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-2- analysls of fluid from A/C ZQ1 and A/C Z02 showed 76 + 1056 500C. The ARB requires a minimum of 80/ 500C for a valid flight test. Shaft Seals; (1425343-JFH) The following cyclohexenyl olefins were synthesized, will be epoxldlzed and evaluated. It Is interesting that the above reaction took plaoe to yield I where the reaction between furan and dlbutyl maleate yielded only starting material. Skydrol Reformulation (RWS-RCR) 1425043 Thermal stability tests were run on THP formulations con taining an AIT enhancer and certain amines. The results were encouraging. THP containing 0.50 percent 2,1,3benzoselenodlazole servived 336 hours in the oxidative bomb test with a final acidity of 0.05. Metal attack was minimal and the fluid was clear and contained no precipi tates. This formulation, see Table I, had an AIT of 825*F, up 125F from THP neat. Those formulations containing 2,6-dlamlnopyrldlne and/or -phenylenedlamlne In addition to the AIT enhancer were much less stable giving rise to metal attack and precipitates. As an alternate to THP based fluids we formulated three potentially lower cost Skydrol LD fluids using TBP/TCP and less expensive VI Improvers. These formulations are given in the table below. Those containing Carbide's FH-25 acrylate VII, and R & H PL 10579 have better shear stability In the 10 hour probe test than Skydrol LD. Shaft seal, thermal stability, and valve tests are planned to evaluate these VI Improvers. HONS 036053 MONTHLY SUMMARY DETAILS - APRIL 1970 FUNCTIONAL FLUIDS - RESEARCH AVIATION FLUIDS Skydrol 500Bi Marketing Technical Service (JFH) Boeing le Installing an AIT apparatus per ASTM D-2155. They asked us to run four fluid samples to check their apparatus. Results are: Phosphate Ester "A" Phosphate Ester "B" Engine Oil "A" Engine Oil "B" 735F 930F 765F 755*F The following fluid samples were analyzed: Fluid: PIA Utility Reservoir Texas International A/C 307 Right Systems Left Systems Vise. 100F 210 "F 7.88 cs 2.60 cs 9.49 cs 3.10 cs 9.32 cs 3.04 cs Acidity 0.29 TAN 0.25 TAN 0.34 TAN Moisture 0.45* 0.30* 0.34* Density 1.0647 1.0591 1.0593 Skydrol 500C Flight Test (1425245 -jfh) The properties of fluid samples from PAA received to date were analyzed by Jack Hlnchen. The following conclusion can be drawn based on the assumption that aircraft top-up was the same for both the 500B and 500 C airplanes. The overall conclusion Is that topplng-up a system with 500B does not affect fluid properties. That Is no reduction In acidity Is shown and the additional stabilizer is rapidly used up. In the 500C aircraft 11/2 top-ups stabilizes acidity at less than 0.4o TAN and stabilizer levels are high and remain that way. The 500B top-up shows no effect on viscosity but 5O0C viscosity approaches new fluid values. The 500B/500C mixtures In aircrafts after two 500C top-ups the moisture level Is 0.30* and remains constant thereafter. The 500C flight test at BOAC In Boeing 707's Is underway. An analytical method wbb developed based on the VI improver's differences to determine the amount of 500C In 500B used samples. The method's precision needs to be refined but HONS 036054 OP-lfZ(cll-l 7a-.Cc% TBP h. h% TcP If. so 7 UF&f / /w>/ a f/A/Jv o- a?7 H>o. V/At'jrzdjj ( *>) (0 o`F a/o *f 3(?6 u.u 3. S3 r&MI-Z. IfZUFl nifrtitf ?.?j7 itP I7.0D 7. PLKfi'j /Ho*?* LiMtyWf 0. it) 7 7=7/ 77*7 fho to.ibV rtf' ll.rff. TzP 7.8.0% FHZT / %brl lu<<*-/ 0. iD'/ F///72- A 77"7 ^-,0. 39/ II.l*) 3.8% /M9 3?7 ' / a3c. oM^i 0. w t. Vjuat, cMjX #7"^ruiv. 7o nuii 3~L. (, 4. /o -i'v,. -- - - Wi 9_>v 163 111 9.V7 *77 l.rl 7.J7 fJtTSs: l. cPx.fF&kit&d&p&.h' . /,.i Ltk: / f/c. c~ ^ aMw3 Sff/lb si. Frias' /Z /?/,) cl ri,.C'(, AU.<xJt *ff sr'f/ U-.L (fdJ( > tcl) x / r- 7o 3- Vistesny or S/'ydi<-,/ UHr r. ( [^ (, fU, l-.i..- J.tXLJ'. ` HONS 03605b -4- (1425243-RWS, RCR) Two shaft seal tests were run on formulations containing 3.4- epoxycyelohexylmethyl acetate and 4-methylcyclohexene oxide. The results of both tests. No. 54 and 55, were good; no leakage and little to no deposit formation. The formula tions were based on DBPP and contained the 500C additive package less PC-98 and Unox 221. The concentration of each epoxide was set so as to give the fluid an initial oxlrane content of 0.35-0.37$. The major effort was directed at scaling up the synthesis of these and other epoxides. 3.4- epoxycyclohexylmethylacetate. This material was Initi ally prepared using m-cnloroperbenzolc acid. A product of high purity (99.5$ by G.C.) but mediocre yield, 51-52$, was obtained. A better procedure was needed owing to the relatively high cost of m-chloroperbenzolc acid (S(23.50/100g). A procedure using peracetic acid was developed, (Peracetic acid Is Inexpensive: go.48/lb in bulk; $1.25/lb In gallons). This procedure is similar to that described in USP 2,838,524 and USP 2,716,123 wherein sodium carbonate and sodium acetate are used to buffer the reaction and retard formation of autoxy compounds. A 84$ yield was obtained. The product distribution was 92$ epoxide, 8$ olefin. This Is similar to the epoxlde/olefln distribution In Unox 221 (89/11). The procedure Is adaptable to the other epoxldatlons we have planned. Methyl-3.4-epoxycyclohexylcarboxylate. This epoxide was prepared using the peracetic acid method described above. The product consisted of 83.6$ epoxide, 16.4$ olefin. The synthesis Is being scaled up to provide sufficient material for several shaft seal tests. Two routes were used to prepare the starting material methyl-3-cyclohexenylcarboxylate. The esterification of the acid in methylene chloride was easy and direct; however, the acid Is expensive ($19/100g). The Diels-Alder synthesis was superior. The product was obtained In 889f yield from the AlCls catalyzed reaction of butadiene and methylacrylate. This procedure follows that described In J.O.C. 30,3567(1965). Future 1. Shaft seal tests will be run on 50OC type formulations containing the following epoxides (prepared via peracetic acid) a. Me thy1-3,4-epoxycyclohexylcarboxylate b. Dimethyl-3,4-epoxycyclohexyl-1,2-dlcarboxylate c. 4-methylcyclohexene oxide 2. Bomb tests at 225 F will be run on fluids containing each epoxide at 0.35$ oxlrane In DBPP at 0.50 HaO. M0NS 036056 r WBte r Zl'ST0 Oxi&ffnVE W>6m& TksryJS OAi T&HexvLPHosPMm FbZjnuL/mbHS. (LomPccrns/J TEST F'/z/Al Mrs. fb Mewl AttAcJc. UZHSTH TA/J_ jp. SOTA/i -QJ. J ccL y ' /9C39&-J | 977 /? TUP(toTI'llTN-lij 33 6 I i i? `It tMur^'yyj ' o-sTJ. 6.S~% 2.li)3-BejJZo?&levA O.OS' /7/3 -6/6 -6 ov -0.07 Moz9u>-A 9i3l mKimiH-lj) 336 ; i`(e% UmyTtjj 0.f'7c [ *,1,3- &e.*pzeJt.vfidiijtliL. \ 0. I It f, i~(.ha. 'm,-A-tpy` nd/rA \ 0.T27, iho, : im%-3 j 97 / THP` / Um^ni ; O, Sb7, 7 j) J-- -y fe. 0-3o/e 0- y!e.tje- dtam/Kt?-* O 3.2$ -^57) f0.0.3 1-0,3/ -/.of -y./y ~0. of 0,72 k/i^ -O.OV^-O.fef '/.>/ -0.3< -0.03 MONS 036057 9i,d]- flip- i.L*], Uvi^l | & A u, / 3 ~~ 0-1*7, 2,U fJLtu/nlfiJO - vyrid,^^ / 0,3Cf,7, 0-fi-..,Jyj\ I Citd 'P.a'.' j O, Tbj, /7,0. j /6? : 6.3^-jW^o ifo.o.2. -6,^6 -2 U -<2. ZZ 3.03 IIS^F (jx/OETive Borne lesntJFj. Epoxids Exfmiffnoti mJ Sboa. Type fim/q. ComPosiTTo/J TEST F/uftL firs 10 fflerm. AttKF- L&JSjTH ~77M/ \o.soW) tf/ a- 131 &?/-! -1L>.V],, VBPP- TotHF4n-(3rt 0^03 ?/'j) 'rthdz); 10.0% (lb% S hkds )j 4. ^7 UtJtom C/]/i.:de C'/v;/4 oc-olcf/lj epo'dde*j Osd7 P7//3X.; 0.14% HiG. Xlot 1.37 ^</o Nil o. 77 -0.33 y-o.t/ A//4 /2/?/-2- m.tol 2>8fp' 7.o7. 3C Q*o32l-> /o. o7. PLHUl'j 2,47* OflUhzterje- oxfdt,- c.r7. Fnriv? c.m7. ^ 0. /> -37r -0.02. -1.19 -O.tfO 4 0./9 40. Ot 121 C 1-3 .! 7?.xj7. tfP; 7,o7tfp7/Zj j/o.o7. pLdZil^ s?7. WKy- | cyc/o/vevyLAiewyt f^erh-n., (c.>S%. pj.&) 3(,o /.Z3 '34 po.o9 ~3-3<P -0.1/ -x# 40,03 3O 3 OU< o -7- Shaft Seal Evaluation (1425235-RLO) Eight DBPP formulations were evaluated for shaft seal leakage and deposit. The two formulations which used diepoxide. Unox 289, caused high leakage and deposit. The six formulations which employed other acid scavengers did not leak although one had some light deposit, A formulation MCS 986, using Epl Res 5014 had light copper transfer from a thrust bearing cage to the races. The Seal Reports 48 to 55 are attached. (Pages 8-15) SST Hydraulics (1409055-RLO) Due to the Hydraunyooll B pump test failure by high wear and copper transfer in the AP10V/280F (3l8F hot Bpot) pump, a lubrication test was devised to screen candidates before pump test. The test employs the LFW machine under the following conditions Test time Test Temp Ring Speed Load 24 hours 280F (or pump test temperature) 200 rpm 8 lbs (53 psl) with conforming Pynalloy 603HT bronze conforming blockB on hardened steel rings. The bronze alloy Is the same as that used on the steel on bronze wearing surface In the AP10V pump. The forging conditions are the same since the test specimens were machined from pump cylinder barrel forgings. The weight loss results are; Test No. Fluid Wt. Loss mgs. 603HT block E9310 ring 1 Used Hydraunycoll B from pump test 36.0 5.1 2 New Hydraunycoll B 32.7 5.6 3 Skylube 450 0.8 0.2 The results for Skylube 450 were so encouraging that a 26o*F/AP10V pump test was started and at 210 hrs there are no operational problems. The wear correlation between the LFW wear and pump test seems to be correct when com paring the 156 hr failure of Hydraunycoll B to the Skylube 450 pump test. If the Skylube 450 pump test is successful, the next test should at low temperature AP10V pump test with a Bendlx valve test in parrallel with the load valve. The low temperature pump test would determine If K-salt mlcell formation blinds filters at the low temperature and the Bendlx valve test will give a measure of the Skylube 450 erosion resistance. MONS 036059 -8- SHAFT SEAL PERFORMANCE EVALUATION Fluid Formulation OR 140381-5 til.73* D3FP (A-D) 3.Hit HF-412 4.551 Unox 289 0,02% Benzotrlazole 0.25 HaO Summary ol Results The total leakage In 2l4 hrs la 478 grams. A heavy resinous deposit covers the stator seal face. Visual Condition AP10V Shaft Seal "Bearlum" Bronze Stator. Leakage path from outer to Inner diameter. A heavy amber reBlnous deposit covers the entire seal face with a heavy concentra tion outside the sealing area on the atmospheric edge. Light wear Is under the deposit. 