Document dybj9gmXbEmL9G72nEVoq180

THE PROPER HANDLING OF AROCLORS AND THEIR MIXTURES IN THE ELECTRICAL INDUSTRY Monsanto __V4_j Monsanto Chemical Co. Organic Div. Sales Dept. 800 N. Twelfth Blvd. St. Louis, Mo. P. G. BENIGNUS MAY I, 1956 HONS 073018 INDEX Introduction Chapter 1 Chapter 2 Chapter 3 Chapter 4 Chapter 5 Chapter 6 Chapter 7 Chapter 3 Chapter 9 The Proper Handling of the Aroolors and Their Mixtures in the Eleotrloal Industry. Procedure for Unloading Tunkears of Arodors and Their Mixtures. A. Description of the Cars. B. Procedure for Unloading the Care. C. Drum Packaging Storage Tanks A. General Description of Storage Tanks. B, Detailed Description of Storage T-nks. Gasketing and Pump Packing. Sampling. Laboratory Analysis and Procedure for Treating Aroclors and Their Mixtures. Test Procedures. Typical Properties. Earth Treatment of Aroclors and Their Mixtures in the Electrical Industry Prior to Use. Dermatology and Toxicology. Attachments: Drawing No. 31-20848, Dome Detail. Drawing No. 31-20847, The Tank Car. Drawing NO. 9C-8170-5. The Horizontal Storage Tank. Drawing No. D-13362, The Vertioal Storage Tank. Drawing No. 9C-B243, The Breather. Drawing No. 9C-8278, The Varec Gauge. Drawing No. 9C-8178, The Unloading Platform. MCNS 073019 THE PROPER HANDLING OP AROCLORS* AND THEIR MIXTURES IN THE ELECTRICAL INDUSTRY INTRODUCTION Monsanto'8 Aroclors*, especially the ohlorlnated biphenyls including types 1242, 1248, 1254 and 1260, uBed alone or in combination Kith ohlorlnated benzenes, are commonly used dleleotrlo materials of the Askarel^ olass. Askarel 1b a generlo name referring to liquid dielectrics derlvedVdSrefe halogenated aromatic hydrocarbons possessing excellent ohemloal and dleleotrlc stability and fire-resistance over the temperature ranges and operating conditions required of transformers and capacitors in the electrical industry. The properties of Aroclors and their mixtures, used as dleleotrlcs are described in detail in Chhpter 7 entitled, "Typical Properties". These dlelectrlos are manufactured under very carefully controlled conditions in order to meet the strict and exacting eleotrloal requirements and properties. The eleotrloal Industry's use of these fluids has been largely in aooordanoe with the Oeneral Electric Company's patents and developments. *Aroclors - Monsanto's chlorinated biphenyls and ohlorlnated polyphenyls. Registered U.S. Patent Office. *F. M. Clark, "Eleotrloal Insulation", Chem. Eng. News 25, 2977 (1947). ------ ----------- 1 HONS C730i0 Resulting from the wide use of these materials In the Industry, trade names have been established to Identify them by different manufacturers of eleotrloal equipment, listed alphabetically the trade names Include, "Chlorextol," Allis Chalmers; "Dlaclor," Sangamo Electrio; "Dykanol," Cornell Dublller; "Elemex," Line Materials; "Hyvol," Aerovox; "Inerteen," Meetinghouse Eleotrlc; "Moflamol," Wagner Electric; and "Pyranol," General Electrlo Company. The purpose of this bulletin Is to assist the Industry With 'theoproper and safe handling of these dleleotrlo materials In their operations. HONS 073021 CHAPTER 1 PROCEDURE POR UNLOADING TANKCARS OP AROCLORS AND AROCLOR MIXTURES A, Description of the Para Aroolor and mixtures of Arodors with ohlorlnated bensenes are shipped by Monsanto In two types of Insulated tankcara both of which are either aluminum lined or zlnc-tla metallized. One type of ear has heating colls Inside of the tank and these are In dlreot oontaot with the produot. The other, a more widely used type of car. Is a double-shell tank with heating oolls between the Inner and outer shells. The steam ooll connections are at the bottom of the oar. Both types of tankcars are tested for 60 pounds pressure and their steam colls are tested for 200 pounds gauge pressure. The oars are top-unloaded by displacement with dry air containing 10 mg. HgO/ou. ft. maximum. There are two or three connections on the tankoar dome depending on the type of oar. Where three connections exist, one Is a two Inch diameter unloading line whloh extends to the bottom of the oar, the second Is a one Inch diameter air Inlet connection and the third Is a two Inch diameter pressure safety vent, whloh la a thin lead disc adjusted to release any pressure In exoess of 60 pounds gaage. This safety vent Is hooded for protection against dust, dirt or accidental bumping. Where only two connections exist on the dome, one Is the two lnoh diameter unloading line and the other Is the safety 3 SONS 07302,2 vent. On these oars. It Is necessary to remove the safety vent and Introduce the displacement air through that oonneotlon. Drawing No, 31-20848 shows In detail the dome of a tankoar with three connections. "A" Is the two inoh unloading line which extends to a small sump at the bottom of the car. "B" Is the one Inch air Inlet oonneotlon. "C" la the hooded safety vent. The oar dome oover with fitted bolts Is shown In the oenter. It Is fitted with a Oarlock 901 asbestos gasket or an ^Aluminum envelope Ooetze gasket. This drawing also shows a bottom opening In the oar. nils oan be opened only from the Inside of the oar and Its purpose Is for oleanlng operations. It has no use at all in unloading the oar. Drawing No. 31-26847 shows the over-all dimensions of the 8,000 gallon Aroclor tankcar. B. Procedure for Unloading the Cars The car should be spotted at an unloading dock similar to the one shown by Drawing No. 90-8178. The car must be level and the brakes set properly. "STOP-Tankoar Connected" signs should be placed fore and aft the car to warn switching crews. If It Is raining or snowing or the humidity Is extremely high. It Is not advisable to open the car. In case the oar must be sampled and opened during bad weather, a canvas canopy must be placed over the dome of the car. It is preferable to unload the cars under roof or Inside the factory. Unless It Is absolutely necessary because of following described situations 4 MCNS 073023 the dome cover should not be opened until ready for sampling. The dome cover is sealed with a standard railroad wire and seal, and Monsanto should be notified if this seal is foundbbroken upon receipt of the car. The first step In unloading Is to lnspeot the dome and clean around the dome cover to remove all loose dirt, water or snow. Wiping rags and a brush should be used to dean before the dome cover and connections are opened. Then, the screwed hood over the alr-lnlet 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 alr-lnlet valve opening and the temperature or the interior of the car determined. If the car temperature Is below the caution temperature Bhown In the following Table 1, It will be necessary to take the special step of inserting a "hair-pin" heating coll through the dome of the oar to preolude rupturing the tankcar seams during the heating period. Product A3TM Pour Point C. TemperatureC. Below which Caution Must Be Deed In Heating Aroclor 1260 Aroolor 1254 + 30 10 + 40 *! 20 Aroclor 1248 Aroclor 1242 Pyranol 1467 Pyranol 1470 Pyranol 1481 -7 +5 - 19 - 10 Pre-heating Is not required* Pre-heating Is not required* Pre-heating Is not required* Except If the material has cooled be&ow -10C. and crystals of scavenger have separated. Then, the material should be heated to 70C. (158P.) until complete solu tion has been accomplished. MONS 07302*1 If the dome of the oar Is to be ppened for the pre-heating operation. It Is necessary that It be covered with a dean canvas. Extreme oare must be taken to avoid getting dirt or moisture Into the oar. It Is due to the relatively hd&h viscosity of some of the Aroclors at low temperatures that it beoomes neoeasary to form a column of molten material from top to bottom of the car. In the oenter, to prevent hydraullo pressure bulld-up whloh may rupture the tank shell If there Is too rapid localized heating when employing the main steam oolls. When such pre-heating Is required, a satisfactory vent hole oan be made by inserting a "halr-pln" coll (1/9 inch diameter brass, galvanized, or stainless steel pipe) Into the open dome of the oar and Introducing steam through the coll until there Is a column of fluid Aroclor from top to bottom. After the vent hole Is melted through the material to the bottom of the oar, the "hair-pin" coll should be removed and the dome cover replaced and bolted. Steam Is then Introduced Into the main colls. It Is recommended that the Bteam pressure be limited to 100 pounds gauge pressure, particularly In the case where the colls are In direct oontaot with the Aroolor. The steam ooll outlet should be trapped or throttled with a valve. It will require eight to twenty hours to bring the material to pumping temperature - depending upon weather 6 SONS 073025 conditions. It Is essential that the air Inlet valve be open during the heating period In order to vent the tank. Some ealoulatlons have been made to Indicate the heat requirements for an Aroolor car. Data for an 8,000 gallon ear of Aroolor 125* are: Specific Gravity = 1.5 Speelflo Heat = 0.26 BTU/lb./'P. Heat requirement for heating Aroolor from 30*C. (86*F.) to 110*C. (230'F.) Is: 8000 x 1.5 x 8.33 x 0.26 x (230-86) - 3.77*,000 BTU. For heating from 30*C. (86#F.) to only 75*C. (167F.), the heat required Is 2,110,000 BTU. A nine horse power boiler operating at 80 pslg produces 263 lbs./hr. of steam with no reuBed oondensate. Returning condensate at 200F. will Increase the steam output to 296 lbs./ hr. at 80 pslg. In the first oase, heating to 110c., the over-all heat transfer oo-effiolent is assumed to be too low to utilize the 100$ oapaolty of the boiler. A value of 1500 for UA with an average T of 144'F. Indicates that the useable steam is 202,000 BTU/hr. or 226 lbs./hr. steam at 80 pslg. In the second oase the ^ T Is lower and the entire output of the boiler Is useable. Table II Bums up the approximate time calculated to heat Aroolor 125*. 7 MQNS 073026 TABLE II Nine HP Boiler Lbs. Steamer. 30-110*C. 30-75-C. 1000 cap.(no reused oondensate) 263 -- 9 Hrs. 750 cap.(no reused oondensate) -- 18 hrs.(86$cap) 12 Hrs. 1000 cap.(condensate 9 200*F.) 296 -- 8 Hrs. 750 oap.(oondensate s 200"F.) -- 18 hrs.(76cap) 11 Hrs. Calculations on a five horse power boiler give heating tines of the following order: Five HP Boiler Lbs.Steam/fcr. 30-110"c. 30-75*C. 1000 cap.(no reused oondensate) 1*6 28 hrs. 16 hrs. 1000 cap.