloxiaatoi ilpk7l aa|ffito aataittod or -- lapriliM e^Mlaim! thorala Mfkt to tto aaaaatlTa agoa* pwdnola* tot daxxatltla Alek ted daralopA mbs im of tha voztaaa la too plot* ' larp Alto rabbito aaoA la asieiai tto patok testa to litolM tto Mtlom cf tto Tarleoa aMm&e&m aatelttod m tit Aim<> fko p>oaafttEra tis to akata tko salael i boom bAera tto pAeh mm appllod ttot tkara wmM It ao brokaa Ms to iatarfara Ato a* to aggravate tto taat f& Material tolag taated mm Mmg Ate atkpl laokol alt tor gattlag a aslvtiam ar a MjiaAoa far Iko pvpM @f AUvtiac tto asttrtd,# fko patok vaa laft <m tm mAom parida Aarlag tto toata -- mm for IIS ten* otbaro fa* <18 ten Ika patok was tkes ronovod ad' tto ozpoaad araa eatokA for toe mki to ba tor* that tha toat u aogatlia* fhla wm im to mil tea aknoa of aot <ti>ervtsg My laftoat ar dalsyai aot ion amh m le taatliM taka plaaa is aaklag patok test0a W@s mm mm irfesmtlom tto aakociala vtttk wm aocatito nn oppUM 1m a esaeaiSgestM faa ia &a?M6et toata to mm if a damatltla olgkt ask daTalop vte tkaaa tiromituaM* ladtpmimt toata mm mM Ate aaok sctwlal aad mm sii on lilfimt daya Aik frotely pimi aeXatloaa to to aora that M amr had oxipt is* Coatrollad toata vara mMa .aaak Mm# Atk tto alookol ad gniaa ad to dato^M wtottor tkoy Aght sot to tto asctlT agtat aMag tto stamt IoAobb* (Km balao ia Riaea rpostf toEisg doAffmtloa Him too v&Amm sisiesiaSs ty tew ItMvok foUwf kjr Sto MMMo fiaaisatim eM mill f Mak Aaolfia aalvtals iroalag IMt 9, wiM ktfora . iroler isigg Xt Ml GSgM) tost* w &-) . tw toiti Ato wantnA smtaiiel les eiss aegaMm M iatwiiaitl iaa itpllfti ^ __. XWf pace lft$ by Bni* ,Aioa1 aai 4>rf atnaaa A atyroM Aak beilan __ _ irealar H ltt latoboek 176t pca ltt aaa aapatlA to all fMta tesleiias tto niuidlnM si, Islnltiiuli -^n\ EXHIBIT mo < A I JHMMxdi 2 0 5D WATER PCB-SD0000031096 \t u /; Mxmhn ipald (Lot l&tmteek Vo. lit, mm t| ynpmA bp cf vq( diphenyl ad Mj( atyra* ad' atyrono M# toilwK (Llqgld itoaia. aalfio awitr Jxoolor Special XftMMic Yo 198* pc* Sr- m ehaleal avo podtla test vllfe took of Ik elskt applications* It Am pn poottlm apltoi Mm Ik fmiM4uil toot* Bo tjpi of domotitla mo ftlA* _ _ iIQ.l 1M (Lot . !. 3/M/M) toil* iMi, Lot f| Ml eicht testa pn o poaltlao rosetta* *ho lolradoaal tost tu Mm positive* A* mitin mo aSMo drooler laii tot 8a sit g/i/i8h '` Imior ims0 lot 9 A elgfeS testa fora a poeltlio roaetla witk this senpoud# tfeo latradaraal teat ms Mm paitiw X fool that tka Aanatltls produced %j tkiaaatexial was prenoua GssafSaMa iMel mao Mm ftooad, to be perttite* fit several teats it did Ml mice its ipimN fa M hours after tko gate! Mi tom naowi# teeolor tM9 (Lot la Iter ground! sale d/m/sili drooler 1S69* lot 8@ vonl dips Ml igMi taata war* negative* *he ia tree of the tee taata ante 11t the ooaooBtwtad Material* fhe latradeaal teat gave reaction*' ' Imkr H89 CM letateek 176* jpege IM4 ppinl bp Barrie* of 96*8J( diphenyl end d*8p etyzene ead etrraao Mil toller -- irp oaotadl drooler iSISo lot notebook 176, pc Ul* <17 vomit Ml eight tosta wore aesetlvo* 'a oaeostrmtei testa veze Mot negative* a klnitiitl test fare apatite reatloe* ' koite UH (Late Sijl>salg Be* Ifi* pig -. - ' &m^ms Mi, Lot Vottbock 176* page Itt* ml gswats Ml el^il teste men opllitt Be tm toota isis vttk ooneankratod mtoiei mre aim aecallvo* Be Ulnltad test gw a aagaftlvo natlab droelor lttt, Let 9# IMtMk 199* 8W IQ Cflw around 1 <! MUit .. - ' gKsaM5? S3S0 lot S Isteteek 5teo ItSf gego Ut GigSsti gsfi!i taste mcgatiWo tt testa rate vlth oonsaatrated odezlal mro 9lm a^tlw fko ialmdaaal taata *va a aaiotlto matloa* 6BRN002056 I WATER PCB-SD0000031097 Mowslueoi / Salons lOOOt fM MQMii a tad la all af l&a aldt tada is dlafc it m aypilai* Si nastloa m llffarnt fmn that of tka tkraa MrnAsm gifiag a poaltlto ataatlaa* af n*a aIM0 kd Ilia adarlal gen am alaazdlta araa* MawftWi * . B&onx Mi ISA tests vltk %Ma aonpomii katk wattilfiiil aaA Ulstif mm mgiMm " ' galwasg #10041 Stolons Mi.g Ml tiiti dtk tkio wMhss&&0 toil Msnatniil ad lilmtej nm mdiatl'Wo Strraaa Dlahlorlflt (Sotabook Io 1ft a.Q Hit . """ ''Sbjjriao 'B&klarlAos mHo ilttMi aat*rl*l mm podtln* It vas artlooA thd tho rabbit foUM mi teas this ahaaleal wao applloA w la tko Allota fan* fhim Am can a olaaratln loolas* ixmlot la4fl Canltl (Batch i6 Ssplo 04 - auto 10/a/sHi Aroolov ms Spaolal Bdak =4k=43 Stoda 10/i/90t Mi Amin gcra a nrj Mh ratatlom dtfc tki ddm bat m and say tkd 1% la pedtiTt* ' Irwlw lgflO (Sot 11,, mfl e/c/a.) i ixoalar U80* Id Sit Bdo ^/as/&)t m Am tasta nra aacatln* ft tmtndoal a iobsibIkM taata nca mAo* lioalag 1S81 flateh BAa lml 7.Ir-6. UAa T/a/N)i Azoolar iSISo Bate* 8A IM T/a/Ns Ml taata nra aagatln* Ite ltM. HMMMi (Irtabook Sa Utjgifa Nil mMff atkjl boasoaa* intitd I9t pa<p SLt Iwsy tost aoAa Mm tkla ndaslal gara a podtln tad* flta laalaa vaa tf n aloardlaa _# ehlflvftadaA Styma. lotobook ltt, pap It VW>* *w*T tad aado Mm tkla fan aa aUardln latfaa* GBRN002057 s WATER PCB-SD0000031098 4 to# IUu'i am**aks are eoploA wMiit w follows* Oaa to Sssggaaeel with the fast tfc* Ml f tbo Mmlem tgMm poslttwe wtttn m off a fkM satara# ittopta wa cafi to ii}i th> aalaala to vvera tel oboorTatiana sate os ooaolads ttat the ssif ttfftrmcc m that tho laal weoM to* iqstai to the hot satfit! gat It vaa i3A `Immm that m seaetlaa share Ml os ufeuui ia clvaa to i emre ' ' Oat wnot tat feel that say stfrwa asipmai whtoh ay to feast to ha preamt as m laporltp la the ibm ef yr troabl** 2 na rathar wf^Mi tick sag ef. the ateiitteA tit aot show m> gi'v nasties* the Ma# It In heea (Mm la no , tawrtigrtiii* that ahlorlae 414 aot piw a toaatltla Am ' mtalllq olootroaoa ww modJbeft^4Llff.Jha.JMAalllau>laato4aa-osio-- rapliaaOj' earhoaTileetrodea# Si theory ms tlul as orcmlo ahlorlae oovouada mm pta4 is tha latter m* X eoolt oocfoot till jo 16% jeer wadlllatloe ayetaa ia plaoes Am fmea are gt^s off# fhrt aeaas be pwHJM for tie aea to take a bath with mm md water if tlay ess la emtaet with the Iff of material ftaaA to be paiMm By ttfa Z mm tf a feels or village went, fha fciiMiefe IdUn eader these olremstaaeea ahoalt ho laalato4 ea 1 fooad that h I Mi eettaa tbs material m ay Mate if X ntd thm tteomtty ao troablo arose# (81fi4) Ifceteriek E0 JMam SBRN002058 WATER PCB-SD0000031099 . ** ,, . . * . ; . j: ? * J V- v' *." - *.;.,`4_.i7*'* >f^.M.. ****** '^J?-' *-*.* **T . S-? ' "r- ?v:\- .2-i-rf * - * *k* f? . .. ***>.' i e> * .<= ^F . jv~; r#* w* i ` *? . ; Medical Research Project No. 1R-45<''"T. THE TOXICITY "AND POTENTIAL DANGERS /^F INgRTZHN * t . > *. . m "*./..I*- . . .. . " "Submitted by - *.*. a,f' *I I ; ^ * :*** `4 V.- ,, . .* ,,V'i-- i'-..t-- > : * Yi. F. von Gettingen, LD.', Ph.D Director Haskell Laboratory of Industrial Toxicology Wilmington, Delaware. : i _ ' .. WESraiSBOUSE ELECTRIC & M?S. CO. cas r i instuunj, i a. IKDJiiUAL H/jib.VS lA-OUATOrr FiL COi*Y. . *.* * -X .#4t WATER_PCB-SD0000031100 the Toxicity and Potential Danger* of Xnria aad Substances, Including a Method of AnjOjil* lor EAloimAt^ ___ .......................................................... . _. V. 7. Ton Oettingoa, M#D# ?h*D. . The toxicological experiments on this problem were arried out by Dr J# & Toulger and Dr. A. J* /lenlng of the' Dpartn- of Toxicology tad the pathological studies were at-do by Dr* 1 * Reed, Jr of the Departs eat of Pathology of the BatSctll Laborer The sateri&l was investigated with oral administration to rets, application to the skin of rats, and in inhalation experl a cats*. The .latter were planned, in such * way. as to approach as closely as possible the actual conditions encountered in the- us of this material in transformers, in order to evtluats the aaxl hazard which nay be encountered in its use for this purpose I comparison, additional tests were mace regards the toxic effect froa inhalation of vapors froa Pyronol and Transforaer. Oil (T?ei inghousej la addition, e method was worked out for the deter mination of Xnerteen in air . . 4 Effect of Oral Adalul.iietlfln .' ' ' ' In order to determine the minimal fatal concentration of Xnerteen for rats, 100 animals tire given by stomach tube sinr dose? of Xnerteen, &s indicated in the table*. . Dose ,Ko. of Bo. of Time of .4eath Per cent cc./kcn. aninala dead mortality 6 treated 1 '. 10-1@49 h& 5 4 4s vithin 5 days 19.2 J\f 15f 6BRN003094 ' 1@5-1.99 2.0-5,49 24 '9 6* 2* 10 5 5% 3 U0 ' 10 e * 5 20 15 15 4* c7. & 50,0 50.0 75.0 WATER_PCB-SD0000031101 s 'la thtss, us la. *uL*quwat sxpsrimeati, an TlI thovtd sipas of discomfort lBacdlstsly following the sdaialatrstioc, lstsr they bscuae depressed tad refused, frequently, wttr and food; within a' feu hour* they beceae teiJc and stuperous, . so that they ttre finally unable to rise. hen this stags wa reached they invariably died* toe of these rats was found to uffer froa albuainuris, oat deTtlopsd tremors of the head nd fore-limbs, end one showed severe hsmorrhuges from the intesti nal tract The table Indicates that with oral cduinis tration the ninimal fatal dose of Inertecn for rati, which Icills 75 per cant of the aniaali within > days, la S*0 to .4 cc# per kilo gram body weight. Upon-- pathological examination of 0 of these auim-ls, those that had died spontaneously showed congestion of the luru:s. Y.hic us'combined vith edeau Mid heu^rrhafe in several instances Tea of the anixuls had mottled gray or yellow livers cad in three instances there res a diffuse pallor with moderate yellowness In 5 out of 6 animals studied cicroscopicully the liver shored narked aid rather extensive hyaline necrosis in the central part of the lobules; the liver cells in this area revealed fatty de generation of the cytoplasm; and in eninali that died 5 and 64 hours after the treatment these cells contained increased nunbera of aitotic figures* In the majority of the animals the mucosa of the intestine v.bS congested and the fecal e-teritl in the -intestines contained' old blood; and in one'instance fresh blood was found in the lov.er third of the ileua, lover Colon, GBRN003095 WATER PCB-SD0000031102 I and sigmoid. Mlero*copiD*Uy the llsatsh of two uxIaU* pr**ot*4 typiexl faonorrhxgic trsfioas of the iueou; aaothwr ahowtd hworrbaglc r#* la the iueak; bad la the rcaulnlag animal* poataortoa changes did sot allow an exact Investigation In order to follow up the toxic effect of Iaertees oa the liver, & group of 50 white rati eta tret, ted In the a use way wit single oral doses of 1*15 to 1,20 ee# per kilogram body weight. Six of these were killed 3, 8, and 11 days, respectively, after the administration* ' "Upon pathological examination it was found that two of the 6 animals killed after Z d^y had. bloody aaterlals in their stomach* cad in 60 per cent of these animals the liver v;as sllchtly yellow In color uiu the liver cells were large and coi tainod ' numerous nitoses tad occasionally there tvs necrosis of cells Immediately about the central veins Animals killed aft8 days presented u slight enlargement of the liver with a ques tienable yellowish color, the liver cells were large, those tx toe central veins were dark, and occasionally there was some ftttydegeneration of these cells Eats killed after 11 days showed no important gross pathology* microscopically, l11 sec tions showed a slight swelling of the liver cells with occtsXc tcuollxfetion o' the cytoplasm. lio other' organs shored paths! changes referable to the exposure. . In orcer to study the effect of reseated oral of Inerteen, 5 groups of 10 rats each were treated In the fol! lng wayi ' 6BRNQ03096 WATER PCB-SD0000031103 4 Ih first froup rcivd fr 0.S5 to 0,84 ec. ptr tllo for' 5 caastcutlr* daj* Ioa of th dl*d ad 6 #r# miw after the Brd treatJaeot for pathologies. #T*twtloc. Si# second croup us fed doses fro* 0d3 to O.M cc, ptr kilo. ' Two died folio-wring the tod'dose End 6 were ldll#d for mxtopgj after the 5r'd adnlni strati on. In the third croup the dose* rtaced from 1C3 to 1T8 cc* per kilo* On rut died after the 1st, three^ after the tod, and four after the Zrd treataeat, and the regaining anisals tero killed four days after the crd treat- atnt* . . . Upon pathological* exsninr.tion the livers of the rets of th< first, group appeared somewhat lighter than usual and one shoved large yellor; cress; there was i diffuse slid swelling of the liver cells v.ith sone polychrostcit; occasionally the cells sho< soae vacuolar ch-Jiges -Ji the eytoplaan, but in general these changes were cot very severe* In 4 n.ts of the third croup ubi died after 3 treatsents the stoaschs vere dilated with food and in tea of these there v.uc also soae old blood present* iiicro- scopictlly, one rat htc sscll infliisaMory ulcers in the fore stonech and another shorc-d bedorrhugie erosions of the pylorus. All shored some fcyperenis. of the liver and in* one rut this v.u3 of Bottled cppeuTence. Hicroscopicully tvo rati.