0 20 40 SO 80 100 120 140 ISO 180 200 -- Tesl Time (Hours) -- MOWS 036060 -9- SHAFT SEAL PERFORMANCE EVALUATION Fluid Formulation OR l4oj8l-4 91.25* DBPP (A-D) 3.4o* HP-412 4.85* Unox 289 0.50* FH-132 0.27* H*0 Summary of Results The shaft seal had a total leakage of 6u4 grams In 212.0 hrs. The seal face has a white flaky deposit and no wear. Visual Condition AP10V Shaft Seal "Bearlum" Bronze Stator. Leakage path from outer to Inner diameter. A moderate amount of white flaky deposit covers the center of the stator seal face. The atmospherlo edge has a black sludge concentration while the fluid Bide edge has no deposit. No wear Is seen under the deposit. 0 20 40 CO 80 100 120 140 160 180 200 -- Tesl Time (Hours) -- MONS 036061 -10- SHAFT SEAL PERFORMANCE EVALUATION Fluid Formulation mcs 966 77.8a> DBPP 7.2* HF 412 In DBPP (30* Sol.) 10.0* PL 4857 in DBPP(30* Sol.) 4.50* Epl Rez 5014 0.05* FH-132 0.22* HaO Summary of Results In 213.7 hrs no leakage occurred. The edges of seal race have dark staining but no deposit 1b found. Visual Condition AP10V Shaft Seal "Bearium" Bronze Stator. Leakage path from outer to Inner diameter. The edges of the seal face have a dark Btainlng while the oenter of the face is dean. Tha seal face has a uniform smearing wear. Test No. 50 800 700- Tester No. C-l 600-h Temp. 225*P Time to 5 grams/hr. 500a 3. 400 -h ~ r 300 4-' Other Stator thickness vari- . atlon is 0.0003 in. Bearing cage had light wear and copper trans- inoL fer to balls and raoes. T ' !-. no leakage 80 100 120 140 160 180 200 - Test Time (Hours! -- MGNS 036062 -11 - SHAFT SEAL PERFORMANCE EVALUATION Fluid Formulation OR 140301-1 76.3* 7.0* 10.0* 6,2* DBPP (A-D) HF-412 In DBPP (30* Sol) PL-4857 In DBPP (30* Sol) Olefin Epoxide 0.5* FH-132 0.24* HaO Summary of Results The seal stator haB light staining and no leakage was observed during test duration of 212.3 hrs. Visual Condition AP10V Shaft Seal "Bearlum" Bronze Stator. Leakage path from outer to inner diameter. A light rust oolored stain oovers the seal face. The stator has light wear. Tst No. 51 Tsster No. C-2 Tamp. 225*F Tima to __ S jrams/hr. Other Stator thickness variation is 0.0003 in. 800 W H -1 1 700 600 tf> ' : S- 500 :. aro <9 - 400 .. : 2 m 300 I:' | -i 1t ! . .. ... ^ - " ' (.......... : 1.. 200 100 i' ' no leakfirc 20 40 60 80 100 120 140 160 180 200 -- Test Time (Hours) -- MGNS 036063 -15SHAFT SEAL PERFORMANCE EVALUATION Fluid Formulation OR l*+o201-2 80.1096 7.0* 10.0* 0.5* DBPP HF-412 (30* Sol) PL-4857 ( 30* Sol) FH-132 2.40* Cyclohexene Oxide 0.24* HaO Summary of Results The leakage Mae 1.6 oc In 22,4 hre. The seal face hae staining and light wear. Visual Condition AP10V Shaft Seal "Bearium" Bronze Stator. Leakage path from outer to Inner diameter. The seal face has a bright copper color surface In the center with rust oolored stains on each side. The center of the seal Is lightly worn. Tost No. 53 Taster No. C-2 Temp. 225 P Time to -- 5 grams/hr. Other Stator thloknesa variation Is 0.0002 in. 800 !ii. 1 ..1 . .:q 700- : .......... " i...... : t/i 600- s : .. .i ...4. . ,|. L. ......... a* ; '! ; 500' 1 ija<Qe . to ...3.1 400- ; ; 1 ...; i. ... .........i--. ^ : 5 300- . .. . i 1 !...,L .1 . 1' . : . 200 100. - In. 1.6 oc leakage 262.J* hre . .! \ 40 60 80 100 120 140 160 180 200 -- Test Time (Hours) -- MONS 036064 -14- SHAFT SEAL PERFORMANCE EVALUATION Fluid Formulation OR 152601-1 78,7it DBPP (A-D) 7.0S HF-412 (30S Sol) 10.OS PL-4857 3.8S 5,4-Epoxycyclohexyl methylacetate 0.5S FH-132 0.22S H2O Summary ol Results The total leakage was 1.8 cc In 254,8 hrs, No deposits were present but the seal face haB pitting and light wear. Visual Condition AP10V Shaft Seal "Bearlum" Bronze Stator. Leakage path from outer to Inner diameter. The center area of the seal face Is pitted and lightly worn while the edgeB have light rust colored stain and little wear. Tost No. 54 Tester No. C-l Temp. 225*F Time to -- 5 ttams/hr. Other Stator thickness variation 1b ,0.0002 in. 800 700- - < i-- . . . V: 600- - B<9 ' ' .a 1 . 500' .. 0># --tI... . . 1 .. ' 2n 1i : ' , 400- -"-:l ' : 1 .......... 1' .. 8 :-| : I r 300' - w - j .... , . 200 - '"rt ' ; 100. 0 20 40 1,8 cc leakage In 238.4 hi _________________________________ J4 60 80 100 120 140 160 180 200 -- Test Time (Hours) -- MONS 036065 -15- SHAFT SEAL PERFORMANCE EVALUATION Fluid Formulation OR 152601-2 80.0* DBPP 7.0* PH-412 10.0* PL-4857 0.5* PH-132 2.5* 4-methylcyclohexene oxide 0.22* HaO Summary of Results The leakage was 1 drop In 200.4 hre. Light deposits and stains are on the moderately worn Beal Pace. Visual Condition AP10V Shaft Seal "Bearlum" Bronze Stator. Leakage path from outer to Inner diameter. The stator face has a light resinous deposit on the atmospherlo half of the dynemlo eeal area. A thin black ataln-deposlt Is on the center area while rust and copper color stains are on the fluid half of the eeal faoe. Moderate wear Is present. Tost No. 55 Tester No. C-2 Temp. 225*P Time to 5 jrams/hr. Other Stator thickness variation Is 0.0002 In. 800 700t--h~' 600 P 500 f- 400* Iw 300 200 4 1001 :.... l-.u... i................... j ; l j- ' ' ' !1 drop ln|2do.4 hrsl _ ; : ..........: i\ : : 0 J. 20 40 60 80 100 120 140 160 180 200 -- Test Time (Hours) -- HONS 036066 -15SHAFT SEAL PERFORMANCE EVALUATION Fluid Formulation OR 152601-2 8c.0 DBPP 7.0* FH-412 10.0* PL-**857 ' 0.5* FH-132 2.5* 4wnethylcyclohexene oxide 0.22* HaO Summary ol Results The leakage was 1 drop In 200.4 hrs. Light deposits and stains are on the moderately worn seal face. Visual Condition AP10V Shaft Seal "Bearlum" Bronze Stator, Leakage path from outer to Inner diameter. The stator faoe has a light resinous deposit on the atmospheric half of the dynamlo seal area. A thin black staln-deposlt 1b on the oenter area while rust and copper color stains are on the fluid half of the seal face. Moderate wear Is present. Test No. 55 Tester No. c -2 Temp. 225*P Time to -- 5 gtoms/ht. Other Stator thickness variation is 0.0002 in. BOO j 700- -p ... 600- r> <6o -- ___ l_! 500- -a- s 400- US J ..... 300- ..a ... ! .!.. . , th- -. J-.- i J:__ i__ ;... i .. :-.. |1 :. -- j :1 . .. ... M-t - -!....... : ;1 1 ZOO . ...\ too. t ........ 1 drop In 200.^ hrs. _ \ 0 __________________ 0 20 40 60 80 100 120 140 160 180 200 -- Test Time (Hours) -- MONS 036067 -16- Metals In Solution (1425235-RLQ) A 24-hr. LFW/280F/200 rpm/8 lbs load test using Mueller Bronze Alloy 603HT on E9310 steel was performed on Skydrol LD, QL 30. The metal combination Is the same uBed on most sliding bronze on steel surfaces on the AP10V pump. The bronze test block was conforming to the steel ring which allows wear with little change in geometry which Is more simulative of pump wear than the 4-ball test. The weight loss results are: 0.3 mgs on the 603HT Block 0,4 mgs on the E9310 Ring A 72 hr test under the above conditions will be run too. If wear Is accelerating and to determine If copper solubility Is accelerating between 24 and 72 hrs. Skylube 450 (1432159-SLR) A Skylube 450 production run was made In the W-Bldg. facilities, totalling 2000 gal In 5 batches. Some plugging of the final cartridge filter was experienced, but It was determined that thie was not due to the fluid, but rather to rust and scale in the system. All five batches were satisfactory on foam, Pb corrosion, Ryder and 0 & C. Two additional batches, representing reworked QM-5, an earlier batch that had been double-charged with amines, gave high Mg corrosion In the 0 & C test. A lab reworked sample gave a good 0 & C test. The W-Bldg reworked batches will be further checked. Analyses (by RAL) on the latest samples of used Skylube 450 from the Northeast Utilities Industrial Jets Indicate continued satisfactory performance. One engine has over 620 hrs since oil drain. Stauffer Jet II Is seeing considerable service in Industrial engines. The lower viscosity of a sample of Stauffer's used oil compared to our sample of fresh Stauffer Jet II suggested that a VI improver might be present in their oil, but sonic shear and other tests do not Indicate the presence of a VI Improver. Analysis of the base stock shows it to be a PE ester of butyric (9.5^), hexanolc (0.5%) and heptanolc (90%) acids. Analysis of the additive package is Incomplete. We have prepared complex ester salts In which chloromethylphosphonlc