Document e5w0RYnXv2Rn8kBqkd84QVmqp

DEVELOPMENT of a new electrical INSULATING TL'JVj A. J. Rutkowskl**-and E. 0. For^ccr** ABSTRACT One of the results of worldwide attention on environmental effects produced by synthetic organic chemicals was an accumulation of evidence that. Polychlorinated Biphenyls, PCB's, are widely dispersed in the environment and that they exert; both adverse toxicological and ecolo gical effects. Since PCB's are widely used in the capacitor and trans former Industry, In late 1970 a study was begun to develop a suitable electrical Insultaing fluid without these adverse properties. This study culminated in the development of dllsononyl phthalate (ENJ-2065) as a dielectric fluid for the capacitor Industry. It Is now In commer cial use in the U.S.A. To be presented Japanese Institute of Electrical Engineers I September 18, 1974 * Chemical Intermediates Technology Division, Exxon Chemical Company, P. 0* Box 536, Linden, New Jersey 07036. Corporate Research Laboratories, Exxon Research and Engineering Company, P. 0. Box 45, Linden, New Jersey 07036. M0NS 039586 2 Introduction ' Polychlorinated biphenyls, PCB's, have been In commercial ure as electrical Insulating fluids for over forty years. They gained prominence in capacitors and transformers because of the property and performance advantages they showed over the hydrocarbon dielectric fluids. FCB's are non-flammable, have a reasonably high dielectric constant, and a high degree of stability. These properties enabled manufacturers to produce relatively non-flammable smaller else capacitors and transformers with longer life performance than could be obtained with conventional hydrocarbon fluids. Over the years, more than 90 percent of the electrical utility and smaLler Industrial type capacitors have been impregnated with PCB's^. Commercially, PCB's arc manufactured by chlorination of biphenyl. This procedure results in a complex mixture of isomeric chlorobiphtnyls with varying chlorine content. Trace quantities of TCB's were reported present in environmental (*>) samples in 1966 . In following years, PCB contamination was found to be widespread including human milk and adipose tissue' . Definitive toxologlcal properties, as regards humans, remain poorly known. A detailed bibliography of the current status of toxicological data arc given in^\ As a result of the environmental end toxicological considerations, the use of PCB's has recently been either limited or banned altogether in many countries. So far in the U.S., PCB usage has been limited to those systems which are closed, e.g. capacitors and transformers, to minimize or olimlnate environmental exposure. In May 1972, Japan totally banned the use of PCB's in any product either produced or imported into their HONS 039567 - * .. country. Member European couutrlc.6 l;\ the orgM^U.aticr for Economic Cooperation and Development (OECD) reached an ageeament i n i 0 73 to rucc:.-cn#.id the restx'lcted use of PCB ' e . Physical and Electrical Properties of Insulatiny rhrid_s Electrical Insulating (dielectric) fluids are important as impregnants in tranformers, capacitors and other electrical devices. Tn addition to their electrical, functions, the fluids may also be used for cooling and arc quenching. For use in capacitors with cellulose pape.r as a dielectric, the important properties of the fluid are: 1, High Dielectric Constant. A desirable dielectric constant Is one which closely matches that of the paper dielectric. A close match reduces electric field i.nhomogencites, Increases dielectric strength and thus improves the useful life of the unit. Although liquids with dielectric constants greater than six would be desirable to reduce the size of the capacitor purifying such liquids of conducting impurities, such as water, is extremely difficult. A dielectric constant in the range of four to five appears to be a good compromise to maintain purity while permitting a reduction In unit si?e. 2, Low Dissipation Factor. This iaclor is known to be primarily * a function of purity but molecular geometry may also influence it. A low value is important to reduce energy loss and damaging heat buildup in a capacitor. 