- showed svvellin of the liver cells vith fatty degeneration #of tnose in the cent parts of the liver lobules# tEvo others presented central necro of the liver cells tith hyperplasia c:* the encothelial cells 1b these areas, one shoving in addition, nuaeroua mitotic fir-ires BBRN00S097" WATER PCB-SD0000031104  Xh% liter can* Of' L nti which ^ere kill*! 4 dty foUotiax the. Zt Sinistratlon, o&t h*d ua-11 uBuat of blood in tb gastric content. ' The llrcr* of both ahlaals wp si.rec moderate!; enlarged and deroieopleklly there wts u genertllted tveiliaj or tfa^ liter cells with som polychrosu-slfc. . too rat suffered fro* fairly general Tkcuoler ricgtneration or the liter cells and another presented racuolnr changes in the central part of the lobules. ' In order to compare the toxic effects of Incrteea vith trichlorobensene and ethyl-tetm-penta-chlorobenseae, a croup of 10 rats was glrm daily doses of t.richiorobengine ranginf iron 0#S6 to 0#5B cc. per kilo body weight* One died after, the 1st, four after the tod and four after the Srd administration, the reiaining rat way killed 4 days following the erd axid last trectaent.' . It appears, therefore, that daily qosbj of 0,56 to 0.5B cc, per kilo of trlchlorobenzene killed SC per cent of the animals' rith S coses, whereas it -was found that doses of 0.6E to 1*04 ci per kilo of rtr:vl-tr-tra-ncntachloroberien&. given in the sane way, -killed only 10 per cent, and Inerteer. in doses of 1 to 1.7C cc* per kilo, given in the sane wey, id.lied DO per cent cf the rats, Upon pathological examination, animals which were treated with trlehlorot.en2ent- anc which died & .-ont&neously shoved a passive congestion of the lungs and the liver; the stons-cbs vere distended . ith food; in four soae blood tts prtsent *in the 0 ' GBRNQ03098 WATER PCB-SD0000031105 0 gastric content# ana in an* Instance there 4s a h*anrrlugic eraiion of tb mucosn* In two rats tot iAm honti irregular mottling. Liver ietloo,s of all animals ahow#d acrotia of ' toe liver calls around tot cantral vein# and touae in to* outer part* shoxed vacuolar degeneration. In rat* which died 2 to 4 day# after the first treatment there was soae endothelial hyperplasia in ther.nreas, of necrotic liver call*. One presented an increase ix?"the number of mitotic figures in the lirer cells. . Of the 7 rats treated with bio r ob es z e s t. the one which died spontaneously after tho 5ra dose showed con-, gestion and hemorrhages of the lungs, generalised passive can- gestloa of the spleen, bone marrow anu other viscera, distended stonachi txju moderate yellow mottling of the- liver, tho liver cells being mildly swollen ni showing fine vacuolar degeneration The animals wiiich were killed showed only a questionable enlarge ment of the liver and kidney anu a slight swelling of.the liver cells with occasional vacuolur degeneration, . Lich* changes were . extremely did. .' ' -i5-a>a>fiderably less toxic than trl chlorobenzene, the minimal fatal dose with oral adaihlstratlon, killing 70 per cent of the anlcals, being t:round 3,0 cca nor kilo rritt whereas gthvl-l-.-tra-renta-chiorob'msene does not ;-.ooci r to be nearly ts toxic rlth oral ednlnistratlon. The octholo--ic;.l changes observed after oral ldoinistratlon of Inorteen anoe: r to be fairly consistent and obvious* Lt-rro doses BBRN003099 . WATER_PCB-SD0000031106 7 yUA. JLO^ fc 8 S1T .of the gf -Sht. k gills,jgugm* ti op ' ..yi thu - rl th ' rk t j ' after eight days, cni after eleven davf no definite liver pa^olaglltg S* 2T1*q\\' IJLJ^23aijaiSL^^ Pintle large dose? -moir to be sore Injurious'than such doses glren In fractions. ' * *. .' ' ej^L_gjLA2^ . Ten *hite rst* t-re treated dally with ta application of about 05 cc. ol Inerteeu to the sbeved akin of the htek^'pre cautions being taken ta pxvTent absorption through the gastro intestinal tract by licking and by inhalation. All rats lost weight curing thr experiment but they showed no toxic slims aside from a slight restlessness at the'beginning of the ex periment At the site of the acsinistrution the skin becane dry, thickened and scaled without any fissures being formed. Sinilar reactions were observed on the human skin especially on the hands, cbweks and forehead# One of the rats clou after 11, and three after 12 treatments, the remaining being.killed # Hi hours After the Ibth application. Upon pi. tholo.jical examination the liver of all an intis was found to be dark gray brown in color with notiling on the 6BRN003100 WATER PCB-SD0000031107 *urfe. In those rt,t which died spontaneously there tui Xtitty degeneration of the liter cells with necrosis of those around the central veins and In animals killed at the end of the ezperisent there was c slid swelling of the liter cells ' with occasional vacuolar degeneration In tone. Microscopically the skin at the Bite of application of A rats showed hyperkera- tlnlcation with occasional blister formation, one animal showed perifolliculitis, one. hyperplasia < the eoithellun rather than hyperkeretlnixstion, and in 5 rats there was u nild fibrobltfti- proliferation with some round ceil infiltration' in the tmderlyl connective tissue. It anoe&rs, therefore, that the contact of Inerteen with the skin does not only cause locr.l reactions such ns drvners. thickening uni pc&llng of the skin, but also gvstealc effects a; Indicated by the injurious effect on the liver. Lff(-ct of Inhr.latlon of Vapors. '' In evaluating the toxic effects -of inhalation of vapors liberated fron Inert*.en ut elevated terperntures, attespts v>erc e&ue to reproduce conditions &,oru severe then would ^ be eet in the overheating of & trtnsforner* In these experiments rats were exposed in l limited apace of about 1 cubic foot capacity to the vapors of the boiling material which entered directly into the chamber through a hole in the lottos In each experisent ft ruts wo.re exposed on L5 to G6 occasions for LO aiuutej, twice, d-lly, to vapors fron Inert&en, Pyranol, or BBRN003101 WATER PCB-SD0000031108 9 Transformer Oil (Weetiag'bouee). During this time they *hoed irritation of tot efcin, which' appeared to be most marked on those parts of the body cot protected by b&ir, mu which per* listed for some time after the exposure. Pyranol appeared to produce .the most affect 1b thia respect, followed by Xnerteea and- Transformer Oil, in the order glrm,^ In opposition to the L rate exposed to Pyranol end Transformer Oil, 3 out of 6 rats exposed to Xnerteetx lost weight, but no othor toxic Bipu were observed. It is quite possible that rats exposed in this way absorbed some toxic material through the gastro-intestinal tract by .liching the fur during or after the exposure since the mate rial' had a tendency to condense on the walls of the chamber and on the surface of the aninals. The naxinun concentration of Inertaen to which these rats were exposed was detor-inuu as abou* 0.5 cj. per liter of air# * Uoon pathological exaninction of ruts exposed in this way an 14, 25 and 06 occasions to Xnerteea, no definite pathological signs could bo observed in the liver or other organs which could be referred to the exposure. Two rats treated with 41 exposure;, to the vapors of Pyrano showed no definite cellular changes in the liver -1though in one aninal there was an inure..sed minder of aiitotic figures in the liver cells. . . Two rats exposed cm e4 occasions to the vapors of Trans former Oil (riestinghouse) shoved no definite pathological changes of the internal organs. 6BRN003102 WATER PCB-SD0000031109 10 la rdr to iudyth effects of continue mnTM*- 10 rat* w<ri. axpj4 6 hour* dally on 6 day* t xor 80 'days to coacmtrfatiaa of 0*08 t(, to 0.09 of Irt*c pr liter of air. They ahovad no toxic nor pathological ign referable to the ezuorare; there tin no definite change* f ' the red blood corpuscles or the hemoglobin* The animal *re killed 2 day* after 20 oxporure*, 5 m t ed Ahgr3L-^2a^imigj-J^Ji^ .Qtg g. of latgteTO ver liter elr_. nor continued exposure to concentra tions of 0.05 to 0,09 tat*. per liter eir cause a definite- toxic effect on the liver* - ` . ' *' . Deterainstion of Concentrations of Inertoen In the J-lr. In order to determine the concentration of I&erteen vapors in the air, the following nephelometric sothod was .worked out, after several other procedures had bees considered. A definite voluae of fair to be tested is drara tt t rate of about 1 liter every 4 Blnutes through fa test tube containing cc. of ethyl alcohol, inersed in cry ice-acetone mixture in order to prevent the evaporation of the alcohol At the end of the stapling 1 cc. of. the alcohol v.os nixed vith 10 cc. of dis tilled rater and the resulting turbidity was set sured with & photo electric cell, usin*. fa sodiun vapor Ian? us the source of light. '' * The turbidity of unknown staples was compared to the ' BBRM003103 WATER PCB-SD0000031110 These cx?erle&ts how that the cmcmirtUoa* f la air dtcr#8e rapidly with the distance free the ouret if their producti # . la order to study variations of the concentrations oTer e period of tine and with different temperatures, a current of 10 liter* per alnute of air us passed over the surface of Iner- trn of about 10 square laches, contained in a flask and thenoe Into a bell Jar. Staples were taken froa the Jar at Yarlous intervals after the flow was started and with various teaperature The following concentrations were detersineds . . Tine of Concentration of stapling trichlorobenzene in hour* . in sg. per liter Temperature of trichlorobenzene in flask ' C. f ' ' 6' 1 4 . . 1 Jtti222lE2k2Mffl 0.29 0.61 0.60 1.68 1.70 1.00 ' Inerteen '* S 2 28 bO 50 . 90 * *. 6 058* ` m' . This tabulation shows that the deteralnations made -at ' &ZC and with the 6 hour sample were alaost the sane for trichlorobonxene (0.60 eg. per liter) and Xnerteea (0.58 ag. per liter). This suggests the possibility that the bulk of the vapors liVyrated froa Inerteen at this .temperature aay be ' trichlorobenseaej so that the hazards froa inhalation of Iner teen Vapors are identical r.lth those froa the inhalation of ' 6BRN003104 WATER PCB-SD0000031 111 tricM.robi* to order to conf!m thl*, Mi cc. or Xacrtcon vere ^ubulticd to fraction*.! distHtotiwi nad ^v>* foiloriag rmlts w obtilnortt Fra c Hoc Temperature of dietllletian *C. Tolunt caHei#d cc* . 