and methylphoBphonlc acids replace the phosphorous acid. These salts will be evaluated In Type II formulations. We will be looking especially for possible Improvement in load-carrying properties compared to the phosphorous acid complex ester salts. HONS 036068 -17- Tentatlve Processes (1432259-SLR) We have duplicated the literature preparation of 5-nltrolndazole, a 5-AI precursor. Modifications are being studied to adapt the method to pilot plant size preparations. A problem which may complicate self-manufacture of 5-AI Is availability of an Intermediate, 2-methyl-4-nltroanillne. American Cyanamld has stopped production of this material. Central Purchasing Is seeking other sources. Nyco PluldB (1452359-SLR) We have confirmed that addition of our complex ester salt to Turbonycoll 93, while showing some Improvement In 0 & C tests, does not bring It up to Skylube 450 performance. Comparisons are shown m the accompanying table. CRD acids (14^2459-SLR) Enough Ct and Cs acids are purified and sufficient Cs acids are expected Bhortly from CRD to prepare a base stock sample for Ryder scuff test. Inadequate agitation in the 5-gal glass-lined autoclave will necessitate further modifications or purchase of another reactor for synthesis of large enough samples of acids to make fluids for bearing rig and fatigue teBts. cirri' sacts w r*A6tirre,n 9} d e r firs AtxtrC ,* ", y/y /ire. *1 ZL f* St, c m i c 7~VA6'>*'yCl,L. 73 JP6S 7v*B**YeL. 93 t /(-Sitr /ss- -H.t **,*/ 1MO.OZ -0.7J2 -J1 /o.ti M0,;S mO,X -o. Syyiuse i., Ate tf-sscr S/yyiute Jr* as \ AOACO AC'Vc) t '7( MO, + 0.0? MO.dZ -O.iS `>.11 -o.ol + O.OZ. f 0.0 i -9.3/ ->.>.,)/ HONS 036069 -18- Santomelt (1405343-JFH) Technical data la being collected to present to the Air Force for Santomelt's use at their Tactical Air Bases. The required performance properties required are: Our Results Immersion corrosion Stress corrosion Magnesium corrosion pass pass report The magnesium corrosion data collected is below. mg/ln2 Distilled water (control) 0.45: o.39 10* Santomelt in dlBtllled Ha0(pH-7) 38.4 105# " "" " (pH-10.5) 34.1 25# " "" " (pH-7) 34l 25# (pH-10.5) 320; 343 Since the Air Force is Interested In the 10# solution values our data Is well within their desired values. Santomelt for Commercial Use - The three problems facing Santomelt before complete acceptance are: a) Aluminum Sandwich Corrosion b) Hydrogen Embrittlement/Stress Corrosion c) Magnesium CorroBion The seriousness of the effect of magnesium corrosion Is not completely resolved. Progress was made in controlling the aluminum sandwich corrosion by Increasing the concentration of the sodium meta silicate used. At present It Is a toss-up as to Include the fomamlde In the Santomelt formulation or not from a technical point of view. From a raw material cost picture formamlde should be excluded. A test was developed to evaluate the hydrogen embrittlement area and to ascertain the difference between stress corrosion and hydrogen embrittlement. Work In this area continues In search of a solution. MCS 990: 75# formamlde/20# urea/5# HeO - a deicer developed by Canadian Dept, or Transport, ran into hydrogen embrittle ment problems In Air Canada'b testing. Since we developed a process and agreed to custom manufacture MCS 990 for Canadian DOT, we had the hydrogen embrittlement test checked by an approved Independent laboratory. Test results show the product as manufactured passes but a 1:3 dilution with distilled water falls. HONS 036070 -19- INDUSTRIAL FLUIDS (WHC, PDF, PFH, LFS, LRS) Pydraul Reformulation Pydraul 625A An additive package has been developed to Improve the pump performance of 625A. The V105C pump had a total weight loss of 20.2 mg which Is equivalent to the previous per formance record (Fyrquel 220-18.4 mg total) and signifi cantly better than Pydraul 625 or Fyrquel 550. A process amendment to Incorporate the additives Is being Issued. Samples of the additive version of 625A and Fyrquel 550 have been sent to Alcor for deposition testing. The oil gear test Is at the 450 hour mark with no apparent wear. The raw materials coBt of the latest version of 625A Is *1.77/gal versus *1.79 for 625. Thirty-five gals of Pydraul 625A identified as Batch OR 139046 was blended for laboratory pump testing (V105C). 49.10# wt. 49.50# " 0.30# " 1.00# " 0.10# " + 0.02# 20 ppm Aroclor 5442 Santiclzer l4o Santolube JQA Unox 221 Benzotriazole FC-98 DCF 200, 350 cs The above formulation was tested In the V105-C pump stand with excellent results, total weight loss amounted to 20 mgs. Pydraul 5^0A The V105E results on an additive version of 540A (TBP and Cu Inhibitor) look excellent. A V105C test Is underway. The tentative process for 540A Is being written. The raw materials cost of S^OA Is *.&f/lb vs. Sf.83/lb for 540. Five gals Identified as Batch OR 139051* was blended for laboratory pump testing (V105E). MONS 036071 -20- 59.0056 wt 15.105* wt 52.00# wt 11.00# wt 2.50# wt 0.50# wt 0.10# wt Aroclor 1242 " 5442 Bright Stock 200 TCP TBP Santolube 70A Benzotriazole + 20 ppm DCF 200, 550 c8 The above formulation was pump tested in the V105E screen ing pump with excellent results, total weight loss less than 10 mgs. A second batch of Pydraul 540A (40 gals) was prepared (OR 159055) and is now being pump tested in the V105C pump stand, a portion of thiB fluid is reserved for an 011 Oear Pump Test (scheduled for late May). Oil Oear Pump, Pydraul 625A (OR 60697) has now accumulated 500 hrs.j indications point to a passing test. Pydraul F-9A A screening pump test of the Santicizer 711 version of F-9A is underway. If these results look encouraging, further properties will be gathered. Pydraul A-200A Testing will be completed as soon as possible on the 1242 version of A-200A. Two non PCB versions of A-200A will be evaluated. Highest priority will be given to the TCB/5442 blend. The other will be a Arobromoclor 1252/5442 combination. Pydraul 512A After four runs on the computer we have evolved component viscosities which blend in a linear manner. The latest printout had a measured viscosity at 100F within 2 cs of the pre dicted value. The next round should be within 1/2 cs. Once the linearization of viscosity is accomplished, the computer program oan be used for the calculation of Pydraul 155, 250, 90 and 540 blends. The calculated FR level wsb verified on a limited scale by full scale fire testing. A blend containing Arobromoclor 1251 was equivalent to Pydraul 155 on the FW spray and hot manifold. It waB better than Pydraul 512 aB predicted. The composition of TCB/5442 and Arobromoclor 1252/5442 blend at various levels of FR follows. HONS 036072 -21Pydraul 135A It appears possible to remove PCB's by utilizing TCB/5*>35. However, the sediment formation in 5^35 blends will nave to be stopped. Anniston Is working on the problem. Analysis of the filtrate from a 5^35/TCB blend showed a mixture of mono, dl, tri, and tetra chloro terphenyl with about 70% being dlchloro. Anniston doubts these results and Is running their own analysis. They believe the material to be slightly chlorinated quaterphenyl. The sample of 5035 sent for distillation by QET analyzed as 3^.2% Cl. Anniston Is working on 35-37% Cl materials, dene Arnett feels that the specific gravity changes rapidly enough below 37% Cl to enable process control to + .5% Cl. HONS 0360^3 -22 Ccr'y'mLi'-', , j P V' C p V' t \- j o $\Zfl F.l'')'vK> j 4 ~X '6 - 0.0 a- j i W'.' i ^iTf- Vr o fc^ / o t 320 //)r6c'". Of.5. TB? C t>? TCB . 5442: C'-./c 1a;,'- y`;o'r' A>. CM-Vl Vi'i' /Oo''i~ So.Z% 2.5 4.5 2 4.6 3 8. 2 co J. O fjLs <4 n i Calc bens 1. 16 / Co st / \b fic tud) Cot.iT/Tj 31 /.ol 1 f a h- 2 b - -a 3 S.7 2.5 4.5 34.7 32.0 0 7. Os* (j 5. O S i. 130 AoSl /.IS# 2: /4 - X fc os i.a PJ.-Hvt.i | 4.-J. r-': 4.5 Z4.f> 2 7. 1 6 / r.'' - -- /.oil o7IJ rTCff Br."3. T3P ; CD? ' 8)2 32. 5442. Calc, {/ isc <s i oorf fie t in? 1 Cfi/e. D'- ^,j 1 Cr^t/Uc A-V b''.r'j, t>y Cor. -f/g 5 / 2 1. 3 ?. 5 45 36.7 2 7.0 & l.C^/^c -- 1.2? 3 34.7 2.S 4.G 3 6.4 2 /.4- 4 7.0,* <54.5 S/v 4 (> 7. -r 4 :: 3/0 id 4 / o.-v .... . /. 1 13 ^ 0^?> /. 1 Oo ,,444 / /62 On-f MQNS 0360 74 . -23- pydrawl 625A, Ac-A. AC-A W.Q. 88 Viscosity-temperature curves, Timken loads, relative drop sizes, and Falex Wear and Load were obtained on the rev ised air compressor lubricants for a revised sales brochure. These valueB follow: Pydraul 625A Pydraul AC-A Pydraul AC-A, Winter Grade 28 Timken O.K.Load 30 45 24 Film Strength 11,700 15,100 8,600 Listed below are results of Falex Load and Wear Tests on Pydraul AC-A, Pydraul AC-A Winter Orade 28 and Pydraul 625A. Tests were run by the Chrysler Procedure, Falex Load Test Passing Load Pydraul AC-A Pydraul AC-A, W.Q. 28 Pydraul 625A 4025 lbs 4175 Its 4250 lbs Passing load was determined by the average of two tests. Palex Wear Test Wt, Loss,Pin Wt, Loss, Blocks Pydraul AC-A Pydraul AC-A, W.Q. 28 Pydraul 625A 0 0.6 mg 1.1 mg 0.5 mg 0.9 mg 5.8 mg HONS 036075 -24- Drops/ml at 25C Mobil DTE 24 Mobil DTE 26 Pydraul f-C Pydraul AC-A Pydraul AC, W,G. 28 Pydraul AC-A, W.O. 28 Pydraul 625 Pydraul 625A Fyrquel 550 ' Fyrquel 220 Fyrquel 150 Fyrquel 300 37 36 41 39 39 4o 43 39 37 37 37 37 The new formulations are completely miscible m all portions with' Fyrquel 150, 220, 300, and 550; Houghtosafe 1010, 1120, and 1130; and our new phosphate esters, MCS 030E, MCS 050E, and MCS 0115E. HONS 036076 KINEM ATIC VISCOSITY. C fN TlS TO K C S K IN E M A TIC VISCOSITY, C M NS YOKES KINEM ATIC VISCOSITY, CSIITISTOKES KINCMAVIC VCiCOSUY, " N tM A T IC VJSC0S11Y, C IM TIS TO K tS `5'JVOASIltnD AAIS035IA DUVV.OMM MONS 036079 viscosity, srtvtOLt uinvensAL sccc.vds 9 . -* .it VISCOSITY, S A Y C U ll U llIV tlW A L SICONOS T 0 9 0 SNOW VISCOSITY, SAYUO U UNIVCRSAt. StCOHOS visco sity, sayo it u iiiv n iS A i. slcouos ?0O9O SNOW VISCOSITY. SAYUOIT UIIPVCRSAl SCCOPPOS * v is c o s it y , s a v p o u u m v c ritfA t scco n. o s \ - lf\ I I rv SI SIX. V tX iV_j I M m> M1 M irycraui ivieasureu visvudu:^ i In Sav'jcit Seconds Universal ' Pump manufacturers recommended operating range between 70 SSU and 4000 SSU. i M !ViI\ VI -XX x_ %X ! H 1 V \ V 1X --1--:---- ------ I-----1t x L S V. X\ X __ 1 r PTCCAUL 40 ; PTCRAU1312 PTDRAUL 230 PY0KAUI 135 PTORAU*. 