Document 2jZMaaqMwOgzg7EpBoGaYVpXr

THE PROPER HANDLING OF AROCLORS AND THEIR MIXTURES IN THE ' ELECTRICAL INDUSTRY Monsanto Monsanto Chomical Co. Organic Div. Solos Dopt. 800 N. Twolfth Blvd. St. Louis, Mo. P. 6. 8SNIGNUS MAY 1, 1956 WATER PCB-00049851 906652 2MDB Introduction Chapter 1 Chapter 2 Chapter 3 Chapter 4 Chapter 3 Chapter 6 Chapter 7 Chapter 3 Chapter 9 The Proper Handling of the Aroelors and Their Mixtures in the Sitetrleal Industry. Procedure for Unloading Tankcara of Aroelors and Their Mixtures. A. Description of the Cars. 8. Proetdure for unloading the Cara. C. tt>um Ptctaging Storage Tanka A. Oeneral Description of Storage Tanks. B. Detailed Description of Storage T-nks. Gasketing and Pump Packing. Stapling. Laboratory Analysis and Procedure for Treating Aroelors and Their Mixtures. Test Procedures. Typical Properties. Barth Treatment of Aroelors and Their Mixtures In the Electrical Industry Prior to Use. Dermatology and Toxicology. Attachmentss Drawing Mo. 31-20848# Dome Detail. Drawing No. 31-208*7# The Tank Car. Drawing No. 90-8170-5, The Horlsontal Storage Tank. Drawing No. D-13362# The Vertical Storage Tank* Drawing No. 90-8248, The Breather. Drawing No. 90-8278# The ?art 6aug. Drawing No. 90-8178# The Unloading Platform. GiRN 0002 94 906653 WATER PCB-00049852 - m worn mmlim op moclors and Tmnt stores IN THE 1MCM1CAL BOUSB1Y INTRODUCTION Monsanto's Aroclora*, especially the ohlorlnated biphenyls including types 1242# 1248# 1254 and 1260# used alone or In combination with chlorinated bensenes# are connonly used dieleotrlo materials of the Askarel* olass. Askarel Is a generlo name referring to liquid dielectrics derividkfrefc laiegemted aromatie hydrocarbons possessing excellent chemical and dleleotrle stability and fire-resistanoe over the temperature ranges and operating conditions required of transformers and capacitors in the eleotrical Industry. The properties of Aroelor 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 electrloar industry's use of these fluids has been largely In accordance with the General Electric Company's patents and developments. Aroclors - Monsanto's chlorinated biphenylt and ohlorlnated polyphenyls# Registered U.S. Patent Offloe. Ip. M. Clark# "Slectrloal Insulation"# Che, teg. News 2j>. 2977 (1947). ------ 1 GBRN 000295 906654 WATER PCB-00049853 Resulting from the wide use of those ntterimls in the Industry, trade names have been established to Identify them by different aanufaoturers of eleetrloal equipment. Listed alphabetloally the trade names Include, "Chlorextol," Allis CtaXauwaj "Dlaclor," Sangamo H@etri@f Djtonol,19 Cornell Dubilierj "Elemex," Line Materials; "Hyrol," Aerovozj "Inerteen," Meetinghouse neotrie; tfa^er Eleetrlej and `'Py- ranol," General Bleetrlo Company, The purpose of this bulletin la to assist the Industry ~ proper and safe handling of these dleleotrlo materials In their operations. QBRN 000296 906655 WATER PCB-00049854 6HAMSS 1 FROCH50RE FOI TOttOADINO TACMS Of AROCLORS AND AROCLOR MIXTORES A. Description of the tei Aroelor tad mixtures of Aroclors with chlorinated bensenes are shipped by Monsanto in two types of insulated tankcars both of whloh are either aluminum lined or sinc-tim metallized. On* typ* of oar has heating oolls inside of the tank and these are in dlreot contact with the product. The other* a more widely used type of ear* is a double-shell tank with heating eolls between the inner and outer shells. The ateam ooll connections are at the bottom of the ear. Both types of tankcars are tested for 60 pounds presses md their sterna ceils are tested for 00 pounds gauge pressure. The cars are top-unloaded by displacement with dry air containing 10 ng. IgO/eu. ft. maximum. There are two or three connections on the tankear dome depending on the type of ear. Where three connections exist# one is a two ineh dfameter unloading line which extends to the bottom of the ear* the seoond is a one ineh diameter air inlet oonneotion and the third is a two inch diameter pressure safety rent* whloh la a thin lead disc adjusted to release any pressure in esoess of 60 pounds png. This safety rent is hooded for proteotion against dust* dirt or aooidental bumping. Where only two connections exist on the dome* one is the two inch diameter unloading line and the other is the safety 3. GBRN 00029? 906656 WATER PCB-00049855 vamt. to these ears, it is MOMMaer to mmw the safety vent and introduce the displacement air through that connection. Drawing Mb, 31-20848 shows la detail the dome of a tankear with three connections, "A" is the two inch raloading line which extend* to a swell sump at the bottom of the oar. "B" Is the one inch air inlet connection, "C" ie the hooded safety vent. The ear dome cover with fitted bolti ia shown in the oenter, Zt ie fitted with e Qerlook 901 aabeetoe gasket or an ^Aluminum envelope Ooetce gasket. This drawing also shows a bottom opening in the ear. This @an be cpened only from the _ inside of the ear and its purpose is for oleaning operations, Zt has no use at all in unloading the oar. Drawing Ho, 31-2#847 shows the oversell dimensions of the 8,000gallon Aroclor tankear. B. Froeedure for Unloading the Cars The ear should be spotted at an wmlending dock similar to the one shown by Drawing Ho. 90-8178. The oar must be level and the brakei set properIf, "ITOF-Tankear Connected" signs should be placed fore and aft the oar to warn switching crews. Zf it is Mining or snowing or the humidity is extremely high, it is not advisable to open the oar. Zn ease the oar must be sampled and opened during bad weather, a canvas oanopy must be placed over the dome of the ear. Zt is preferable to unload the oars wider roof or inside the factory, Obless it is absolutely necessary because of following described situations 4 G6RN 000298 906657 WATER PCB-00049856 the done oovtr should not be opened until ready for sampling, me done oover is sealed with a standard railroad wire and seal, and Monsanto should be notified If this seal is foundbbroken upon receipt of the oar. The first step in unloading la to inspect the dose and clean around the dome oover to remove all loose dirt, water or now. Wiping rag* 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 in serted through this air-inlet valve opening and the temperature of the interior of the oar determined. If the car temperature la 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 coil through the dome of the car to preclude rupturing the tankcar seams during the heating period. Product mm Pour Point 5C. Temperatvape06. Below whioh Caution Must Be Peed in Heating_ Area lor 12o 30 40 Aroelor 1254 10 20 Aroclor 1248 7 5 Ar-ocler 1242 Pyranol 1467 19 10 Pre-heating is not required41 Pyranol 1470 Pyranol 1481 Pre-heating is not required9 Pre-heating is sot required9 Exeept if the terial has cooled bettow -1O60. and crystals of scavenger have separated. Then, the material should be heated to 70C. (158P.) until complete solu tion has bean accomplish^. ' GBRN 000299 906658 WATER PCB-00049857 If the dome of the car la to be ppened fop the pre-heating operation, it la necessary that it be covered with a clean canvas. Extreme care must be taken to avoid getting dirt or moisture into the oar. It la due to the relatively high viscosity of aone of the Aroclora at low temperaturea that It becomes necessary to form a column of molten material from top to bottom of the car. In the center, to prevent hydraullo pressure build-up whloh may rupture the tank shell If there Is too rapid localised heating when employing the main steam colls. - When such pre-heating Is required, a satisfactory vent hole oan be made by Inserting a "hair-pin" eoll (1/f inch diameter brass, galvanized, or stainless steel pipe) Into the open dome of the oar and introducing steam through the eeil until there Is a column of fluid Aroolor from top to bottom. After the vent hole is melted through the material to the bottom of the oar, the "hair-pin" coll should be removed and the dome cover replaeed and bolted. Steam is then introduced Into the main colls. It Is recoMended' that the steam pressure be limited to 100 pounds gauge pressure, particularly in the case where the colls ire in direct contact with the Aroolor. Ihe steam coil outlet should be trapped or throttled with a valve. It will require eight to twenty hm to bring the material to pumping temperatwe - depending upon weather 6 GBRN 000300 906659 WATER PCB-00049858 conditions. It It essential that the air lalat Taira ba opea during the heating parled la order to raat the taak. Some ealeulatloas have baaa aada to ladloate tha heat requirements for aa Aroelor ear. Data for an 8,000 gallon ear of Aroelor 125* are: Spaelfle gravity Spaeifle Kaat * 1.5 - 0.26 BTUAb./*F Heat requirement for heating Aroelor from 30*0. (86*P.) to 110*0. (230*FO iu ' 8000 z 1.5 x 8.33 x 0.26 x (230-86) - 3*77*,OOO BTU. For heating froa 30*0. (86*P.) to oalf 75*C. (167*P.)* the heat required is 2,110,000 BTU. A nine horse power boiler operating at 80 palg produces 263 lbs./hr. of steaa with ao reused eondaasate. Returning oondensate at 200*F. will laeraasa tha steaa output to 296 lbs./ hr. at 80 pslg. Ia tha first ease, heatlag to 110*0., tha orar-all heat transfer eo-effleleat is assumed to ba too low to utilize tha lOOjf capacity of tha hollar. A value of 1500 for UA with an araraga ^ T of 1***F. ladieatas that tha useable steaa is 202,000 BTU/hr. or 226 lhs./hr. steam at 80 pslg. Za tha saeoad ease tha ^ S is lower aad tha entire output of tha boiler is useable. Table II suas up tha approximate tlaa calculated to heat Aroelor 115* 7 906660 WATER PCB-00049859 TAILS II Mint IP Boiler Lb>. gfam/te. 30-110*C. 30-75*C. 1000 eap.(mo reused condensate) 263 9 Brs. 750 eap.(no reused condensate) ~ 18 brs.(860eap) If Its. 1000 eap.(condensate 200*F.) 296 ... 8 Hrs. 750 eap.(eondensate 200*F.) ~ 18 brs.(760eap) 11 Hrs. Calculations on a five bora# power boiler give heating times of tbe following orders Fire HP Boiler Lbs.Steam/frr. 30-110*0. 30-75*0. 1000 eap.(no reused condensate) 146 28 bra. 16 hre. 1000 eap.(condensate 200*?.) 