(condensate 200*F.) 16* 25 hrs. 1* hrs. Aroolor oars can be heated by steam (80-100 pslg) to the proper handling temperatures in a reasonable time by uBlng a boiler source oapable of producing 200,000 to 300,000 BTU/hr. The times given here are approximate and will aot as a guide until experience shows the exact time for this operation. MCNS 073C23 8 The proper handling temperature for the various fluids Is given In the following Table III, which Indicates cor responding viscosity values: TABLE III Product Handling and Pumping Temperature C Approximate Viscosity, S.U.S Aroclor I860 95 - 130 100 - 43 Aroclor 1854 Aroolor 1848 Aroclor 1848 75 - 110 50 - 85 35 - 75 100 - 4a 100 - Uo 100 - 40 Pyranol l48l 30 - 75 100-40 Pyranol 1467 Pyranol 1470 80 - 55* 15 - 45* 100-40 100 - 40 *If any of the scavenger Is out of solution, then the material must be heated at 70C. (158 P.) until It has dissolved. Selection of pumping temperatures for any dleleotrlo not shown on this list or which may be developed In the future should be based on a vlsooslty of about 100 Saybolt universal Seconds for aversge pumping and about 40 S.U.S. for fast pumping. Whan the material has been heated to pumping temperature, a one-half Inch diameter pipe "cross" arrangement containing a pressure gauge, air Inlet, pressure relief valve to relieve at 30 PSIO, and vent connections, should be connected to the dome air Inlet pipe. Then the unloading line should be oonneoted. 9 aoas C7308S (At this point a sample is taken as described in Chapter 4,) Dry* air is then Introduced Into the tankoar and pressure built up to 15 pounds gauge. The two lnoh valve cock on the Btand pipe Is opened and the discharge pipe observed to be sure the liquid Is being uftloaded. To proteot the Beams In the tankoar, the pressure must not exceed 30 pounds. The car will begin to unload at about 12 pounds pressure, When the oar la empty, the air pressure will drop off rapidly and air will blow out of the vent on the reoelvlng tank. The air flow may be stopped at this point and the tankcar pres sure released through the vent valve on the .\sross" arrange ment. After Inspecting the car to be sure that It has been completely unloaded, all connections and dome cover should be dosed 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 dehumldlfylng unit suoh as soda lime, activated alumina or similar dehydrating agent drying unit. It may be necessary to reoharge the dehumldlfylng unit each time that a oar Is unloaded. For unloading a tankcar of Arodar within three hours, 15 standard oublo feet a minute of air at 15 pounds per square lnoh gauge pressure -arta -loop, 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. M. Kemp Mfg, Co., 405 E. Oliver Street, Baltimore 2, Maryland and Pittsburgh Lectrodryer Corporation, Foot of 32nd Street, Pittsburgh, Pennsylvania. 10 HONS 073029 step. It Is desired that a standard railroad wipe 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 be replaced as received. Adequate care should be taken In preparing and sealing the car for return shipment. Unloading with dry air as described Is the preferred and recommended procedure because It Is done with the car dome closed which avoids contamination. If the car Is unloaded by pumping out of the top, which required opening the dome. It 1b most desirable that the car be set Inside of a building. If this cannot be done, then, a canopy or roof should be provided over the oar dome, and the unloading should be done when the weather is clear. A centrifugal pump with minimum capacity of kO gpm. Is suggested. It will be necessary to prime the pump and only dean Askarel should be used to do this. Another method for priming the pump Is to use a Penberthy steam Jet, No. 22* available from Penberthy Injector Co., 124a Holden Ave., Detroit 2, Michigan. ^____ If a flexible unloading line Is used. It should be e flexible metallic hose. Rubber hose must not be used. 11 HONS 073030 C. Drum Packaging ' Drum paokaglng Is made with new and carefully Inspected 55-gallon drums. Itoese Bteel drums are lined with a specially seleoted baked phenolic coating. An example Is NESCO No. 3 lining offered by the National Enameling and Stamping Company, Long Island, New Tork. contents of the drums should not be heated by dlreot application of flame or strip heaters. Radiant heat from steam colls or hot air in a heated room Is to be pre ferred. The screw plug In the drum head Is fitted with a metal oap as a safe guard against tampering. 12 MENS 073031 CHAPTER 2 STORAGE TAKES A. General Description The Btorage banka should be a minimum of 10,000 gallons and preferably 12,000 to 15,000 gallons capacity to accommodate the normal 8,000 gallon tankoars. It Is preferable to locate the tanks above ground where they are easily accessible for any ohanges or repairs. Under ground looatlon presents difficulty In this respect. Especially in cold climates. It Is preferable to locate the tanks Inside of a building. The tanks should be located conveniently with reference to the tankcar unloading facilities and the area where the dielectric Is used. Although Aroclors are non-oorroslve to metals, oorroalon or rusting of Iron and steel equipment (by oxidation) may occur resulting In contamination of the produots. The resis tance of Aroclors to materials of construction is given in Monsanto Technical Bulletlon O-P-115, entitled, "The Aroclors," Page 6. Stainless steel tankB are very satisfactory but relatively expensive. Stainless steel pipe Is relatively difficult to fabricate and It la difficult to make tight leak-proof connec tions. Storage tanks may be of steel construction If properly metallized with zlnc-tln or aluminum on the Interior surfaces 13 SONS C73032 coming In oontaot with the Aroclors. The metallizing should be done according to the following procedure: 1. Clean an area of the surface by sand blasting, or a similar method, to give a perfectly clean and roughened surface. The area oleaned should not be greater than can be completely metallized within a few hourB after cleaning. 2. If zlnc-tln metallizing Is used, a coating of zinc 0.005 Inches thiok should be sprayed on to the cleaned surfaoe. This is followed Immediately by a coating of tin 0.007 Inches thick. 3. Aluminum metallized surfacing should be about 0.01 Inch thick. The detailed procedure for metallizing and cleaning is outlined as follows: a) Sand blast, b) Coat with iron, 0.005 Inches thick. (The purpose of this coating 1b to provide a rougher and better bond for the finish coat of aluminum or the zlnc-tln combination.) o) Apply the seleoted 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 dlreotly onto the metallized surfaoe of the tank.) e) Drain the tank, f) Fill with cold water andfraln. 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 the tank, allow It to cool and pull dry air through It using a dehumldlfylng breather In the air line, heat again etc. until the tank Is full of comparatively dry air. 1) Spray about 100 gallons of new, electrical grade Aroclor (not high 14 MCNS 073033 In vlsoosity) or electrloal grade trlchlorobensene onto the Inner walla of the tank, washing the walla thoroughly (avoid breathing any fumes). J) Attaoh the circulating pump, the llnea used, and the filter preaa fitted with dry paper and cir culate the fluid through the ayatem and the tank. Inatall new dry filter paper several times In the preaa during this dry ing and cleaning operation. Discard the dlelectrlo fluid used for cleaning, k) Partially fill the tank with new Aroelor dleleotrlo and analyse It eleotrleally and ohemlcally to de termine whether It meets speciflcatlona. If all teats are met, then fill the tank with the dleleotrlo. The tanka should be Insulated using, preferably; glass foam beads as supplied by Dow-Cornlng or Llbby-Owens-Ford. The suggested thickness of the glass Insulation Is one Inch mini mum to two inches maximum. The glass Insulation may be covered with tar material commonly used for weatherproofing. Another type of Insulation which may be used Instead of the glass Is 8556 Magnesia-Wool which should be oovered also with the weather proofing tar. The advantage of the glass insulation Is that It Is not moisture sensitive as 1b the case with Magnesia-Wool. If the storage tank 1b located outdoors. It Is best that the Insulation be oovered with riveted or bolted tin sheeting painted with aluminum paint. This type- of metal surfaoe weathers well and Is cleaned easily. All piping must be gal vanised and sorewed fittings must be back brazed to assure 15 SONS G73034 ' I tightness. All handling pipe lines must be traced with steam I lines and Insulation applied over the two lines In order to keep the handling lines and the material up to the desired I pumping temperature. Usually a one-fourth Inch copper steam r line running parallel with the handling line will suffloe. e Under very severe conditions of low temperatures. It would be desirable to wind the steam line around the handling line e about two turns to the foot. i the tanks must be provided with ample pressurized heating B coll surface to Bupply sufficient heat to the material to bring B It to the proper temperature for pumping and handling as Indi cated In Table III. Heating colls should be either metallized P steel, or preferably steel colls which have been galvanized b after fabrication. It 1b recommended that the steam pressure on all heating colls should not exceed 100 pounds per square p lnoh gauge; lower pressures may be used where practicable. t It Is essential that all steam oollB be completely free from even minute leaks since thlB will Introduce water Into the 0 product. 0 The steam colls may be Introduced as "halr-pln" colls through a manhole at the side and bottom of the tank, or as 1 Is most often done. Inserted through the manhole at the top I of the tankrand then looated 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 colls, 16 073C35 The storage tanks may be fitted with a stirrer, either through the top, side, or bottom of the tank and the propeller blade should be located near the bottom of the tank. However, insertion of a stirrer through the Bide offers possible source of a leak and since these materials are homogeneous, it is not essential to provide such agitation for the purpose of mixing. Adequate circulation can also be accomplished by using a centrifugal type pump. Gear pumps or other equipment where wear or chipping of metal parts may introduce contamination should not be used. The pumps must be of the type designed to handle hot oil. All wetted pump partB should be either stainless steel or bronze. The centrifugal pumps must be provided with a deep stuffing box and proper packing used, as described in Chapter 3. As examples of pumps found com pletely satisfactory for thlB service, reference is made to Worthington Worthlte pumps. Blaokmer pumps, and Dayton Dowd Type C pumps for handling hot oil. Also, a very satisfactory arrangement for mixing or circulating and pumping the fluid from the storage tank is to use a vertical sump pump such as a Taber pump. All storage tanks must be amply provided with a dehumldlfylng breather such as soda lime, activated alumina, etc., units. This is essential to prevent moist air from coming in oontact with the dlelectrlo. A moisture content above 35 ppm 17 SONS C73036 adverse!/ affects the electrical resistivity of these pro ducts. Provision should be made to preclude possible leakage df the drier material back into the storage tank and the drier should be Inspected periodically to make sure that It Is open and not plugged. B. Detailed Description Drawing Ho. 9C-8170 shows the detailed construction of a horizontal 15*000 gallon Btorage tank for Aroolor and its mixtures whloh has been found completely satisfactory. The various nozzleB on this tank are used as follows, con sidering them In order from left to right on the drawing: 3" nozzle Inlet for reolrculatlon 24" nozzle For future agitator lfzequlred (not used) 3" nozzle For soda lime or oalclum ohlorlde breather connection 36" manhole For Inspection, etc. The float gauge Is located In the center of this manhole. 