3, High Dielectric Strength. High values are required to improve the service life of the units by permitting exposure to short * periods of abnormally high stresses without breakdown. MONS 0395B8 .. /l - 4. low Gassing Tendency. Low values are desirable to avoid the production of gases, such a? hydrogen, which car lewd rc che buildup of pressure in sealed vmif-3. In. practice of aror.iatic molecules has been found to be beneficial in reducing gas evolution (4) 5. High Chemical and Thermal Stability. The equilibrium concen tration of water present in ccllulosir paper and the oom.il operation of capacitors at elevatnd tan:pcraturca dt-mar.c a high order of stability of them*, fluids to prevent or minimize failure of capacitors In use. 6. Low Viscosity. For ease of complete impregnation and filling of capacitors, a low viscosity fluid is desirable to eliminate voids of air pockets. 7. Low Degree of Toxicity. This property is mandatory to over come objections of governmental, environmental protection organizations, and other private agencies. 8. Ecological Compatibility. This requires an accepiuble fluid to be readily.biodegradable by microorganisms in soil U'd water. If biodegradation to carbon dioxide and water is not complete, the degradation products should be relatively nontoxic or no more toxic than the parent fluid. The above requirements apply primarily to capacitors. In practice PCB's have also found use as dielectric* fluids J.n transformers particularly in those used indoors where limited flammability is an important requirement. In these transformer applications the magnitude of the dielectric constant is of less Importance than the fluid's heat transfer ability. MONS 039589 -5 The search for a suitable dielectric fluid to replace PCB's In capacitors has been undertaken l.n many laboratories. Organic esters, fluorocarbons and silicones have received much attention n ' 71 . The organic esters studied generally had either low dielectric constants, showed poor dielectric strength or were either hydrolytically or thermally unstable. The esters which received the most attention were derived from either straight chain alcohols, e.g. butyl sebacate or mono-bronched alcohols e.g. dl(2-ethyl hexyl) phthalate CHOP). Esters from these type alcohols would be expected to have a lower hydrolytic stability in capacitor applications since a higher degree of branching in the alcohol Is believed to improve (7C) hydrolytic stability . The fluorocarbons were generally more volatile and expensive than PCB's, and decomposition products are expected to be toxic. Silicones have the disadvantage of low dielectric constant and some deteriorate rapidly under electric arcing. , , Vith these general considerations in mind, it Is possible to focus on the myriad of possible ester types of polar dielectric liquids. As will be shown in the following sections, we believe the choice is limited to a few types of compounds, with special emphasis on esLcr$ from branched chain alcohols if one is to stay within the realm of readily available, stable and economically practical materials. Experimental .\ . The fluids used in this study were cither experimental materials prepared in the laboratory or were supplied by*the Exxon Chemical Company U.S.A. (see Table 2). The sample of PCB (42% Cl) was obtained from the Monsanto Chemical Company. In the preliminary screening studies, they vere used as prepared or received (seo. Table 1A, IB). In . the later stAges MONS 039590 -6- of this investigation, the samples were carefully purl.'ied (see Table 3) and the preferred purification method be described later. A. Dielectric Measurements The dielectric measurements were carried out in two types of cells. When evaluating liquids alone, a Balsbaugh cell, Type LRC-l (manufactured by Balsbaugh Labs, South Hingham, Massachusetts and con forming with ASTM D150) was used, together with a GE built high voltage bridge (Direc Read Capacitance Bridge) capable of operating at up to 5000V. For the evaluation of the interaction of the