164 25 bra. 14 bra. Aroelor ears ean be beated bjr steam (80-100 palg) to tbe proper handling temperatures la a reasonable time by using a boiler souree eapable of produelag fOO^OOO to 300,000 STUAr. Tbe times given here are approximate and fill aet as a guide until experience sbous the exaet time for this operation. (CRN 0Q03C2 8 906661 WATER PCB-00049860 The proper handling temperature for the various fluids la given in the following Table III, which indicate* cor responding viscosity valuesi TABIZ III Produet Bailing and Piping Tsnperitwe C Approxima Viscosity, ! Aroelor 1260 95-130 100 - 43 Arcelor 1254 75 - 110 100 - 42 Aroelor 1246 50 - 85 100-40 Aroelor 1242 ` 35 - 75 100-40 Pyranol 1481 30 - 75 100-40 Pyranol 1467 20 - 5# 100-40 Pyranol 1470 15 - 45* 100-40 If any of the scavenger is out of solution, then the material Bust be heated at 70C. (158 P.) until it has dissolved. Selection of punping temperatures for any dielectric not shown on this list or whloh nay be developed in the future should be based on a viscosity of about 100 SayboIt universal Seconds for average punping and about 40 S.U.S. for. fast punping. When the asteri&l has been heated to pvmping temperature, a ae-half inch diameter pipe *@pess* arrangement containing a pressure gauge, air inlet, pressure relief valve to relieve at 30 PSXO, and vent connections, should be connected to the done air inlet pipe. Aten the unloading line should be oonneoted. 9 bBfth o0303 906662 WATER PCB-00049861 (At this point a staple 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 cook on the stand pipe is opened and the discharge pip* observed to be sure the liquid is being unloaded. To protect the teams in the tankear# the pressure mist not exceed 30 pounds. The car will begin to unload at about li pounds pressure. When the car is empty# the air pressure will drop off rapidly and air will blow out of the vent on the receiving tank. The air flow my be stopped at this point and the tanks&r pres sure released through the vent valve on the JHnfoss" arrange ment. After inspecting the ear 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 oar is unloaded in order to keep the ear filled with dry air during return shipment. As a final It is essential that the displacement air used for unloading be dried thoroughly by some dehumidifying unit euoh as soda lime# motivated alumina or similar dehydrating agent drying unit. It may be neoessary to recharge the dehumldlfylng unit each time that a ear is unloaded. For unloading a tankcar of ArocSer within three hows# 15 standard cubic feet a minute of air at 15 pounds per square inch gauge pressure *adia 10F# 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 self-contained reactivating heater is suggested. Two manufacturers of air dryers of this type are: C. N. Kemp Mfg. Co., 405 I* Oliver Street# Baltimore f# Maryland and Pittsburg Deetrodryer Corporation# Foot of 32nd Street# Pittsburgh# Pennsylvania. 10 00030* 906663 WATER PCB-00049862 step, it Is desired that t standard railroad wire seal be in serted through the slotted bolts of the oar fittings. Steam should be released from the oar oolls and all condensate re moved from the oolls by blowing with air with the steam trap by passed. All connections must bs replaced ae received. Adequate care should be taken In preparing and aeallng the car for return shipment. Unloading with dry air aa described la the preferred and recommended procedure because it is don with the oar dome closed which avoids contamination. If the oar is unloaded by pumping out of the top, which required opening the dome. It Is moat 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 car dome, and the unloading should be done when the weather is clear. A centrifugal pump with minimum capacity of 40 gpm. is suggested. It will be necessary to prime the pump and only clean Askarel should b used to do this. Another Mtbd for priming the pump Is to use a Penberthy steam Jet, No. 22A available from Penberthy Injector Co., 1242 Bolden Ave., Detroit 2, Mlohlgan. If a flexible unloading line la \aed, It should be a flexible metallic hose, Rubber hoae must not b used. GBRN 000305 11 906664 WATER PCB-00049863 C, Dnaa Packaging ' Dmm packaging ia made with mw and artfully inapeeted 55-gallon druse. Hies steel dnw are lined with a specially elected hiked phenolic coating. An example ii NRSCO Ho. 3 lining offered by the national Enameling and Stamping Company, Long Island, Hew fork. Contests 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 pre ferred. The screw plug ia the drum head is fitted with a metal oap as a safe guard against tampering. GBRN 000306 12 906665 WATER PCB-00049864 I CHAPTER 2 STORAGE TAMES A. general Description Tm storage tanka should be a minimus of 10*000 gallons and preferably 12,000 to 15#000 gallons capacity to accomodate the noraal 8#000 gallon tankoara. It la preferable to locate the tanks above ground where they are easily accessible for any changes or repairs. Under ground looation presents difficulty in this respect. Especially in cold climates# it is preferable to locate - the tanks Inside of a building. The tanks should be looated conveniently with reference to the tankoar unloading facilities and the area where the dielectric is used. Although Arodors are non-corrosive to metals# corrosion or rusting of iron and steel equipment (by oxidation) may occur resulting in contamination of the products. The resis tance of Aroolors to materials of construction is given in Monsanto Technical Bulletlon O-P-115# entitled# "The Aroolors," Page 6. ` Stainless steel tanks are vary satisfactory but relatively expensive. Stainless steel pipe is relatively difficult to fabricate and it is difficult to males tight leak-proof connec tions. f. Storage tanks my b of steel construction if properly metallised with line-tin or altmism on the interior surfaces 13 GBRN 000307 906666 WATER PCB-00049865 coning In contact with the Aroclors. The metallizing should be don according to th following procedure: 1. Clean an area of the aurface by sand blasting, or a similar method, to give a perfectly clean and rou^ened surface. The area cleaned should not be greater than oan be completely metallized within a few hours after cleaning. 2. If line-tin metallising is ud, a coating of fine 0.005 inohea thick should be sprayed on to the eleaned surfaee. This is followed immediately by a coating of tin 0,007 inches thick. 3. Aluminum metallised surfacing should be about 0.01 inch thick. The detailed procedure for metallising and cleaning is ~ outlined as follows: a) Sand blast, b) Coat with iron, 0.005 inches thick. (The purpose of this coating is to provide a rougher and better bond for the finish ooat of aluminum or the zinc-tin combination.) 0) 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 urfaoe of the tank.) a) Drain the tank, f) Fill with cold water and drain, g) Wipe dry 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 beneficial to heat th tank, allow it to cool and pull dry air through it using a dahtMidifylni breather in th air line, hat again ato. until the tank is full of comparatively dry air. 1) Spray about 100 gallons of new, electrical grad Aroclor (not high 14 * 00308 906667 WATER PCB-00049866 in visoosity) or eleotrieal grade trichlorobenzene onto the inner mil* of the tank, washing the walls thoroughly (avoid breathing any fumes). J) Attaoh the circulating pump, the lines used, and the filter preaa fitted with toy paper and clreulate the fluid through the system and the tank. Install new dry filter paper several times in the press during this dry ing and oleaning operation. Dlaoard the dlelectrlo fluid used for cleaning, k) Partially fill the tank with new Aroclor dleleotrlo and analyze it electrically and chemically to de termine whether it meets specifications. If all tests are set, then fill the tank with the dlelectrlo. The tanks should he insulated using, preferably? glass foam beads as supplied by Dow-Corning or Libby-Owtns-Ford, The suggested thickness of the glass insulation la one inch mini mum to two inches maximum. The glass insulation may be covered with tar material oommonly used for weatherproofing. Another type of insulation whloh may be used instead of the glaais Magnesia-Wool whloh should be oovered also with the weather pm oflng tar. The advantage of the glass insulation is that it la not moisture sensitive as is the ease with Magnesia-Wool. If the storage tank is located outdoors, it is best that the insulation be covered with ribeted or bolted tin sheeting painted with alumina* paint. This type of metal surface weathers well and is oleaned easily. All piping must be gal vanised and serewed fittings must be back brmied to assure 15 GBRN 000309 906668 WATER PCB-00049867 tightness. All handling pipe lines Bust be triced with steam lines and Insulation applied over the two lines In order to keep the handling lines and the staterlal up to the desired pumping temperature. Usually a one-fourth Inch copper steam line running parallel with the handling lint will suffice. Under very severe eondltlons of low temperatures, it would be desirable to wind the steam llna around the handling line about two turns to the foot. The tanks must be provided with ample pressurised heating ooil surface.to supply sufficient heat to the material to bring it to the proper temperature for pumping and handling as indi cated in Table III. Heating colls should be either metallised steel, or preferably steel colls which have been galvanised after fabrication. It is recommended that the steam pressure on all heating colls should not exoeed 100 pounds per square inch gauge; lower pressures may be used where practicable. It is essential that all steam oolls be completely free from even minute leaks slnoe this will introduce water into the product. 1 The stem colls my be introduced as *halr-p&n" 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 tankr.and then located near the bottom. External heating oolls located in the Jacket of the tank may be used but this construction is more expensive and less efficient than the internal oolls. 16 ' GBRN 000310 906669 WATER PCB-00049868 * The storage tanks may be fitted with a stirrer, either through the top, side, or bottoa of the tank and the propeller blade should be located mar the button of the tank. However, insertion of a stirrer through the side offers possible source of a leak and since these materials art homogeneous, it Is not essential to provide suoh agitation for the purpose of nixing. Adequate circulation can also be accomplished by using a centrifugal type pusp, dear pumps or other equipment where wear or chipping of metal parts may Introduce contamination 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, Ihe centrifugal pumps must be provided with a deep stuffing box and proper packing used, as described in Chapter 3. As examples of pumps found com pletely satisfactory for this servloe, reference is made to Worthington Worthlte pumps, Blackmer pumps, and Dayton Dowd Type C pumps for handling hot oil. Also, a very Satisfactory arrangement for mixing or elreulmtln*- and poping the fluid from the storage tank is to use a vertical sump pu^ such as a Taber p\np. All storage tanks must be amply provided with a dehumidlfylng breather such as soda lime, motivated Alumina, etc., imits, Tht* is essential to prevent moist air from coming in contact with the dielectric, A moisture content above 35 pp 17 . GBRN 0003U 906670 WATER PCB-00049869 adversely affects the electrical reaiativity of these pro duct*. Provision should he Bade to preclude possible leakage 46 the drier material back Into the storage tank and the drier should be inspected periodically to sake sure that it la open and not plugged. B. Detailed Description Drawing No. 90-8170 shows tha detailed construction of a horizontal 15,000 gallon storage tank for Aroclor and its mixtures which has been found completely satisfactory. The various nozzles on this tank are used as follows, eon? sidering them in order from left to right on'the drawing: 3" nozzle Inlet for reclroulatlon 24" nozzle For future agitator if wqulred (not used) 3" nozzle For soda lime or calelum ohiorIda breather connection 36" manhole For inspection, eto. The float gauge is located in the center of this manhole. 