3" nozzle Hot UBSd 24" nozzle For future agitator If required (not used) 3" nozzle Hot used 3" nozzle 18" X 26" Oval Nozzle Filling Inlet oonneotlon For sump pump 3" nozzle For thermometer well (see detail) The two 24" nozzles were originally Installed for Installa tion of agitators. If required. However, It has been found 18 HONS 073037 unnecessary to use agitators in the storage tanks, and these nozsles could be omitted. It has been found that circulation of the fluid by the sump pump, and Into the nozzle at the opposite end of the tank, for several hours gives satisfactory blending of the tank contents. Por pumping the dielectric from the storage tank, a "Taber Pump Co. all bronze 2-1/2" X 2" vertical sump pump with monel shaft has been found to be quite satslfaotory for the applica tion. The liquid level gauge used In the storage must be gastight. The storage tanks are equipped with Vapor Recovery Systems Co.'s "Varec," gas-tight, automatic tank gauge as shown by Drawing Mo. 9C-8278. The storage tanks should be provided with an operating plat form suitable to the customer's conditions of operation. The dehumldlfylng units used as breathers on the storage tanks can be constructed as shown by Drawing No. 90-8248. The upper portion of the chamber Is charged with anhydrous soda lime or another drying agent. Periodic Inspection of the drying agent will show the formation of a oake 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 No. 90-8248 may be used for the breather units. Drawing No. D-13362 shows design detail of a 15,000 gallon 19 MQNS 073036 vertloal storage tank. Hie vertical type tank would seem especially desirable when Insufficient space Is available to accommodate the horizontal type tank. 20 MCNS 073C39 CHAPTER 3 QASKETIM3 AND POMP PACKING Aroclors and their mixtures soften and swell natural rubber and many of the synthetic "rubber" materials. Such material not reoommended for use, lnolude Hyoar P, Koroseal, Perbunan, Neoprene, eto. These materials are known sources of contami nation. Suggested types of packing and gasketing materials Include: 1. For Welded Flanged Pipe Connections: Carlook Packing Co., No. 901 or No. 7021, 1/8 Inch asbestos fiber sheet. A ring of thin aluminum drawn tightly at the flange conneotloos may be used satisfactorily also. 2. For Pumps: Oarlock NO. 234, No. 431, and Cheveron No. 7050-C are satisfactory packings. Likewise, Durametalllo's spiral asbestos fiber may be used. Johns-Manvllle and others have comparable packing materials. 3. For Valves: Oarlock No. 117 braided packing or Its equivalent Is suggested. 4. Other Resistant Materials: It Is Indicated that duPont's Teflon, poly tetrafluoroethylene Is not attacked by hot (l30c.) Aroolor and Is to be recom mended as a gasket material. Dow-Cornlng's Sllaatlo, Silicone 160, Is very resistant to Aroclor and Is suggested for gasket purposes. 5. In boom cases cork Impregnated under pressure with Chrysler's Cycloweld 55-9 or Armstrong Cork Co.'s 1162-J and cured at 170C. may be used as a gasket material. These are baked phenolic type coatings. 6. Pipe Thread Compounds: When necessary to use pipe tnread compounds, the following should be satisfac tory If care Is taken to prevent the pipe oompound from getting on the Inside of the pipe. (a) Plastic Lead Seal--manufactured by Durametallic Corp. (b) Ordinary white lead . 21 SONS C73040 Usually It Is not necessary 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 HONS 073041 CHAPTER 4 SAMPLING METHODS 1.) The ASTM Standard Method for sampling electrical Insulating oils Is described In ASTM Designation: D923-49. This describes glass and metal thlefs for sampling drums, cans, and tankoars. A specially designed thief or bomb for sampling tankcars Is described, also. A very good Instrument of this type Is the stainless-steel Baoon Bomb Thief with which samples of the liquid can be drawn from any level of the tankcar. The ASTM procedure describes sample containers, their oleaning 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 bb the surrounding air, because cold oil may oondense 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 oholoe, as it may be neoessary to procure samples from a tankcar when the temperature Is not above the surrounding air. On suoh 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 peroent, and samples shall never be taken In the rain." S3 MOMS 073042 At the plants of several eleotrloal manufacturers using Aroclor dleleotrlcs, the praotlce Is to switch the tanlccars directly Into the plant building or under roof before sampling and unloading. These precautions In handling are taken to avoid any contamination of the fluids which are manufactured under very strict specifications. For example, the specification for lonlzable chlorides allows no more than 0.10 parts per million. Moisture may not exceed 30 to 33 parts per million. Tankcars are oleaned and prepared under close Inspection before they are filled. When filled, and analysis shows the material In the oar 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 tankcars have been unloaded In the Industry, It Is requested that the dome fittings should be sealed with a railroad wire and seal. 2.) Monsanto Methods used for sampling tankcars differ somewhat from the ASTM procedure. The modified techniques are used because of their greater simplicity and they have been entirely satisfactory as employed over many years. A sample Is never taken when It Is raining or snowing or when there Is any chance of contaminated atmosphere moving in the dlreotlon of the car. However, in oase of an emergency, during Inclement weather, a oanopy Is plaoed over the car dome before sampling. 24 MCNS 073043 A satisfactory sample bottls Is a five pint, round amber glass, paoker type oontalner fitted with a 38 millimeter Beke- llte sorew cap with an aluminum or tin oup liner. Bottles of this description oan be purchased from the Northwestern Bottle Company, 3144 North Broadway, St. Louis, Missouri aooording to their No. A-7253. Only new bottles and oaps are used, when a shipment of bottles Is reoelved, the bottles are capped immediately and stored in their receiving oartons, prior to use, the exterior of the bottles Is wiped with a clean doth. The simplest sampling devloe used Is a clean stainless steel or aluminum dipper. However, this Is not a generally preferred device because It permits sampling the oar from the near surface, only. The sampling devloe oommonly used consists of a stainless steel tube, seven feet long with one end bent Into a hook, to serve as a handle and on the other end there Is a stainless steel buaket with a perforated bottom. This buoket Is about 5-1/4 lnohes Inside diameter and 6 inches deep to hold the five pint bottle. This bottle Is held firmly by a stainless steel collar made to slide along the shaft of the sampling devloe. This oollar has a damp attachment for fixing It tightly Into plaoe where desired around the neck of the bottle. When a oar la to be sampled, a new sample bottle Is damped firmly In the buoket. All dirt la brushed and wiped away from the car dome ares using a dean rag. , -25- BONS 073044 The car dome la opened and the cap la then removed from the sample bottle. The sampling device la Inserted into the oar so that the neck or the bottle Is at least twelve to eighteen inches below the surface of the fluid. The sample taken Is dis carded as Its purpose Is to rinse the bottle. A portion of the sample 1b used to rinse the Interior of the bottle oap. This procedure Is repeated until a minimum of three rinses has been made; each time the sample'taken Is not put back Into the oar. These rinses should be discarded. Then the sample Is taken and the oap of the bottle Is screwed down tightly. When the sample has been obtained, the car dome lsireplaced, Immediately. The exterior of the sample bottle Is wiped with a clean doth and when returned to the laboratory it Is further clean ed with a cloth dampened with pure trlohlorobenzene. If the sample Is to be shipped, the cap Is taped with Sootch Tape. The sampling device Is also cleaned with pure trichloro benzene and Is stored In a duet free, air condltlofledroora. 3.) Drum Sampling. A glass thief, thoroughly cleaned with pure trlohlorobenzene and dried Is used to sample drums.* 26 *CHS 0 7304S CHAPTER 5 LABORATORY ANALYSIS AND PROCEDURE POR TREATINO AHOCLORS AND THEIR MIXTURES WITH EARTH A sample of the Aroelor or Aroolor mixture taken from the tankoar, or druma, as described In Chapter 4, Is analyzed In the laboratory to determine Its quality In accordance with the property values given In Chapter 7. For oapacltor use, usually the important properties tested are resistivity, power factor, chlorides, and moisture. Por transformer use dielectric strength, resistivity, moisture, and ohlorldea are the Important properties. If the sample Is out of line with the shipping specifica tions, It Is lndloated that the sample has become contaminated. In this case, another sample is to be taken and the properties redetermined. If still out of specifications, the sample should be given treatment with earth. Treatment of the dielectric with conditioned Attapulgus earth will bring the eleotrloal properties to the maximum attainable values. While there Is complete agreement on the benefits derived from treating with conditioned earth, there Is difference of opinion on details of the method, arising from factors such as the following. No doubt, there are differences In the absorbent power of various types of dlatomaoeous earth with respeot to removing moisture. Impurities and additives such as stabilizers or scavengers from the dielectric 87 MOhS 073046 materials. The alee of the earth particles, temperature and oondltlona of activation of the earth, the concentrations used and the temperature, the degree of agitation and time Interval at whloh the dleleotrlc la given earth treatment are all possible variables which are still being studied In various laboratories. The method used by Monsanto for treating the fluid with activated earth In the laboratory Is: The absorbent Is minus 200 mesh Attapulgus* earth 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 Eleotrodes, O.E. Cell and Accessories". The flask or beaker Is fitted with a glass or stainless steel agitator. Heat is applied using either a hot plate or a Olas-Col mantle and Is controlled by a thermostat such as a Penwal thermo switch with a stainless steel sheath. About 0.1 to 0.2$ of the activated earth, based on the weight;of\.the liquid Is added. Attapulgus Division, Minerals te Chemicals Corp. of Amerloa, 210 West Washington Square, Philadelphia 5, Pennsylvania 28 SONS 073047 The more vlacoue dlelectrlos such aa Aroolora 1248 and 1254 are heated at about 70 to 80C. (1580 . 