90 P/JXA'-'C AC-'A*, w"*rf f 1 --1-- 1----- ---- ,----1 ----- 1----'------------- ; 1 --!-- ------ ! Xv -~v rv jv N \-x | v . \N \ [X S'i S [\l --r^r VnU V \X s \ VI1 Xk \ V S X>kS \ X XX V 1 '..i Mill JJ : i 1i ii --i 11 i -- vs X rx > V 'l V i * X\ X i X X XX X x Xs --1 5X X X > sx V X | M M m m m m m n m m mm mm HtwmmmmMt* mm ,, nKPtMTUH, ottins ruiaaMSiT ' Jj -31- Oerman Mine Fluid A Tentative Process was written for Pydraul 28l, a revision of Pydraul 280 which provides improved low temperature performance and eliminates the use of Aroclor 1260. Fluid Recovery and Reclamation Initial work to assess recovery of PydraulB from customer effluent streams has been started on samples from Johnson Motors, Central Dlecastlng, Lester Castings, and Timken Bearing Co. Qualitative results Indicate large amounts of solid material present with the oily layer. Flltratlons have been difficult and relatively large amounts of fluid remain with the solids. This work will continue to provide more data on quantity and quality of fluid recovered as well as suggesting methods for recovery. Turbine and Air Compressor Lubricants European Steam Turbine Control Fluid Samples of Qelgy Reolube TF 90, Reolube HYD 110, and trlxylyl phosphate were screened for possible use as steam tur bine control fluids in Europe. Of these the TF 90 material was considered the best candidate at this time. Tests run to date Included 350F 0 & C, beverage bottle hydrolytic stability, and a screening pump test and wick fire tests on the TF 90. MCS 979 The field trial at the AQTL Cremona station has passed 800 hours with no problems. The Inner bearing on the DeLaval booster has reached 192F on several occasions and AQTL is keeping a close watch on the situation. Tom Oneson has requested us to formulate a lower vlBcoslty fluid In antici pation of warmer weather. We would then be going back to essentially the same fluid as MCS 97^. Perhaps an AIT enhancer could be utilized to upgrade the FR of MCS 971* but It Is roughly equivalent to Pydraul 135 now. Water/Qlycol Fluids A Tentative Process for Santosafe W/Q fluids blending using Carbide concentrate and thickener has Issued. A capital project for equipment to blend these fluids at JFQ plant has been approved. A possible relationship between lubricating properties of W/Q fluidB and the oloud point at higher temperatures has been checked, (polyglycol thickeners have an Inverse sol ubility and come out of solution at higher temperatures.) HONS 036083 -34- oatlon. HONS 036086 ^ j(sAyC.-^t -35- fzJLo^d! C^^fj>^-4zu j**d*Zs Vdt``Al iSOCp iqi~Z00F (J/ja U.^m^ wo m yt**/ ^ / y I ytt/J/-*, Z 1/ Ut*\ /5oi r l4n*ff4cZZ+-o/-<L. 5*Z0 flos-Z/Z. ) 5-Z TLo 3 4* Pol/lA* w/G / oo FK, /50505 fctM. MWac fr z.oo \^/aJ?'f,t'A* WS&** tAtxy k'&y^ 6 ?-o >&/j F-/~" 3 / 3 >l~5 tn-h* XZ2> ^O-CfZ >2?*<P &o -Z/o 5 nt'i*- ^ r G > 7 l**fcr* 8" t " / O Vt^pcvT. *8&*^&**^c* W^G f 5 <0<w4,'Vc wf& ^D 36urtr^ 3o j^M*/>-' l4/j/<3 C^ckrf.t'tZL' fsj<t-Z/7 -- -- *.'y-z/* -- -- ---- >z3o -- -- HONS 03608 7 -36- Phosphate Eater Hydraulic Fluids Pump teat results on the pilot plant prepared cumylphenyl nonylphenyl phosphate ester are listed below. MCS-050E (OR 142228)(NCPDPP Ba. #1)- 220 SSU which was pre pared by D. L. Kocher was pump tested In the V105C pump stand with excellent results. Total weight loss was less than 20 mgs which Is comparable to Fyrquel 220. MCS 050E (OR 139050) 220 SSU which Is Identical to the above formulation, but using Pilot Plant Batch #2 (NCPEPP) was pre pared - 65# NCPDPP Ba. 2 35# TPP This formulation is presently being pump tested in the V105C pump. Preliminary Inspection Indicates a reproducible test. V105C Pump Stand "J" is presently being modified for testing phosphate ester fluids. MCS 030E Is scheduled to be pump tested In this stand; start-up Is scheduled week of 4-26-70. Phosphate Ester Hydraulic Concepts (1315635-RLO) Two base fluids NCPDPP and OXDPP, one fluid with a surfactant additive NCPDPP + 0.04# PC 98, and two competitive fluid formulations Fyrquel 220 and Fyrquel 150 were Investigated on the Boeing streaming potential apparatus. The results indicate that Fyrquel 150 and Fyrquel 220 are similar In streaming potential and wall current while NCPDPP has lower streaming potential and higher wall current. The addition of FC 98 reduces the streaming currents and potential. OXDPP has stream currents similar to the Fyrquels. The attached graphs have streaming potential and wall current data vs. volume flow rate through the apparatus. o3608 *0NS V O LTA C S & ffl- IM P E O A K jCE -yr- MONS 036089 E ^T i.'/i 38 MONS 036090 -39- MQNS 036091 -4o- (., .i 2 5 1 S 0 7 # 5 10O0 1 3.1 S Q I 8 'J 1 Iv Flow Fatf cc /.'w/*' MQNS 03609i -41MONS 036093 -42- Thermal Stability of Cumylphenol (P.P. SPL. 37) (H. Luebke & E.Emery) INTRODUCTION ' Thermal stability data for curaylphenol were requested to provide process safety information for operation in the Pilot Plant. A maximum pot temperature of about 280oC is used for the distilla tion. SUMMARY The thermal stability of a Pilot Plant sample of cumylphenol (Spl. #37, 3-5-70) has been determined with the Monsanto built pressure DTA apparatus. The experiment was run under a nitrogen atmosphere. Only a very minor exothermic reaction was observed above about 280'C. Gas evolution was detected at about 210*C and a rate of 0.4g - millimoles/min/Kg (9cc/min/Kg, STP) was measured at the maximum proposed pot temperature of 280"C. A plot of gas evolution rates vs temperature is attached. Gaseous decomposition products were identified by GC/MS as carbon dioxide, methane and 2 and 3 carbon hydrocarbon fragments. We foresee no serious process hazards due to thermal decomposition of this compound. The rates of gas evolution are low and the slope of the curve is quite flat, indicating a small temperature coefficient. Reference - DTA #70-28 mums 03*094 -44- Marketlng Support Cltgo FR-2? A recent Cltgo fluid similar to Pydraul 512 has been characterized aa follows: 1) 65 Aroclor 1248 13# Phosphate ester; 4iS triphenyl 9% cresyldiphenyl 10.5% Petroleum Oil (Same MW & MVI distribution as found in Cltgo CHX-604) 1.5% VI improver, (same type as found in Cltgo CHX-6o4) 2) Cltgo CHX-604 Cltgo FR-23 Vis at 100oF, cs: TO.93 Vis at 210F, cs: 7.122 V.I. 48.4 Sp.G. at 25C 71.6 7.67 71.5 1.28 3) FR of subject sample as defined by the 'Wick Test' (insufficient sample for normal FR determinations) indicates an Improvement over Cltgo CHX-6o4 which was in turn rated a definite pass by the F/h Hot Channel and H.P. Spray tests. Basically we are dealing with the same components as found in their earlier fluid, CHX-604. The Increased FR noted is undoubtedly due to less petroleum fraction as compared to the earlier fluid. (See 10/9/69 memo WRR from PFH) Both of these fluids are in the 300 SUS range; hov.'ever, the VI 8a. of FR-23, is roughly 20 points higher indi cating a more potent VI improver and possibly more shear stable since it was reported that oheardown was a problem with the CHX-6o4 fluid. We do not plan tc characterize the VI improver at this time- It is our opinion that they have incorporated more potent and possibly a more shear stable VI improver and have reduced the oil content to achieve similar viscosities. HONS 036096 -45- Hamworthy Compressors/Pydraul 625 Three compressor parts from Hamworthy Compressors were tested for compatibility with Pydraul 625 and Pydraul 625A. The parts were of a perspex compound and the results were negative. The parts were cut In half and then partially Immersed In each fluid for 168 hrs at 158F. - The parts did not change greatly In dimension but aome dissolving did occur. This caused the fluid to become very slimy. Another part which was a gasket for a flow meter became very swollen and Boft. These parts would not be recommended with either fluid. Recovered Pydraul 312/0,M. Bedford Recovered Pydraul 312, Flndett lots CF 56 and CF 57 appear to be nearly equivalent to new Pydraul 312 as Judged by the Factory Mutual Spray fire test. Pydraul 135 Acidity/Republic Steel Laboratory degraded Pydraul 135 and new fluid were furnished to R. R. Klinge of Republic Steel to serve as standards for measuring fluid acidity. Attached arc typical titration curves for these tv:o samplea which indicate the differences expected as fluid Is degraded. The AS'fi'i V-G6`i