liquids with capacitor-grade paper a glass cell having flat parallel platinum electrodes with cell constant 0.1 (manufactured by Beckman's Industrial Instrument Division as Cell A01) was used. Tills cell was supplied with a ground glass joint so that the liquid and paper could be sealed in the cell for the duration of any test. All dielectric measurements reported in subsequent sections represent the average of measurements on at least three different samples. Constant temperature of the cells was maintained in an oven into which dry nitrogen was circulated. The temperature in the oven could be controlled to within + 1C. The capacitor paper was always dried under vacuum at A- 90C for at least 48 hours prior to Impregnation with the liquids under study. Physical Measurements . The physical properties of the fluids were determined according to ASTM methods unless stated otherwise. To evaluate the thermal stability .. * '. of the fluids, a simple screening test procedure was developed. It con sisted basically of an evaluation of the dielectric constant and loss factor at 25C. Then, while still In the measuring cell, the samples were heated to 90C. After two hours at 90C, to reach thermal equilibrium, HONS 039591 the dielectric properties of the fluid were determined. The system was allowed to cool to 25C overnight. When thermal equilibrium at 25C was reached, the dielectric properties were again measured. The data were evaluated according to the following criteria: The dielectric constant at 90C hod to be less than that at 250C both before and after heating. The dielectric loss factor should not exceed 0.5 at 90C and its value at 25*C should not change by more than a factor of two as a consequence of the heating cycle. As a rule, properly purified liquids were found to satisfy readily these requirements and their long term thermal stability was found to be quite satisfactory. The purification of these fluids is discussed in the following section. Purification Esters, particularly those used in electrical applications require purification if they are to maintain their chemical and physical integrity. Such purification involves the removal of trace moisture, unreacted alcohol and organic acids as well as half (acid) esters and possibly catalyst residues, since their presence could adversely affect the dielectric fluid's stability and performance. Examples of the effect of residual alcohol and moisture on conductivity are shown in Tables 3 and 4 respectively. The efficiency of any purification process is usually determined by conventional macro- and microanalytical techniques. When dealing with fluids for use in electrical equipment auch as capacitors, these conventional techniques prove to be insufficient and experience has shown that electrical measurements are a more sensitive means for evaluating the state of purity of such liquids. Various purification methods were evaluated but eventually the method involving percolation of the ester through a packed column was se lected as the most convenient and efficient.. As packing material, activated MOWS 039592 -8- Attapulgus clay (30/60 mesh) proved most effective. Activation of the clay was achieved by heating it to.250*C for a minimum of I? bra while Hewing nitrogen through the column. The gas inlet and outlet were connected to bubblers to prevent back mixing of moist nir during the cooling period. The liquid esters were gravity fed through the clay bed at ambient temperature while maintaining a dry inert atmosphere. In general the first 57. of fluid coming through the column was recycled. . A typical example of a run is shown In Table 5. No attempt was made to optimize flow conditions. In Table 2 are sumnarized the electrical and physical properties of the various purified phthalate esters used in this study. Results . ''] y '. In order to obtain a general understanding of the interrelation between molecular structure and dielectric properties a significant number of mono and dibasic esters were examined. Their dielectric constants as well as conductivities arc shown in Tables lA and IB. Within a group of