3" nozzle Not used. 24" nozzle For future agitator if required (not used) 3" hois! Not used 3" nozzle Filling Inlet connection 18" X 26" Oval Nozzle For ip pwitp 3" nozzle For thermometer well (see detail) The two 24" nozzle* were originally installed for Installs tlon of agitators, if required. However, it has been found 18 GBRN 00C3U 906671 WATER PCB-00049870 unnecessary to uae agitators la the storage tanks, and these nozzles oould be omittsd. Zt has been found that elroulatlon of ths fluid by the susip pump, and Into the nossle at the opposite end of the tank, for several hours gives satisfactory blending of the tank contents. For pumping ths dieleotrio from ths storage tank, a "Taber Pump Co. all bronze 2-1/2" Z 2" vertical tump pump with monel shaft has been found to be fuit sataifaetery for the applica tion. ... - The liquid level gauge used in the storage must be gas- tight. The storage tanks are equipped with Vapor Recovery Systems Co.'a "Vsrec," gas-tight, automatic tank gauge as shown by Drawing Mo. 9C-0278. The storage tanka should be provided with an operating plat form suitable to the customer's conditions of operation. The dehumldlfylng unite used as breathers on the storage tanks can be constructed as shown by Drawing Mo. 0-0248. 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 con struction similar to that shown on Drawing Mo, 90-0248 My b used for the breather units. Drawing No, D-13302 shows design detail of a 15*000 gallon 19 ' GBRN 000313 906672 WATER PCB-00049871 vertical storage tank, ftie vertical type tank would seem specially desirable when insufficient space la available to acconsodate the horizontal type tank. 20 GBRN 000314 906673 WATER PCB-00049872 CHAPTO 3 Qksmnm and pcmp pactoo Arcelor* and theto slxtures soften and swell natural rubber and many of the aynthetlo "rubber" materials. Suoh material net rec<ended for us, Include Hyear P, Koroseal, Perbunan, Neoprene, eto. These materials are loom souroes of eont&alnatlon. Suggested types of paoklng and gasketing materials Include: 1. For Welded Flanged Pipe Connections: Garloek Packing Co., No. 901 or No. 7021, 1/8 lnoh asbestos fiber sheet. A ring of thin aluminum drawn tightly at the flangeconnections may be used satisfactorily also, 2. For Pumps: Garloek No, 234, No, 431, and Cheveron No. 7050-C art satisfactory paeklngs. Likewise, Durametallle's spiral asbestos fiber may be used. Johns-Manville and others have comparable packing materials. e 3. For Valves: Oarlook No. 117 braided packing or Its equivalent Is suggested. 4. Other Resistant Materials: It Is Indicated that duPont's Teflon, poly tetrafluoroethylene is not attaoked by hot (130c.) Aroolor and is to be recom mended as a gasket material. Dow-Cornlng's Silastic, Sllloone 180, Is very resistant to Aroolor and is suggested, for gasket purposes, 5. In some oases eork Impregnated under pressure with . Chrysler's Cycloweld 55-9 or Armstrong Cork Co.'s 1162-J and oured at 170C. may be used as a gasket material. These are baked phonelie type coatings. i, Pip# Thread Compounds: When necessary to use pipe thread compounds, the following should be satisfac tory If cart is taken to prevent the pip# eompound from getting on the Inside of the pipe. (a) Plastic Lead al--manufactured by Durametallic Corpe (b) Ordinary whit lead 21 ' GBRN 000315 906674 WATER PCB-00049873 Usually It la not neoassary to use pipe thread com pounds since all screwed pipe fittings should be sealed by back brazing. 7. All new lines and fittings should be cleaned thoroughly by steaming (for two hours) and dried with air or heat. 22 6BRN 00Q3LO 906675 WATER PCB-00049874 CHAHBR 4 SAMPLDO METHODS 1.) The ASTM Standard Method for sampling electrical Insulating oils la described la A3TK Designation: D923-49. This described glass and metal thief for sampling drums, cans, and tankears. A specially designed thief or bomb for sampling tankcars la described, also, A very good Instrument of this type la the stainless-steel Moon Bomb Thief with whioh samples of the liquid oan be drawn from any level of the tankcar. The ASTM procedure describee 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 oholes, as It may be neoessary to prooure samples from a tankoar when the temperature is not above the surrounding air. On such occasions, the temperature of oil and air, also the humidity if possible, should be noted in the report of test results.) It is unde sirable to do any sampling when the relative humidity of the atmosphere exceeds 75 percent, and samples shall never be taken in the rain." 23 &BRN 000317 906676 WATER PCB-00049875 At the plants of several eleetrioal manufacturers using Aroclor dieleotrlos, the praotice is to switch the tankcars directly into the plant building or under roof before sampling and unloading6 These preemptions in handling are taken to avoid any contamination of the fluids whioh are manufactured under very atrlot specifications. For example, the speolfloatlon for lonisable chlorides allows no more than 0.10 parts per million. Moisture may not exceed 30 to 35 parts per million. Tankears are cleaned and prepared under close inspection before they are filled. When filled, and analysis shows " the material in the ear to be satisfactory, the oar is then sealed with a standard railroad wire and seal inserted through the slots of the dome fittings. Likewise, after the tankears have been unloaded in the industry, it is requested that the dome fittings should be sealed with a railroad wire and seal. g.) Monsanto Methods used for sampling tankears differ somewhat from the ASTM procedure. The modified techniques V 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 ef contaminated atmosphere moving in the direction of the ear. However, in case of an emergency, flu?inf inclement weather, a canopy is placed over the ear doe before sampling. GBRN 000318 906677 WATER PCB-00049876 A satisfactory sample bottlt Is a fIva pint, round amber glass, paokar typa oontainer fitted with a 38 llllmeter Bake- llta so raw oap with an alualnua or tin oup liner, Bottlaa of this daaorlptlon oan ba purohased from tha Northwestern Bottle Company, 31bt North Broadway, St. Loula, Mlaaourl aooordlng to their No. A-7253. Only naw bottlaa and oapa ara used. Whan a shipment of bottlaa la raoalvad, tha bottlaa ara capped Immediately and stored In their receiving cartons. Prior to use, tha exterior of tha bottles la wiped with a olaan cloth. The simplest sampling devloe used Is a clean stainless ~ steal or aluminum dlppar. However, this la not a generally preferred devloe because It permits sampling the oar from the near aurfaoa, only. The sampling device commonly uaed oonslata 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 la a stainless steal buoket with a perforated bottom. This bucket Is about 5-1/4 inohes Inside diameter and 6 Inches deep to hold the five pint bottle. Tfela bottle la bald firmly by a stalnlaaa steel collar made to elide along tha shaft of tha sampling devloe. This oollar haa a elamp attachment for fixing It tightly Into plaoe where desired around tha naok of tha bottlt. When a ear la to ba sampled, a naw sample bottle la 0lamped firmly In the buoket. All dirt la brushed and wiped away from the oar dome area using a olaan rag. -25- GBRN 00u 319 906678 WATER PCB-00049877 The car dome Is opened and tha cap is then removed from the sample bottle. The sampling davlea la Inserted into the oar ao that the neck of the bottle ia at least twelve to eighteen inches below the surfsee 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 prooedw9 is repeated until a inim\m of three rinses has been made; eaoh time the sample*-taken is not put back into the oar. These rinses should be discarded. Then the sample is taken and the cap of the bottle is sorewed down tightly. When the sample has been obtained, the ear dome ^re placed, immediately. The exterior of the sample bottle la wiped with a olean cloth and when returned to the laboratory it is further clean ed with a eloth dampened with pure triohlorobensene. If the sample la to be shipped, the eap is taped with Sootch Tape. The sampling device is also cleaned with pure triehlorobensen and is stored in a dust free, air oon3ifeided.:>reoii. ' .' 3.) Pngs Sampling. A glass thief, thoroughly cleaned with pure triohlorobensene and drtd is used to sample dsnas. 26 GBRN Q0C320 906679 WATER PCB-00049878 ' CHAPTER 5 LABORATORY MALTS IS AB5 PROCEDURE FOR TOMTIia JUtOCLORS AXD HEIR MOTOTB WOT EARTH A sample of tii Aroelor or Aroelor mixture taken from the tankcar, or drums, as described la Chapter 4, is analyzed la th* laboratory to determine its quality in accordance with tha property values |lrn in Chapter 7. For eapseitor use, usually ths important propsrtiss tasted are resistivity, power factor, chlorides, and moisture. For transformer use dieleetrie strength, resistivity, moisture, and ohlorldts 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 ease, another sample is to be taken and the properties redetermined. If still omt of spsoifiestions, the sample should be given treatment with earth. Treatment of the dieleetrie with conditioned Attapulgus earth will bring th eleetrieal 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 suek as the following. Mo doubt, there are differences in ths absorbent power of various types of dlntonnesous earth with raspest to ramoving moisturs, impurities and additives sueh as stabilisers or seavsngers from the dielectric 27 GBRN 000321 906680 WATER PCB-00049879 materials, fh* slit of the acrth partielea, 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 la given earth treatment are all possible variables which art still being studied in various laboratoriese Re method used by Monsanto for treating the fluid with activated earth In the laboratory 1st fhe absorbent is minus 200 mesh Attapulgua* earth ac tivated Just prior to use by heating in shallow trays for four hours at 400C. (752P.) 