procedure v.'ns followed with the end point taken at pH 11, Total acid nvabors (T.VJ) In r.illli~rn:,.ws of KCIt nor from of fluid ..era calculated to bo 0.17 for new fluid and 0.29 for the degraded fluid. Two characteristics are noted for degraded fluid. The Initial n" dropa lower and may eventually get into the strong acid region below r,!I Ji. Also, more weak acids are being formed and the titration curve flattens and extends to pK 11. NONS 036097 -47- Asslstance to Manufacturing Recovered Aroclor 1242 for Pydraul Blends Specifications for Aroclor 1242 returned by O.E. and Westlnghouse for use In Pydraul blends were suggested (see following page). Steps are being taken to allow the plant analytical lab and manufacturing department to work directly with Flndett on approval of recovered fluids for use In Pydraul blends. Pydraul 320 Customer Complaint Dross separation of Pydraul 320 was reported In Japan. This appears to be caused by exposure to low temperatures. About 45# is in the top layer and 55 below. These layers remix readily at room temperature (75?). Fire resistance of the two layers as Judged by a pipe cleaner wick test Is similar to the complete fluid. Interim recommendations will be to remix fluid, at room temperature before using. Further attention will be given to this problem as these fluids are reformulated to eliminate PCB's. Pydraul Acidity Specification Limits Currently produced Santolube 70A has a slightly lower acidity than the old Santolube 70. This results In problems meeting minimum acidity spec limits for some Pydraul blends. Each 0.1# of Santolube 70A contributes 0.05 to 0.06 TAN to acidity of finished fluid. Specification limits will be changed as needed. MQNS 036099 -48- RECOVERED AROCLOR 1242 TENTATIVE SPECS FOR USE IN PYDRAUL BLENDS Recovered Aroclor 1242 for use In any Pydraul or Santosafe Recovered Aroclor 1242 restricted to use In Pydraul 312 and Santosafe 300 Series* JFQ Method No. Color, ASTM P-1500 Appearance, visual Neutralization Number, mjjKUH7gm ' Moisture, KF m methanol Sp, Gravity 25/25*0 Viscosity, cs at 100F Oxlrane Oxygen OLC Analysis 1.0 max 3.0 max Clear, light yellow liquid free of sedi ment. Clear, yellow liquid free of sediment. 0.03 max 0.03 max ## 100 ppm, max. 100 ppm, max 1.380-1.395 16.1-18.6 1.350-1.395 16.1-18.6 0.1$ max. 0.1# max. a) 0.2# max area low boiler peaks near new 1242 peak envelope. b) no low boiler peaks far re moved from new 1242 peak envelope. v same c) other peak typical of new 1242, V 16-B 80 -E 78-1 116-I 126 -f * Includes Pydraul 312, 135, 790, 230, and 320; Santosafe 300, 150, and 100, ** Water contents as high as 180 ppm should make Pydraul with acceptable moisture and appearance; however at this water level Aroclor 124s alone Is very cloudy. *** procedures to be supplied later. being run by Research. Currently HONS 036100 DIELECTRICS -*9- Biodegradable Capacitor Fluids (R. H. Munch) A modified Aroclor 1242 designated Aroclor 1242B has been produced by fractionating Aroclor 1242 to reduce the pcnta and tetra chlorinated components to a minimum value. The new product has only . 16% p*ita, 2.3% of the amount in standard Aroclor 1242 and 16. 3% tetra, 67% of the amount in the regular material. Biodegradaliility data for the new product are tabulated below along with similar data for standard Aroclor 1242 for comparison. Biode gradability Peak 1 Peak 2 Peak 3 Peak 4 Aroclor 1242 Amount Remaining (after 1 week) Nil 66% 64% 42% Aroclor 1242B Amount Remaining (after 1 week) Nil 10% 33% 1% These data seem to indicate that the Aroclor 1242B is significantly more biodegradable than Aroclor 1242. The attached sheet gives the specification properties for Aroclor 1242. Those which have been determined for Aroclor 1242B are given on the same sheet. These data indicate that the new fluid could be substituted for the old in capacitors with no modifications in capacitor design or processing methods required. Arrangements have been made to produce 500 to 1,000 gal. of the Aroclor 1242B. The fractionation is to be carried out in the Dayton MRC pilot plant because no suitable still exists in our St. Louis pilot plant. The adsorbent treatment will be done in the St. Louis pilot plant if the truck strike docs not interfere. The large sample of the new product is to permit use tests in capacitors by our customers. Preliminary work indicates that a product having amounts of p<nla chlori nated biphenyl too low to detect and tetras reduced to about 1. 3% can be produced by fractionating Aroclor 1132. The fractionation must be done so as to reduce the concentration of tho 4,4' dichlorobiphcnyl isomer to 2.0 2.3%. If this is not done crystallisation takes place. Further work will bdone to determine the best procedure for making a product of this type. HONS 036101 LonStiTiO OAOANIC CHCMICAl. OIVI.ION V.N'NJSTON':and krummrich. ,, FINISHED PRODUCT SPECIFICATION P. E. Heisler IlkCI W. E. Ault CNCA*L.OCCllriOM ,' AAODUCT -50- Aroclor 12-12, Electrical Grade -MODUCT COOC |UL WGK, Ann, S Lt'FkCTIVt; 81101 - 82612 U*L.a COOL IOCPT. 2-16 S - lea 6/17/66 APPMOVAU HCSUAHCH 1040-240-04/11/16-03/09 R. W. Bucknell OUAC.ITV CONTROL (Chll Chtmlit) O. x!. jJOlin W. J,1 Gresham ... , , CHEMICAL POMMULA - Also>. known as Pyranol 1499 ' 27 E MOL WT. 4-13 -62 AMPLE POM ANAL Wife 3 x 5 pt Amber Bottles . LIMITS hiliaD ay UNRESTRICTED INFORMATION ' . ' 'lifii.S WGK J. P. Prader METHOD Anniston (R) Color (APHA) (R) Condition 40, 'max. 1 , Clear 10084 10084 (R) (R) (R) (R) (R> ,<3i Sp. Gr. @ 25/15.5`C, 1,381-1,392 K3t7 10114 Acidity (mg, KOH/g,) Moisture (HjO) 0. 010, max. . .1 ; 35 ppm,; max. 10087 10620 Refractive Index 325*C. 1,6240 - 1.6260 10125 Inorganic (Free) Chlorides 0. 05 ppm,, max. 12741 Pour Point -14*C, or Lower - 14'c, 10115 Dielectric Constant (1000 cycles @ 100*C, ) 4,70 - 4.90 . 1: ' 9.S7-2<v&H608 . . Resistivity '500, min. Itfi*oc y/0'11607 (500 VDC <8 100*C, O. 1" Gap) As OHM-CM x 10v . t.>* sv1*. /.*. F+uV*' * 0 K, Otf-ff , (R) Hydrolysis Stability-Test ' . , 0,5 ppm, max,' 12672 (R) (As Chlorides) Monsanto Stability Test ' ... : . ' I 0, 4 ppm,, max, ' ' 11503 (As Chlorides)^ j; . . <R) Distillation Range ' : 10117 (ASTM D-20, Corrected) 10% Distilled by wt. 325*C., min. Jl(f <- 90% Distilled by wt. -360*0., max; 539 E- Suliate s None " ' , 12169 Dielectric Strength <8 25 c. 35 KV, min, . 11605 Flash Point (*F) 338 - 392, - 10123 Fire Point , . None . 10123 ^ * Corrosion Test . ' .1 1. 10126 (6 hr*, @ 210*C, with bright , aluminum foil) Change in wt, of AE % 0.0 ' A.C. Color (APHA) 60, max. 10084 A.C, Condition T Clear , 10084 " A.C. Acidity (mg. KOH/g.) 0, 010, max. , 10087 A.C/ Inorganic (Free) 0.05 ppm,, max. O; Chlorides - . % , Vise. @ 100'F.. (SUS) (Over), . , 12741 a 14-44-54 G-l 14-49-54 14-42-54 14r53-54 14-34-54 014 14-47-54 14-36-54 14-35-57 0)0 14-61-57 14-31-54 043 , 14-28-54 14-28-54 14-55-57 14-44-54 G-l 1 14-42-54 014 14- 4-52 1 ' * MONS 036102 GENERAL, INFORMATION ' ,i i -51 Specific Heat @ 25*C, Coefficient of Expansion (25 - 65*C) . Fixed Chlorine Powor Factor @ I00*C, 60 cycles 1000 cycles .0.30 0,0006 Scc/'C. 42.5 - 53,5% \ ' ( Typical Values) S' ' . 0.30 1% ,01 SPECIAL, CUSTOMER REQUIREMENTS General Electric . Thermal Chemical Chlorides 0.65 ppm,, max, Westinghouse Hydrolizable Chlorine (Westinghouse Stability Test) 1,0 ppm,, max. 12722 T-2219 s~ MOMS 036103 L -58- Synthesls of Capacitor Fluids (1630459-QET) n-Butyl pentachlorophenyl ether, synthesized last month, had an unexpectedly low power factor along with a reasonable dielectric constant. We are following up this lead by pre paring butyl ethers of various lower chlorinated phenols and by modifying the alkyl group In pentachlorophenyl ethers. Compounds prepared to date Include n-butyl-2,4-dlchlorophenyl ether n-butyl-2,4,6-trlchlorophenyl ether and n-heptyl pentacKlorophenyl ether. The latter melts at 8*C while n-butyl pentachlorophenyl ether melts at l6C. The relatively Klgh melting points of the pentachlorophenyl ethers indicate a necessity for use of mixtures or a significant modification of the alkyl portion of the molecule to lower the melting points. Capacitor Fluids (RWW) A second batch of dlchlorodlphenyl ether (5 Kg) was prepared. Yield Is considerably Improved (7056) but all too low. Air sparging after chlorination Is Buspected to cause polymer formation. This will be checked out on a smaller scale preparation. Electrical properties for chlorinated or-methylstyrene dimers are attached. The dlchloro derivative showed good resistivity and dielectric constant; however, the pour point is much too high. We will try blending to improve low temperature properties, Aroolor Defense (RWW) Only one experiment In the hot tube without catalyst was run. Very little Isomerization of 4,4'-dichlorobiphenyl was noted. A Suggested Procedure was written for bromine recovery from HBr off-gaB In Bromo Aroclor production. The process comprises scrubbing demisted HBr with agitated calcium hydroxide slurry to pH 4-5, oxidizing with chlorine and steaming out bromine. Saturated bromine with 0.056 water is withdrawn from bottom of receiver and dried with activated oaloined alumina to 20 ppm water level. The aqueous supernat ant from the receiver is recycled. Overall bromine recovery will be better than 986. This process Is preferred over oxi dation of the much more corrosive HBr. Industrial Hydraulic Fluids and New Dielectric FluldB A new batch of Bromo Aroclor 1232 is prepared by bromlnatlon of Aroclor 1223. This material exceeded desired Aroclor equivalence (^1237) and will be blended in new Pydraul 312. Properties are summarized In Table II. This material will be purified and tested for electrical properties. MONS 036104 ,, -53- .LiI'CacX X /(^ 0^! U'vj-^r */{- >00"C p/` iV 7kcJ'>* Zj~.J:l.