osters it wsb noted that generally both tho dielectric constant and the ac conductivity decreased with increasing molecular weight. Exceptions to this trend were found among the aliphatic dibasic acid esters, which may be due in part to impurities in the various ester. In selecting some potential candidates for use as electrical insulating oils, thought was given to availability of the material, its physical characteristics as well as such special properties no gassing tendency under high electrical tresses. Since It is well known tbnt**Aromaticvcompounds perform better than aliphatic ones in this latter aspect and to Assure availability at reasonable cost, the selection was narrowed to the phthalate esters shown in Table 2. Among these six esters, diieononyl phthalate (ENJ-2065) vie* the most promising candidate in terms of overall properties. UNJ-20C5 HONS 039593 9 is manufactured in the United State.; by the Exxon Chemical Company, u.s.A., from phthalic anhydride and an approximately 60/20 mixture of branched and isomeric alcohols. ENJ-2065 wes selected as the final candidate for a more thorough and exhaustive study on the basis that It has (1) An advantage in Its loss characteristics relative to the lower molecular weight dihexyl and dioctyl phthalates, (2) a higher dielectric constant than the higher molecular weight phthalates, (3) a relatively high flash point, and (4) a more highly branched ester group than dihexyl and dioctyl phtholates to improve hydrolytic stability. The other physical and electrical properties of ENJ-2065 also offer a good balance of perfor mance characteristics* It is well known that electrical Insulating fluids have to remain chemically unchanged when subjected to temperature cycles. For this reason It is desirable first to know what- effect certain contaminants might have on the stability of the material, secondly how one could remove these contaminants and thirdly what protective additives might be useful in en hancing its stability. To provide answers to the first point the effect of . adding small amounts of alcohol and water on the material's conductivity was evaluated. The results shown in Tabless 3 and 4 respectively indicate that less than 0.1 wt % of alcohol and less than 0.01 wt % of water could probably be tolerated without adversely affecting performance. To obtain an answer to the second point it was decided to use a percolation technique to eliminate these contaminants as well as others such as residual catalyst. In Table 5 are shown the results of such a purification process using activated Attapulgus Clay. Under the conditions used, the column could handle about 22 to 23 gallons before the clay lost its activity and breakthrough HONS 03959<* - 10 - of conducting impurities occurred. In search for a solution of the third point, it was deemed expedient to take a look at the additives used with polychlorinated biphenyls^. In general. It was noted that epoxide type compounds were compatible with ENJ-2065 and indeed Imparted beneficial effects to its long term performance. ' - In the next phase of the study, the gassing tendencies of ENJ-2065 were evaluated and the results are shown in Table 6, Although its gas absorption tendency was not as good as that of a typical FCB capacitor fluid, it waa judged sufficient for the intended purposes. .. ' ' " The preliminary test results indicated the suitability of ENJ-2065 for use in capacitors. Its compatibility with other componen ts forming a capacitor needed to be evaluated. In Table 7, a comparison is shown of a long term stability test run in the presence of regular capacitor paper. Over the test period of 600 hours, the dielectric loss decreased and was considerably below that of the FCB. The presence of aluminum or nickel foil did not show an adverse effect on the long term stability of ENJ-2065. For an overall evaluation, six capacitors designed for a nominal 30 /(Id, 370 VAC in PCB (427. Cl) were impregnated with ENJ-2065 containing 0.3 wt.