176P.) and the leas vlaoous materials suoh aa Aroclor 1242 and Pyranola 1481, 1467* and 1470 are heated at about 50 to 60 c. (122 to 140P.). After heating and atlrrlng the sample for about four hours. It 1b filtered using a clean Pyrex glass suotlon flask and a buohner funnel fitted with a Whatman No. 1 or No. 3 filter paper. This apparatus and the bottle Into which the treated sample of dielectric Is transferred should have been cleaned In a manner similar to the oleanlng procedure de scribed In Chapter 6. The earth treated and "up-graded" sample Is then ready for final analysis of Its eleotrloal properties. 29 SONS 073046 CHAPTER 6 TEST PROCEDURES A. General Information The Monsanto test methods desorlbed here with the special equipment used are some of the control tests employed to main tain the quality of Aroolors for dielectric use. They are suggested as a guide for test work needed to lndloate the quality of the dielectrics used In the manufacture of electrloal goods. The most significant eleotrloal tests made on Aroclors for oapaoltors are: 1. Dleleotrlc constant. 2. Power Paotor. 3. Resistivity. For transformer use the most significant tests of Aroclor mixtures are: 1. Dleleotrlc Strength. 2i Resistivity. In both oases a significant ohemloal test Is corrosion chlorides. The following terms are defined: Dielectric Constant: The dleleotrlc oonstant (sometimes called spec If18 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 SONS 0 73049 dielectric to the oapacitance when there is a vaovium between the conductors (for all practical purposes air at ordinary pressures may be used Instead of a vacuum). Dielectrio Strength: Dielectric Strength is the rupturing strength of an Insulating material when subjected to voltage stress under speclflo conditions and expressed In kilovolts. Breakdown varies with the shape of the electrodes and does not Increase directly In proportion to the thickness of the dielectric. Power Paotor: The power factor 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 ohmscentlmeter of an oil Is the ratio of the d-c potential gradient In volts per centimeter paralleling the ourrent flow within the sample, to the current density In amperes per square oentlmeter at a given Instant of time and under prescribed conditions. Volume resistivity Is expressed In ohm-cm. The analytical procedures described In detail Include; 1. METHOD HO. 11,751, "PROCEDURE FOR CLEANING OF ELECTRODES, O.E. CEDE AND ACCESSORIES." 2. METHOD NO. 11,608, "DIELECTRIC CONSTANT AND POWER FACTOR." 31 MOMS 073050 3. METHOD NO. 11.605. "DIELECTRIC STRENGTH." 4. METHOD NO. 11,607, "RESISTIVITY." 5. METHOD NO. 10,126, "CORROSION AND CHEMICAL STABILITY." 6. METHOD NO. 10,118, "INORaANIC 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. "PROCEDURE FOR CLEANINQ OF ELEC TRODES, O.E. Cell and Aooessorles. a. The Eleotrode Cleaning Procedure: 1) Plaoe the electrodes In hot eleotrloal grade Trlohlorobenzene for ten minutes. 2) Wash with unheated TCB. 3) Rinse twice with methanol and twloe with tap water. 4) Plaoe the eleotrodes In hot \0% Trl Sodium Phosphate solution. 3oak and heat for ten minutes. 5) Wash thoroughly with''.tap water. CAUTION: After Step 5-- DO NOT TOUCH THE ELECTRODES WITH HANDS! 6) Wash with distilled water twice. 7) Dry In drying oven for at leaBt two hours at 120C. b. The O.E. Cell Cleaning: 1) Reolean the cell before use, when more than 8 hours have elapeed since the previous cleaning. 2) Follow the procedure for the electrodes starting at Step 4. 32 MCNS 073051 0. Cleaning of the Accessories: 1) Apply the same cleaning procedure as given for the electrodes (Steps 1 to 7) to prepare the glass spacer and beaker for next test. 2) Clean the thermometer In the same manner as the electrodes, except for Step 7. 3) Place the wet thermometer (after Step 6) dlreotly In position In the temperature Heating Unit (Modified Fisher Isotemp Oven) and allow to dry. METHOD NO. 11,608. "DIELECTRIC CONSTANT AND POWER FACTOR." 1. Apparatus A. Oscilloscope: Heathklt Model 0-6. B. Constant Temperature Heating Unit: Fisher Isotemp oven. Model 13-245A, modified to Include inter wall oonneotors, 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. Capaoltance Bridge: General Radio Co. Capacitance Bridge type 716-C. F. Test Cells: O.E. type, concentric cylinder eleotrodee Catalog #1,559.663. 0. Class B driver transformer: This 1b used for 60 oyole measurements to excite the bridge directly from the domestic power line. It has 50 volts output with a 4800 ohm resistor In service. H. Tuned Clroult Filters: General Radio Type 1231-P* (400 and 1000 oycle) and 1231-P3 (60 cycle). These filters aid In obtaining a more accurate frequency for the measurements by removing harmonics, noise, hum, etc. 33 MQNS C 73052 II Adjustment of Controls on Eleotrloal Apparatus A. On Panel Wo. 1 (Top Panel, Amplifier and Hull Detector) a. Turn the 4-way (main power) switch on the upper right hand side to the #3 position to determine the Dleleotrlo Constant at 1000 cycles. Turn this switch to the #2 position for measurements a to oycISs. b. Allow the equipment to warm up 10 minutes. 0. Turn "OAIN CONTROL" to 6. d. Depress "INPUT 0.03V." button. B. On Panel No, 2 (Oscilloscope) a. Turn "INTBN." to about the 12 o'clock position. CAPTIONt 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" oontrols center the Image on the screen. c. Adjust "FOCUS" for sharp line. d. Turn "FREQ. SELECTOR" to LOOKC. e. Turn "FREQ. VERNIER" to 80. f. Turn "VERTICAL OAIN" to 5. g. Turn "VERTICAL INPUT" tO "10 VOLT MAX.". h. Turn "HORIZONTAL OAIN" to about 20. 1. Turn "SYNCHRONIZING" to + 20. J. Turn "SYN." to "EXT. SYN." k. Turn "OEN." to "SWEEP OEN." 34 MGNS 073053 C. On Panel Mo. 3 (Capacitance Bridge) a. Turn "RANGE SELECTOR" switch to "100 C" for 60 oyole measurements and to "1 Kc" for 1000 cycle measurements. b. Turn "METHOD SWITCH" to direct. o. Turn "DISSIPATION FACTOR" selector switch to "0". T. On Panel Mo. A (osolllator) a. Disregard this panel for measurements at 60 oyoles. b. On 1000 cyole measurements, depress the No. 10 "MUI/TIPLY BY" button. . 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 Paotor. III. Determination of Constants for the Apparatus 1. Carefully assemble the cell which has been cleaned and dried within the last 8 hours. Refer to Method NO. 11,751 for the procedure to use In oleanlng the oelis. 2. Plaoe the cell assembly in the Fisher oven whloh 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 MONS 073054 4. Connect the cable from the capacitance bridge to the terminals on top of the oven ao that the Inner wire of the oable goes to the bade terminal and the outside mesh casing of the cable (the ground) goes to the front terminal. 5. Remove the thermometer from the top of the oven before going on with the test. TCTs~Ta important. 6. Make all adjustments on the eleotrlcal apparatus as dlreoted In Part I of thlB method. 7. Balance the bridge by rotating the "CAPACITANCE" and "DISSIPATION FACTOR" dials on Panel No, 3 until the wide vertical band on the oscllllscope Is adjusted to a minimum width. 8. Reoord the sum of the readings on the "CAPACITANCE" dial and vernier and call this value A. 9. Remove the beaker containing the cell from the oven and fill it with C.P. benzene, to a level 0.737 Inches (ca.3/4 Inch) above the top of the eonoentrlc cylinders of the oell. 10. Adjust the temperature of the benzene to 25C. while stirring with a thermometer. 11. Replaoe the oell In the oven (at 25C.) and make the same eleotrlcal connections as In Steps 3 and 4. DO NOT Interchange connections. 12'.. Balanoe the bridge again as In Step 7. 13. Reoord the sum of the readings on the "CAPACITANCE" dial and vernier and oall this value B. 14. Calculate the oell constant by the following equations Cell Constant, K B - A (this Is usually 2.27 u l.o around 70 mmfd.) 15. Remove the oell from the oven and balanoe the bridge as In Step 7 with the "CAPACITANCE" and "DISSIPATION" "FACTOR" dials. 3f MGNS 073055 16. Record the sum of the readings on the "CAPACITANCE" dial and vernier..and call this value F, (capacitance of oonneotlng oable.) ~ 17. Caloulate the CELL LEAD CAPACITANCE by the following equation: CELL LEAD CAPACITANCE, 0 . A -F - K (this Is ~ usually around 3 mmfd.) WHERE: A : CAPACITANCE OF ENTIRE SYSTEM IN AIR (SYSTEM CONSTANT) 0 > CAPACITANCE OP THE CELL LEADS (CELL LEAD CONSTANT) F - CAPACITANCE Of CABLE AND WIRES WHICH CONNECT THE CELL AND CELL LEADS TO THE BRIDGE. (CONNECTOR CONSTANT) K . CAPACITANCE OF THE CELL ALONE (THE CELL CONSTANT) Tabulate the system Constant (A), the Cell Lead Con stant (0). the Connector Constant (F), and the Cell Constant (K) on a piece of stiff paper and post them near the instrument Where they can be easlly?referrsd to for comparison and calculations. These constants must be oheoked at least once every three montho and In all cases where the Dielectric Constant and/or Power Faotor are out of specification. Measurement of Dleleotrlo Constant and Power Factor on Ardolors. pyranols, Inerteens, and Trl-Jetraohiorobensene Blends. A. Test Run on Cell to Determine whether It Is Clean and properly Aligned. 1. Carefully assemble a cell which has been cleaned and dried within the past 8 hours. 36a MGNS C 73056 NOTE: Refer to method No. 11.751 for procedure to use in cleaning oells. 2. Adjust the oven control to hold at a temperature of 100C. for all materials except Trl-Tetra Blends. If a Trl-Tetra blend Is to be tested, adjust the oven to hold a temperature of 25C. 3. Plaoe the empty cell assembly In the oven and oonneot the back wire lnalde the oven to the lead on the lnner~cyllnder of the oell. and connect the other1 (front) 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 oable goes to the back terminal and the outside metal casing (ground)goes to the front terminal. 5. Allow 15 minutes for the oell to reach temperature equilibrium Inside the oven. 6. Remove the thermometer from the top of the oven before taking any measurements on the bridge. This is Important. 7. Hake 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 oeollloscope screen Is adjusted to a minimum width. 9. Record the sum of the readings on the "CAPACITANCE" dial and vernier and oompare this value with the SYSTEM CONSTANT determined In Part II of this method. IMPORTANT! If the value obtained In Step 9 does not agree with the System Constant A (Part II) within 5 uuf, the cell must be re-cleaned, re-drled, re-assembled, and the test run for the System Constant must be repeated. NOTO: Although the above test run must be made prior to eaoh analysis, the value obtained In Step 9 Is not to be used In calculations but Is to be used only as a~oheck on the cleanliness and alignment of the ceil. 37 HONS 073057 B. Procedure for Testing Materials 10. Remove the oell from the oven and fill the beaker with the material to be tested to a level O.737 , Inches (ca 3/4 Inch) above the cylinders of the oell. 11. Adjust the temperature of the sample to 100C. (use hot plate) for all materials exoept Trl-Tetra blends. For Trl-Tetra blends, adjust the tempera ture of the sample to 25C. uBlng an Ice-water bath If neoesaary. NOTE; Stir sample continuously with a thermometer while adjusting the temperature. 