-,; ^ H lit1*J roo v Zk. . UiV>r Jt cZ**nt - c?. *0* ,00 12C < . 00 t 11,10 6 7y %tc va y 11 *? 2v*-^w Xv*-&-fv- /Of U3I Va ciHi-t-v - .** Ci /(JO a*o* Jr. /i. $.3 3 /.i7 MW. w :*; t.iSr /. Joi- C^u. >1 f^/- /Z3C /* vo MOWS 036X05 -54- Dielectric Liquids - H. Vodden, C, Coleman . RUABON 76Q.12.722.bl ulactrioal ,`lulde C'fb. a visit to Mioufil* *.urich elucidated tho * tuiitior. in r-.^pect of tneir ilcenoeee. Voltas* India are nlruady *n production aim *ere uuid to i<* using , rodeieo in reliant#. '.lektrosbrija* ijeo^rad *re not in ,x<xtuotion am i rv not expeoted to bo Tor perhaps *. yours. ..unuuai, Italy and .ioncm* ...tin nave no oonnuotion with lonfil. Laohurost wan visited tc. fino out tho nuu- n lui u.uir ciucont.-nt with . ousanto. Vheir rdtin rwaucn wim the u!lla>.<tul> Ji jA.,,tti.jn factors obtamud on dru.i doliverisa of .rocior l?4d. V;.ic **o a.nu to hi Ivx tiaui on ooujitftitivo produo ts from deyer and .rodeieo, and also to be hi,thjr than the value of l.,,, quoted as u typical vain* in our .'iJ. < vim cp <utt \X JJU'M* pGU* was sniu to have been obtained or* 2'..C.7''. - ...a back* and although the result# on t/at art not c.ncluei/c, i.--. I//.* t> indent# that our dissipation f*otor is higher than is dssirubU or exjfctnd* it is recoautendeu that the uisuipation factor of future cci,a*,;u...ut# t mil* ciuiUrntr Shculd be Ciiookud before buint; uis, i'.che<* oo `.hut vu /i;r > t , . volu* <-X t tis sta"W. Two ..lCL MlI U dieloctr e toot colic nave been , for uiu..*to.`: to Heavy "ilsctrioals, India* this exneuots our present stock *.ni It m not proposed to havs any more m*'de because of the ch.-iipe over t.v . ' t ilu nneh method of i*a&a^rer.iont uaiv.;; ti c hnlsbaut/1 cells. 760.12.022.44 electrical . laatio Ellina* A further .naetin;; eitn uCL took ; lice in Lonr.ra cr 1.y:>. j t *** tt.;ain siaphaStSua that :iuL require Monsanto oet s,>ecifior\tlons for poly n> . io.tc filo Deonuae of tue cost of their dsvelo;;ia*nt work. It wa.-f . r*^. * this ouln be oospleted oy the end of April. In the meantime we h&ve experienoeu a uetbaok in the testin' T tun coiSj atlbllity of the jCj. expux.menlal samples* Leek of re-rsus.ii.iity ^ne obtained and the osuhq has been truoed to the electrode cluanjup stommnee, hut not positively identified. as a temporary sxi j.'iunt, \-it tin restin' n.'ency of this work* the teet le bain*; o/irrieu out uaitig the Cl cell. .i vi.lit to .11.' muuarcli* London v<as made for the purpuNo of tf.Air OApfioitcr winding* iaA*rt!jiiatii^ m.u testiiq; nijur^LiOJit. .is * vj.alt uf t..eir rooomibuadutiom) v'ilncap# uttur ;;aay<m wuj viiiitod in cx.ior i) i-v** v/e.r de*. n of windlu.j naoiiine in operation. .mciunas . ,.our *<' i' d \i all /tr foruuuoublrt ro ( ureutcn-ju but;, f - a ril;- ..ici .. .'.u : .v-jac.,* i : , ,/OJi pi lit .'hi'.i -`'J' .l; i. i. iri not y t *.;t.:.ou o...J';w-r *.: ....'a ' . h- r . I. r>: HONS 036106 -55- ailcotrloal i'laatlos Hiil, borat jrogrvse has bran made on tooting the sanplea submitted by 'W and 12 aanplea out of 44 hbve bean tacted to Unto. Joi.r rupeatnbillty la being exiarianoad end present affnrta are hi reot.d to fiml tha oauoa of tl.ia. dissipation factor ia being measured (it 500 voltn hecuueu the eonaltlvi ty of tho Lneood bridge ia lnaufflolant at volte. Milvary of the .1 701 bridge la audited. A nueting with UCL took place on 17.2.70. They euutod det.Jla of ooute to equip theueolvee for Oarrylng out n eoaplete range of tnetu on thoir eleotrioal films, including compatibility with forcolor. 'They alao lntena to aet up a oapaoitor testing operation. They require froa Morieanto a oooiplete epeolfloatlon for alaotrioal filu ao that thoy onn nmnufncture to thin. Thuy nlun require Monsanto to tall than tha tMokn.ise ana type of f. lm ulmra tho Market opyortunitlee will ba unet favourable, bearing In wind that they era lata In t.ne field ana their oonpotitore have already uainbli-hod thnslvee in thiuktmaxoa of H> "ilorone and above. They lnoluna to the view that tha grant.1st o.vortjiltins lie with oapaoitora with a single layer of raetiilllced file b..t ln.-rugnato.l rutnor than dry. They are particularly lntereated in Hon.mnto'a development! in liquids that an suitable for uae under self-healing oondltlona in auoh oapaoitora. 'lacellaneoua pevslonaanta. A vlalt to i'.'ilA diaelorad that negligible progress has been cuius on our privately-sponsored project to test Mdii 717 and an Aroclor 12d?/pj!> blanu In polypropylene flln oapaoitora. The roaeon (rlvwn was rtnlrya 1. exiting up their la, ro&iation ayataa. The raeulta wore promdend for tha end of April. One aspect of their generally-aponaorad project oovara the tonting of soavengera in aakarala. In addition to the email sample of j.vranol i that wa have supplied, they will require a quantity of 40 - 50 gallons for larger triale. At prevent we ara unable te supply this boeauae it ia too aueh to supply froa the laboratory and no pilot plant la awallable. , 2.45. .HI1 ,*? ATMlMli Three further modified saaplaa have been received fur electrical teats, da ears told that attempts to refine the previous sample nave nut been euooeeaful. eleotrioal fluids UTS CoanlUae Work. A nesting of KHA SQ1K4 wae attended in London. Thin masting was Mostly conoorned with allloone fluids. A 2 day nesting of bXTA in AYankfUrt was attendee. Thia nan solely Outiuemed eith toxicity prohl..ie and tha Flatter of apecifi cation., nnicli enneerned .. rodeleo, vaa not dieoueeed. Jay Intends to aval with thin tnntlor by oorreepondenoe. HONS 036107 -56- /<>. .if . . ^ (Vi j____loi ukj-_.________ r-js_. *'T.V .... .OJM ; Iii .`OtJ' )t:r V**i' : r. r * nrittf ci.iteri nlB iiMve he^r* x-t, i. , ..rnHo^ .-a.' o t or.rnot. '.-ut *vnr tie r.io* tv. . ..... n > j ., it.'UOll Itlli): kill: I.O'tt 1*0 " ' ' ' '! t C1 ). 1 v'*' t ;ii.\ *r* "* 1 be '.-m *u.v. r. . ;0c u.* ut . . Kid tJ.imu, m.-^u u ii. r 11. # U` ' ' Job No. 760,12,722.51. Electrical Fluids CTS. The following customers were visited*- 1. ICAR, Monza, Italy: They have tested our impregnants A275 and A230 in their aluminium metallized polypropylene film capacitors and the results are unsatisfactory. It was found that corona discharges eroded the metal coatings resulting in a reduction in capacitance during ageing tests. The mechanism of this effect is not readily apparent and further investigation is required. 2. Zanussi, Pordenore, Italy: They requested further information to enable them to change from Aroclor 1254 to 1242. They also want a sample of # purified Unox 206 sufficient to 'dope' 25 gallons of Aroclor 1242 for a trial. They do not use polypropylene film. 3. CGE Milan, Italyi They prefer to continue to use Aroclor 1242 from the USA. They use P2 for motor capacitors using paper now but are looking at polypropylene film both metallized and non-metallized, They are expanding rapidly and may produce power factor correction capacitors in the future. 4* BICC, Helsby, England: Met Richardson during a visit for another purpose and he asked if I knew about a new Prodelec product called 'Metaline' with a DK of 4*2. He also mentioned that Newport dissipation factor readings were high compared with theirs, 2 to 5$ for Newport corresponding to 1 to 1.5^ at BICC. 5. LIFASA, Barcelona, Spain: Requested further information on design of a purification column and suppliers of components for a measuring system. A small manufacturer, but highly advanced technically, who usee Aroclor 1242 with Superad. 6. Bianchi, San Sebastian, Spain: Having problems with dust contamination so wish to defer change to 1242 until these are overcome. Requested details of automatic machine for injecting epoxy resin capacitor seals. Wanted further visit when they change to 1242 said to be 8 months hence. Advised them to run pilot trials to te3t sealing. Don't use polypropylene film. ' HONS 036108 I -57- 7. Fecha* Madrid* Spain: Having so much trouble with Aroclor 1242 that they are considering changing back to 1254 Use Superad with Aroclor also. Have made trials with polypropylene film from La Cellophane and Kalle but not using it at present. Personnel difficulties are hindering progress. 