% epoxide stabilizer. Conventional techniques were used to dry and impregnate the units. The results of these tests are shown in Table 8. v ..A substantial amount of safety evaluation has been carried out on dilsononyl phthalate. A sunmary of these studies is presented in Appendix 1 end Its implications are discussed la'Cer on. Discussion . ' . The results presented in the preceedlng section indicate that ENJ-2065 possesses all the necessary characteristics of a capacitor' impregnating fluid. Although its dielectric constant is not as high as MONS 039595 r - - 11 - . that of typical polychlorinated biphenyls (PCB), It is sufficiently high to be useful in capacitors designed for use with PCB's and has the advantage of being ecologically acceptable. It may be argued that some lower phthalate esters have high dielectric constants but at the same time their conductivities are higher and their thermal stability and flash points are lower than that of ENJ-2065. The branched structure of the e9ter group in ENJ-2065 provides an increased measure of hydrolytic stability for improved service life of paper wound capacitors. Thus, ENJ-2065 represents a dielectric fluid with the best overall balance of physical and electrical properties for capacitor applications. . ,t .. ':'v.h;.'v.-' ' .. . . - Another important aspect involves the potential danger involved 'in disposing of this material. Although much has been written about the . biodegradation of phthalate esters, only recently have studies been carried out on neat phthalate esters Saeger and Tucker evaluated the biodegra dation of phthalate esters using'(1) a semi-continuous activated sludge test, and (2) a River Die Away test. Comparisons were made to controls including a readily degraded surface active agent, LAS, and a poorly degradable insecticide, DDT. . . ; , vr The test results of Saeger and Tucker "clearly demonstrated that the phthalate esters and their intermediate degradation products are all rapidly degraded by readily available bacteria In our environment. For this ..reason, these compounds should not be classified as persistent materials but rather as a class of industrial chemicals which are easily recycled by natural biological processes". - .. ! phthalate esters also have been the subject of considerable toxicology studies. In the. period 1971-72 much concern was voiced regarding their occurrence in- the environment ami ih bank blood. At'e <, 4 ; :: . : , HONS 039596 12 result of this concern, the National Institute of Environmental Health Sciences sponsored a meeting in Pinehurst, North Carolina, on September 0-7, 1972. The information presented at the meeting showed that there is a vast difference in degree in the types of problems presented by phthalates as compared with those related to polychlorinated biphenyls^. . '' At the Pinehurst meeting after hearing papers on such diverse aspects of environmental consequences as "...Phthalate Esters in Aerospace Technology", "...Toxicity via Ingestion", and "Toxicology in Aquatic Organisms", Mr. Lloyd Tepper, Associate Commissioner for Science of the .FDA commented in his review that we are in a "...clearly preferable position (over PCB's and mercury which were found to be the source of overt disease) of having an etiology which is searching for a disease". .' . * /O \ ' A similar symposium in March.1973' ' reaffirmed the Pinehurst conclusion that phthalates present no immediate hazard to the public health. Although there are no data to suggest imminent hazard, more work should be preformed to Insure that there are no long term in-house effects. An FDA fish-sampling study recently completed (917 gives cause for.further optimism that phthalates are not accumulating in. the environ ment since only 20% of the fish sampled contained phthalates and thoso at such a low level that the FDA abandoned further fish sampling. ./ V- In summary, ENJ-2065 represents a dielectric fluid with the best overall balance of physical, electrical, toxicological and environ mental properties to meet the current .needs, for.capacitor applications. MUN5 039597 REFERENCES (1) Polychlorinated Biphenyls and the Environment, Interdepartmental Task Force on PCB's, Washington, D. C. May 1972 (COM-72-10419). (2) Jensen, New Scientist 32, 612 (1966). . (3) J-. Acker and E. Schulte, Naturwisscnschaften 57, 497 (1970). (4) See for example U* S. Patent 3,549,537. (5) V. W. Sacger and E- S. Tucker III, "Phthalate Esters Undergo Ready Biodegi*adation," Plastics Engineering, August 1973. (6) See for example U.S. Patent No. 3,754,173. (7) a. Insulating Materials for Design and Engineering Practice, F. M. Clark, John Wiley and Sons p. 246, (1962). b. L. L. Jackson, "Industrial Organic Chemicals ns Alternative Dielectric Fluids", IEEE Conference Paper **C74 265-5 (1974). c. J. S. Hurley and A- Torkeleon, "Silicone Dielectric Fluids for Liquid Dielectics", IEEE Conference Paper #C74 264-6. d. R. F. Burrow and G. A. Vincent, "silicone Fluids vs. Hydrocarbon Oils; A Comparison of Thermal and Electrical Performance Capabilities", At IEEE Conference Paper #C74 258-0. . U-S- Patent 3,740,625. (8) Flexible Vinyla and Human Safety: An Objective Analysis, Regional Technical Conference of the Society of Plastica Engineers Inc., March 20-22, 1973. . (9) Association of Official Analytical Chemists, national Meeting, October, , 1973, Washington, D.C. ., . MOMS 039598 TABLE 1A ' DIELECTRIC PROPERTIES OF DIBASIC ACID ESTERS r'v <2S'C> 1000 Hz) Aromatic Dibasic Acid Esters Ester and its Empirical Formula M.W. Dihcxylphthalata : c6h4[cooc613]2 ' Dllsooctylphthalate c6ha[cooc8ii17]2 / Dl(2-ethylhcxyl)phthalate ' C6IIa[COOC8H17]2 .. 334 ; .. . 350 , 390 Dilsononylphthalate . C6Ha[COOC9H19]2 ; 418 Dllaodacylphthalate . c6h4[coocioH2i]2 Ditridecylphthalate . :, C6H4[COOCi3H27]2 ` . . ... . ; V ' :' ' .. 446 ' . '' ; ; . 520 Di(ethyl-neo-decanoyl)phthalate . C8H4[COO-CH2CH2-0-CO-C9H19]2 ' ,562 D1 (ethyl-nco-decanoyl)tercphthalate C6H4[C00-CH2-CH2-0-C0-C9H19]2 562 Dielectric Constant 5.62 Conductivity (ohm-cm* M 9.0 x 10"U 4.97 1.3 x 10-H 5.n 2.1 x 10-11 4.66 2.9 x 10`12 4.45 2.0 x 10-12 4.08 , 4.3 x 10"13 5.59 2.3 x 10*13 4.53 1.8 x 10-13 Aliphatic Dibasic Acid Esters Ester and its Empirical Formula Di(cthyl-nco-pentanoyl)maleate .. [HC-C00-CH2-CH2-0-C0-C(CH3)3]2 . 372 Dl(ethyl-neo-decanoyl)raaleate (HC-C00-CH2-CH2-0-C0-C9H19)2 . 512 Dlliononylmalcate (HC-C00C9H19)2 ' " ,1- *. 368 Di(ethyl-neo-decanoyl)adipate (ch2-ch2-coo-ch2-ch2-o-coc9h19)2 . 542 D1(othyl-neo-docanoyi)azalato (CH2<CH2>3COO-CH2-CH2-0-COC9lii9) 584 Dlisooctyladlpatc (cm2-cii2-cooc9h19)2 ' ' 393 ,, * 6.61 2.5 x 10-1 5.20 2.3 x 10-H 4.27 4.79 5.0 x 10-13 1.1 x lO'12 4.63 8.9 x 10-13 3.91 6.2 x 10"12 HONS 039599 TABLE IB ` DIELECTRIC PROPERTIES OF HOLLAS :lC ACID ESTEPS <25"C,, 1000 Hr.) Mono-Ester (Alcohol-Acid) M.W. Hcxyl-neo-decanoatc Tridccylproplonatc Didecylvalerate Dodocyl-noo-pentanoate laooctyl-neo-decanoate Tridecylheptanoate Hexdccyl-neo-pentanoate Hcxylatoarato Tridecylmyriatate llexadocylmyristate Hcxadccylpalmitate Hexadecylstearate , 256 v . . ; 256 , / . v 270 . . 270 . ` - 5 . 284 .. , 312 . . /:/326 ' 368 * ' . ' 410 ` - 452 480 . - . 508 Dielectric Constant 3.61 3.62 3.36 3.40 3.52 3.26 3.28 3.07 2.95 2.88 2.86 2.86 01 K CO Conductivity (ohr.i-cm* 1.7 x 10-12 1.3 x 10-12 2.1 x 10*12 1.2 X 10-12 2.8 x 10-13 6.2 x 10-13 2 x 10-14 4.2 x 10-14 3.8 x 10-14 2.6 x lO-14 . 9.4 x 10-14 Di-Ester (Glycol-Acid) ' Ethylene Glycol-bis-neo-pehtanoate Ethylene plycol-bis-neo-decanoate 230 370 5.23 3.86 ** 7.4 x 10-11 1.4 x 10-13 MONS 039600 TABLE 2 ELECTRICAL ASP PHYSICAL PROPERTIES OF PKTHALATE ESTERS yPhthalate Ester _ -. \" ' V _. V- - * . Dielectric Constant Tangent Delta "V AC Conductivity . 10-H (ohn-cm) -1 , Breakdown Voltage > (KV/0.1 inch) - - . Boiling Point-mid (? 5 na fig, *C Pour Point, #C -' . viscosity, cps. 20*C . . Flash Point, COC, 'F .7- Fire Point, COC, *F ' Dihexyl 5.64 9.0 210 -33 50 . 380 ' . 420 ' D1-2-ethylhexv1 5.33 0.14 2.1 28 230 -50 81 425 475 :' Diisooctyl 4.97 0.30 1.3 27 235 -45 83 430 485 Dlisononyl Diisodecvl 4.66 0.05 0.29 4.45 0.02 0.20 30 36 252 256 -48 -50 95 110 430 452 495 515 Di-tridecyl 4.08 0.01 0.04 29 286 -37 230 470 555 oz CO * o u Oo' TABLE 3 - effect of residual alcohol on cokpuctivitv of f.m.t-2065 Tempornturc, Cycle (1000V, CO il7.