12. Place the oell and sample In the oven and make the aaae oonneotlons from the oell to the bridge as In Steps 3 and 4. DO MOT Interchange oonneotlons. 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 1b important. 13. Make the adjustment of oontrols on the electrloal apparatus as directed In Part I of this method. 16. Balanoe the bridge by rotating the "CAPACITANCE" and "DISSIPATION PACTOR" dials on Panel No. 3 until the wide vertloal band on the osolllosoope screen Is adjusted to a minimum width. 17. Reoord the sum of the readings on the "CAPACITANCE" dial and vernier, and oall this value X. 18. Reoord the sum of the readings on the "DISSIPATION FACTOR" dial and switoh. Call this value D. Calculations> Dleleotrlc Constant X-9-0 ------ K------ Where; X s Capaoltanoe reading from Step 17. F Connector Constant (Determined in Part II) 0 .Cell Lead Constant (Determined In Part II) K - Cell Constant (Determined In Part II) . 38 MUNS 073058 When assembling this booklet, a mistake was noted In the num bering of the pages. No 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 MGNS 013059 # Power Factor f x D ~^6 Where: f m Teat Frequency (60 cycles or 1000 cyolea) f0 Frequency of "Range Selector" on Panel Ho. 3 D Dissipation Factor reading from Step 18. NOTE: When D (dissipation faotor) Is lesB than 0.1, the dissipation and power factors differ by less than 0.0005. Therefore, for our measurements, power faotors and dissipation faotors are equal. Precision: (Reference: Oeneral Radio Manual for Model 716-C Capacitance Bridge) a. Capaoltance readings are preolse to i 2 mmfd. x mul tiplier reading (i 0.2# of full scale for each range) when the dissipation faotor Is less than 0.01. b. Dissipation Faotor (power Faotor) readings are pre cise to i 0.0005 or 1 2# of the dial reading which ever Is larger, for values lesB than 0.1 for D (Dissipation Factor). 3. METHOD HO. 11,605, "DIELECTRIC SIRENOTH." a. Apparatus and oeneral Information The eleotrlcal equipment necessary to provide high voltage to permit the determination of dleleotrlc strength of liquid dlelectrlo at commercial power frequencies Is basloally quite simple. The equipment assembled In the laboratory oonslsts of a high voltage transformer of good design and with a ourrent capacity of 2.43 KVA and with equip ment for control Of the voltage and a means of measuring the voltage and to provide safety for the operator. 40 HONS 073060 It 1b 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 compiled with. The door on rear of cabinet must be dosed. The cover over the oil must be all the way down and the voltage oontrol must be at 0 position. Pallure to comply with these requirements will prevent any action when the red button Is depressed. The test cup* Transformers, Voltmeters, and Accessories The askarel testing oup type No. 224809 supplied by Oeneral Eleotrlo Company Is mounted on the top rear of the oablnet. It Is protected by a heavy plastic oover, hinged at the rear for accessibility to the receptlcal. It Is equipped with safety contactor so placed that the circuit energising the high voltage oontaotor cannot be completed unless the protective oover Is completely lowered and In place. It Is Impossible for the operator or anyone else to touch the testing cup when high voltage Is applied. 4l WCNS 0730b1 The High Voltage Transformer manufactured by the Kelly-Koett Manufacturing Co. la of the closed core, oil Immersed, Bhell type design. Rated 9 81,000 volt 9 40 mlllaapers. It was recovered from a used X-ray machine, purchased quite Inexpensively. An auto transformer from the same X-tay 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 cf a 2-1/2 KVA poweratat variable auto transformer supplied by the Superior Electric Company. Power to the powerstat Is controlled by a 4 con tact 30 amp. solenoid circuit breaker. The voltmeter mounted on top near front edge Is connected across the powerstat secondary and Is calibrated to read directly In Kilovolts in the range of 0 - 50 K.V. The overload clroult breaker consists of a small relay connected between one Bide of the high voltage transformer secondary center tap and 42 SONS 073062 ground. It 1b adjusted to break contact on a current drain of about 50 mllliampers. The circuit for the ooll of the Bolenold circuit breaker la wired through the contaots of this relay. Safety and Operating Controla 1) Door Interlock awltoh located on rear door. 2) Test cup cover Interlock switch. 3) Powerstat awltoh mounted on rear of unit arranged ao that high voltage contactor cannot be closed unless powerstat is at zero position. 4) Main power switch on front panel 5) Powerstat voltage control on front panel. 6) High voltage oontaator 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 (4 0.5)C. NOTE; Testing at other temperature Is likely to give variable results whloh may be misleading. 2) Shake the sample container so as to thoroughly mix the askarel before filling the test cup. NOTEi This operation Is especially Important with used Aroclor as the Impurities may settle to the bottom and the test may be misleading. 3) Rinse the testing cup three times with small portions of the sample to be tested. 43 HONS 073063 4) Immediately after final rinse, fill the oup to a height of not less than 20 mm. (0.787 In.) above the top of the dectrodea. 5) Rook the cup a few times In order that any entrapped air may escape. Close cover over oil test oup. 6) Allow to stand 3 minutes, CAUTION: THIS IS IMPORTANT. ----------- 7) Turn main toggle switch on front panel to "ON" (or up) position. Both green and amber pilot lights on the top at either side of the voltmeter will now glow. NOTE: The green signal light Is connected aoross the 115 volt ln-put and denotes that line voltage has been applied to operating control circuit. Amber light Is connected In series with sensitive switch located under high voltage oontactors and connected to Its armature. It Indicates that high voltage contactor Is In Its rest position and away from oontaots energizing auto transformer, 8) Turn voltage control (large knob on front) to extreme counter-clockwise position. 9) Depress red button on front. This energises high voltage transformer and olrcult breaker and is lndloated by amber light going out and the red light dlreotiy over voltmeter will light; ^ 10) Watch the voltmeter and, while holding the button "IN", turn the voltage control at such speed that will cause voltage as lndloated on1voltmeter to 'rise at a fate of 3 K.V. per second. 11) Note and Record the voltmeter reading at breakdown. 44 MO ItS 073064 IS) Repeat the teat until two successive break downs occur on each of two fllllngB of the teat cup which do not differ by more than 10J<. Report the average value of these two readings (Step IS) as the Dleleotrle Strength, if the limit of the Instrument la readied before breakdown. report the Dielectric Strength as 50 K.v. at 25C. Cleaning of the test cup; After the test Is completed, drain the oup. Flush the oup with benzene. Then fill with Aroolor 1248 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 cleaned with benzene and carbon tetrachloride before and after running the test. The electrodes: The testing oup has two electrodes. Both electrodes are movable and have twenty threads to the lnoh with index notches on both the electrodes and the look nuts. To set the flap: Arrange one of the electrodes and the look nuts with the index marks In line. Hove the other elec trode until It oomes In firm contact with the first electrode and lock It, 45 HONS 073065 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 teat cup free of carbon coating: The following ASTM method of cleaning 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. CAPTION: It Is Important to avoid touching the electrodes with the finger or with portion of the tissue paper whloh has been In oontaot with hands. Rlnae the electrodes and oup with dry lead-free gaso line, Stoddatf Solvent (or dry, waterwhlte Kerosene) until they are entirely clean. Care should be taken not to touch the electrodes or the Inside of the cup after oleanlng so as to avoid possible contamination. 46 HONS 073066 I*. METHOD NO. 11,607. "RESISTIVITY. " a. Apparatus: Qeneral Radio Company Megohm Bridge Type 544-B. This la 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 aocuracy of the Instrument In the range en countered In the measurement of Aroclor resis tivity, 100 to 1000 megohm Is 4 &$, 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 6-1/2" wide, 22-1/2" long and 8" high. Approximate weight--26 pounds. 47 MCNS 013061 Teat Eleotrodes: Two concentric nickel cylinders with feet, obtained from General Electric Company. The Inner electrode .has outside diameter of 2.8" and a height of 3.25" with area of 184 sq. cm. The outer electrode has an Inside diameter of 3" and a height of 3.25" with area of 198 sq. cm. The distance between electrodes is, therefore, 0.1" or 0.254 cm. By theory, electrode constant (K) area/length Is 191/0.254 or 752 where average area is 191 sq. cm. Also K 36 x 10" x C (farads with air as dielectric) or 11.29 x C (nmfd. with air as dielectric). Glass Plate; Pyrex about 3-1/2" diameter with concentric grooves to assist In spacing electrodes. Obtained from General Electric Company. Heating Unit: Assembled in the laboratory and Is the same unit described In Dielectric Constant Apparatus (see Method Mo. ll,608j Equipment). b. Procedure: l) Assemble the teat cell. Place the recently cleaned (within the last 8 hours--see Method Mo. 11,751, Step 9) electrodes In an 800 ml. beaker. j*e MOMS 073068 2) Measure the capacitance of the test eell (cc) according to Method Ho. 11,608 (Dielectric Constant and Power Factor Measurements.) 3) Pill the cell assembly until the liquid level Is 3/4 Inch above the top of the electrodes. 4) Heat the assembly on the hot plate to 100 ( 0.5)c. 5) Plaoe the assembly Inside of the testing oven. 6) Attach top lead ( + ) on the megohm bridge to Inner electrode. 7) Attach other lead to outer electrode. 8) Throw the three switches at the top of the megohm bridge to "ON" position. 9) Allow 10 minutes for assembly to reaoh temperature equilibrium inside the oven. DANGER) Make sure control knob la In "CHECK" position. Otherwise, painful shock will result If leads are touched. 10) Bring the galvanometer pointer to zero by turn ing the "ZERO ADJUST" knob In the direction In which the pointer of the galvanometer should move. 11) Turn the control knob to "CHARGE" position for 30 seconds. 12) Turn the control knob to "OPERATE" position and return the galvanometer pointer to zero by ad justment of the "MULTIPLY BY" switch and the megohm dial. 13) Read after 30 seconds. Calculations Resistivity* - Megohm dial reading (Step 12) x "Multiply By" reading (Step 11) x oapaoltance of cell (Step 2) In mmfd. x 11.29 x 0.001. 