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, O.E. Cell and Accessories". Ifce flask or beaker is fitted with a glass or stainless steel agitator. Beat is applied using either a hot plate or a Olas-Col mantle and is controlled by a thermostat such as a Fenwal thermo twitch with a stainless steel sheath. About 0.1 to 0.2% of the activated earth, based on the weight sof*;.the liquid is added. Attapulgua Division, Minerals ft Chemicals Corp. of America, 210 West Washington Square, Philadelphia 5# Pennsylvania 28 . GBRN 000322 906681 Jir, WATER PCB-00049880 The im viacoua dielectrioa such as Arodors 1248 and 1254 art heated at about 70 to 800. (158 - 176F.) and the less viscous materials such as Aroclor 1242 and Pyranols 1481, 1467, and 1470 are baated at about 50 to 60 c. (122 to 140P.). After heating and ittolag the Maple for about four hours, it is filtered using a elsan Pyrex glass auotlon flask and a buohner funnel fitted with a Mhatnan M 1 or Mo. 3 filter paper* Thia apparatus and the bottle into which the treated sample of dleleotrle is transferred ahould have been cleaned in a manner similar to the 0leaning procedure de scribed In Ohapter 6. lfee earth treated and "up-graded" sample la then ready for final analysis of Its eleotrloal properties. 29 gSRN 000323 906682 WATER PCB-00049881 CHAPTER 6 TEST PROCEDURES A. General Information The Monsanto teat methods desorlbed here vlth the special equipment used are iom of the control tests employed to mintain the quality of Aroolors for dleleetrio use. They ere suggested as a guide for test work needed to indicate the quality of the dielectrios used in the manufacture of electrical goods. The most significant electrical tests made on Aroolors for capacitors are: 1. Dielectric constant. 2. Power Pactor. 3. Resistivity. For transformer use the most significant tests of Aroolor mixtures are: 1. Dielectric Strength. 2i Resistivity. Xn both oases a significant chemical test is oorroslon chlorides. The following terms are defined: Dielectric Constant: The dielectric constant (sometimes called specific induc tive capacity) of any substance is equal to the ratio of the capacitance of a condenser when that substance is used as the 30 . GSKN 0 C G 3 2 906683 WATER PCB-00049882 dielectrio to the oapacltance when there i a vacuum between the conductor* (for ail practical purpose* air-at ordinary fwiiwifi my be used Instead of a mew*), Plelectrlo Strengthi Dielectric Strength Is the rupturing strength of as Insulating material when subjected to voltage streis under specific conditions and e^ressed in kilovolts. fceakdown varies with the shape of the electrodes and does not increase directly in proportion to the thloknees of the dielectrio. Power Factors " The power faotor of a dielectric is the ratio of the ener gy loss in the dielectric to the "apparent power" in the di electric. Resistivity; Resistivity is electrical resistance offered to the pas sage of a steady current. The volume resistivity in ohas- oentimeter of an oil is the ratio of the d-c potential gradient in volts per centimeter paralleling the eurrent flow within the sample* to the eurrent density in amperes per square centimeter at a given instant of time and under prescribed conditions. fhluM resistivity is expressed in ohm-em. The analytical procedures described in detail includes i. itrae hd. li/fsi* BmociDW rm ciMMxnm v msssmsum, o.s. eng tm Aocssaoftss, t. iao> ho. ix*f8* "sazzcmic constant m power FACTOR," ' 31 GBRN 00032f> 906684 WATER PCB-00049883 3. METHOD HO. 11,605# "DIELECTRIC STHENOTH." 4. METHOD NO. 11,607# "RESISTIVITY." 5. METHOD HO. 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)." Detailed Instruction and Testing Methods. 1. METHOD NO. 11,751, "FROCEDOTE FOR CLEANING OF ELEC TRODES, O.E. Cell and Accessories. a. The Electrode Cleaning Procedure: " 1) Place the electrodes In hot electrical grade Trlohlorobenzene 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 with4:tap water. CAUTION J 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. m O.E. Cell Cleaning: 1) Reolean the dell before use, when more than 8 hours have elapsed since the previous cleaning. 2) Follow the procedure for the electrodes starting at Step 4. 32 6BRN 000346 906685 WATER PCB-00049884 c. Cleaning of the Aceessorlea: 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 Pisher Isotemp Oven) and allow to dry. METHOD HO. 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. Generator: General Radio type 1302-A. D. Amplifier and Null Deteotor: General Radio type 1231-B with type 1261-A power supply. E. Capacitance Bridge: General Radio Co. Capacitance Bridge type 7l6-C. F. Test Cells: G.E* type, ooncentrlo cylinder electrodes Catalog #1,559*663. 0. Class B driver transformer: This is used for .60 oyole measurements to excite the bridge directly from the domestie 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 eycle) and 1231-P3 (60 cycle). These filters aid In obtaining a more accurate frequency for the measurements by removing harmonics, noise, hum, stc. 33 GBRN 000 3Z 7 906686 WATER PCB-00049885 II Adjustment of Control* on Electrical Apparatus A. On Panel No. 1 (Top Panel, Amplifier and Null Detector; "" a. Turn the way (main power) switch on the upper right hand aide to the #3 position to determine the Dielectric Constant at 1000 cycles. Turn this switch to the #2 position for measurementB~y5U cycles. b. Allow the equipment to warm up 10 minutes. 0. Turn "SAIN 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. 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 SO. f. Turn "VERTICAL GAIN" to 5. 1. Turn "VERTICAL INPUT" tt "10 VOLT MAX.", h. Turn "HORIZONTAL GAIN" to about 20. I. Turn "SYNCHRONIZING" to + 20. J. Turn "SYN." to "EXT. SYN." k. Turn "GEN." to "SWEEP GEN." ^ GBRN 00C328 906687 WATER PCB-00049886  C. On Panel No, 3 (Capacitance Bridge) a. Turn "RAMIE 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 cyoles. b. On 1000 cycle measurements, depress the No._ ' ` 10 "MULTIPLY BY" button. d. 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. III. Determination of Constants for the Apparatus 1. Carefully^ assemble the oell which has been cleaned and dried within the last 8 hours. Refer to Method No, 11,751 for the procedure to use in cleaning the cells. 2. Plaoe the cell assembly In the Fisher oven which has been adjusted to 25C. 3. Conneot 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. 35 GBRN 00032 906688 WATER PCB-00049887 4. Connect the cable from the capacitance bridge to the terminals on top of the oven so that the Inner wire of the oable 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 goTng^5n"'wifR"Th^sfT" fEXsTa"Uportant. 6. Make all adjustments on the electrical apparatus a* directed in Part I of this method. 7. Balance the bridge by rotating the "CAPACITANCE" and "DISSIPATION PACTOR" dials on Panel No. 3 until the wide vertical band on the oacllllscope Is adjusted to a minimum width. 8... Record the sum of the readings on the "CAPACITANCE41 dial and vernier and oall 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 cylinders 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 t'he sum of the readings on the "CAPACITANCE" dial and vernier and oall this value B. 14. Calculate the cell constant by the following equation: Cell Constant, K B - A (this is usually 572T"5"CT around 70 mmfd.) 15. Remove the cell from the oven and balance the bridge as In Step 7 with the "CAPACITANCE" and "DISSIPATION" "FACTOR" dials. 3* GSRN 000330 906689 WATER PCB-00049888 16. Record the sum of the readings on the "CAPACITANCE" dial and vernier, and call this value P, (capacitance of connecting cable,) " IT, Calculate th CELL IZAD CAPACITANCE by the following equation: CELL LEAD CAPACITANCE, 0 . A - F - K (this is " usually around 3 tmnfd.) where: A - CAPACITANCE OP SNT3HE SYSTEM IN AIR (SYSTEM CONSTANT) ,Om CAPACITANCE OP THE CELL LEADS (CELL LEAD CONSTANT) - P - CAPACITANCE OP CABLE AND WIRES WHICH CONNECT THE CELL AND CELL LEADS TO THE BRIDGE. (CONNECTOR CONSTANT) K m CAPACITANCE OP THE CELL ALONE (THE CELL CONSTANT) Tabulate the system Constant (A), the Cell Lead Con stant (G), the Connector Constant (P), and the Cell Constant (K) on a piece of stiff paper and post them near the instrument where they can be easily?referred to for comparison and calculations. Wiese constants must be cheoked 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 XroeTors, Fyranoie,..Inerteens, and fri-Tetraohiorobenaene mends'. .. A. Teat Run on Cell to Determine whether It la Clean and "Sfroper'i y"' Al ignedl 1. Carefully assemble a cell which has been cleaned and dried within the past 8 hours. 36A GBRN 000331. 906690 WATER PCB-00049889 NOTE; Refer to method No. 11,751 for procedure to use m cleaning cells. 2. Adjust the oven control to hold at a temperature of 100C, for all materials except Tri-Tetra Blends. If a Tri-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 ^rront) wire to the lead on the outer cylinder. 4. 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 anSF the outalde metal oasing (ground)goes to the front terminal. - ' *' 4 5. Allow 15 minutes for the cell to reach temperature equilibrium inalde the oven. 6. Remove the thermometer from the top of the oven before taking any measurements on the bridge. This la 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 vertloal 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 oell 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. 37 6BRN CC033 906691 WATER PCB-00049890 B. Proeedwe for Tenting 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. e 11. Adjust the temperature of the sample to 100C. (use hot plate) for all materials except Tri-Tetra blends. Por 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 temperatwe. 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 WOT Interchange connections. - 13. Allow fifteen minutes for the cell to reach tempera ture equilibrium Inside the oven. 14. Remove thermometer from the oven before taking a measurement. This is".important, .~~. 