1 240 40-254 s 864-280 4 80-500 EesidsM above WO SB 41 45 SO 180 Specific Boiling Gravity Politic of fraction. 1.468 1.478 1*488 1*877 1.88S COS-218 EM 40 69 Since ,.the opocific gravity of trichlorobenzene is 1.466 . and the boiling point QBC.-219*C., it is evident that up to 240C the vapor consist exclusively of trichlorobenzene and that for this reason the Lhove statement Is justified, naselr. thfet for iao3t~ conditions the hazards froa vcoors of Inerteen t-.r*! Identical wl th those froa trlchiorob.ensene> ' ' ' Beaune. .. The experiments discussed in this report ahow that vith oral administration Inerteen is considerably less toxic than trichlorobenxene, .the ainiaal fatal dose Killing froa 70 to . /' 75 per cent of t, he rats being around 30 cc. per kHogr&a body weight and 1.4 to 1.8 pw kilogram body weight, respectively. Fatal doses rill cause passive congestion of all viscera, ex tensive degeneration of the liver, nd ulceration of the gas trl nuc' osa, Fith su!lethal doses these effe cts# ere loss severe end there Is evidence that they rill heel then no further exposure occurs* . BBRN003105 WATER_PCB-SD0000031112 Continued application of Inert& to the akin 0f rats end humans causes drynsss of the gJdA# thickening tnd sealing; and the observations Wide In rats indicat that sufficient e quantities c&y bo absorbed through the idn to product injuri ous effects a the liver* . Repeated inhalation for short periods of concentrations of 0*5 mg. of Xaerteea*vapors per liter of air, or repeated, inhalation for 6 hours of concentrations of 0*05 to 0*09 ng, per liter of air causes no definite injurious effects in. rats* Vapors liberated from boiling Pyraaol, Inerteen, and Irons- former Oil (Westinghsuse) are irritant tad the irritant action decreases froa Pyraaol to Transformer Oil (Vestinghouse), In erteen being Intermediate in this respect* It has been shjva that vapors liberates froa Inerteen under conditions approaching those as night be encountered in transformers consist n&ialy of trichlorobenzene. ' . jh. simple method for the determination of Inerteen (tri- chlorobeazone). vapors in air is given* If 10 liters of air arc dram ut a rate of about 1 liter every cinutcs through & test tube containing 1 cc* of ethyl alcohol, cooled in dry ice or in in let' sc.lt mixture, aid the tlcohol is then poured care fully on the surface of o fov cubic .`centimeters of water in & test tube", l ring of turbidity is produced .if the concentra tion of Inerteen (trichlorobenxene) is over 0.05 iag. per liter of tir. If under these conditions a white ring is produced, 6BRN003106 WATER_PCB-SD0000031113 the air tested ahoold be regarded nth suspicion ud shanifl be improved ty more effective ventilation*. .. . . It was found that the concentration of Inerteea (trl- chlorobenseae) in a closed fp&c* 14 inches above the surface ; of boiling Inorteeu is 4.6 g, ptr liter and in an.op space : 5 inches abort the surface of boiling Xnerteea is 0*56 ng* ptr liter, and when the temperature in a transformer, standing in a closed room (vault), rises to B0C. the air may contain 1,9 mg per liter of air, . Proa 'the s-uiaal experiments^reported, it appears that concentrations below 0.05 fig per liter of nir will cause no ^ _i"ii # toxic signs or synptons even v.ith continued exposure. Regards preventive seesures. the following nay be suggests ` It appear*' to be cf paraatount inport:nce that the conttai- nttioa of the air be reduced to concentrations below 0.05 mg pe liter of air by adequate forced ventilation at the site of the ' production of such vapors ' Greatest personal hygiene is not less important. Contani mation of the skin should be avoided by wearing proper protectiv 'garments. such as gloves, caps, and coveralls* In case of tccide or vith exposure to higher concentrations of and above 0#2 eg p liter, respirators or open air masks should.be worn. The akin shoal'd be kept isxaculutely clean and ointaents such as lanolin or Aquafor should be applied to the skin after washing the hands In view oi the heputotoxic action of this compound, indi viduals suffering from Injuries of the liver, syphilis, and hear / GBRN003107 WATER PCB-SD0000031114 ihould bt xcludtd fra* operations in vhich I* hndld* ' . . Vorttrs hinrtllng Inrt*u or *ith frequent exposure to It* vapor* should `have periodic enril nations, special attention should be paid to their nutritional caaciti# ind tht coalition of the liver m.j be checked by aeteralnln,, the Icteric Index la the blood, tal the urobilin and urobilinogen excretion in the urine* . `. Regards the trectaent of toxic effects produced by exposur to Inerteea, it appears tdrisable to Increase the resistance of the liver by carbohydrate diet; i4mIMjtrtion of glucose and insulin may be advisable, ana duodenal lavage with nagnesiua sulfate aay be tried* Local irritation of the skin produced by Inerteea should be treated i.ith blend ointaents after the toxic, caterial has been reaoved by intensive vasiiin,; and scrubbing. In case Inerteea has been taken by noutb, the- toxic naterie.1 should be removed froa tha stoaach by eaetics ouch ts soap water or maturd'fitter, and this should be followed by gastric lavage with a suspension of activated charcoal in water and saline . cathartics such as Epson salts. '' co28 38 4* ' BBRN003108 WATER PCB-SD0000031115 IEE TOXXCOL0P1 OF UHOT AMD MLk?X isa 6UJ.CK IHCIUDLVG 1 UITEOG wF MAU816 TO? Bi!.v.n i*r> a vc v. _ r * ' A* J. TlmiMt * ' Ihe Toxicology of X&ortoon w%* lavoatlgated by oral adsAniatratioa, axis ppliCition# and lahalatioa experiment* in rat* la the latter an attempt m sad# to the aubatance in a wy relative to ita uaa in tranaforaera and to determine toe xaxlsua hazard that night ariaa should toa aubstanea be used for that purpose* The minimum fatal dose was determined by oral edslniatratlon and to* affect of repeated oral doses was studied and compared with toe effect of similar doses of trlchlorobenaena and e thylte^pi^pnta-chlorobeniene. A tethod cf air analysis'for th hmlogcaaf d hydrocarbon! was devised and air an&lysaa were made to determine the con centrations of Inertaan in to* air near open and closed contain ers when the substance was heated to various temperatures and when samples were taken at varioua distances from the source. A statement of the problems incident to the toxicology of Inerteen and the answer# to these problems will be found in the conclusions and sunnary at the end of the paper MuMm (1), Single Doaea The substance was given in single graced doses to several groups of rets to determine the minimum fatal dose cnnnAfii 300021 WATER PCB-SD0000031116 ^j| @##f @ 8?8g o ft * OT rrmvr c* CJ 1C cr B KO fyt c ffv V c 0) c> gk g a a c&c-.* H &* t i* r f* 0 O - 0> W w w a < fc M fe ^ HZ NMci HPC H e 0 W t*3 tn . t* IS C O tt t *1 fBt c ma m> n- C'000^^ 300022 WATER PCB-SD0000031117 . Th tmult* r eonvaaitatiy tabulated in tabla l. ' Ai oot#d| * dosa of to 8.5 ee. par kllocrut !# a 75 par east ortality* fvwty-nro of till* group of ^inii virt *u taps lad. Aaothar group of BO r*Vs was glrca 1b;1 oral dosaa ranging from 1*15 to l.3 ee p*r kilogra*. Six of theaa nn kill ad Z day* after treatment and axaninad by tha pathology dapar^eat for possible liTer dm{, flz wart till ad 6 days &ftc treatment and examined for possible kidney change and 6 ware killed 11 days after treatment, and examined for poaslbla brain damage. K \ ' U) Eeoaetad Poses ' Thirty rats were divided Into groups of ten* The first group received Iron 0.35 to 0.56 cc. per kilogram for Z treatments. Sone died and 5 ware killed for autopsy within 4 hours after tha 3rd treetsent. la the second group, the dosage ranged from 0.63 to 0.66 cc. per kliogran. Two died after the second treatment and 5 were killed for autopsy 4 hours after the last treetcaht. In the third group the dosage ranged free 1.22 to 1,76 cc. per kilo. One died after 1 treatment, 3 died after treataenta, and 4 died after 'toe 3rd treatment. AH animals in this lest group vere autopsied within 4 hrs of the last treetsent. ' Ir/'general all rats behaved toe sene following oral # administration of Inerteen. They proceeded at- once to eat as if to allay the discomfort caused by the substance. Following this they became depressed and would not eat and often would net ' 300023 WATER PCB-SD0000031118 drink. litJaiii stupor generally rupirvta^ within fr hour* until the eninai*.. could no longer rise for jood wttir. Ii;ud nr taken, however, if administrated and for a fee minutes following administrstlon the smlaalt parked up a Mi Tha improvement was only iimporary tad tha oataone, when they had thus far proirus^, m invariably fatal One anlsal howtd an altoua*nurlt (testad poat mortem) Mid on* de veloped trnori of to# hee.d,. and front limbs. On* hmA eevere hemorrhages from toe rectum and to* autopay indicated the bleeding was from the lower and of tka smell bowel. Comparison of Incrtaan with tr1chiorobensana mad gthyl-tetra-pentc-chloifiiniflf.................. 1 group of 10 aninels was glvan repeated doses of trlchlorobenzane ranging from 0.56 to 0.68 cc* per kilogroe. One died after toe 1st treatment, 4 died aftar toe fad, and 4 died after the 3rd The remaining animal was killed 4 day* after toe 3rd and last treatment. All animals were autopsied. Similar groups were treated with Inerteen and ethyl-tetra-penta chlorobenzene and the following noted! Daily doses of 1.23 to 1.76 cc per kilogram of Inerteen killed 60 per cant of the animals, when 5 doses were given, while dully coses of 0.36 to 0.56 cc per kilogram of trichlorobenzene killed 90 per cent of the animals with 3 doses On the other hand daily doses of ethyi-tetra-penta-chlorobenxen ranging fros 0.62 to 1.04 cc. per kilogram*killed 1 rat in a group of 10 with 3 doses. . . Conclusion! fnnna54 Tne sir.ims fatal dote of Inerteen appears to be ' 300024 WATER PCB-SD0000031119 -4- around 3.0 oc. per JtUojm, d dates of Inert*as were fatal ta eoneactrations betwen O.SS asd 1.71 et. p*r kHofma, while repeated doata of txichlorotM*a were fatal la ee- tratio&j between 02 tod 0fi ae. p*T fcllefran Xthplatetra* Pmia-ehl0TbnJt does net appear to ba umxlj m Uxie by pal adalnlatratloa* flalf a oublc centimeter of Inerteea ati applied deil; to the ahaved backs of 10 pit* by ttani of a a mall glass cup filled with a piece of cotton wool soaked in the rubatance. The whole waa strapped to the aniaels with adhesive tape. Ont rat i died after ll treatments. Three died after 13 treatsents and to retaining aniaels were 'allied for autopsy 14 hour* after tna 151 treatment, All rats lost weight during the experiment, but out side of a slight restlessness at the beginning of the experiment showad no other signs. The Xnerteen acted locally on the shin, producing an txcasalve dryness with subsequent thickening and scaling without any fissures being foraed. The sane effects wer noted on the human skin with respect .to the drying and slight scaling and were cost notable on the hands, cheeks and forehead. lahilaUoa . An attespt was cade to reproduce conditions core sever than would be ret in the overheating of a transformer and expos ing rats to these conditions for 0 ninutes trice a day. 0 300023 WATER PCB-SD0000031120 .1 I- tha aXorsietaf id&SYm. riprtiuti a box ef *bou\ t 1 oufcdcfoot aapGlt7# in one eorner of which l tot i wifro a |lui flask