49 RONS 073069 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, 100C and 500 volts DC. NOTE; It is important that the produot under test, eleotrodes, and beaker be at uniform temperature for this determination. Temperature variations In different parts of the sample mill cause the galva nometer eero to ohange constantly and give mlsleadlr results. CAPTIONi Inasmuch as measurements must be made at a potential of 500 volts DC a shock 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 electrodes. 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 precaution -- Painful Shook. .METHOD NO. 10,126 "CORROSION AND CHEMICAL STABILITY." a. Apparatus: 0.8. Corrosion Apparatus consists of the following: 1) A Corrosion Flask - It Is a 300-ml. pyrex flask 50 SONS 073010 Kith a ground glaaa 24/40 Joint equipped with a 12-lnoh straight tube aa an air cooled con denser. The alr-oondenser is painted on the outside Kith aluminum. 2) The Corrosion Apparatus: A transite box 32" long x <J" Kioe x 5" deep, me top of the box represents a split transite board Kith 5 holes out to fit the flasks. The box is heated by two 500-watt, 15 volt O.E. Strip heaters with off-set terminals at one end (23.5" overall length). The heating length of the heating element is covered by a copper atrip 19-1/2" long x 4" wide x 1/4" thick. The temperature is controlled by an automatic thermostat with temperature setting lndloator. It. Procedure: 1) Roll a rectangular (2" x 4") piece of aluminum foil so that It will pass through a ground glass 24/40 Joint of the oorrosion test flaek. CAUTION: Be oareful that after rolling the specimen 3oes not touch Itself at any point. 2) Hash the aluminum foil (Step 1) scrupulously with acetone, distilled water, acetone, benzene, and chloride-free ether. 3) Then place the foil on a clean watch-glass and dry in an oven at 110c. for 30 min. After cleaning handle the specimen with tongs or Poroeps only. 4) Heigh accurately on an analytical balanoe the specimen (Step 3) at room temperature. 5) Drop the weighed aluminum foil into the chloridefree oorrosion flask of the "O.E. Corrosion Appa ratus," Rinse out flask with sample and rinse end of condenser with sample. MCNS 073071 6) Add 200 ml. of the product under teat 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. 18) Heat the flask for 6 (t 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 plate. 12) Remove the flask from the hot plate and cover all of the flask with aluminum foil (when the flaBk 1b 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 nlohrome tongs, remove the aluminum foil specimen (Step 5), 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 MOMS 073072 METHOD NO. 10,118, "INORGANIC CHLORIDES." a. Preparation of Standards: 1) Make a primary standard of 100.0 ppm by weighing 0.1648 g. c.P. Nad Into a chloride-free 1 liter volumetrlo 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 le considered the very faintest beam perceptible to the eye between 15-45 eeoonds after adding the AgNO- solution. If the beam Intensity Is not vlslble^at all, or If easily visible (too strong), discard the solutions and make new standards. 2) Weigh 20.0 g. C.P. AgN03 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 eaoh funnel In a test tube Which has been rinsed with chloride-free water. Test these aliquots for Tyndall beams by adding 3-5 drops of AgN(>3 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 HNO3 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. Heat the water In both funnels to boiling. (Hold stopper while heating as steam may causa stopper to fall.) 52 HONS 073073 3) Transfer 50 ml. of the sample from the sample bottle at a temperature of 95-1006C. Into the separatory funnel oontalning the 50 ml. of boiling water. (As a precautionary measure, pour some of the sample ; from the sample bottle into a waste beaker before adding the 50 ml. to the funnel.) 4) Stopper the funnel and shake vigorously for at least 1 minute, venting frequently through the stopcock. (Care must be exerolsed at all times to touch neither the lower part of the funnel stem not the ground part of the stopcock.) D 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 seoond separatory funnel.) It may be necessary to heat the sample when transferring the sample to the seoond funnel; e.g., Aroclor 1260. 6) Repeat step 4 and allow the layers to separate. Then drain off the sample Into a waste beaker. 7) Combine both water extracts In one funnel and shake thoroughly. El 8) Take approximately a 10 ml. aliquot of the water extraot out through the bottom of the funnel Into .>J1 a 3/4" x 6" test tube. Again, first allow a few ml. to drain out before taking the aliquot. (The test tube used should be rinsed with chloride-free water several times before using.) l, t 9) Add approximately an equal portion of chloride- y free ether. (The ether la tested by shaking a portion of It with chloride-free water and testing for Tyndall beam at the end of 45 sec. If beam la i present, wash ether several times with ohlorldefree water until washings show no beam after adding 3-5 drops AgNC>3). i 10) Shake the ether-water mixture until the emulsion in the sample disappears and the water layer la completely beam free before adding AgN03. If emulsion is difficult to break, add sample dropwise through the ether and then shake. 53 MOMS 073074 11) Add 3-5 drops of 10{t AgNO* solution and tast for chloride beam for 45 sec. exactly. If no beam Is present at the end of 45 seconds, report as ^0.1 ppm. The very faintest of beams Is considered 0.1 ppm. If beam Is stronger It will be necessary to compare with etandarda of 0.15, 0.20 up to 1.0 ppm, adding the 3-5 drops of AgNO? and comparing at the end of 1*5 sec. The method Is precise to the nearest 0.1 ppm. Report results to the nearest 0.1 ppm. 7. METHOD NO. 10,007, "ACID NUMBER." a. Reagents: 1) Nitration grade bensol. 2) Anhydrous methanol. 3) A saturated solution of phenol red (phenol sul- fonphthaleln) In methanol (approx. 0.1%). 4) A 0.01 N solution of KOH In methanol, b. Procedure: 1) Place 100 ml. of benzol, 100 ml. of methanol and 0.5 ml. (pipette) of phenol red Indicator Into one of two dean dry 500 ml. Brlenmeyer 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 la still neutral, divide It equally between the two flasks. If not, repeat steps 2 and 3. 4) Weigh (1 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 matcoes the blank. o.. Calculations: Acid NO. (mg. KOH/gram sample) > ml. 0.01 N KOH x t).56 Sample weight 54 HONS 073C75 Report the results to the nearest 0.001 If they are below 0.1, otherwise to the nearest 0.01. The method Is precise to + 0.002 for acid numbers below 0.01 and to + 0.01 In the range of 0.1 to 0.01. ROTE 1: To convert mg. KOK/gram to mg. NaOH/gram, multiply by 0.715. 8. METHOD (MODIFIED NO. 10,620, "MOISTURE (WATER)". a.Introductory Comment: The Karl Fischer Reagent titration method UBed In the analytical laboratory Involves uBe 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" potentlometrlc 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 Reagents: 1) Karl Fischer 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. = 1 mg. H20) Fisher Scientific Company, 2800 Jeffer son Avef, St. Louis, Missouri. 3) Karl Fischer Reagent Solution No, SO-K-2, Fisher Scientific Company. o.Standardisation of Karl Fischer Reagent Into a 500 ml. clean, dry Erlenmeyer flask, place about 100 ml. "Anhydrous" methoanol (commerlcally available, 99.95J<). 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 hons 07301b Moisture value of K.F. reagent In terms of grams HgO per ml. (Moisture value of stand(Ml. Standard HgO solution) ard water solution In gm. per ml. stated on ______________________________ label.) ml. Karl pisoner 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 Pyranol 1488 1467 Pyranol 1481 Pyranol 1495 All Aroolors 0 ml. 100 ml. 100 ml. 100 ml. 110 ml. 300 ml. 200 ml. 200 ml. 200 ml. 190 ml. e. Prooedure, "Visual End Point." 1) Place 100-300 ml. of dry solvent mixture (0) In a dry 500 ml. ground glass stoppered Erlenmeyer flask. 2) Titrate the solvent with K.P. reagent to the vis ual endpoint, l.e., the first change from the yellow to reddlBh orange that persists for 30 seoonds. Refill the burette. 3) Using a beam balanoe, weigh to the nearest 0.1 gram by difference, a sample containing 0.03 to 0.06 grams HgO Into the flask. 4) Stopper and shake until the Bample Is In solution. 5) Titrate the solution with K.P. reagent to the endpoint described In Step 2. Record the volume of K.P. reagent used. Calculation: ft HgO ml, of K.F. reagent x HoO factor x 100 sample Weight References: Mitchell, J. and Smith, D.M., Chemical Analysis, Vol. Aquametry, Intersolense Publishers, Inc., New York, (1 9^8) 56 HONS 073077 CHAPTER 7 TYPICAL PROPERTIES The 1200 series members of the Aroelor family are chlor inated biphenyls, and are made by ehlorinatlng biphenyl to approximately the percentage of ohlorlne, by weight. In dicated by the last two digits of the serial number. Por example, Aroolor 1254 Is approximately 54$ ohlorlne on a weight basis. Accordingly, these Aroolors are not single or simple compounds. They are a mixture of isomerlo com pounds oomposed predominately of the chemical compound In dicated below as being their approximate equivalent: Aroolor 1242 Aroolor 1246 Aroolor 1254 Aroolor 1260 Trlohlorobiphenyl Tetraohloroblphenyl Pentachloroblphenyl Hexaohloroblphenyl For transformer use and some oapacitor use where lower viscosity Is required for better low temperature operation than offered by the above Aroolors, these produots are mixed with pour point depressants, particularly trlohlorobenzene resulting In various oeneral Eleotrlo Company Pyranols described briefly as follows: Transformer Pyranol 1467* 60$ of Aroolor 1260 40$ of Elec. Orade Trlohlorobenzene 0.125$ of Tin Tetraphenyl Transformer Pyranol 1470* 45$ of Aroolor 1260 55$ of Eleo. Orade TrichloroTetrachlorobenzene Mix ture 0,125$ of Tin Tetraphenyl *Dse of trl-tetraohlorobenzene and tin-tetraphenyl scavenger Is subject to O.E. patents and lloense: Royalty arrangements should be oheoked before using. Questions about lloense concerning the use of anthraquinone stabilizer for DC capaoitors should be referred to Western Electrlo, 195 Broadway, N.Y.C. 57 HONS 073078 Capacitor Pyranol 1481 755* of Aroolor 1254 25# of Eleo. Grade Tri chlorobenzene Detailed propertlea of all of these produots are given as follows: AROCLOR 1242 PROPERTY TYPICAL Vlso. 8 37.8C. (ASTM D88) Speoiflo Oravlty 8 25/15.5C. (ASTM D287) Color, APHA Condition Acidity, mg, KOH/g. Pour Pt., C. (ASTM D97) Inorganlo Chlorides, ppm. Refraotlve Index 8 25 C. Distillation Range (ASTM D20) Correoted for Btem and barometrlo pressure Corrosion 82 - 92 seoonds Saybolt Unlver. 1.381 - 1.392 100 max. Clear 0.01 max. -14 or lower 0.10 max. 1.6245 - 1.6265 10% 325C. min. 90% 366C. max. After heating with aluminum for six hours at 210c } 10oc, the aluminum must not be cor roded either on visual or weight Inspection and the Aroolor 1242 should meet the following spees: Color, APHA 150 max. Aoidlty,mg.KOH/g. 0.01 max. Inorg.Chlorides,ppm 0,10 max. Condition Clear Water Content, ppm 35 max. Resistivity 100C. 500 volts DC 8 0.1" gap 500 x K>9 ohm-om., min. Dleleotrlo Constant 100C. 4.7 - 4.9 8 1000 cycles (ASTM D924) Flash Point Clave. Open Cup* 160C., min. Fire Point C.