8. Cenemesa, Cordoba* Spain: Introduced Pyroclor 5 and after initial adverse reaction they appeared to accept what satisfactory experience of Westinghouse Canada indicated that it would be acceptable. Will place an initial order for trial quantity and make measurements on a transformer. Requested information on a source of supply of epoxy resin impregnated paper for transformers. BEAMA Conference on insulating materials held at Earl's Court* London during the Electrical Engineer's Exhibition was visited and a paper entitled 'Transformer Askarels* was read. Only interest was from Castrol! Other papers on polypropylene film in capacitors aroused considerably more interest and many capacitor manufacturers from UK and overseas attended. Laboratory work: The following TSLR reports have been issuedt- L7003-1611: Heavy Electricals, India - Assembly and calibration of 2 MCL Mklll dielectric test cells. This exhausts present 9tocks of components and it is not proposed to order further stocks in view of the change to the Munch Method, L7001-1611: Insulating Sleeves and Tapes Ltd. L7001-2711: Westinghouse Brakd and Signal Co. Ltd. L7002-1711: Bruce Peebles Ltd. RTW and AIM visited Newport plant for 1 day and 4 days respectively in order to carry out tests using their ESI 701 bridge and compare results obtained at Ruabon. This is part of the project to attempt to reduce excessive variability now being observed at Ruabon when following the Munch method of measuring dissipation factor. Job No, 760.12.022.44. Electrical plastic films. ' The work of testing the BCL samples continues and about JO$ have been completed. In view of the difficulties in obtaining reproducible results with the Balsbaugh cells and the low rate of testing* we have temporarily reverted to using the MCL cell and cleaning procedure. The solution method No.2 is still being followed. We have been given a suggested limit for compatibility of the film with Aroclor using this method, but the other properties of the film which are required to draft a specification for BCL are still in doubt. MQNS 036109 -58- The visit to Italy was made in the company of Mr. J.L. Unsley-Hood of further Provsome samples of 8 micron film for the 5 manufacturers. A ^ nn? !*?! ! ? "T!" fllm for ICAR is still waited from BCL. I CAB did not give details of their requirements or prices paid. manufaoturer^visited^US reqUiJ'e"'Cnt m" &t lhiS "" ^ Spanish longer^rcquire "" ^ ^ CRc ICAR Metallized Plastic Fllm Capacitor Fluid (RHM) Icar has inquired about the availability of 2-butoxyethyl-2-chlorophcnyl ether and 2-dichlorophenoxy methyl tetrahydrofuran, presumably for trial in their metallized plastic film capacitor project. These arc fluids which Monsanto patented as dielectric fluids. Icar apparently discovered our patents while searching the patent literature looking for leads to help Bolve their problem. I have secured copies of our patents and read them carefully. I find that the 2-butoxyethyl-2-chlorophenyl ether is listed as having a dielectric constant of about 5.8 and a power factor of 0.3% measured at 100C and 10K Hz. It would therefore probably have a power factor of about 60% at 100C 50 Hz. The 2(dichlorophenoxymethyl)tctra\ydrofuran was found to have a dielectric constant of 6. 3 and a power factor of 1.7% at 100C and 10K Hz, or about 340% at 50 Hz. If my assumption that Icar wants to make capacitors for use at power line frequencies is correct, they would have no interest in such a material. Moreover, neither of these materials is available even in sample quantities. Because it has been our feeling that minimum gassing under electrical stress was one of the important requirements of the Icar application, we have subjected a number of our materials to ASTM D2298-64T which is designed to determine stability of insulating oils under electrical stress. The data obtained are shown in Table I. Included in the table are data for Dialla Oil, a transformer oil, and Wcmco C, a capacitor oil. Duplicate runs were made for each sample. The table gives the initial dissipation factor and resistivity for each sample, the dissipation factor and resis tivity for each at the end of the experiment, and the average gassing co efficient in microliters per minute (AGC). HONS 036110 -59- Thc data in Tabic I shed some light on the problem of selecting a fluid suitable for use in a metallized paper or film capacitor where the capaci tor is expected to be self clearing by burning the thin evaporated film away from the area of a short circuit. There arc two requirements. First, minimum degradation of the dissipation factor and resistivity of the fluid. Second, minimum gas formation. If the degradation of dis sipation factor and resistivity is too great the fluid in the vicinity of the fault will become conducting and the capacitor will fail completely. Data in the table show that the resistivity of Aroclor 1242 decreased by a factor of about 6 x 10^ in this test. This is the reason a chlorinated impregnant is not suitable. The other requirement is that the amount of permanent gas formed during the clearing process must not be enough to form a permanent gas bubble which would lead to breakdown. Thus, of the materials listed in Table I, Dialla Oil would be the least desirable. HB40, and mono isopropyl biphenyl would be relatively desirable, with HB40 being the more desir able because its resistivity is less degraded than that of the mono iso propyl biphenyl. Of course other factors would influence the choice in practice. There * may also be some question as to the validity of ASTM D2298-64T for this purpose. However, I don't know of a better test except capacitor manu facture .I I believe that we have done about all that we can do to help Icar in their search for an impregnant. If we want to try to do more we should have direct contact between their technical people and ours to make certain that we have correctly understood their problem. HONS 036111 HONS 036112 TABLE I STABILITY OF INSULATING OILS UNDER ELECTRICAL STRESS BY ASTM D2298-64T Dialla Oil (Transformer Oil) D.F. @ 100 C 60 Hz Initial Final .00054 .09936 .11136 Rs, 500Y 100'C Initial Final 519 x 1012 .41x 1012 . 44 x 10^ Wemco C (Typical Capacitor Oil) .00072 .01374 .03918 52 x 1012 4 x 1012 1.4 x 1012 A-215 (Alkyl Benzene) .00012 .041* .50844 Mono Isopropyl Biphenyl .02910 . 167* . 161* HB-40 Aroclor fz42 .00102 .60120 .50628 .00060 . 58** . 59** 28,349 x 1012 .09 x 1012 1.27 x 1012 0. 74 x 1012 .01 x 1012 .01 x 1012 393 x 1012 .25 x 1012 . 31 x 1012 170 x 1012 .00003 x 1012 . 00008 x 1012 * Measured at IK Hz ** Measured at 10K Hz ACC 91.9 90. 3 58. 6 60. 2 22. 1 22. 1 1. 6 2.4 1. 6 1.6 1. 6 1.6 -O9- -61- AROCLOR DEFENSE (EST) PCB, chloride, chlorine and total organic chlorine analysis of the gas samples collected during the thermal oxidation studies at the John Zink Co. established that Aroclor 1242, Inerteen PPO, and Aroclor 1260 can be successfully disposed of in this manner. The preliminary data has been sent to CRD and a report Is being Issued. Sixteen sediment and water samples have been received from WOK for PCB analysis. Their analysis will be completed by May 15. The WGK analytical laboratory has ordered the neces sary gear which will allow them to do their own PCB analysis and are scheduled to be on Btream by July 1. Along these lines we will familiarize one of their personnel with the required techniques during the month of May. Two 7-lb Mississippi River carp have also been supplied to us by WOK and are being prepared for PCB analysis. Samples of these fish will be returned to WOK for mercury analysis. It is also planned to examine the carp extracts by GC/Mass to see what others chemical residues can be observed. Water and sediment samples from six accounts employing Pydraul fluids have been analyzed for PCB's. The results Indicate that all plants are discharging low ppb to high ppm amounts of PCB's to associated sewers, streams, and lakes. The companies so far monitored all Johnson Motors (Waukegan, 111.), Lester Castings (Bedford, Ohio), Central Diecasting (Chicago, 111.), Wheellng-Pittsburgh Steel (Steubenville, Ohio,), Wisconsin Steel (Chicago,111), and Timken Steel (Canton, Ohio). This information is being generated to help guide a potential recovery and recycle program evaluation by Fluids' Marketing. Muratlc acid (HCl) from Monsanto Central Drumming has been analyzed by EC/GC for PCB's. Low levels of compounds having similar retention times to the lighter chlorinated biphenyls were observed. A larger sample has been extracted for GC/Mass confirmation of the susplcloned presence of PCB's. Two other products, food grade fumarlc acid and saccharin are also presently being analyzed for PCB contamination. These re sults should be available early this month. If positive, no doubt, other products will have to be examined closely. OC/Mass and EC/QC analysis of silo paint scrapings and raw milk extracts submitted to us by the State of Ohio, Dept, of Agriculture, Foods, Dairies and Drugs Laboratory confirmed the presence of PCB's In these materials. The silo scrapings contained 2.87% unaltered Aroclor 1254, the raw milk extracts contained an estimated PCB level of 0.6-0.7 ppm. Although the Isomer distribution of the PCB's In the milk was altered with respect to Aroclor 1254, the Isomers present were those that occur predominately In Aroclor 1254. Strikingly similar Isomer alterations have been observed earlier in the electron capture chromatograms of an extract of a human fat biopsy sample, supplied to us by WARF Institute and In extracts of HONS 036113 -62- raw milk samples supplied to us by the Maryland Cooperative Milk Producers. Both organizations had suspicloned PCB contamination; unfortunately, in both cases GC/Mass con firmation could not be obtained because of the limited amount of sample available (WARP) or the low level of