containing tot lubftuei balng lnTeatigatod, Xn rt#o, Pyrt^l or traaa6zs*r til (WeatLaghouja) tnrf pilc^ in tha flK mad brought to a tell Iw r*tt vara pi*cd j la to* box and allovvd to rtouLla for 10 minute*, during w^ich tlaa a gtn*rtii*td Itching of to* shin app#ax#d which v* *t i *xk#d In tot part* of tha body not protected by hair* Tha itchlnavs parilated for aoeatlaa After tha animals vara remove* fro* tha box* fyrmol aeesad to product tha eoat affact to this raapaet with Inartaan and Irmjforatr *11 foUowlnc In tot 1 i ordar mad. Thrtt out of 6 of tot Inartaan traatad rata lot wifht vhlla toe Pyranol ud Transformer oil traated rata gain waight ( rats only in tacn of toe laat too group!), It It quit# possible that these tnlaala ingested a considerable amour, of these substances by licking their fur after rasoval froc toe J box. lo rarked change In respirations were noted, although the anlsals one* or twlca breathed faster than norael and occasion ally the extremities were slightly blue. At autopay bo gross pathology was noted. The saxisua concentration of Inartaan to which these rats ware exposed was about 0,5 ng per liter Tha box was aired betwaan readings, but not washed out. 0 With Inartaan too rats received 8 treatments, two received .3,5 treatments and too received 66 treatments. With Pyranol two rats received <2 treatments and with Transformer Oil too rats received 44 treatments 300026 WATER PCB-SD0000031121 6- . A group of t*n riti ni for io 4*j tig^t 41 . hour* par day to aaaeratritioaj of Z&irtacs la th% tlr rm*lnx fro 00S to 0,09 ag. ftr UUr. Ill nt irr kHl4 f0r p%tm>l9gj wltMn two day* following the &0th dty of traatM&t* light of thl* group gil&wd weight, o&* loit walgbt tad mi showed no changa, 71t* *hovd a flight 4rop la th r*4 blood count, three fhow*d an Increased rwd blood fount and two hov#<! no chang*. Ih* ehaafti in th* hemoglobin paralleled th* ehan{e< in th* red blood eount* f 9 c ft r bon . Considerebl* difficulty we* experienced in ostaining a satisfactory atthod of air analysis for these su&stancaa and a nephelometric cethod was finally adopted. In this, a definite volume of the air to b* tested ui drawn at t rate of about 1 liter every four minutes through 5 cc. of ethyl alconoi cooled In a cry ice-acetone mixture. The latter being necessary to prevent evaporation of th* alcohol. One cubic centimeter of alcohol was toen mixad with 10 cc of distilled water and th resultant turbidity measured with a photo *l*ctric cell, using a sodium vapour laap as a sourc* of light The turbidity of un known samples. was compared to toe turbidity produced by known standards made up of trichlorobenzene and ethyl alcohol, This method gave a satisfactory range of readings for concentrations varying from 0.30 eg. per liter to 0.03 fig** per liter which, when the original dilutions were taken into account, was suffi cient to detect a* low as 0.03 mg* per liter of Inerteen in the air tested. The method is not specific for the various members of the halogenated hydrocar Dons. COOOA5V7 30002/ WATER PCB-SD0000031122 7 lairttc. . . " Tha affect f ary lux the distance at wtlcn aaaplas war# tax an froa a cLoiti apace onr boiling laaptjaa wm da tar* mlntd wltt tha foLlaartax f#*uii#s Pi a tone* Cooaantratlon 14 4.50 to 1.56 19* 1.14 1.14 Similarly tha affect of warylng the distance at which Basplas were taken orar an open beaaer cf boiling Inertee: was deternined with tha following results; Plstanca Concantratlon s 0.56 10 0.4i 15 O'U to 04 The concentrations fall off rapidly and If any cool* ins surface is aDove the Xnertean and no air currents are blow ing oTtr the surfaca of toe Xnertean, there if ouch leas chance of any appreciable amount escaping into the atsosphere as frcn container like ^transformer. . CflOO&FiR ' gaggling at Various fise..latjjxi.ls_ and Xfrj.perat'Jres. Mr at 10 liters per minute was passed' over a surfact of Xnertean (about 10 *c inches) contained in a flack and toenca into a bell jar" Samples were taken frog the bell 3nnnoo WATER PCB-SD0000031123 Jtr at various intervals after the air flaw sma a tar tad and under various conditloas of temperature. Til* of CoaemtriUoa of Temperature of a*pllag . IriohLorbasn* Triahlorobenjunt At M*C. 1/i bmr 0.19 m * 0.81 m M I0C. 1 0.80 i.ea u to 4 1.70 to At 90C. 1 1.90 0 Lnartaan at 0C, 6 0.&S tz Trem the foregoing it will be noted that toe 6 hour staple with trichlorobanzane at 3C gives alaost the sane con centretion (0*60 ag, par liter) as did tha six hour lample with Laertee:; at 3C, (0.58 ag, per liter) This suggests the poas bility that toe bulk of the stuff coning off the Xnarteen at that temperature say be tricklorobeasese and that the hazard* o In6rteen Bay thus b tha hazards of trichlorobanzane fraction al distillation of about 335 ec. of Inerteen was carried out Is a distilling flask with a 300C thersoseter reaching to the level of the side are. The distilling flask was attached to a Liebig condenser end e collecting flask Samples were collects over temperature ranges from 4DC to 300C, (The temperature reco'rded being that of the vapor* .around toe .thernoneter bulb Tne distance between the bulb and the surface of'toe liquid vac about 6 inches. Although the liquid boiled vigorously several minutes elapsed before the'vapor reached the bulb). The bcil- snnnoQ WATER PCB-SD0000031124 lag poiat and pacific fxivlty wj nitrurtd for mea fraction ooUiet*4# Temperature of Bo 11live Point Fraction Condensing Liquid Fraction Bmo, Grav. I, Mo. *c. 1 5 4 Residue MO * C40-454 54-160 . 83-200 .Above 200 B06 - 119 IU ' 140 MB To (!')( 1,476 1,492 1,877 1.59E 118 45 48 m 110 .Fraction #1 m probably triehloroberueae (6pci- flc gravity 1.466, boiling point 06 - *19C.), In investigating the toxicology of Inerteen answers to the folioring questions were fought and are 'here given es far as posslolt, * (1). What i the composition of the Taper* liberate Iron Inerteen at a saxlaus working teapereture of 8DC# Trichlorobenzene only. v () What is the m&xlBua concentration of 'toil fraction to which workers sight possibly be exposed, . (a) In a closed space 14* over boiling Inertee: 4.5 ng# per liter. . OWUUGO (b) In an open space 5* over boiling Inerteen # 0.56 eg. per liter. ' (3), *hat eight be toe at* Inrun concentration in a room where transformers are placed when toe tespenture of the transformers- are 90C, and the air has a chance to get eatusnnn :<n WATER PCB-SD0000031125 _ 1.1 14 Pr liter* (4) that li a safe oamnirtIon n ahem by Animal Azptrimmsti* Coaildfring the hazard if 4u, wmd#r rdinary wiltlac eonditione to trichlorobeastot ilu| - (a) Fro* irichlorobemimf data previously btelaed, #0M mg* per liter. ' (b) From Inerteen data - ,048 i^.pir liter ' The laat figure has been trifled by expoaing rata for 8 hour* par day to juch concentration! over a period of wteJcs* . > (5) la thar a staple test that alii detect con* centratioua of Inerteen below .048 mg, per liter* s lea. if 10 liters of air are drawn at a . ratt of about one liter every cinutea through 1 cc* of ethyl alcohol (cooled in . dry ice or an ice salt mixture) and the alcohol poured over the surface of a few cc. of distilled water in a teat tube a ring of turbidity will be produced if the . concentration is over 0.03 &g* per liter If a ring is produced* the air.tested should be regarded with suspicion and increased ventilation provided. *# (6). that is the minimum fatal dote orally! 5 to 3.5 cc per .k.il.ogram. m #-- : - * t (7) Is there any thin hazard? Constant exposure sake* the akin excessively dry, and long continued^^r^osure WATER PCB-SD0000031126 - 1& mj radr ytraoo* xpos4 rutotptlbla to thaaa iinHiom mie&s-i proa* to irlit la iaslfiy dry ilclait 8/&8/M 4* fC r- ,w> - *" 300032 WATER PCB-SD0000031127 - ? Iff*ct of Intrtmas and IffiPtl )Ulatad ttbit*nct f^qa tfa* Whit* Eat* _______ W ? 4aad| Jr| M+D* In#rt*aa, a aixtura of trlchlorobtsisa, pantfe-chlorobmaunt imd chloriMiad diphaByi, was adjainlstr*d to whit* rat* orally, by akin application, and by lnhalatioc. In addition a*veral animal* *r txpoaad to trichlorobaaaana anJ tthyl tetra-pinta-chlorobmitaf taperatalja ' Two rata were tploy#d to itudy the effects of inhalation of t coapound known as Pyranol, and two other anlmala r axposed to vapor* of lastinghou** Tranaforoer Oil* Intrttia OrsI adninUtratlon. Tcwnty-four white rats received cingle doses fro= 1.L1 to 5,44 cc. per kilogram of body weight Follovinj treetnent death occurred in C to 54 hours. One died Immediately follow ing treatment, the arterial having beta partly Introduced into the lungs. Gross Pfatholory. Lung a i *ost of the animals that died show congestion vith or rithout edean tno beaorrhag. "4f EXHIBIT NO_____ fnnn-sfi3 liven Ten rata have mottled gray or yellow livers Ihrte animals show l diffuse pallor with aoderate yellowness, '0 Gtomtchi In 17 rats the stomach contains blood Kine of these present grossly visible erosions of the pylorus Intestine! In the majority of the animals the fecal cu.ter contains old blood In one animal killed 54 hours aft treatment the lower third of the Ileun contains bloody a; terial. There is congestion of the nucosa The lower colon tno sigaoid also contain bloody material. 300033 ,,< o WATER PCB-SD0000031128 t Mlcrgfcoslc HU^locr. ' in rtti are xmalm*d MitologiaiJJLy, Liven fIt* ho> wncid ana. rather ulcilTt byaLLn nweros; In th central part of tie lobules. The livwr ctHi atx thin araaa preaent fatty dwgwntration of the cytoplasm. In two animal a lirlag B& and b4 hours after treataaat ti are iacrsaswd numbers of mitotic figurts. Etomachi Two animals pre'aant typical hamorrhagic wroslona c tie mucosa, another baa hemorrhagic area* In the mucoaa. The raft of th animals show post mortan chinra which partially maaka prwctdiag pathology* The raaalndar of the Tlscera presents no chances that ere thought to be of importance* Eighteen rati were given l dose of 1*1S to 1,E0 cc. per kilogram body reight. Six of these animals were killed tb day* after treatment Six anis&ls %re killed 8 days after treatment Six animals were killed 11 days after treatment. Orois Pathology# Stomach* In of the 6 animals killed after L days there is bloody material in toe stomach. LiTeri In half of the animals killed after S day* the lire are slightly pale yellov in color Those killed after days present slight enlargement of the liver with a ques tionabli yellowish color* Rats killed after 11 days present no important nethology* Mi e r a 8 e e e., P a_th o1 o gy * Liver* Exposure 5 days The liver cells are large v.itfa numerous mitoses. Occasionally there is necrosis of cells immediately about the central veins. Exposure 6 days The liver cells are large . Those . about the central veins ere dark Only occasional fatty degeneration is seen. Exposure 11 days All of the- sections- show slight swelling of liver cells with very occasional vacuoliiati of liver cell cytoplasm. ^000 None of the other viscera present pathology of importance to the exoerinent* 30003d WATER PCB-SD0000031129 l CO i . Tvioty-^oe rati fotivd multiple triUcti by mouth. Th# amount of k single dost Tariea frea 0*40 to 1,75 cc, pr kilogram body wilght The aalmls studied histologically r#3 Group 1 4 rats, 1,84-1.75 cc per jdlograx. Di*d mftmr Z dally treatments. Oronp L. t rata, l.f-l.Cb cc par kilogram. Killed 4 daji after 5.daily tmtautii Group 2 ft rate, 04-0*48 ec. per kilogram. Killed 4 day* ' after 5 dally treatment*. Gr3A$.