15. Make the adjustment of oontrols 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 I, 18. Record the sum of the readings on the "DISSIPATION FACTOR" dial and switch. Call this value D. Calculationsi Dielectric Constant I-------F1--- -0 Where: X s Capacitance reading from Step 17. P Connector Constant (Determined in Part II) 0 .Cell Lead Constant (Determined in Part II; K Cell Constant (Determined in Part II) 38 GBRN 0333 906692 WATER PCB-00049891 Mhtn assembling this booklet, a mistake was noted In the num bering of the pages. Ho page of contents Is missing. Only number 39 was skipped. We are pleased to insert number 39 as .a blank page for your conveni ence for notes, if you care to make any. 39 gbrn 000334 906693 WATER PCB-00049892 % Power Factor f x D Where ? f Teat 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 measurements, power factors and dissipation factors are equal. Precision: (Reference: Oeneral Radio Manual for Model 716-C Capaoltance Bridge) a. Capacitance readings are precise to 2 mmfd. x mul tiplier reading (4 O.Sfg 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 i 0,0005 or 2j( of the dial reading which ever is larger, for values less than 0.1 for D (Dissipation Factor). 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 dlelectrio 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 capaolty 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. 40 GBRN 000335 906694 WATER PCB-00049893 It Is enclosed In a steel gray crackle finished cabinet measuring 42 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 oontrol must be at 0 position. Failure to oomply with these requirements will prevent any action when the red button Is depressed. The test cups. Transformers, Voltmeters, and Accessories The askarel testing cup type Ho. 224809 supplied by Oeneral Electric Company Is mounted on the top rear of the oablnet. It is protected by a heavy plastlo cover, hinged at the rear for accessibility to the receptleal. v It is equipped with safety oontactor so placed that the elrcult energising the high voltage oontactor cannot be completed unless the protective oover 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. 41 66RN 0CQ33o 906695 WATER PCB-00049894 The High Voltage Transformer manufactured by the Kelly-Koett Manufacturing Co. is of the closed core, oil immersed, shell type design. Rated 9 81,000 volt 0 40 mlllaspers. it was recovered from a used X-ray machine, purchased quite Inexpensively, 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. voltmeter mounted on top near front edge Is connected across the powerstat secondary and is calibrated to read dlreotly In Kilovolts in the range of 0 - 0 K.V. Hie overload circuit breaker consists of a small relay connected between one side of the high voltage transformer secondary oenter tap and 42 GBRN 000337 906696 WATER PCB-00049895 ground. It ii adjusted to break contact on a current drain of about 50 milliampers. Hie circuit for the coil of the solenoid circuit breaker la wired through the contacts of this relay. Safety and Operating Controls 1) Door Interlock switch located on rear door. 2) Test cup cover interlook switch, 3) Powerstat switch mounted on rear of unit arranged so that high voltage oontactor 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. Procedure 1) Ascertain that the temperature of the material under test is 25 ( 0.5)C. WQT81 Testing at other temperature is likely to give variable results which may be misleading. 2) Shake the sample container so as to thoroughly mix the askarel before filling the test cup. WOTS: This operation is especially Important with uled Aroclor as tne impurities may settle to the bottom and the test may be misleading. 3) Rinse the testing cup three times with small portions of the sample to be tested. 43 feBRN 000338 906697 WATER PCB-00049896 4) Immediately'after final rinse, fill the cup t a height of not less than 20 an. (0,787 in.) above the top of the Aectrodes. 5) Rock the cup a few tinea in order that any entrapped air may escape. Close cover over oil test cup, 6) Allow to stand 3 minutes. CAUTION: THIS IS IMPORTANT. 7) Turn main toggle switoh 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. NOTE: The green signal light is connected across the _ ' 115 volt in-put and denotes that line voltage has been applied to operating control elroult. Amber light is connected In series with sensitive switch located under high voltage oontactors 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 lighn T " 10) Vatoh 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 breakdown. 0339 906698 WATER PCB-00049897 12) Repeat the teat until two successive break downs occur on each of two fillings of the test cup which do not differ by more than 10%. 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. Plush the cup with benzene. Then fill with Aroelor 1246 and let stand, until the next analysis. NOTE: An exception, when samples of oil from the plant are brought in for test, the cup must be thoroughly oleaned with benzene and carbon tetraohlorlde before and after running the test. The electrodes: The testing oup has two electrodes. Both electrodes are movable and have twenty threads to the inch with index notches on both the electrodes and the i lock nuta. To set the Jl2: Arrange one of the electrodes and the look nuts with the index marks in line. Move the other elec trode until it oomes in firm contact with the first electrode and look it. 45 GBRN 0003*0 906699 WATER PCB-00049898 Now unscrew the electrode with the Index marks In line (Step 1) 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 oleaning shall be followed when it is apparent from visual inspec tion that the electrode discs of the cup are coated with carbon. Wipe clean with dry calendered tissue paper the electrodes and the test cup. CAUTION: It is Important to avoid touching the electrodes with the finger or with portion of the tissue paper which has been in contact with hands. Rinse Jthe eleotrodes and oup with dry lead-free gaso line, StoddaaB Solvent (or dry, waterwhite Kerosene) until they are entirely clean. Care should be taken not to touch the electrodes or the inside of the cup after cleaning ao as to avoid possible contamination. 46 0003^ 906700 WATER PCB-00049899 '4. method NO. 11,607, "RESISTIVITY." ' a. Apparatus: General Radio Company Megohm Bridge Type 544-B. This is a combination of Wheatstone bridge and vacuum tube voltmeter for Indicating null. The direct measurement of resistance up to 1,000,000 megohms is made possible by the use of a vacuum tube detector which absorbs negligible amount of power. The voltage applied to the unknown resistor is held approximately constant, regardless of the value of the unknown resistance. This condition is necessary to measure resistance properly. The accuracy of the Instrument in the range en countered in the measurement of Aroclor resis tivity, 100 to 1000 megohm is k 6^. 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. 47 GBRN 0003^2 906701 WATER PCB-00049900 Test Electrodes: Two concentric nickel cylinders with feet, obtained from General Electric Company. The inner electrode has outaide diameter of 2.8" and a height of 3.25" with area of 184 sq. ea. The outer electrode has an inside dlaaeter of 3" and a height of 3.25" with area of 198 sq. ca. The distance between electrodes is, therefore, 0.1" or 0.254 ca. By theory, electrode constant (E) area/length is 191/0.254 or 752 where average area la 191 sq. ca. Also K 36 x 10" x C (farads with air as dielectric) or 11.29 x C (mnfd. with air as dielectric). Olaas Plate: Pyrex about 3-1/2" diameter with concentric grooves to assist in spacing electrodes. Obtained from General Electrlo Company. Heating Unit: Assembled in the laboratory and is the sane unit described in Dielectric Constant Apparatus (see Method Vo. 11,608; Equipment). Procedures 1) Assemble the teat cell. Place the reoently cleaned (within the last 8 hours--see Method Mo. 11,751, Step 9) electrodes in an 800 ml. beaker. 48 GBRN 000343 906702 WATER PCB-00049901 2) Measure the capaoitance of the test eell (cc) . according to Method Mo. 11,608 (Dielectric Coaatant and Power Factor measurements.) 3) Fill the cell assembly uatll the liquid level is 3A inch above the top of the electrodes. 4) Heat the assembly on the hot plate to 100 (t 0.5)8c. 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 egohn bridge to "01* position. 9) Allow 10 minutes for assembly to reach temperature equilibrium inside the even. ,, DAMPHR: Make sure control Ismob is in "CHECK" position. otherwise, painful shock will result if leads are touched^ 1 10) Bring the galvanometer pointer to sero by turn ing the "ZERO ADJUST" Jamah 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 galvamaaeter pointer to sero by ad justment of the "MULTIPLY BY" switch and the megohm dial. 13) Head after 30 seconds. 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. 49 GBRN CCC344 906703 WATER PCB-00049902 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, 100eC and 500 volts DC. NOTEt It Is Important that the produot 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 aero to ohange constantly and give misleading _ results. CAOTIONs Inasmuch as measurements must be made at a potential of 500 volts DC a shook hazard exists in the handling of this apparatus. 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 eleotrodea. Do not attempt to handle the electrodes . of the test leads unless the oontrol knob is in the "CHECK* position. Possible penalty for failure to observe this preeautien Painful Shock. .METHOD NO. 10,126 ''CORROSION AND CHEMICAL STABILITY," a. Apparatus i 0.8. Corrosion Apparatus consists of the following! 1) A Corrosion Flask - It is a 300-ml. Pyrex flask 50 GBRN 000345 906704 WATER PCB-00049903 with a ground glass 24/40 Joint equipped with . a 12-inch straight tube as an air cooled con denser. The air-eondenser is painted on the outside with aluminum. 2) The Corrosion Apparatus: A transits box 32" long x 8" wide x 5'1 deep, The top of the box represents a split transit board with 5 holes cut to fit the flasks. The box is heated by two 500-watt, 15 volt Q.E. Strip heaters with off-set terminals at one end (23.5" overall length). The heating length of the heating element la covered by a copper strip 19-1/2" long x 4" wide x 1/4" thick. The temperature la controlled by an automatic thermostat with temperature aettlng indicator. Procedure 1) Roll a rectangular (2" x 4") piece of aluminum foil ao that it will peas through a ground glass 24/40 Joint of the corrosion test flask. CAPTION: Be careful that after rolling the specimen (Soesnot touch Itself at any point. 2) Wash the aluminum foil (Step 1) scrupulously with aoetone, distilled water, acetone, benzene, and chloride-free ether. 3) Then place the foil on a clean watch-glass and dry in an oven at 110C. 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 oondenser with sample. 51 feSRN 0003*6 906705 WATER PCB-00049904 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. 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 ( O.l) hours at 210 5) C. The temperature of the liquid in the test flask is mea sured indirectly using a thermometer inserted through a cork stopper and into similar liquid contained in an iden tical 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 the hot prate. 