* None to boiling point Sulfates (ASTM-D117-31)* N__o_ne Fixed chlorine oontent (Carius)* 41.5 - 42.5$ Specific Heat 8 25C.* 0.29 Evaporation 8 100C for 6 hre,* 0.4js max. Dleleotrlo Strength (KV) 35 Min. (ASTM D877)* *N0t determined unless by special request. 58 MCNS 073C79 AROCLOR 1248 PROPERTY Vise. 54.4C. (ASTM D-88) Spec. Oray. 0 65/15.5C. (ASTM D-287) Color, APHA Condition Aoidlty, mg. KOH/g. Pour Point C. (ASTM D-97) Refrao. Index 0 20C. Cist. Range (ASTM D-20) Water Content, ppm. Reels. IOOOC. 500 v D.C. 0 0.1" gap Dleleotrio Constant,100C. 1000 oyole Dleleotrlo Strength 25c.* Plash Point, (C.O.C.)* Fixed Chlorine (carlus)* Speolflo Heat 0 25C.* TYPICAL 73-80, sec.Saybolt Unlver. 1.404-1.414 100 max. Clear 0.01 max. -7, 1.630-1.631 343 - 373C. 35 500 x 10^ ohm-om., min. 4.6 35 KV min. 1930. 47.5 - 48.5* 0.27 Not determined unless by special request. HONS 073080 AROCLOR 1254 PROPERTY Vise. 9 98.9C.(ASTM D88) Specific Qravlty 9 65/15.5C. (ASTM D207) Color, APHA Condition Aoldlty, mg.KOH/g. Pour Pt. C.(ASTM D97) Inorganic Chlorides, ppm, Refraotlve Index 9 25C. Distillation Range (ASTM D20) Corrected for stem and Barometrlo Pressure Corrosion TYPICAL 44-48 seo, Saybolt Dnlver. 1.495 - 1.505 100 max. Clear 0.01 max. 7-12 0.10 max. 1.6370 - 1.6390 10* 366-- 3786C. 50* 372 - 3830c. 90* 383 - 396C. After heating Nlth aluminum for 6 hours 9 210C. plus or minus 10C, the aluminum must be oorroded either on visual or weight Inspection and the Aroelor 1254 should meet the following specs: Color, APHA 150 max. Acidity,mg.KOH/g. 0.01 max. Free Chlorides,ppm.0.10 max. Condition - Clear Water Content, ppm. 35 max. Resistivity 10OC.,50O v D.C. 9 0.1" gap 500 x 10^ ohm-cm., min. Dleleotrlo Constant, 100c 4.15 - 4.35 1000 eyolee Dleleotrlo Strength 25C* 35 KV,, min. Burn Point (ASTM D92)* Higher than 350C. Sulfates (ASTM D-117-31)* None Fixed Chlorine Content (Carlus) 55 I 0.5* Evaporation 9 100C. for 6 hrst 0.4* max. Stability* There shall be no liberation of chlorine or chlorides when the material Is heated 9 100C In glasB vessels In contact with air for periods of at least one month. Ageing Characteristics* No Iobb in resistivity over original value on heating In air for 96 hrs. at 100C. Specific Heat 9 25C. 0.26 Not determined unless by speolal request. 60 SONS 073081 AROCLOR 1260 PROPERTY TYPICAL VIbo. 0 98.9C.(ASTM D88) 72 - 78 Seo. Saybolt Univ. I Specific Gravity 9 90C,fl5.5C 1.555 - 1.566 (ASTM D287) Color, APHA 150 max. I Condition Aoldlty, mg.KOH/g. Clear 0.01 max. Pour Pt,,C.(ASTM D97) 25 - 34 B Inorganic ohlorldee, ppm. Refraotive Index, 25C. 0,10 max. 1.6455 - 1.6470 Distillation Range (ASTM D20) 10J< 385 - 398*C ;s Corrected for stem and barometrio pressure. 50* 390 - 404C. 90* 400 - 420C. Corrosion After heating with aluminum 0 for 6 hrs. 0 210C. t 10C, the aluminum must nof be cor roded either on visual or E weight inspection and the Aroolor 1260 should meet the p following speos: Color, APHA 150 max. Free Chlorides,ppm, 0,10 max. b Aoldlty,mg.KOH/g. 0.01 max. Condition Clear c Water oontent, ppm. Resistivity,100C. 500 volts P.l" gap _ 35 max. 500 x lO^ ohm-om., min. Dleleotrlo Strength 50C.* 30 KV., min. g Dlelectrlo Strength 100C.* Dleleotrlo Constant 100C. 30 KV , min. 3.6 - 3.8 a 9 1000 oyoles* Burn Pt. (ASTM D92)* Sulfates (ASTM Dllf-31)* Higher than 350C. None Fixed ohlorlne oontent (Carius)* 60 4 0.556 a Evaporation 0 100C. for 6 hrsj* 0.2)1 max. Stability* There shall be no liberation of ohlorlne or chlorides when . 1 the material is heated 0 100C. in a glass vessel in oontaot with air for periods of at least one month. Speolflo Heat 0 25C.* 0.23 Not determined unless by special request. 61 HONS 073082 PYRAHOL 1481 PROPERTIES TYPICAL Vleooslty 9 37.8C. 70 - 82 sec. Saybolt Unlv. Spao. Gravity 9 15.5/15.5C 1.525 - 1.535 Color, APHA 150 max. Condition Clear Acidity, mg. KOH/g. 0,01 max. Pour Pt., c. -15 or lower Inorganic Chloridea, ppm. 0.10 max. Refractive Index 9 25C. 1.6205 - 1.6215 Olatlllatlon Range Corrected for atem and barometric preaaure. Plrat drop 205C. min. 25* max. Below 270C. 90* 380 - 395C. Corroelon Teat Change In Weight 0.0* Color, APHA 200 max. Acidity, after teat,mg,KOH/g 0.01 max. Free ChlorIdea,ppm. 0.10 max. Condition after teat Clear Water Content, ppm. 35 max. Resistivity 9 100C 500 volts, DC, 0.1"gap 100 x 109 ohm-em.,mln. Dleleotrio Constant (100C., 1000 cycles) 4.1 - 4.6 62 HCNS 073083 FYRANOL 1467 PROPERTIES TYPICAL VIbo. 9 37.8C.,(ASTM D88) ,, 54 2 sec. saybolt oniv. Speolfio Gravity 9 15.5/15.50 (ASTM D-287) 1.560 - 1.568 Color, APHA 150 max. Condition Acidity, mg. KOH/g. Clear 0.01 max. Pour Point, C. (ASTM D-97) -32C. or lower Inorganic ChlorldeB, ppm. Refractive Index 9 25C. 1.0131 - Distillation Range (ASTM D20) 1st drop - 200C. min. Corrected for stem and Below 270C. - 40% max. barometric pressure 90* - 395 - 4l5C Corrosion After heating with aluminum for 6 hrs. at 200-220C,,the aluminum must not be corroded either on visual or weight In spection and the Pyranol should meet the following speos: Color, APHA 200 max. Acidity,mg.KOH/g. 0.01 max. Inorganlo Chlorides 5 max. ppm. Condition Clear Water Content, ppm. 30 max. Resistivity, 100C. 500 volts, 0.1" gap 100 x 109 ohm-cm.,min. Dleleotrlo- Strength, 25G. 35 KV., min. Dleleotrlo Constant, 100 C., 1000 oyoles* 3.7 - 4.0 , Tin Tetraphenyl* Bum Point, (ASTM D92)* 0.125% 4 0.01% by weight None up~to Bolling Point Fixed Chlorine* 59.1% min. Aro Formed Oases* ,, Less than 1.0% (Oxygen Free Liquid 9 25 C.) Total combustible gases Including oarbon monoxide, hydrogen and volatile hydro carbons . Not determined unless by speolal request. 63 HONS 073084 PYRANOL 1470 PROPERTIES TYPICAL Viao. 9 B7.SC. (ASTH D88) Spec. Gravity 9 15.5/15.5,SC., (ASTM D287) Color, APHA Condition Aoldlty, mg. KOH/g. Pour Pt.,C., (ASTM D97) Inorganic Chlorides, ppm. Refraotlve Index 9 250. Distillation Range (ASTM D20) Distillation Range (ASTM D20) Correoted for stem and barometric pressure First drop 35# 55# 65# 95# Corrosion 41-45 Seo. Saybolt Onlv, 1.563 - 1.571 150 max. Clear 0.01 max. -44C., or lower 0.10 max. 1.6075 - 1.6085 2100c., min, 238 - 256C. 275 - 345C. 380 - 400C. 390 - 4l5C. After heating with aluminum for 6 hrs. 9 200-220C., the aluminum must not be corroded 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 max. Resistivity, 100C., 500 v., 0.1" gap ,, 100 x 10^ ohm-om., min. Dleleotrlo Strength, 25C. 35 KV., min. Dleleotrlo Constant, 100C., 1000 oyoles* 3.8 - 4.3 Tin Tetraphenyl* 0.125# * 0.01# by weight Bum Point, (ASTM D92)* None up"to Bolling Point Plxed Chlorine* 60.5 * 0.5 Aro Formed Oases* Total"eombustlble gases In (Oxygen Free Liquid 9 25C.) cluding carbon monoxide, hydro gen and volatile hydrooarbona. Eleotrloal Stability* After heating for 96 hrs. 9 100C In a dosed container, the resistivity Bhould not deorease more than 10# *Not determined unless by speolal request. 64 *CNS 073085 PYRANOL 1488 Viso. @ 37.8C. Spec. Orav. 9 15.5/l5.5C. Color, APHA Acidity (Mg KOH/g) Water, ppm. Condition Refrao. Index 9 25C. Pree Chloride, ppm. Pour Point, C. Reals. 9 100C., 500 v D.C. 1" gap Dleleotrlo Strength (25C.) Corrosion: Lose of Aluminum 54-- 2 Seo. Saybolt Onlv. 1.560 - 1.568 150 max. .014 max. 35 max. Clear 1.6137 - 1.6147 0.10 max. Lower than -32C. 100 x 10^ ohm-cm min. Over 35 KV None Heating with aluminum for 6 hrs. at 200-280C. The Fyranol after heating should meet the following specs: Color, APHA 200 max. Aoldlty(MgK0H/g) .014 max. Pree Chlorides ppm .10 max. Condition Clear Dleleotrlo Constant 9 1000 oyoles 9 100C.* 3.7 - 4.0 Distilling Range (corrected)* 1st drop 200C, min. Below 270C. 4056 max, 90$ point 295 - 4l5C. Burn Point (ASTM D-92)* None up to boiling point Fixed Chlorines* 59.1* min. Aro Formed Oases* Less than 1.0* total com (Oxygen-free liquid 9 25C.) bustible gases Including oarbon monoxide, hydrogen, and volatile hydrocarbons. Not determined unless by speolal request. 65 HONS 073086 CHAPTER 8 EARTH TREATMENT OP AROCLOR IN THE ELECTRICAL INDUSTRY PRIOR TO USE. Aroolors and their mixtures supplied to the electrical Industry must conform with most strlot requirements sepolfled by the Industry as shown In Chapter 7. Slnoe 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 oapaoltors or fill transformers. Common contaminants to be avoided lnolude moisture, ionlsable Impurities, metallic Impurities, auoh as rust or oorroslon products from storage and handling equipment, and contaminants suoh as oils (mineral oils), lubrleating oils or greases common ly used In equipment or other processes In the eleotrloal Industry. Care must be taken to avoid contamination from oontact with Improper gaskets or packing materials. Including natural and synthetic rubber and most plastic exclusive of oertaln Sllloones and Teflon. Rosin solder fluxes, eto. may also lntroduoe traoes of deleterious Impurities. The dieleotrlcs are also susceptible to the harmful aotlon of ultra-violet light and, therefore, exposure to dlreot sunlight should be avoided. The adverse effect of lonlzable Impurities Is especially pronounoed In the low viscosity Aroolors such as Aroclor 1242 66 MCNS 07308J or Aroelor mixtures suoh as Pyranol l48l. In the oase of more viscous fluids, suoh as Aroelor 1234, the lonizable im purities are not so free to move about in the fluid and, con sequently, the more viscous fluids ean be handled Kith less oare than required for the thinner fluids. This is especially pertinent in oapaoltor manufacturing. When using the thinner type Aroolors to make oapacltora that offer superior low temperature operation, the following types of traoe contamination affecting the electrloal properties of the dlelectrlo have been experienced. Occasional droplets of perspiration from operators, when winding the oapaoltor oores, have fallen onto the paper oauslng contamination in the finished units. Small amounts of Olyptal reBin and simi lar sealing compounds used to seal tiny leaks in the vaouua 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, whereas it may not have as much adverse effect on the more viscous dleleotrlos. To be oertaln that the fluids are free from traoes of contamination, it is standard praotloe to treat them with con ditioned dlatomaoeous earth and then to filter immediately be fore use. Treatment with this earth by removing trace contam inants results in "up-grading" the electrloal values, e.g,, 67 SONS 073088 the volume-reslstlvlty nay be brought up considerably beyond the speolfloatlon minimum or the normal values of the dleleotrlo as received. Likewise. Improvement In power faotor may be ao oompllshed. The earth treatment recommended for use by the eleetrleal manufacturers Is qualitatively the same as used In the produc tion of the Aroolors and their preparation for shipment to the eleotrloal Industry. Treatment of the Aroolors with earth by the electrical manufacturers Is a step required to assure that traces of Impurity or contamination that may have been Introduced during storage or handling In the eleotrloal Indus try have been removed and that maximum eleotrloal values have been attained Immediately before the dleleotrlo Is introduced Into oapaoltors or transformers. It Is lmpraotloal for the manufacturer to furnish these dleleotrlos to the oustomer at the maximum attainable eleotrl oal qualities because even with oareful packaging, shipping, sampling and handling In the eleotrloal Industry, these fluids may easily plok up traoes of oontamlnants from opened tankcars, drums, pipe line, pumps, etc. However, as supplied according to the specIfloatIons, the fluids are readily "up-graded" by the earth treatment. The type of dlatomaoeous earth used Is known as Puller's Barth, supplied by the Plorldln Earth Company, Warren, Pennsyl vania, or the Attapulgus Division, Mineral & Chemicals Corp. of Amerloa, 210 West Washington Square, Philadelphia 55, Pa., 68 HONS 073089 or their equivalent. Usually a minus 200 mesh size, regular volatile. Is used and the qjallty should be specified as for use by the eleotrloal Industry. (Code 73122) The earth as reoelved 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 la desirable that the earth be used Immediately after It has been activated. Aotlvatlon Bhould be done by heating the earth contained In stainless steel shallow trays for four hours at 400C. In a muffle furnace. 