-MShS>lMiy Group 1, Stomach: All are dilcted tl th food . In there is aoae old blood present in the content liven All present soae hyperemia. In 1 the surface hts a mottled appearance* Group L Etonw-ch* One unlatl has t small amount of tlcoc in toe gastric content, LiTeri Both present moderate enlargement Group 5 LiTeri Hie livers appear somewhat lighter than usual In one there are large yellow areas Microscopic Pe tholo.rr. Group 1 Stomach* One rat has small inflammatory ulcers of the fore-stomach* another presents hemor rhagic erosions of toe pylorus. Liver* Two animals shov swelling oi liver cells with fatty degeneration of cells in the cent? part of the liver lobules Two animals prese central necrosis of liver cells with hyperpla of the endothelial cell! in these areas In of these animals numerous mitotic figures are found in liver cells. Group 2. rnnn^rrz I i MII l-r*o Liver! Ther^ is l .generalized swelling, of liver cells with some polychrontsia.- In one rat th is n fairly generalized vacuolar degeneration liver cells. The other presents vacuolar chn: in the central part of the lobules. 300035 WATER PCB-SD0000031130 4 Group 5 ~ !*! ?*: There is u dlffu**, *2d *f Liver etna with *o u&tiiii in atoH < *. utility. wc&B3lqntl liter etUi pre*ot cuoIat ch*afi la the cjtopLtm, Piiholoo' of aH of the udsdi i ml crni. teisaiaato The pathology resulting froa oral in^ettion of Inerteen ii fairly consistent and obviou.1. Large doses *tJ.ch nr* lethal In one or tvo day* cause a terainel passive congestion of riscere, extensive degeneration of the liter, v.itL necrosis about the central reins ana local ulcerations o: the gastric bucose. If sub-lethal coses are given and the a&ia&Is sacrificed it different tine intervals, the resulting pathology 1st Z days - gc.stric irritation, hepatic degeneration and active regeneration* 6 cays - mild degenerative changes in the liver vith foci of regenerated liver cells 11 days - indefinite liver pathology. ' In the group of animals gives repeated oral treatments, those that dies present gastric ulceration and hepatic degenera tion similar to those receiving & single lethal dose *wo ruts surviving 5 successive treatments shot similar changes but to & less severe degree. The croup of rats receiving c daily doses of Inerteea, the total of '.-hie'.-, amounted to lethal or sub-lethal level, presents aild to uod.erate degenerative changes in the liver. ('WVMfiS Other visceral pathology has not been included because it is considered to be coincidental in character It nay be nen- o a a '> p WATER PCB-SD0000031131 akin Savr. rets received about 0*5 ec. of Iaartaan dally to the ihirei akla of the bach* This was protactad by a flai rtn# md adhesive tap* to preTsat licking* tee animal diad aftnr 11 treatments, the reat were killed after 15 applica tion* Sl22JLL^J!AXl2L* ' Liven All of the liters are dark gray brown in color with mottling of the aurface* Bklm Hu gross chnngc is observed excent in the that died Here the area of application is oft and necrotic in appearance. This anLoud also presents pulmonary congestion# &iaaea^ie,,kihalogy The animal that died presentsi Livers Petty degeneration of liver cells with necrosis of those about the central veins Skins fiyperkeratlniration with blister formation and leucocytic infiltration There are die inflnsaatory chnuges i& the underlying connective tissue In the six animals killed there isi Liven Mild awelline of the liver cells in all of the animals with occasional vacuolar degeneration in some of the liver cells* cnnn&67 Skim There is hyperkeratiniration in 4 rats with oc casional blister formation* Bair follicles are increased in number in three and decreased in oat One anintl also presents peri-folliculitis. One of the animals has a hyperplasia of the epithelium rather than kyperkeratinlzotion. In 3 rata there is olid fibroblastic proliferation with some round - cell infiltration in the underlying connective tissue There is no question that skin application produces eone absorption o: the materiel. In one animal this was sufficient to produce death, Lince there is injury to the akin the degree of absorption nay r.ell depend on the amount of *Q-0-^ V WATER PCB-SD0000031132 !< Group 1, Two rats were girm maximum cunceatra tiaaj of vtpor* i of Inertemn (abwat 0*4 mg. per litar) with exposure twice daily for 0 minutes eh ihe a&Asalfl tsrt killed l days after 14 treatments* Group Two rats were given vapor* containing about 0.4 mg. per liter. This was given twloe dally for M tmw> ) Bents. One `died, the the- animal cat fcillsd* (i Group 5. Two rats received two daily exposure* for 0 aimites each of vapors containing about 0*4 mg. per liter. These animals were killed after 66 treatments* j Group 4. Ten rata received 8 hour erporures 5 day* a week of ' 1i vapor* containing an average of 0.057 and 0.061 age par liter. These an1 mils were killed after 20 treat ments* The animal that died 1b Group 2 presents b coincidental infection* In the rest of the enltails there trr tape rorn Infesta tions of the liver and two nts hive puluutiury Infections No pathology of importance is sera. Mlcr 3JLC Croup 1 lo striking pathology. One animal presents bronchitis* ' Croup In the animal that died the bone sirrow, liver <uji& spleen suggest coincidental infection* Group Z, The liver shows questionable swelling of cells Fat stains arc entirely negative for degenerative changes* Group 4. * Lungs Bronchitis or t ronchormeucoaib or both i re found in 4 animals* spleens Five rats present fairly oir^eu erythro- ph&giA . *. Font. Uerror* In those ar.lcc.ls that have pulaomr inf c-ct ions there is hyperplasia of-cells of the granular series*. COOOAfyft 300038 WATER PCB-SD0000031133 7 hile the incidence of 1m* infections la hirh in the ruts exposed to Inerteec by inhalation of vapors, it cannot be said that this Is directly due to Xart<m There la do definite liver dua| and no other pathology that i* of ny significance* finurr Oral administration of Inerteen may produce local gastrle ulceration tad hepatic degeneration particularly of the central' part of the lobule*. Generalised passive congestion is produced ki t terminal event la lethal cases* Follorlng single oral treatments there is evidence of hepatic regeneration in about k to 5 days milch becoses complete in about 10 days to k veeks. Bkin application results in injury to the Sidn ;md absorp tion of Inerteen, the anount of absorption presumably depending on the amount of cutaneous damage* . Inhalation of Inesteen produces no definite pathology of the viscera* Trl chlorobenzene Nine rati received daily oral treatments vith trichloro benzene, the individual dose varying fron 0*c6 to 0.59 cc. per kilogram body veight* Two rats died overnight after 1 treat ment; tro died 4 hoars after the 2nd'treatment;' one died over right after 2 treatments; one died 4 hours after Z treatments; rnooflRQ ' 300033 WATER PCB-SD0000031134 8 two died ovrrJ,ht After 2 tr&s tsesta; and oce ret vu mu^ 4 day* After 3 treatments* Qr^gg Patholorv. _ In ell enl *1s that died there is massif* congestion of the luaii end liter, Staa*cht In ill mlaili th* touch If ovsrdistended *ith food In four there if eoae blood present in the geit content* Liveri In Addition to passive congestion tv>o rats aho% an irregular yellow mottllag* hlcroscpplc Pathology. Liven 1 111 aections reveal necrosis of liver cells about the central veins of the lobules, the liver cells in the outer part shot-, vacuolcr degeneration. If decth occurred early hyperemia is also severe. When the animal died 5 or 4 days after the first treats eat, endothelial hyperplasia is seen in the areas of ne crotic liver cells One animal presents increase in number of mitotic figures in liver cells Staadchi In one animal there is hemorrhagic erosion of the cucosa* Ethyl-tetra-penta-chlorobenscnc ' Seven rats received dully doses from 062 to 0*94 cc per kilojraa body v. eight of ethyl-tutra-penta-chlorobenzene. One rut receiving the highest uost died after the Srd treatment. Six ruts aere killed 4 days after treatments* Oresi Pathology ' She animal that died reveals* Livers -jdcrate yellov, Bottling# e Stonuchi dilated vith food Lungss Congestion and hemorrhage. C000 /0 '- 300040 WATER PCB-SD0000031135  Ix rat* killad p?*sat qnae datable aalarg*ant of Kidney *&4 llTir. llxa&fla&fi-iifaalag> It the rat that died there l nild iihh; 0f liver eella with fine vacuolar degeneration. Generalised pmiTi congestion of iuag, epleea, boat marrow and other Tltoirt, In the anlaala that war* killed th*r ii . Liven Blight rwelliag of liver e*llt with occaeloaal acuolbr degeneration. The changes are extreaelj slid. ' fiaaasai The hepatic chaises following trlchlorobenxene are identical with those seen after Inert .an* thyl-t;tra-p antfachlorobenzene produced relatively little oarphologickl change in the seven tnlmtls examined. The one animal that died pre sents aainly generalized Tiscaral passive congestion Kith only slid degenerative changes In the liver# . EmssI Two rats ware exposed' to vapors from distillation of Pyr&nol Exposura ves given twice a day for 20 ninutea. Forty-one treatsants were given* Mo definite pathology la seen# ^Icr6se3^1e_,g&th3leg.y ' , :l )c4 / ' In one animal there .are increased nunbers of mitotic figures in the liver. The liver, however, presents no defi nite cellular chenge. 30004 WATER PCB-SD0000031136 10 ' Swa rti ir to u^tri of diatliiiw# fr*a- former OH This *sa {1td E0 minutes, tvice daily for 44 treatments* ' fliaii-Ellhalttir* lo definite pathology it een* Microscopic Pathology. ^ ' Lung I In one animal ttTaral of the bronchioles contain macrophages filled with eosin staining granules or small refractile droplets* No striking pathology is b*trr#d in either animal. o.L5cB 4* ?*"*> 300042 WATER PCB-SD0000031137 * February 14, 1950 Dr. Louis W. Spolyar, Director Division of Industrial Hygiene Indiana State Board of Health 1098 'feat Michigan Street Indianapolis 7# Indiana Dear Dr. Spolyar: I enclose an application bulletin on our Arodors. Cn page 19* there la a summary of almost all our toxicology Information on this compound. 0 If the case you refer to la in Brazil, Indiana, oar company has had some contact with the problem; This--p.arfclcular Installation used a temporary heat transfer system, and thus did not make tfie~Ihotairat"Xoh air tight. This la contrary to our expressed Instructions when Aroclor Is to be used at elevated temperatures. Upon hearing of the Illness, one of our development engineers went to the plant and gave his recommendations, and then I called the plant physician to try to obtain some Idea of what the Illnesses were. Aa far aa 1 could determine, two men suffered from gastrointestinal upset. I suspected . the possibility that the* Aroclor fumes might have caused liver damage, but was unable to obtain this Information over the phone. X was also unable to contact the employee's physician. The toxicology of Aroolors is somewhat confused. The experimental work was done by Dr. Drinker at Harvard about 12 years ago, and was done In connection with chlorinated naphthylene, chlorinated diphenyl, and chlorinated diphenyl high boiler. Both of .these last two are Aroclors. In the particular work at Harvard, Dr. Drinker found that Aroclor 1263, which means ihenyl chlorinated to 66, was of low toxicity. The confusion existed In his findings that Aroclor 1254, which Is the diphenyl chlorinated to only 54., was considerably more toxic on Inhalation. We did not supply him with this material, and I was never convinced that some error might not have been made In the sample. ., At any rate, ve have advised protection against all Aroclor fumes when an elevated temperature Is used. I will appreciate It If you will let me know the result of your investigation, if one ia to be made. Very truly yours RFKirg B CCi Mr. 