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 for* a Appearance. Color, and Condition. b Inorganic (Free) Chlorides--Apply Method No. 10,118 c Acidity (Acid Number) - Follow Method No. 10,087 14) With a pair of clean, straight nlchrome tongs, remove the aluminum foil specimen (Step 3), wash thoroughly, dry and weight 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 0.0001 g. and the Chemical Stability, as Indicated by the ana lysis of the products "After Corrosion Test", in the same way as reported for the original (as received) material. 51 A GSRN 0QQ34 7 906706 WATER PCB-00049905 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, NaCl 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 mix well. A 0.1 ppm beam is considered the very faintest beam perceptible to the eye between 15-45 seconds after adding the AgNO, solution. If the beam intensity is not vislble^at all, or if easily visible (too strong), discard the solutions and make new standards. _ --* * 2) Weigh 20.0 g. C.P. AgNOj into a chloride free dark bottle. Add 20 ml. C.P. HNO- (chloride-free). Dilute to 200 ml. with water. 3) All solutions should be freshly prepared every two weeks and stored in glass-stoppered Pyrex bottles. b. Light Source: Employ the 2 battery Penllte flashlight, having a 3-4 mm, light aperture. New batteries must be used fre quently in order to perceive beams properly. c. Procedure: 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 ehlorlde-free water. Test these aliquots for Tyndall beams by adding 3-5 drops of AgNO? 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 HNOj and repeat Step 1). 2) When funnels are beam-free, drain out all the water exoept 50 ml. in one and 25 ml. in the other. Beat the water in both funnels to boiling. (Hold stopper while heating as steam may cause stopper to fail.) 52 SBRN 000346 906707 WATER PCB-00049906 3) Transfer 50 ml. of the sample from the sample bottle at a temperature of 95-100&C, 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.) k) 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 not the ground part of the stopcock.) 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 120. 6) Repeat step A 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 10 ml. aliquot of the water extract out through the bottom of the funnel into a 3/^" x 6" test tube. Again, first allow a few ml. to drain out before taking the aliquot. (The teat tube used should be rinsed with chloride-free 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 1*5 sec. If beam is present, wash ether several times with chloridefree water until washings show no beam after adding 3-5 drops AgNO-j) o 10) Shake the ether-water mixture until the emulsion in the sample disappears and the water layer is completely beam free before adding AgNO^. If emulsion la difficult to break, add sample dropwise through the ether and then shake. 53 GBRN 000349 906708 WATER PCB-00049907 11)Add 3-5 drops of 10 AgNO? solution and test for . chloride beam for 45 aec.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 AgNO? and comparing at the end of 45 aec. J The method la precise to the nearest 0.1 ppm. Report results to the nearest 0.1 ppm. METHOD HO. 10,087, "ACID NUMBER." a. Reagents: 1) Nitration grade benzol. 2) Anhydrous methanol. 3) A saturated solution of phenol red (phenol sulfonphthaleln) in methanol (approx. 0.1). 4) A 0.01 N solution of KOH in methanol. b. Procedure: 1) Place 100 ml. of bencol, 100 ml. of methanol and 0.5 ml. (pipette) of phenol red indicator Into one of two clean dry 500 ml. Erlenmeyer 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 squally between the two flasks, ~ If not, repeat steps 2 and 3. 4) Weigh (i 0.05 g.) into one of the flasks a 75.0 T 5.0 g sample and titrate with the 0.01 N, KOH until the sample matones the blank. 0.. Calculations: Add No. (mg. KOH/gram sample) ml. 0.01 N KOH x D.56 sample weight 54 bBRN 000350 906709 WATER PCB-00049908 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 4 0.002 for acid numbers below 0.01 and to 4 0.01 In the range of 0.1 to 0.01. NOTE 1: To convert mg. KOH/gram to mg. NaOH/gram, multiply by O.715. . METHOD (MODIFIED NO. 10*620, "MOISTURE (WATER)". a.Introductory Comment: The Karl Fischer Reagent titration method used in the analytical laboratory involves use of an analytical ba lance 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 _ sues..a purchased standard water solution as described below. Also, in the laboratory a "Dead Stop" potentiometrlc method for determining 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. b.Apparatus and Reagentst 1) Karl Pischer Burett, Automatic Pyrex No. 5750, 25 ml. capacity. Ace Glass Company, Vineland, New Jersey. 2) Water Standard in Methanol. No. SO-W-2 (1 ml. z 1 mg. H0) Fisher Scientific Company, 2800 Jeffer son Aver, St. Louis, Missouri. 3) Karl Fischer Reagent Solution No. SO-K-2, Fisher Scientific Company. ^Standardization of Karl Fischer Reagent Into a 500 ml. clean, dry Brlenmeyer flash, place about 100 ml. "Anhydrous" methoanol (commerically 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 watersolution 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. 55 G&rn 00035 906710 WATER PCB-00049909 Moisture value of K.F. reagent in terns of grams - HgO per ml. (Moisture value of stand- (Ml. Standard HgO solution) ,ard water solution In gm. per ml. stated on ........... label.) ml. rtarl Fischer Reagent d. Solvent Mixture: Slnoe the solubility of the different askarels varies, the following solvent mixtures are suggested: Material Anhydrous Benzene Anhydrous Methanol Pyranol 1478 Pyranel 1488 1467 Pyranol l4Sl Pyranol 1495 All Ar00lore 0 ml. iQ ml. 100 ml. 100 ml. 110 ml. 300 nl. 200 ml. 200 ml. 200 ml. 190 ml. Procedure, "visual End Point 1) Plaoe 100-300 ml. of dry solvent mixture (c) in a dry 300 ml. ground glass stoppered Erlenmeyer flask. 2) Titrate the solvent with K.F. reagent to the vis ual 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 IgO 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.F. reagent used. Calculation: % HgO ml, of K.F. reagent x BqO factor x 100 J Sample Weight1........ References: Mitchell, J. and Smith, D.M., Chemical Analysis, Vol. 5> Aquametry, Intsrsolenoe Publishers, Inc., New York, (1948 56 . 6BRN OCG 3 5 906711 WATER PCB-00049910 CHAPTHl 7 TYPICAL PROPERTIES The 1200 series members of the Aroclor family are chlor inated biphenyls, and are mad 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 la approximately 54^ chlorine on a weight basis. Aeoordlngly, these Aroclors are not single or simple compounds. They are a mixture of isomeric com pounds composed predominately of the ehemloal compound in dicated below as being their approximate equivalent: ` Aroolor 1242 Aroclor 1248 Aroclor 1254 Aroolor 1260 Trlohloroblphenyl Tetraohloroblphenyl Pentachloroblphenyl Hex&chlorobiphenyl For transformer use and some oapaoltor 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 trlohlorobenzene resulting in various General Bleetrie Company Fyranols described briefly as follows: Transformer Pyranol 1467* 60^ f Aroclor 1260 40 of Blec. Grade - Triehlerobenzene 0,125^ of Tin Tetraphenyl transformer Pyranol 1470* 450 of Aroolor 1260 55* of Blec. Grade TrichloroTetrachlorobenzene Mlxturi 0.125^ of Tin Tetraphenyl *0s@ of tri-tetraehlorobemene and tin-tetraphenyl scavenger is subject to G.E. patents and licenses Royalty arrangements should be checked before using. Questions about license concerning the use of anthraquinone stabilizer for DC oapaoltora should be referred to Western Electric, 195 Broadway, N.I.C. 57 GBRN 000353 906712 WATER PCB-00049911 Capacitor Pyranol l48l 75* of Aroclor 1254 25$ of Else, Grade Tri- ehlorobenzene Detailed properties of all of these product# are given as follows: AROCLOR 1242 PROPERTY TYPICAL Vise. 37.8c. (ASTM D88) Speoifio Gravity 25/15.5C. (ASTM D28?) Color, AFHA Condition Acidity, mg, KOH/g. Pour Pt.,C, (ASTM D97) Inorganic .Chlorides, ppm. Refractive Index @ 25 C. Distillation Range (ASTM D20) Corrected for stem and barometric pressure Corrosion 82 - 92 seconds Saybolt Univer 1.381 - 1.392 100 SAX, Clear 0.01 max, -14 or lower 0.10 max. 1.6245 - 1.6265 10* 3252c. min. 90* 366C. - After heating with aluminum for six hours at 21000 2 10C, the aluminum must not be cor roded either on visual or weight inspection and the Aroolor 1242 should meet the following speca: Color, AREA 150 max, Aoldlty,mg. KQH/g. 0.01 max. Inorg.Chlorides,ppm 0.10 max. Condition Clear Water Content, ppm 35 Resistivity 100&C, 500 volts DC 0.1" gap 500 x 109 ohm--om., min Dleleotrio Constant 100C, 4.7 - 4.9 <8 1000 eyelee (ASTM D924) Flash Point Cleve. Open Cup* 160C., min. Fire Point C. None to boiling point Sulfates (ASTM-D117-31)* None Fixed chlorine content (Carina)1 41.5 - 42.5* Specific Heat 25C.* 0.29 Evaporation 100C for 6 hrs.* 0.4* max. Dieleotrlo Strength (KV) 35 Min. (ASTM D8r?) Not determined unless by special request. 58 GBRN 00035<t 906713 WATER PCB-00049912 AROCLQft 1248 PROPTOTY Vise. Q 54.4C. (ASTM D-88) Speo. Qrav. G 65/15.5C. (ASTM D-287) Color, APHA Condition Aoidity, ag. KOH/g. t four Point C. (ASTM D-97) Refrao Index 0 20C. Diite Mng (ASTM D-20) Water Content, ppm. Reels. 10OC. 500 v D.C. 0.1" gap Dieleetrie Constant,100G. 1000 o>ole Dieleotrio Strength 25C.* Flash Point, (C.O.C.)* Fixed Chlorine (Carlus)* Specific Heat 25C.* TYPICAL 73-80, seo.Saybolt Univer. 1.404-1.414 100 Clear 0.01 -7^ I.630-I.631 343 - 373C. 35 500 x 10^ ohffi-om., min. 4.6 35 KV Bin. 193C. t 47.5 - 48,5^ 0.27 Not determined unless by special request. 59 ooo3^5 906714 WATER PCB-00049913 AROCLQR 1254 PROPEOT TYPICAL Vise. 9 98.9C.(A5TM D88) Specific Gravity 65/15.5C. (ASTM D207) Color, AFHA Condition Acidity, mg.KOH/g. Pour Pt. C.(ASTO D97) Inorganic Chlorides, ppm. Refractive Index 9 25C. Distillation Range (ASTO D20) Corrected for stem and Barometric Pressure Corrosion 44-48 sec. Saybolt Dnlver. 1.495 - 1.505 100 max. Clear 0.01 7-12 0.10 max. 1.6370 - I.6390 10* 366.- 3785C, 50* -l2 " 31830c. 90* 383 - 398C. After heating with aluminum for 6 hours 9 210C. plus or minus 10C, the aluminum must be cor roded either on visual or weight Inspection and the Aroclor 1254 should meet the following specs: Color, APHA 150 max. Aeidlty,mg.KOH/g. 0,01 max. Tree Chlorides,ppm.0,10 max. Condition Clear Water Content, ppm. 35 max. Resistivity 100C.,500 v D.C. 0.1" gap 500 x 10^ ohm-cm., min. Dielectrio Constant, 100C 4.15 - 4.35 1000 oyoles Dlelectrlo Strength 25C* 35 KV., min. Bum Point (ASTM D92)* Higher than 350C. Sulfates (ASTM D-117-31)* Hone Fixed Chlorine Content(Carlus )* 55~t 0.5* Evaporation 9 lOO^C, for 6 hrst 0.4* max. Stability There shall be no liberation of chlorine or chlorides when the material Is heated 9 100C in glass vessels In oontaot with air for periods of at least one month. Ageing Characteristics* No loss in resistivity over original value on heating in air for 96 hra. at lOO^C. Specific Heat 0 25C.