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 eleetrloally heated oven at 230C. Another method used Is to pan dry and aotlvate by heating at 100C. and using a strong vacuum, about 6 mm. of meroury. This latter method Is used In oonnsotlon with transformer work and the former methods are usually used for oapaoltor work. In the plaoe 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 dlffloult to handle In the subsequent filtering operations. It Is the consensus that the earth should not be heated above 400c. as this may oause collapse of the partlales. 69 MQNS 073090 The amount of earth used la usually 0.1JK to 0.3$ baaed on the weight of the fluid. Larger amountB of earth oan be used If the fluid Is oompoaed of only Aroclor or a mixture of Aroolor and ohlorlnated benzene or other pour point depressants. However, larger amounts of highly aotlve earth. In the range of 2% or 3, would be expeoted to selectively adsorb scavengers or stabilizers rrom the fluids containing these additives. This Is especially of oonoern In handling the transformer fluids whloh usually oontaln 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 vaouum, about 6 mm. of meroury. Not more them about 0.1 of earth based on the total weight of the transformer fluid should be used. For treatment with earth, the fluid Is put Into a suitable tank fitted with an agitator, heating coll, and a eover. The proper amount of freshly conditioned earth Is added and the mixture Is agitated thoroughly and heated for about four hours. The more viscous dleleetrlos suoh as Aroclors 1248 and 1254 ire heated at about 70 to 80 C. (158 to 176F.) and the less viscous materials suoh as Aroolor 1242 and Fyranols 1401, 1467, and 1470 are heated at about 50 to 60 c. (122 to 140P.) 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 suoh as supplied by 70 HCNS 073091 Carl Sohleioher and Sohuel Co., Ino., Keene, N.H. The paper la usually 25 mils thlok and must be dried at lOOOC. to remove a moisture, prior to use In the filter press. The filtered dleleotrlo material Is then ready for Impregnating capacitors r or filling transformers. In some oases, especially for AC oapaoltor work where s the dleleotrlo does not require addition of stabilisers and T aooordlngly there Is no danger of removing suoh additives by repeated earth treatment, good practice Is to use continuous C earth treating, circulation and filtration with constant read c ing of the resistivity or the filtered dleleotrlo. In Chapters 1 and 2 selection of proper materials of t oonstruotlon for the tankoars and storage tanks was dlsoussed. It Is equally Important to seleot proper materials of oonh truotion for the prooesslng tanks used In the oapaoltor and t transformer Industries and also for the lmprgnatlng chambers r used in making oapaoltors. It Is preferable that this equipment be made of stain r l- less steel or aluminum, or , If It Is of steel oonstruotlon, L the Interior should be either slno-tln metallised or aluminum lined. ( While Iron or steel equipment Is not regarded as de I sirable for handling the fluids, this type of oonstruotlon Is used In some of the plants. Here the possibilities of rust ing or oorroslon cannot be overlooked. If the equipment Is kept free from water and If a film of clean dleleotrlo adheres 71 SONS C730S1 to the surface of the metal, e.g. when the tanks are empty, then satisfactory operation oan be experienced. However, a number of faotors must be kept In mind and to cite an example, reference la made to the Impregnation of capa citors by the ohamber method. Hie moisture oontent of the paper used in the oapaoltor oores may easily Introduce several gallons of water Into the average Impregnating ohamber. nils water Is removed from the oapaoltors prior to Impregnation -- usually by heating the chamber to about 130C. under efficient vaouum, 100 microns or less. If the ohamber la not made of the preferred materials of construction, slight corrosion may ooour and the film of fluid on the Interior surface of the tank may be contaminated and In turn Introduce traoes of Impurities into the treated and clean dielectric subsequently Introduced Into the chamber for Impregnating the capacitors, in faot, beoause of this possibility of contamination. In some operations the oapaoltors are conditioned and dried preparatory to Impreg nation In a separate oven or ohamber and when thoroughly dried they are then transferred Into a seoond ohamber used for impreg nation. In the case of relatively large size oapaoltors, suoh as power faotor correction units, a manifold pipe system may be used to handle each unit Individually rather than by the batohehamber method. The unimpregnated oapaoltorB are placed Into an oven and vaouum is applied to the individual units attaohed to the manifold. 72 HONS 073093 When conditioned and dry, the dielectric 1b introduced into the unit through the manifold. Care must be taken that nolet air or contaminants do not oolleot in the branch through which the dleleotrio is introduced. In addition to removing moisture, another purpose of the heat and vaouum conditioning treatment given the capacitor units prior to impregnation is to remove traoes of impurities suoh as residual solvent from the metal cleaning operations and from solder flux, etc, Hie fluid is introduced hot into the evaouated capacitor units. The more viscous Aroolors, such as 1248 and 1254, are usually Impregnated at 85 to 130C. The less viscous and more volatile dleleotrlcs suoh as Aroolor 1242 and mix tures of Aroolor with ehlorlnated benzene may be Introduced best at lower temperatures -- about 50C. optimum, 80<. max. Table IV indicates desirable minimum resistivity values of the dleleotrio materials when earth treated and ready for oapaoltor impregnation and similar values of the material following the process. TABLE IV Dielectric Volume Resistivity Ohm-om at 100C. and 500 volts DC. Prior iT TO-------- Impregnation Impregnation Aroolor 1254 2.500 x 109 800 x 10$ Aroolor 1242 1.500 x 109 600 x 109 Pyranol 1481 600 x 109 400 x 109 73 MONS 073<m In the case of new and freshly filled transformers using Aroolor dielectric mixtures. It seems reasonable that the power faotor of a sample of the fluid drawn from the trans former should be In the range of about 5 to 12 per oent, measured at 60 eyoles and 100C. With field service of the transformer the power faotor value Is expeeted to lnorease somewhat. However, suoh a power faotor Increase alone does not seem to have harmful effeot on the operation of the transformer. A more usual measurement used for transformer fluid Is volume-resistivity. This value of the new dleleotrlo prior to filling the transformer should be about 500 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 10^ ohm om. With long field service volume-reslstlvlty values de crease somewhat but seem to level off around 10 x 10 ohm-om, with satisfactory transformer qperatlon. However, If the voiumereslstlvlty of the fluid falls below 10 x 109 ohm-om, the matter should be looked into. 74 HGNS 0730S5 CHAPTER 9 DERMATOLOGY AND TOXICOLOGY Skin patoh testa using Aroolor 1254 (biphenyl Chlorinated to the extent of 54)6 by weight) applied to gauze and placed in oontaot with the Bkin showed no primary lrrltanoy or sen sitization. The tests were oonduoted under oompetent medical supervision and the standard procedure reoommended by Ere. Louis Sohwartz and Samuel M. Peok, 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 oontaot with hot Aroolors, the burn should be treated the same as any ordinary burn. Aroolor adhering to the burned area need not be removed immediately unless treatment of the burn demands it, in whioh case use soap and water or repeated washings with a vegetable oil. At ordinary temperatures Aroolors have not presented industrial toxloologloal problems. If Aroolors are used at elevated temperatures In open systems, methods must be designed to exhaust any vapors arising. Experimental work on animals Indicates that the maximum safe concentrations of vapors in workrooms Is In the range of 1.0 to 2.0 milligram per oublo meter of air. This applies to all of the liquid Aroolors. 75 HONS 073050 Laboratory technique merely requires keeping the hands free of the liquid and handling It under a well ventilated hood. LooAllzed or spot ventilation together with general work room exhaust la recommended for plant operations. When sampling tankoars. canvas gloves and safety glasses or goggles should be worn. No special dothing is required but the worker's garments should be laundered at least weekly and ohanged In oase Aroolor or Aroclor mixture Is spilled on the olothes aooldentally. If workmen are exposed to Aroolor vapors at relatively high levels, as may be the case when opening a heated capacitor Impregnating ohamber. a respirator should be worn during these short Intervals. The many years of satisfactory and safe use of Aroclors and their mixtures with ohlorlnated benzenes in the eleetrleal industry for Impregnating capacitors and filling transformers has demonstrated the Industry's ability to handle these fluids without hazard to the workmen. It Is a simple matter and In line with good "housekeeping" and personal cleanliness to exerolze the suggested and required precautions In all oases. . 76 HONS 073097 o e 9 9 HONS 073098 HONS 073099 nau- r-g' Xtrgitenr >*./<' flonmU LhaiiBd Lmpuqr 4ft 42- ANMtrrQM. AM AMMitTOX' rms 0>M<tirrb *<** >Mt T<m fc- 'III 1-11.41 DWG. NO. 9C-S246 HONS 073100 'I HONS 073X01 HONS 073102 HOMS 073103 y.iv ty **>**//fw o a MONS 073104