'Paul Benlgnua . St.. Louis 900973 WATER_PCB-SD0000031138 V ".A . State or Iipsana o TAT* BOARD OF MKAL.TH February 28 # JJ80 Dr. R Eastt lallj . Mileal Dir*eter Monsanto Chemical Company St Louis 4, Missouri . Dear Dooter tallys ' Thank you very ueh for your-jmjqt^infonaatlTa lattar of Febru ary 14, relative to tha usa og^Iroclors)in industry lha plant under question la the Brasil plant mentionad in your lattar lha chief oeaplaints ware Irritation of the upper respiratory traot plus possible liver daat(a At tha time of our study Aroolor was oiroulatad in galvanized pipes and moat pipes ware leaking* It waa suggested that new plpaa be lnatallad and loeal exhaust amployad Plant rapipad with copper tubing and lnatallad a loeal axhaust ays tarn ovar oxtrudar rolls Witt this improvement very little Aroelop vapors ware osesping This probably will aolva thair pro- blosi. Further the plant ia considering building an onolosuro around the extruder and roils so that this equipment will ba both anoloaod and exhausted Thanks again for your help* Vory^truly yours. /miM ImfifAn/ Hal 8 ga VJ W. Spolyar, M B, Director Division of Industrial Hyglsna Indiana Stata Board of Health UO003211 MOCM MtALTM IS "TUt AW AMO SCttMCS um *a pcesovica p;jwot@*3 ams ueaJst see> cismct TMaouM oaAMSSo c--mwmot sraaav.** a. ((- l/ * r* 41 EXHIBIT NO.^L. tuz WATER PCB-SD0000031139 It. Louis December 12, 19(6 AROCLOR SWEDEN Mr. D. Wood BRUSSELS I 3?< -- atJLo^ r-* A. tepin - anossiLg 0 1 Buchanan - mwn D.V.N. Hardy - LONDON R. A. stmsnrod - isteb X do not believe that w can glibly accapt Aroclora m a synonym for polychlorinatad phanols that vara disouasad at tha meeting of solantlata at tha Wannar-tiren Cantra in Stockholm on November 27. Thara ara polyohlorinatad phanols which presumably could inaluds derlvltives from, or impurities in pantachlorophanol and, aspaolally, 2,4-D and 2,4,5-T. These compounds would ba such mors liable to appear in salmon, pike* and saa aaglaa than any derived from Aroclors. Thara ara many chlorinated polyphenyla that mn ba formed durinc tha manufacture of 2,4,5-T and probably pantachlorophanol, aa vail* Our only problem is whether or not va want to bring theee facts up and hams our harbieida program receive another black aye* This, X will have to leave to your judgment. I think the question hare is primarily an analytical problem* How oan ve find out what product Mr. Jensen is talking about? Can wa compare thasa chromatographic peaks that Mr. Jansen Is describing with anything found In Aroclors, pantachlorophanol, 2,4,3-T, ate? X adult I am out of my depth hare but 1 think another compound Is indicted rather than Aroclor. $ MEK/ln R. Emmet Kelly, M. D. NEV 023924 733979 WATER PCB-SD0000031140  * *. T ' X attack a egfpg5 # & lottor cocoivod fea QXa Ralsi 1a ffeoeldholm Z tew Mat oopiao of tMs Lttor aim to tko ^propriAtu dapartauti wltMa oor iasa orgaoiootloo* Xm ooosidoratioo of tko i*prtc tea osd piiieisf es, 4arvl0p*ifc _ t3i.a Iwidijli aorkot foclxedar ipoor ooot f1t yxs* w vold bo fxatofsl ye ao14 arxmag Ss Eklo imfaaofclao to bo eaooidorod by tko *pyropritJi dopartoo&ts f ft* bools s$i fckix OHBiMts tzoosaittod to os as o m ffmmiM.a ^ ^dMtham to tko gfdtle ^oMmm mamtianmA m Sls&ae&l' 2 aood otoriols* no nU tea iatemtad to loaxa low tMs prbhLoo 4 ImmMjsA tm lociift* Xm tko S.X. mb? aafuifla bonro bnNa Mrytaf . 0iStegiaX> la <asmiSc? Hittfjjd ia fetes 4m-- barlag boos. borb*4 late WATER PCB-SD0000031141 c c : v- r - w ^a m ^ ^ W TM ( RISING &. S X R A M Q OP/BO AKTI Q UAQ mXTQM 34 #1 1 39 44 43 mat 1434. 9#^. SVCAVAM 4f November 28 ,, Monsanto Zurooe muSSLS 3 Belgian Per the attention of Hr. D. WOOD Dear Davids yg; ABCCLOHS As mentioned, there has been sms publicity in Sweden concerning investigations made at the Institution cf Analytical Chemistry at the Stockholm University. These have revealed that a i^cup of products called iUpL--iA* Polychlorinated 31- Phenols f PCS fer short - accumulated- in certain orsanH"o? amaala. They-ays said to b* ; related to DOT and equally poisomous. ; The findings were discussed at a meeting of scientists at the Wermer-Gren Centre in Stockholm on November 22. Below please find a translation of an article in the ; Swedish daily paper "Dagens Nyheter" "It is found in saloon and in pike. It.is found in sea eagle living on fish. It Is found.' on the^sur- face of the needles of the fir treesi that isTSdi the air. It is found is the hair of -five norths baby... " ' *3 ! . * *..* . The scientists working with biocides have for colons time seen this something as unlacwn "peeks? on /their gas chromatographs and at a meeting-4t the Wtoair Gren Center, Research Assistant Sdrea `Jensen of the Institution for Analytical Chemistry at the Stock holm University could reveal the identity of these peeks. It has been found that they consist of a group of poisons. Polychlorinated BlofaaaaXs. (for snort PCS) which are closely reiaCrT7si equally poisonous as, DOT. FC3 is broken down considerably slower than DOT and gives rise to damagybf liver and sidn. PCS is not SIR 017391 WATER PCB-SD0000031142 rising a strap*. MESA, Brussels - Mr. D-. *( c. used as a herbicide. It 1S; not; manufactured in- Sweden but is supposed to- used by the industry' to quite some extent-. No special, industry 'can aa far be aecuaed._of.._bfting the aca^a^-o^-cscxanJ-aaCion.. ' Research, Asst. S. Jessea has tested 20Q fishes and. m rijaber of birds. He has takes, several samples cf air and has reached the conclusion that BC2 Ls equally eomm la Nature as chlorinated hydrocarbons; of the type of DDT, BCE, and Lindane. Even fish in Laddjaiaur* la Upland contain PCS. Hr. Jensen has. also found that ?C3 does not appear in animals living on a vegetarian diet, such as the elk. In the course of his work, Mr. Jensen has not found anything indicating-.that the source of contamina tion ccmes from agricultural additives. It Is, however, obvious already now that K3 is mcsc frequently found in organisms living in water or feeding frcm water animals. In all examined pikes PQ was found. Is a sea eagle found dead cucside Stockholm It was found that the liver contained. __ .10 jag of mercury cer_tCilo, 76 mg PET and consider" ablT more--PC3. Th exact figure has sot yet been ~determined. PC3 is found in water and in air, and not only in' the Swedish air, but also in e.g. LcacoG, air. Mr. Jeasea has. not yet been in London for sampling but could identify the poison by studying a ehrcmaca^sm of air published in a British techni cal ^otthaX. 1 Mr. Jensen bar also examined the fair of his family and himself red has found PCS on all samples. Most PC3 was found in. the hair of his wife but nose sensational was that the girl aged 5 months bad mere PCS a her hair than her brothers and sisters of 3 and 6 years. Probably the girl had got the poison via the mother" s milk. to the State Jftxaeua Mr. Jensen has examined the-, whole collection of sea eagles dating beck to lSSO. By testing it could be established taat ?C3 was present only is birds from 1944 and thereafter while birds collected before 1944 were quite free ft** PC3. The use of PC3 in Sweden is not established in detail. According to American sources these types of products axe used in the manufacture of a variety of heat- resistant materials. They are used for electrical insulation, for fire-proof heat transport in hydraulic oils, in lubricating oils used at high -3 "> iOD STR 017392 WATER PCB-SD0000031143 I s t P C 4 S T P A fM Q M ssels - Mr. "s { w' ;c temperature and pressure* in paint-s; and as; pig ments in various plastics. ?C3 is not- importedonly as such. It is also part of several" finishedproducts. Nothing is known as to the way in whichit reaches the water and the air. According to Mr. Jensen* products containing PCS should have this openly declared. PCS is equally harmful whether absorbed via. the skin, through the food, or by inhalation. In con tact with the skin it can cause dema. For DDTthe highest permissible concentration in the air has been set at 0.5 - 1 mg/cu.metre. For PC3 it has been mentioned to be 0.5 mg/cu.metre. Mr. Jensen will now try to get more complete analytical material. Ke hopes eventually to be able to disclose the source of the contamination and will also increase his cooperation with tcxccologists and genealogists." Another daily paper, Sveaska Dagbladet, has a similar article. Here it Is mentioned that Mr. Jensen* work ing under Lab orator (Professor) Gunnar Widmark, hasdisclosed facts which will have far-reaching- importance, since the findings have proved a new source of pollu tion of the nature. One of the participants at the meeting was Dr. A.V. Holden of Scotland, scientific contact man between the twelve G.Z.G.D. cambrics, who has established coordinated analysis of chemicals used and found in nature.I I suppose there is no doubt that what has been termed Polychlorinated Biphenyls is equal to Aroclor. There la also no doubt that the published facts will cause considerable unrest In several quarters. We probably will have to have Aroclor registered with the Swedish Board of Poisonous Substances and the industry will have to be particularly careful in handling the'material. The problem in seme eases of course may be the disposal of used material. I understand that there hardly exists a convenient method of destroying Aroclor and that possibly burying umaeable material my be the only answer. We shall be glad to hear from you soon. Yours sincerely. nsNQi STRAMD .1 O i SIR 017393 WATER PCB-SD0000031144 I *4 I I 10 7' ,, 12th January, 1967 Aroolor - Sweden mm/m PG Benignus, St. Louie G.R. Buchanan, St. Louis BS Cameron, Brussels Br. R fimet Kelly, St. Loula GR. Graham, New York R.A. Steenrod, St Loula . B. Wood, Brussels J.A. Evans, London R0A0 Baxter, Ruabon 'JAN : 6 1967- On 2nd January 19^7 Hr A Richardson of Shell Chemicals1 IHmstall Laboratory, Sittingbourae, Kent talked with me over the telephone concerning the Swedish Press report relating to the identification of "Polyclilorlnated Biphenols" as trace contaminant in sea birds, fish etc. Richardson has been working for some years on the similar problem with insecticides such as BBT, which are known to have wide distribution in trace quantities He had already found that the chlorine-oontaining residue contained substances more stable than BBT and Just as StJren Jensen reports he has obtained spectrographic evidence that these are very similar if not identical with Aroclors* He has obtained samples of Aroolors 1242, 1254s 1262 and 54&> from us,' and would now like to have small samples of any chemically pure Aroolor constituents which we may be able to supply Milligram quantities would suffice for his purpobe Mr Richardson was quite sure that the compounds reported to be "polychlorinated biphenols" are really meant to be polychlorinated biphenyls and as support he has sent me a copy of the synopsis of a paper entitled "Pesticide Analysis1 Presence of Polychlorinated Biphenyls at Residue Anal/Cyeis of Biological Samples" by SBren Jensen and Gunner Widmark (photocopy attached)* . 