* 0.26 Not determined unless by special request. 60 GBRN 000356 906715 WATER PCB-00049914 ABOCLQR I860 PROPERTY TYPICAL Viao. 0 9fl9Ce(A3TM D88) 72 - 78 Sec, Saybolt Unlv, Specifio Gravity 0 90C./15.5C 1.555 - 1.566 (ASTM D287) Color, AFHA 150 max. Condition Clear Acidity, mg.KOH/g. 0,01 max. Pour Pt.,C.(ASTM D97) Inorganic chlorides, ppm. 25 - 34 0.10 max. Refractive Index, 25C. 1.6455 - 1.6470 Distillation Rang (ASTM D20) 10< 385 - 398C Corrected for stea and 50* 390 - 404C, barometrio pressure. 90* 400 - 420C. Corrosion After heating with aluminum for 6 hrs. 0 210C. 4 10C. the alxsainum must nof be cor roded either on visual or weight inspection and the Aroolor 1260 should meet the following specs Color, APHA 150 max. Free Chlorides,ppm. 0.10 max. Acidity,mg.KOH/g. 0.01 max. Condition Clear Water oontent, ppo. 35 max. Resistivity,100C 500 volts P.l" gap . Dlelectrlo Strength 50C.# 500 x 10^ ohm-OB., min. 30 K7., Bin. Dielectric Strength 100C,* 30 KV., Bln. Dleleotrlo Constant 100C. 3.6 - 3.8 0 1000 cycles* Bum Pt. (ASTM D9S)* Higher than 350C, Sulfates (ASTM DI17-31)* Mone Fixed chlorine oontent (Carlus^ 60 4 0.5* Evaporation 0 100C, for 6 hr# 0,2* Bax. Stability* There shall be no liberation of ohlorine or chlorides when . the naterlal is heated 0 100c. in a glass vessel in oontact with air for periods of at least one month, Specific Beat 0 25C.* 0.23 Not determined unless by special request, 61 GBRN 000357 906716 WATER PCB-00049915 PYRANOL 1481 PROPERTIES TYPICAL Viscosity 9 37.8C. 70 - 82 seo. Saybolt Dniv. Speo. Gravity 9 15.5/15,5C 1.525 - 1.535 Color, APHA 150 max. Condition Clear Acidity, 02. KOH/g. 0.01 max. Pour Pt,, C. -15 or lower Inorganic Chlorides, ppm. 0.10 max. Refractive Index O 25C. 1.6205 - 1.6215 Distillation Range Corrected for stem and barometrlo pressure. First .drop 205C. min. 250 max. Below 270C. 90% 380 - 395C. Corrosion Test Change in Weight 0.0* Color, APHA 200 max. Acidity, after test,mg.KOH/g 0.01 max. Free Chlorides,ppm. 0,10 max. Condition after test Clear Water Content, ppm. 35 max. Resistivity 9 100C 500 volts, DC, 0.1"gap 100 x 109 ohm-om.,mln. Dielectric Constant (100C., 1000 oyoles) 4.1 - 4.6 62 (,BKN 000353 906717 WATER PCB-00049916 FYRANOL 1467 properties TYPICAL Vlso. @ 37.8C.,(ASTM D88) 54 4 2 sec, Saybolt Univ. Speoifio Qravity # 15.5/15.5C (ASM D-287) 1,560 - 1,560 Color, APHA 150 max. Condition Clear Acidity, mg, KOH/g. 0.01 max. Pour Point, C. (ASTM D-97) -32C,, or lower Inorganic Chlorides, ppm. 0.10 max. Refractive Index t 25C. 1.6137 - 1.6147 Distillation Rang (ASTM D20) lit drop <- 200C, min. Corrected for stem and Below 270C. - 40% max. barometric pressure 90% - 395 - 4l5C Corrosion After heating with aluminum for 6 hra. 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 200 max. Aeldlty,mg.KOH/g. 0,01 max, Znorganio Chlorides 5 max. Ppm. Condition Clear Water Content, ppm. 30 max. Resistivity, 100C. 500 volts, 0.1" gap 100 x 10^ ohm-em.,min. Dielectric Strength, 25C. 35 K7., min. Dleleotrlo Constant, 100C, 1000 oycles* 3.7 - 4.-0 Tin Tetrapheny1*` 0.125% 4 0j01% by weight Bum Point, (ASTM D92)* None up"te Boiling Point Fixed Chlorine* 59.1% min. Aro Formed Oases* _ Less than 1.0% (Oxygen Free Liquid 25C) Total combustible gases including oarbon monoxide, hydrogen and volatile hydro carbons. Hot determined unless by special request. 63 GBRN 000359 906718 WATER PCB-00049917 FYRANOL 1470 PROPERTIES TYPICAL Vise, 37.8C. (ASIM D80) Spee. Gravity 15.5/15.5*0., (ASTO D287) Color, APKA Condition Acidity, ng. KGff/g. Pour Pt.,C., (ASTM D97) Inorganlo Chlorides, ppm. Refraotive Index t 25C. Distillation Range (ASTM D20) Distillation Range (ASTM D20) Correoted for stea and barometric preasur First drop 35* m >5* 95* Corrosion 41-45 Seo. Saybolt Unlv. 1.563 - 1.571 150 max. Clear 0.01 max. -44C., or lower 0*10 max. 1.6075 - 1.6085 210C,, min. 238 256C. _ 275 - 345C. 380 - 400C. 390 - 4l5C. After heating with aluminum for 6 hr, 200-220C., the aluminum must not be eorroded either on visual or weight inspection and the Pyranol should meet the following specs Color, APHA 200 max. Acidity,mg.KOH/g, 0.01 max. Inorg. Chlorides,ppm 5 max. Condition Clear Water Content, ppm. 30 Resistivity, 100C., 500 r,, 0.1" gap _ 100x 10^__________ o. ho-cm., min, Dleleotrlo Strength, 25C. 35 Sny7,,. mnlinn. Dieleotrio Constant, 100C., 1000 4roles* 3.8 -4.3 ,, Tin Tetraphenyl* 0.125* * 0.01* by weight Bum Point, (ASTM D92)* Hone up"to Bolling Point Fixed Chlorine* 60.5 4 0.5 Are Formed Oases* Total eombustlble gases in (Oxygen Free Liquid 25C.) eluding carbon monoxide, hydro gen and volatile hydrocarbons. Eleotrioal Stability* After heating for 96 hrs. 100C in a closed container, the resistivity should not decrease more than 10* Hot determined unless by special request. 64 GBRN 000360 906719 WATER PCB-00049918 PYRAUQL 1488 Viac, 0 37.8C. Spec. Qrav. O 15.5/15.5C. Color# AFHA Aoidity (Mg KOH/g) Water# ppm. Condition Refrac. Index 0 25C. Free Chloride# ppm. Four Point# C. Bella. 100C., 500 v D.C. Dielectric Strength (25C.) Corroalont Lose of. Alumlmn 54-- 2 Seo. Saybolt Unlv. 1.560 - 1.568 150 sax. .014 max. 35 max. Clear 1.6137 - 1.6147 0.10 max. Lower than -32C. 100 x 10^ hm-om min. Over 35 K? None - Heating with aluminum for 6 hr, at 200-220C. The Fyranol after heating should meet the following epees: Color# AFHA 200 max. Aeidity(MgKOH/g) .014 max. Free Chloride ppm .10 max. Condition Clear Dielectric Constant 9 1000 cycle 9 100C.* 3.7 - 4.0 Distilling Range (corrected)* 1st drop 200C. min. Below 270C. 40J8 max. 9658 point 295 - 415C. Bum Point (ASTM D-92)* Fixed Chlorines* . *None up to boiling point 59 1 min. Arc Formed Oasei Less than 1.0* total com (Oxygen-free liquid 9 25C.) bustible gases including carbon monoxide# hydrogen# and volatile hydrocarbons. Not determined unless by special request. 65 GBRN 0003o1 906720 WATER PCB-00049919 CHAPTBi 8 EARTH miAOTT OP AROCLOR IN THE ELECTOICAL INDUSTRY mim to ose, Aroolors and their mixtures applied to the electrical industry must conform with most strict requirements stpoifitd by the industry as shown in Chapter 7* Since these products are sensitive to contamination from traces of impurities, they require careful handling in the industry when sampling or storing or using the materials to impregnate capacitors or fill transformers. Common oontaminants to be avoided include moisture, lonizable Impurities, metallic impurities, such as rust or corrosion products from storage and handling equipment, and contaminants suoh as oils (mineral oils), lubricating oils or greases common ly used in equipment or other processes in the electrical industry. Care must be taken to avoid contamination from contact with Improper gaslQsts or peeking materials. Including natural and synthetic rubber and most plastic exclusive of certain Silicones and Teflon. Rosin solder fluxes, etc, may also introduce tracts of deleterious impurities. The dielectrics are also susceptible to the harmful action of ultra-violet light and, therefore, exposure to direct sunlight should be avoided. The adverse effect of lonlzable impurities is especially pronounced in the low viscosity Aroolors suoh as Aroolor 12^2 66 . GBRN 000362 906721 WATER PCB-00049920 or Aroelor mixtures such as Pyranol 1481. In the east of more viscous fluids, such as Aroelor 1254, the lonlzable im purities are not so free to move about In the fluid and, con sequent^, the more viscous fluid* can be handled with less ear than required for the thinner fluid*. This li especially pertinent in capacitor manufacturing. When using the thinner type Aroelor* to make capacitors that offer superior low temperature operation, the following types of trace contamination affecting the electrical properties of the dielectric have been experienced. Occasional droplets of perspiration from operators, when winding the capacitor cores, have fallen onto the paper causing contamination In the finished units. Small amounts of Glyptal resin and simi lar sealing compounds used to seal tiny leaks in the vacuum impregnating equipment or storage tanks have caused contamina tion. Also, small amounts of mineral oil entering the system have caused similar trouble. A small droplet of any of these materials in one or several liters of the thinner type fluids results in noticeable contamination, whereat it may not have as much adverse effect on the sore viscous dielectrics. To be certain that the fluids are free from traces of contamination, it is standard practice to treat then with con ditioned diatomaoeous earth and then to filter idiately be fore use. Treatment with this earth by removing trace contam inants results in "up-grading" the electrical values, e.g., 67 6BRH 000363 906722 WATER PCB-00049921 _ the volume-resistivity may be brought up considerably beyond the specification minimus or the normal values of the dielectric as received. Likewise* improvement in power factor may be ao compllshed. The earth treatment recoamedded for use by the electrical manufaeturers is qualitatively the tame as used in the produc tion of the Aroolors and their preparation for shipment to the electrical industry. Treatment of the Aroolors with earth by the electrloal manufacturers is a step required to assure that traces of impurity or contamination that may have been introduced during storage or handling in the eleotrieal indus try have been removed and that maximum electrical values have been attained immediately before the dielectrio is Introduced into capaoltors or transformers. It is impractical for the manufacturer to furnish these dielectrios to the customer at the maximum attainable electri cal qualities because even with oareful packaging* shipping* sampling and handling in the eleotrloal industry* these fluids may easily piok up traces of contaminants from opened tankcare* drums* pipe line* pumps* eto. However* as supplied according to the specifications* the fluids are readily "up-graded" by the earth treatment. The type of diatomaoeous earth used is known as Puller's Barth* supplied by the Plorldln Barth Company* Warren* Pennsyl vania* or the Attapulgus Division* Mineral ft Chemicals Corp, of America* 210 West Washington Square* Philadelphia 55* Pa.