> 25'C 90'C : 25*C Conductivity n.0~12 ohm-cm"!) Wt% Alcohol Added 0 O.U1 0.1 0.78 1.97 1.98 40 65 320 `3 4 12 i table a ; ' EFFECT OF RESIDUAL WATER ON COHDL'CTIVITY OF EXJ-2065 Temperature, Cycle (1000V. 60 lie) \ 25'C 90* C ' 25* C Conductivity (10" ^ ^ ohn-cri . Wt% Hater Added 0 0.001 0.01 0.1 A. 0.78 2.7 . 3.7 135 .4 165 >400 >400 3 10 25 70 HONS 039602 ; TABUE 5 , '' " PURIFICATION OF ENJ-2065 BY PERCOLATION THROUGH ACTIVATED ATTArULCUS CLAVO) - DIELECTRIC PROPERTIES DURING TEMPERATURE OVOTF Vol. of ENJ-2065 Effluent * ('Gallons) V'v ' .. " ' ' ;. 1 . . V. -1 . DK (1000V) 25C 90 C 25C 4.58 4.50 4.58 Conductivity y. 10' 12 nooovi 25 C 90" C 25C 2.1 55 4.0 ", ' .io ' 4.59 4.39 ; .4.58 ?'; 4.58 ' - , 4-37 4.58 .i , * . .::V.; 20 ' , 4.58 : 4.27 ' " '4.60 ' 4.34 i.59 4.59 1.9 1.6 - 1-6 . 7 1.3 37 35 yf 35 3.4 2.7 2.8 2.8 :"V\ ` /;. ' M " 'y. -22 ' :v/'C- 4.60 ' 4.53 4.59 '23 ' ' ' ,-y, .4.59 ' "V";.vr.26':,:'.5;: 4.60 4.40 - 4.57 9.21 4.64 . 10 1.0 2.6 53 ' 48 330 6.5 6.3 14 i*1* , ,* V (1) Attnpulgus clay 2250g in 3M x 48" glass column. I TABLE 6 A COMPARISON OF THE GASSING TENDENCIES OF ENJ-2065 AMD PC3 (42 Cl) _____ Doblc Cassing Tendency Ceil. ASTM 1 2300, proc. B 65C, 10 KV Results Expressed in Microllters/Min Test Period_______ SO min 100 min ENJ-2065 : FCB (427. Cl) -23.3 . -36.0 . -20.5 -26.8 'TAB IE 7 A COMPARISON OF LONC, TERM STABILITY OF Ei:j-2065 90'C, 1000 V, 60 Hz, Regular Capacitor Taper, No Additives Time. Mrs. 0 ' 96 168 408 504 600 . . .. - TT -4.2 4.1 4.0 4.1 4.0 4;o ENJ-2065 % Loss 21.7 15.5 14 15 14 9.5 PCB (427. Cll J=7 '/ 9.1 * .9.1 8.3 7.2 , 6.9 7.1 . 78.8 78.9 53.6 52.1 46 47 MONS 039604 TABLE 8 CAPACITOR SCREENING TEH' RESULTS W Copacitancc, [lF% LogsC2) A. Initial Measurements 'lOO'C, 300 V/mil 27.5 0.435 B. Life Test 500 hrs, 80-C, 460 V/mil One failure after 190 hrs C. Post Test Measurements 100-C, 300 V/mil 27.5 1.23 (X) Capacitors unit designed for nominal 30 uF and 370 VAC, . after drying at "lOO'C were filled with ENJ-2065 + 0.3 wt.1. Epoxide. .. .' ' (2) Average of six units. , . HONS 039605 APPENDIX I I. Acute Toxicity and Irritancy Studies on ENJ-2065 : .' Acute oral toxicity (rats) - There were no deaths at any dose * level up to 10 g/kg of body weight. There were no significant findings . at necropsy. v, '' Acute dermal toxicity (rabbits) - There were no deaths or signs of systematic toxicity at any dose level up to 3.16 g/kg of body weight. t There were no significant findings at necropsy. - ` Acute eye irritation (rabbits) - There was no systematic effect following instillation of 0.1 ml into the conjunctival sac. Treated eyes were not irrigated. Irritation was slight and confined to the conjunctiva. All signs of irritation cleared by 72 hours. XX Subacute Toxicity Studies on ENJ-2065 ' Six-week repeated dermal application - rabbits - ENJ-2065 -applied dally to intact and abraded abdominal skin of rabbits 5 days/week or 6 weeks at doses of 0.5 and 2.5 ml per kg of body weight. ' . There wss no evidence of compound-related systemic toxicity at 1 either dose level. Dermal irritation was slight. ` :Thlrteen-week dietary feeding study - rats - Rats were fed ENJ-2065 at dietary levels of 0 (control), 50, 150, and 500 mg/kg/day. The 50 and 150 mg/kg/day levels were clear "no effect" levels. The 500 mg/kg/day level was a beginning "effect" level In both sexes - ' Thirteen-week dietary feeding study - does - Dogs were fed ENJ-2065 at dietary levels of 0 (control), 0.125, 0.500, and 2.0% for 13 weeks. After the eighth week the 2.0% level was Increased. " . The 0.1257. level was a clear "no effect" level In both senes. The 0.500% level was a questionable "no effect" level in both sexes. The only effect noted for the males wss a slight Increase in liver weight and ratio to body weight In two of four animals. The finding was not associated with any histopsthology. The 2.07, dietary level (raised to 4% after 8 weeks) was a clear effect level in both sexes. ., An examination of all the data shows that ENJ-2065 has a low order of acute and subacute toxicity add la without any meaningful lrrl' tatlon on the skin of experimental animals. M0NS 039606