1 discussed with Richardson the soundness of Jenserfs claims, and was assured that Ms work and findings are sound Jensen ie on the staff of the. Institute of Analytical Chemistry, University of Stockholm A note on the staff and work of the Institute is attached. Prom this you will aee that Jensen is wholly conoeroed with the analysis of chlorinated pesticides and with the work of stations for routine analysisI I would be glad if Br Baxter and to Buchanan would arrange to send me milligram samples of any pure Aroolor constituents that may be available at Ruabon and St Juis respectively. WATER PCB-SD0000031145 We recently sent you a translation of a Swedish newspaper article referring to the identification in nature of polychlorinated biphenols. Because some of the uses claimed for the materials fell in line with the uses of our own chlorinated diphenyls, we made a point, during our recent visit,to Sweden, of visiting the research institute involved and discussing their particular programme of work. To e 1 im in at e_ any earlier confusaon that there may have been, I~^hourg~TIki~^o~empHasTse that there -is no j3oub't~tKa""the eHe^TTcaT~which~Ts~Th~ubject~~of~the~ investigation and~the newsrelease, is chXorxnaWct dl~pHSnvrT7iT~Aroclor. '1 The company that supplied the mass spectrometer which was used in the research programme, in fact have recently put out a press release on this work. Although I am horrified by some of the headlines in t^iis press release, it does basically describe the' research programme carried out in Sweden, and describes in clear terms how chlorinated diphenyls were identified. I therefore, enclose a copy for your files. ' Jensens only aim in life as an analytical chemist, was to identify the substances found in his research work on the occurrence of insecticides in nature. The unfortunate'aspect of the situation is the comments which have been added to Jensens work. He showed what was present and unqualified people have made f 1 statements as to the possible effect of what he has found. Summarising the publication position, there were original articles covering the Stockholm conference in the Swedish daily press, and these reports were picked up also by the Danish press. You will have seen from D.V.N. Hardy's memo of the 12th January that it has also been picked up by the Shell Chemicals Laboratory `in Kent, U.K. Jensen also divulged that he had been contacted by the Swedish American press agency who intended to include information about this research work in their monthly review "The Swedish American Journal". There is additionally the press review issued by LKB Productor AB which 1 imagine to have been sent to a numbetechnical journals. M-3. h NEV 022156 ./. .. 732211 WATER PCB-SD0000031146 G. H. Buchanan St, Louis 2 26th January, 1967 Effect in Sweden . , ' This matter was raised with us by every capacitor manufacturer in Sweden that we visited. Fortunately there has not been , 'too much adverse comment as yet from plant workers since : they have not associated the polychlorinated biphenols mentioned ; in the article with Aroclor or Pyralene used in the Swedish \ factories. Jensen, however, stated that he had bee_n.approached personally by^everaT~woB^^LAsj5.ociate.d_,.with~'c'hlorinated diphenyls for non-electrical uses and these workers were quite .v)orratr^s to the possible eFfei:tr^n--th`erf~Hialth.. ^Future Research . ` \ Arrangements are being made in Sweden -for this work to be taken over by one of the medical institutes who hope to study the toxicology of the poloychlorinated diphenyl residues at the levels of Concentration found by Jensen. Additionally ' a geographical survey is to be carried out to try and determine where the highest concentrations of residue are appearing and, if possible, to detect from this the method of escape so that more security precautions can be taken. We were asked by Jensen if it was possible for Monsanto to supply any samples of the pure isomers of chlorinated diphenyl since his work indicated at the moment that the lower chlorinated isomers are fairly easily metabolised, and the potentially more dangerous constituents are the more highly chlorinated members. If he can get hold of pure isomers, he would like to carry out some work on comparitive rates of metabolisation. Jensen is forwarding me copies of his mass spectrographs and '' details of sample preparation so that we have all the details : of his research work. The point that 1 have made to Jensen is the need for`care in any further publication of his work which is made. He accepts : that the toxicology of chlorinated diphenyls should only be ` discussed with detailed information about exposure concentrations T and exposure times and that generalised statements out of context can only arouse undue public, concern. If any technical 'journal takes up the press release from the LKB Productor Company, there is little that Monsanto could, or should do. in the way of publishing rebuttals. We do not want, personally as Monsanto ' to get too involved in this question. I am hopeful that we NEV 022157 -7009'! 9 WATER PCB-SD0000031147 Go R Buchanan St, Louis -3- 26th January, 1967 . might persuade Jensen himself to write a letter defining the true extent of his own research work and placing his results in their proper perspective. It would certainly be helpful in gaining his further support if we were able to make available to him any small quantities of pure isomers. Since we are not alone in supplying polychlorinated diphenyls to the Scandinavian market, I have drawn this matter to the attention of the other askarel manufacturers in Europe. As you will see from the press release one of the major " points that is made is the difficulty in 'disposing of waste chlorinated diphenyls and again I must mention that constructive recommendations of the safe disposal of our materials would be most helpful :.i `.V : N6V 022158 ' 732213 WATER_PCB-SD0000031148 Gene V/Ufie - General Office# February 13$ 1967 LTH* PUBLlClTJf CM cac^niiirVffa) buwwls R, Eaaot Kelly, M, E. It, M. ftu*a V, F, Voychcf? 0. tt, Suclkcum ^J7(i Research - R. E. Keller !i.-re i & brief imuy of nbai we diBcuOTed durlnfi sw nodlng February 0 in your office# i/c reviewed the iufontim we tmm reotttwd ao ftur m Mm oaverse publicity to Europe ca j^ychlorimtcd blpiheuylft* For tiw rocordj wc taw received tbo following publiobed isformtioa* letter frets Danner HMasrk of the laetitute of Analytical Chemistry* University of fitockboXn^ toted toaster 29 about hie Mr, Jensen fefiaiag tone of , toe unknown in Mi aualyticDl volt ee polychlorimtett biphenyls, Attached to tola letter woe a report od the . presence bf polyckloilimted hipheryls at msMm . analysis of biological. ans^lea wittea bp Mr, Jpamm wa& Dunnar Vitexk tewe Wood of cur Srueaels office seat us Mm USB pevee release of January S% 1967, about the Swedish eueceee itt detecting the ^y^ortetofl biphenyl. A Mcao written by Save Hood dated Jtomty 26 sunoailKliiB 111* Tiftit with S Jto*y 3P* l^T# iesue of chealcl BociiwrerliiK. jsttG 52. taste* cement about Wpheoyls to ftmdoa* Shle wm the first pihUthttA ' fiPn*^wn^n"=8rMwaswdt.vbolwmp Iihipnit. Ofhw* tL L" , ' 8soooft*r 1% 1566* the Swr Belog&lwt rtmsipe* cwtoi en *rfelcl about a nowr the wort that h4 been 4oo bp the Ootwraity of SbA jri^ .- _ ' KswttfetiiJJy, sU/ef town# report# wa4 the mm Mmm Sue to the ^wtame# of the Aewtar pwAicrt# to the Qrguil* ' Division, we tootoa oa the fblloMltm #* of action, Stacw ell f the notion njtai4 Adis wttola the ef pour sutboeltar* you accepted to# swgpcntib&llty to folic* |hww# on the folXMiaet NEW 024083 734138 WATER PCB-SD0000031149 a 1. Prepare a etatemani or letter for woo by Maz^ettos with custeoors uho ia^ulre about this publicity* 2 You viH talk to ten Porrestol on prcjxiring a jresw> rdoarc aa-fi )>olU it until such a tix that we foe! as though it Should be releoood. 3* Olva wm thought to kw i*e would OEprooth this prohlea on & ioxioo&oeleal and plan^ologleel t* Stalk to to BCE '$eqflja after ve define to perom "to - 5 Armafft tor contact with Bayer nfi troMm 2Vo g,uestloos tot toopt coatac tack to our n$Me during to uMting ` wro that la all of the pQfp3&oAii thcr* haa W nothing abewt to levels tot toi teen fowafi particularly la 'to atr and no cue he# 4#tn4 k^|btoa about stmt level wmM be cwtaF*A karmftiL,, Ballaar brought out the Uict' tot tow wust have ' teen other products found to to* olle analysis and be tfouM be totereata !ta knowing what otor things wara Jtauwl* . All of tbaee actions wd tewfilate attention with the eeejiiiaf of courts, of to ^fchertog of to tosleoloQ^cttl ai tdmtsuMlogical H#&#t to let ka tea if tore is tu^iMug 1 mn. to or ouaor way 1 eaa help to ffstMag, tMm mMma *ua ttiiog ewe infonaetlca ioestiwr oo that ve coa sake aura our feodor bucinooo Is not affected by this evil publicity. .. . gim .. ; ' :V NEV 024084 \ / `'. ' ' ` , 734139 WATER PCB-SD0000031150 ho.-" Monsanto Chemical Company At St. Louis, Mo. Dit 12, 1956 ' Kr. H.X. Nason-M.0. Hr. R.E. Soden-Nltr . L.C. Weger-Nltr M-- V To Dr. R. Emmr.t Kelly * - , Vo * Cc-- Dept Reference j C_CH LORA N~ CAS! SubRd DUB TC 7?: Persons; Present : Dr. H. Oettel Dr. K. T. Hofmann A . Palm (Ph.D.) W. Seen ksen (Plant Supt., parrt-tine) On the 17th or November, 1933, Bacische was producing a batch of 1 trich'lorphenol from tetrachiorbenzene when the process exceeded centre pressure and temperatures similar to our incident at Nltro, No one Va injured at the time. Vithin one week, as clean-up was being carried out, the first cases of chicracnc developed. Fifteen or sixteen cases (6 serious) developed within the next 1-2 months and additional cases showed up during the next 10*12 months until there was a total of 50-60 cases. I did not see our most severe Nitro cases nor have I seen photographs of these cases. The photographs of the worst Badische cases show _ horrible skin eruptions with nearly blister-like welts and seme ulcere lien where infection ensued. Areas Involved included the face, neck, arms, ?r.d upper half of the body. It is my Impression that their 1 severe* cases were much worse than ours. In idlticn to the skin mani festations, their men reported all the addition--- symptoms as exper iences In our workers, i.e, fatigue, vertigo, loss of libido, painful Joints, etc. About ten days following the Incident, and after initial clean-up. Dr. Oettel was asked to expose animals to' the workroom atmosphere. Rat bits (in oj>en wire cages) were placed in the operating area for 2^-U8 hours. There were no obvious symptoms, which developed in the animals | until one week after exposure - when they died. Autopsy showed liver necrosis. Cettel thought there might be virus infection or some othei: cause for death until he exposed additional animals in the department,' others in cages suspended inside the "decontaminated" autoclave, end some in the adjacent department. All died within 1-2 weeks following exposure. Subsequently, animals placed in the cages which had pre viously been in the department died of liver necrosis. A thorough systematic investigation lias isolated impurities in the tr'chlorphenol process (or residues) which will cause zne same effects In rabbits. Liver necrosis will develop in rabbits at the following doses of the indicated materials: 15-20 mg. of pent&chior naphthalene 1 ms- of chlorinated diphenyl oxide 0.1 mg. of residue from trichlorphenol disti.iation 0.01 mg. of residue fraction from trichlorphenol (above 230C) .