* 68 906723 WATER PCB-00049922 op their equivalent. Usually a minus 200 mesh size, regular volatile. Is used and theqiality should be specified as for use by the eleotrloal industry, (Code 73122) The earth as received needs to be conditioned and acti vated, after which It should be stored only a minimum length of time (about a day at the most) and In hermetically sealed containers, prior to use. It Is desirable that the earth be used Immediately after it has been activated. Activation should be done by heating the earth contained in stainless steel shallow trays for four hours at 400C. In a muffle furnaoe. If a muffle furnace is not available or the capaolty by this method may not be great enough, the earth can be activated by heating at least twelve hours in an elec trically heated oven at 250C. Another method used Is to pan dry and aotlvate by heating at 100C. and using a strong vacuum, about 6 nm. of mercury. This latter method is used In oonneotion with transformer work and the former methods are usually used for papacltor work. In the plae of pan drying, rotary driers may be used but their aotlon should not be so severe as to break the earth par ticles to the extent of producing powder which Is difficult to handle in the subsequent filtering operations. It Is the consensus that the earth should not be heated above 400c. as this may cause collapse of the particles. 69 906724 WATER PCB-00049923 - The amount of earth used la usually 0.10 to 0.30 based on the weight of the fluid Larger amount* of earth ean be used If the fluid is composed of only Arcelor m a mixture of Aroelor and ohlorlnated benzene or other pour point depressants. However, larger amounts of highly active earth. In the range of 20 or 30# would be expected to selectively adsorb scavengers or stabilizers from the fluids containing these additives. This is especially of concern in handling the transformer fluids which usually contain scavengers such as tin tetraphenyl. For transformer work it Is suggested that the earth be condi tioned and mildly activated by heating It at 100C. under va cuum, about 6 mm. of mercury. Not more than about 0,10 of earth based on the total weight of the transformer fluid should be used, Por treatment with earth, the fluid la put Into a suitable tank fitted with an agitator, heating coll, and a cover. The proper amount of freshly conditioned earth is added and the mixture Is agitated thoroughly and heated for about four hours, ,, The more viscous dielectrics such as Aroclors 1248 and 1254 Are heated at about 70 to 80 C. (158 to 176F.) and the less vlsoous materials such as Aroelor 1242 and pyranols 1481, 1467, and 1470 are heated at about 50 to 60 C. (122 to l4oP.) After about four hours oontaot the material is filtered through a sparkler or Sweetland or a comparable filter press previously fitted with filter paper liners such as supplied by 70 GbRN 000366 906725 WATER PCB-00049924 - Carl Schleicher and Sohuel Co,, Inc., Keene, N.H. The paper Is usually 25 oils thick and must be dried at 100c. to remove moisture, prior to use In the filter press. The filtered dielectric material is then ready for Impregnating capacitors or filling transformers. In some oases, especially for AC eapaoltor work where the dleleotrlo does not require addition of stabilizers and accordingly there Is no danger of removing such additives by repeated earth treatment, good praotloe Is to use continuous earth treating, circulation and filtration with oonatant read ing of the resistivity of the filtered dleleotrlo. In Chapters 1 and 2 selection of proper materials of oonstruotlon for the tankoars and storage tanks was discussed. It is equally Important to select proper materials of con struction for the processing tanks used In the eapaoltor and transformer Industries and also for the lmprgnatlng chambers used In making capacitors. It Is preferable that this equipment be made of stain less steel or aluminum, or , If It is of steel oonstruotlon, the interior should be either sine-tin metallised or aluminum lined. While Iron or steel equipment Is not regarded as de sirable for handling the fluids, this type of construction is used In some of the plants. Bare the possibilities of rust ing or corrosion cannot be overlooked. If the equipment is kept free from water and If a film of clean dielectric adheres 71 ' GbRN 000367 906726 WATER PCB-00049925 to th surfac# of the metal* e.g when the tanks are empty* then satisfactory operation oan be experienced. However* a number of factors must be kept in mind and to cite an example* reference la made to the impregnation of capa citors by the chamber 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 capaoitors prior to impregnation -- usually by heating the ohamber to about 130C. under efficient vacuum* 100 microns or less. If the chamber is not made of _ the preferred materials of eonatruetion* alight corrosion may occur and the film of fluid on the interior surface of the tank may be contaminated and in turn introduce traces of impurities into the treated and clean dlelectrlo subsequently introduced into the chamber for Impregnating the capacitors. In fact* because of this possibility of contamination* in some operations the capacitors are conditioned and dried preparatory to impreg nation in a separate oven or chamber and when thoroughly dried they are then transferred into a second chamber used for impreg nation. _ Xn the case of relatively large size capaoitors* such as power factor correction units* a manifold pipe system may be used to handle each unit individually rather than by the batch- chamber method. The unimpregnated oapaoitora are placed into an oven and vacuum is applied to the individual units attaohed to the manifold. 72 GBRN 0Q03OB 906727 WATER PCB-00049926 - When conditioned and dry* the dielectric is Introduced into the unit through the manifold, Care must be taken that moist air or oontaminants do not collect In the branch through which the dielectric is introduced. In addition to removing moisture* another purpose of the heat and vacuum conditioning treatment given the capacitor units prior to impregnation la to remove traces of Impurities uoh as residual solvent from the metal oleaning operations and from solder flux* ate. Th fluid is introduced hot into the evacuated capacitor units. The more viscous Aroelors* such as 1248 and 1254* are usually Impregnated at 85 to 130C. The less vlsoous and more volatile dielectrics such as Aroolor 1242 and mix tures of Aroolor with chlorinated benzene may be introduced best at lower temperatures -- about 50C. optimum* 30%. max. Table IV indicates desirable minimum resistivity values of the dielectric materials whan earth treated and ready for oapaoltor impregnation and similar values of the material following the process. TABU IV Dielectric Volume Resistivity Ohm-om at 10QC. and 500 volta DC. Prior fo After Impregnation Impregnation Arodor 1254 2,500 x 109 800 x 109 Aroolor 1242 1*500 x 109 600 x 109 Pyranol 1481 600 x 109 400 x 109 73 GBRN 000369 906728 WATER PCB-00049927 In.the ease of new and freshly filled transformers using Aroclor dleleotrlo mixtures# it seems reasonable that the power factor of a sample of the fluid drawn from the trans former should be in the range of about 5 to 12 per cent# measured at 60 eyoles and 100C, With field servioe of the transformer the power factor value la expected to Increase somewhat. However# suoh a power factor inoreaae alone does not seem to have harmful effect on the operation of the transformer. - A more usual measurement used for transformer fluid la volume-resistivity. This value of the new dielectric prior to filling the transformer should be about 300 x 109 ohm-om. at 1#000 eyoles and 100C. The similar value of the fluid taken from a new transformer should be at'least# about# 50 x 10$ ohm-cm and no lower than 25 x 109 ohm cm. With long field service volume-resistivity values de crease somewhat but seem to level off around 10 x 10^ ohm-cm# with satisfactory "transformer qperation. However# if the volume-resistivity of the fluid falls below 10 x 109 ohm-cm# the matter should be looked into. 74 6BRN 000370 906729 WATER PCB-00049928 . ClAFriR 9 DSWATOLOOY U TOXICOLOGY Skin patch tests using Arcelor 1254 (biphenyl Chlorinated to the extent of 54$ by weight) applied to gauze and placed In contact with the skin showed m primary Irritancy or sen sitization, Th tests wore conducted under competent medical supervision and the standard procedure recommended by rrs. Louis Schwartz and Samuel M, Peek# Reprint No, 2552, Public Health Reports# Vol, 59# No, 19 (April 28# 1944) was used, _ If Aroolors are.spilled on the skin# the skin should be washed In the usual manner with soap solutions. If accidental burns eeeur from contact with hot Aroolors# the bum should be treated the same as any ordinary bum, Aroolor adhering to the burned area need not be removed Immediately unless treatment of the bum demands it# in whloh case use soap and water or repeated washings with a vegetable oil. At ordinary temperatures Aroolors have not presented industrial toxicological prob1m*, If Aroolors are used at elevated temperatures in open systems# methods must be designed to exhaust any vapors arising, teperimental work on animals indicates that the maximum safe concentrations of vapors in wortooems is in the range of i,0 to 2,0 milligram per cubic meter of air. This applies to all of the liquid Aroolors. 75 GBftN 000371 906730 WATER PCB-00049929 Laboratory technique merely requires keeping the hands free of the liquid and handling it under a well ventilated hood. Loeglised or spot ventilation together with general work room exhaust la reeomended for plant operations. When sampling tankoars, eanvaa gloves and safety glasses or goggles should be worn. No speolal olothing Is required but the worker's garments should b laundered at least weekly and oh&nged 'in ease Aroelor or Aroeler mixture is spilled on the olothes accidentally. If werlmen art exposed to Aroolor vapors at relatively high levels, as may be the ease when opening a heated capacitor impregnating chamber, a respirator should be worn during these short intervals. The many years of satisfactory and safe use of Aroolors and their mixtures with ohlorinated bensenes in the electrical industry for impregnating eapaeltors and filling transformers has demonstrated the industry8 ability to handle these fluids without hasard to the worloea. It is a simple matter and in line with good "housekeeping* and personal cleanliness to exercise the suggested and required precautions in all cases. 76 GBRN 000372 906731 WATER PCB-00049930 906732 WATER PCB-00049931 906733 WATER PCB-00049932 IP 'HP, I! I mg if-- i r*- 4*-j<t U- I1 Ij rr-( R* IE f& zzzr^l 5f& W :t*cn k f ...c.. :-r":rtt*\-J!^o i ^- : ^|i | 2 1 GBRN 000375 906734 WATER PCB-00049933 GBRN 000376 906735 WATER PCB-00049934 906736 WATER PCB-00049935 GBRN 000378 906737 WATER PCB-00049936 i 000379 906738 WATER PCB-00049937