\" ; Cl 5579 % WATER PCB-SD0000031151 Dr. Oetiel believes that the nest potent chxoracnogen Is a comoour.d 3onewhat similar to chlorinated diphenyl oxide, ' a c I y with d G d 11 j na. .^6o L>OU ;1 --- at "cio in ir.e mole cuiss. He ha a : r- i- 'r.v. f 'ne:' reached the came cc: 1 . 1 e ential of chi :rinated t: , Oettsl beliw-a, fur i;.-:-.', lor-. any cr.-orl.-.ated :/r. > c rracne which has been cue .orpne; cr. .ateo oluhc.-.v. Dr. Cestel has nc fait:, cr. ir.v animal skin tests for isolating chi ora cr. c-gens. He was very Interested in Kettering's work er.d was not awa of the publication referred to in Dr. Suski.nd's first report ar.d L l > * ch describes the cyclic skin development in new-bern rats. (Refer enc e: Parnell, J.P.: Postnatal Development and Functional Kistolcgy of the Sebaceous Glands in the Rat, Am. J. Anat., 8pAl, 19^9). He i con vinced that the Bronsulphaiein test reported in the attached repri Is significant. In this regard, Badische routinely uses this test on each batch of trlchlorphenol which they now purchase from Bayer, a, nrd refuses to accept materia 1 which fails to pass the animal testa, also learned at Bayer that- they have experienced chi oracne during production of trlchlorphenol but have now licked the probier." CC ending to Dr. Manser, (chemist - Research Director At Zlberfeld)'; Badische has been able to reproduce in the laboratory the conditions which lead to the incident such as theirs and ours at Nitro and v&3 quite surprised that we had not been able to do so. I was not given the Nitro process information, i.e., temperatures and pressures, but if I had had this information I am sure that I conic h2*ve obtained Badische's. One of their chemists, a Dr. Palm, sat in ch our dis cussions and was prepared to go into details. Ke did mention that "with 3 mo Is of trlchlorphenol, methyl alcohol, and alkali, ar.d a ten perature of 180C" the process gets out of control. His remarks are in quotes because he does not speak English and I'm not certain of his remarks. . Dr. Oettel would be very happy to receive samples of ar.y of cur materials for Investigation. He would like particularly: i (1) Samples of any of the materials involved in our 19^9 incident including tetrachlorbentene, trlchlorphenol, or N& salt and any residues from the autoclave or material cleaned from the equipment and structural members. (2) Trlchlorphenol (or Na salt) from regular production. (3) Any samples from raw materials,- intermediates, and final product 'which may have been involved in our cases which developed during our normal 2,^5-T production in the years following the initial incident. CONFIDENTIAL P.1 ^KQl\ WATER PCB-SD0000031152 He would ce happy to exchange freely any and all information with us and Kettering. It was ny suggestion that thl: be direct with Dr. Duskind tc eliminate "third parties.' He w :A routinely send ; and we could request Dr. Su ski n.d C-- likewise. r .hat this night save u .n-u-ss ary 6.i?' i cat Mr. of eff; ;lu.-.bl*' lr f'mat li ana -c expense, > . Ir. J*, VS * . s.cci t. i or. t r.vestiger 1 ,\c r on ^^i'i r i n.vc: 1 m.Jgh t cbta ..-.g h U,Ti 3-T. v;.`. unVers . 2 left with Dr. Oe' cooies of the following: {':) The five (5) reports from tr.e Industrial Hygiene Foundation v.hich discuss their rahoit ear tests. (2) ne^v^er^ng s udc: NJtro, 1953 'Clinical and Environmental Survey at (3) Kettering's report - "Environmental Survey Carried Out In' Building 30, Monsanto Chemical Company at Nitro, February 2, 10$6." Wc reviewed thoroughly Mr. Weger's excellent "History ci'^Chlorac.ne" which he sent to me with covering me no dated May'up, iS5d, and which Included descriptions of Kettering's reports on their human and animal research. I did not give Dr. Cettel a copy of thl3 account becaus., I did not have permission to do so. As a result of my visit, it may be desirable tc edit this report somewhat and add further ' process information before forvjarding this to Badische. Ar.vv Srpe reccnr.enda.tl are implied in the above narrative accouJ of my visit to 3adisehe and must be based on an agreement beat full ar.d complete exchange of information with Badische is desirable and ocssible. EPW;dh Attachment Elmer P. Vfneeler 0>*** X * . ^' \. fS, ' * *v pi WATER PCB-SD0000031153 This document has been retyped for clarity. From Monsanto Chemical Company Ate St. Louis, Mo. Mr. H.K. Nason-M.O. Mr. R.E. Soden-Nitro Mr. L.C. Weger-Nitro Date June 12, 1956 To Dr. R. Emmet Kelly At Medical Dept. Reference subject CHLORACNE CASES AT BADISCHEN ANILIN DUE TO TRICHLORPHENOL Person Present: Dr. H. Oettel Dr. H. T. Hofmann A. Palm (Ph.D.) W. Soenksen (Plant Supt., part-time) . On the 17th of November, 1953, Badische was producing a batch of trichlorphenol from tetrachlorbenzene when the process exceeded control pressure and temperatures similar to our incident at Nitro. No one was injured at the time. Within one week, as clean-up was being carried out, the first cases of chloracne developed. Fifteen or sixteen cases (6 serious) developed within the next 1-2 months and additional cases showed up during the next 10-12 months until there was a total of ' 50-60 cases. I did not see our most severe Nitro cases nor have I seen photographs of these cases. The photographs of the worst Badische cases show horrible skin eruptions with nearly blister-1 i.ke welts and some ulcera( tion where infection ensued. Areas involve included the face, neck, arms, and upper half of the body. It is my impression that their severe cases were much worse than ours. In addition to the skin mani festations, their men reported all the additional symptoms as exper iences in our workers, i.e., fatigue, vertigo, loss of libido, painful joints, etc. About ten days following the incident, and after initial clean-up, Dr. Oettel was asked to expose animals to the workroom atmosphere. Rab bits (in open wire cages) were placed in the operating area for 24-48 hours. There were no obvious symptoms which developed in the animals until one week after exposure - when they died. Autopsy showed liver necrosis. Oettel thought there might be virus infection or some other cause for-death until he exposed additional animals in the department, others in cages suspended inside the "decontaminated" autoclave, and some in the adjacent department. All died within 1-2 weeks following .exposure. Subsequently, animals placed in the cages which had pre viously been in the department died of liver necrosis. . A thorough systematic investigation has isolated impurities in the trichlorphenol process (or residues) which will cause the same effects in rabbits. Liver necrosis will develop in rabbits at the following doses of the indicated materials: 15-20 mg. of pentachlor naphthalene 1 mg. of chlorinated diphenyl oxide 0.2 mg. of residue from trichlorphenol distillation 0.01 mg. of residue fraction from trichlorphenol (above 230C) This document has been retvned for -?*#-.# WATER PCB-SD0000031154 This document has been retyped for clarity. Dr. Oettel believes that the most potent chloracnogen is a compound somewhat similar to c! 1orinated diphenyl oxide, ---------- . y-----------v but, Cl Cl 0 probably with additional oxygen atoms in the molecules. He has cor responded with Don Irish at Dow who either reached the same conclusion independently or, in mentioning the potential of chlorinateddipheny1 oxide, influenced Oettel's reasoning. Oettel believes, further, that this impurity can show up in the production of any chlorinated phenol allegedly to chlornapthalenes, pentachlorphenol, chlorinated biphenyl, etc. Dr. Oettel has no faith in any animal skin tests for isolating chloracnogens. He was very interested in Kettering's work and was not aware of the publication referred to in Dr. Suskind's first report and which describes the cyclic skin development in new-born rats. (Refer ences Parnell, J.P.s Postnatal Development and Functional Histology of the Sebaceous Glands in the Rat, Am. J. Anat., 85:41, 1949). He is convinced that the Bromsulphalein test reported in the attached reprint is significant. In this regard, Badische routinely uses this test on each batch of trichlorphenol which they now purchase from Bayer, and refuses to accept material which fails to pass the animal tests, (I also learned at Bayer that they have experienced chloracne during the production of trichlorphenol but "have now licked the problem" according to Dr. Hansen (chemist - Research Director At Elberfeld). Badische has been able to reproduce in the laboratory the conditions which lead to the incident such as theirs and ours at Nitro and was quite surprised that we had not been able to do so. I was not given the Nitro process information, i.e., temperatures and pressures, but if I had had this information I am sure that I could have obtained Badische' s. One of their chemists, a Dr. Palm, sat in on our dis cussions and was prepared to go into details. He did mention that "with 3 mols of trichlorphenol, methyl alcohol, and alkali, and a tem perature of 180C" the process gets out of control. His remarks are in quotes because he does not speak English and I'm not certain of his remarks. Dr. Oettel would be very happy to receive samples of any of our materials-for investigation. He would like particularly:1 2 3 (1) Samples of any of the materials involved in our 1949 incident including tetrachlorbenzene, trichlorphenol, or Na salt and any residues from the autoclave or material cleaned from the equipment and structural members. (2) Trichlorphenol (or Na salt) from regular production. (3) Any samples from raw materials, intermediates, and final product which may have been involved in our cases which developed during our normal 2, 4, 5-T production in the years following the initial incident. This document has been retyped for clarity. WATER PCB-SD0000031155 This document has been retyped for clarity. He would be happy to exchange freely any and all n format ion with us and Kettering. It was my suggestion that this be direct with Dr. Suskind to eliminate "third parties." He would routinely send carbons of any correspondence to us and we could request Dr. Suskind to do likewise. It is my opinion that this might save unnecessary duplication of effort and expense. In addition, Kettering might obtain valuable information to further their investigation involving human volunteers. I left with Dr. Oettel copies of the following: (1) The five (5) reports from the Industrial Hygiene Foundation which discuss their rabbit ear tests. (2) Kettering's report - "Clinical and Environmental Survey at Nitro, 1953." (3) Kettering's report - "Environmental Survey Carried Out In Building 30, Monsanto Chemical Company at Nitro, February 2, 1956. " We reviewed thoroughly Mr. Weger's excellent "History of Chloracne" which he sent to me with covering memo dated May 15, 1956, and which included descriptions of Kettering's reports on their human and animal research. I did not give Dr. Oettel a copy of this account because I did not have permission to do so. As a result of my visit, it may be desirable to edj t this report somewhat and add further process information before forwarding this to Badische. Any specific recommendations are implied in the above narrative account of my visit to Badische and must be based on an agreement that full and complete exchange of information with Badische is desirable and possible. EPWsdh Attachment EPW Elmer P. Wheeler This document has been retvoed for olarltv WATER PCB-SD0000031156