contamination (MCMP). The Bio-Test Laboratories has been contacted to arrange for the transfer of the tissues from various feeding studies they have conducted for PCB residue analysis. A rough estimate from them indicates that they have approximately 1000 cu. rt. of freezer space that is now filled. For this reason it was requested that a laundry list be prepared so that selected samples could be sent. We presently have only about 30 cu. ft. of storage space in St. Louis and see no reason to duplicate their facilities. Air samples from the Appleton Coated Paper Co., Appleton, Wls. have been received and analyzed for PCB's. Low levels were detected, but the amounts present in terms of mg/ms cannot be calculated until the actual number of liters or air passed through the scrubbers is obtained from them. If their sample sizes were on the order of 100 1. or more, the calculated amounts will probably be less than the recommended "safe" level. An informational PCB problem review of the analytical methods and the data so far generated was held for representatives from Westlnghouse. A first quarter report has been written reviewing the results of the preliminary river die away and some continuous actlvltated sludge degradation of Aroclor 1221, 1242, 1248, 1254, and Arobrom 1228. In brief, the results were as follows, the only Aroclor which was degraded to any extent in the river die away experiments was Aroclor 1221. Isomer alterations accompanied by the disappearance of 0.3-1.0 mg per 24 hr. periods were observed with all Aroclors (compared to 20 mg of LAS Dodecene-1 which is consumed in 24 hrs) feed to the semi-continuous activitated sludge units. The actual interpretation of this data awaits the evaluation of nonblodegradatlon routes which could account for the bulk of the Aroclor lost. This experiment is currently in progress. In the past these experiments (adsorption, volatilization, etc.) have been hampered considerably by our inability to analyze the large number of samples required to obtain enough data points to compensate for the large variance generally encoun tered in biological experiments. In the future, this should be compensated for by the additional manpower which has been assigned to this portion of the project. The Physical Chem istry Group is currently setting up the necessary equipment to carry out biodegradation studies on Aroclors and Aroclor replacement products. M0NS 036114 -63- Electron capture chromatograms of recombined laboratory distillation cuts of Aroclor 1130 and 1142 (Aroclor 1242B) Indicate that most of the "refractory" PCB isomers can be removed in this manner. Figure I compares the EC chromato grams of these potential substitutes with our current Aroclor 1242 production material. Figure II shows the isomer alter ation that can occur via degradation of Aroclor 1242 in the semi-continuous activitated sludge units. Figure III shows the isomer alteration that occurs in a mammalian system (cow). It is important to note that the isomers present in the fractionated materials are those that appear least "refractory". The following additional reports have been written and will be issued soon. 1. Relative Retention Times and Electron Capture Response Factors of Some Polychlorinated Biphenyl Isomers Relative to DDE. 2. A Study of the Completeness of Thermal Oxidation of Polychlorinated Biphenyls at John Zink Pollution Research. 3. The Partition of PCB Between Hexane and Various Organic Polar Solvents. 4. Extraction of Aroclor 125^ From Painted Surfaces by Water. 5. A Study of the Open Air Combustion of Paper Containing Aroclor 1242. 6. Determination of PCB Residues in Fish from Lake Michigan. T. Solubility of Aroclor 1242, 1248, 1254 in water. 8. A Study of Aroclor Chemical Clean-up procedures for Use with Electron Capture, Oas Chromatography Methods. MONS 036115 -64- AP1/LISD SCIENCES Environmental Aroclor Project (Keller-Tucker-Emery-Dietrich) It appears that disposal of PCB's can be accomplished successfully by thermal oxidation. This conclusion was made after analysis of ga9 samples from John Zink Company. They were analyzed for PCB, chloride, chlorine, and total organic chlorine. Data were sent to CED and a report is being Issued. Additionally, heats of combustion of the PCB's were estimated for CED evaluations. Water and sediment samples from 6 Pydraul customers were analyzed for PCB's. It is concluded that PCB's are finding their way to Bewers, streams and lakes inasmuch as amounts ranging from low ppb to high ppm were determined. EC/GC determinations for PCB's showed low levels of materials in muriatic acid from Monsanto's central drumming facility. These contaminants appear to be lower chlorinated biphenyls. Confirma tion studies are underway. Paint scrapings from silos and raw milk extracts showed presence of PCB by GC/Mass and EC/GC analysis. The paint scrapings contained 2.87% Aroclor 1254. The raw milk contained an estimated 0.6-0.7 ppm PCB, probably originally Aroclor 1254 but with an altered isomer d is tribu tion. Analytical methods and data collected to date were discussed with Westinghouse in an informational meeting on the PCB problem. A preliminary report on biodegradation of Aroclor was written. Tentatively, Aroclor 1221 degrades in river die-away experiments. Higher Aroclor products may not. More conclusive experiments arc underway. A current study involves removal of certain fractions from Aroclor products which might be intractable to biodegradation. Electron-capture chromatograms suggest that most refractory material can be separated by distillation. We are continuing to assist the WGK Plant in monitoring bromine content of chlorine they use to make Aroclor products. Seven samples, collected in the past month, were shown by XRF to contain 250-400 ppm bromine. Wc are preparing to determine the presence of dioxins in the prescnc of other chlorinated materials. GC studies show that octachlorodiben2o--dioxin can be determined but that the tetracbloro isomer will have interference from the components in Aroclor 1260. A better method to determine percentages of various components in undistilled Aroclor is necessary. A suitable GC method appears to have been developed as a consequence of studies made on 60 distilla tion cuts from 4 Aroclor samples. HONS 036116 -65- SKYDROL 500 Flight tests are currently being performed on Skydrol 500C by various airlines. Only tests involving at least 80% Skydrol 500C will be declared valid. The. other component presumably would be Skydrol 500B, heretofore employed. A gravimetric/precipitation method depending upon interaction with the disparate VI improvers is aa t i s f,ac tory for new fluid blends but not for used fluids, because of degradation of the VI improvers. We are attempting to develop anNMR method whose success may hinge upon relatively comparable rates of the decomposition of the VI improver. A hard deposit from a Northwest Orient Airlines shaft seal was shown by IR to be constituted of a heavy metal* degraded polymeth acrylate VI improver and hydrolyzed phosphate ester. We have frequently observed such a material. It is apparently derived in part from Skydrol 500B in the aircraft hydraulic system. OS-59 We determined by IR that a sample of our OS-59 returned by Maxwell Laboratories had no detectable contaminants. This tends to confirm our advice to Maxwell that OS-59, per se, is not suitable for making capacitors. Maxwell thought their poor experience might be ascribed to contaminated fluid. MCS 524 By NMR, we showed that a commercial phenyloctadecanoic acid consisted of at least two isomers. TYPE III, IV CANDIDATES L-77, said to be a superior wetting agent for Teflon, aluminum and stainless steel was shown by IK and NMR to be a siloxnne and that methyl groups and glycol ethers and/or methoxy groups are present. MCS 571 We received a deposit from an MCS 571 system at Dalton. IR analysis showed that 96Z consisted of inorganic salts, primarily bicarbonate as well as silicate. The balance of the sample was a carboxylate salt but not related to any components of MCS 571. Conclusion: the fluid did not contribute to deposit formation. MONS 036117 -66- PYDRAUL 625 Canadian Liquid Air, Ltd. sent us two deposits collected from an exploded air compressor serviced with Pydraul 625. Extractions with hexane, chloroform, acetone and methanol left a highly magnetic residue. The extracts were shown by IR to contain carbonyl and carboxylate salt compounds containing phosphorus. Exact source of these products could not be determined. SILICATE FLUIDS The dielectric strength, power factor, resistivity and dielectric constant of Coolanol 25A and MCS 825A were measured to provide data for a product bulletin. ^ CUMYLPHKNYL D1PHKNYL PHOSPHATE Timely' analytical support via GC was provided to the pilot plant production of -cumylphenol. NASA TENSIMETER Ue received a purchase order from NASA for a recording tenslmctcr. This instrument will be identical to that which we presently use for vapor-pressure and decomposition-temperature measurements on fluids. The components and materials for construction were ordered. CAPA ClTOR-LIFE-TKS T APPARATUS Components were ordered for an apparatus for life-testing of capacitors incorporating experimental dielectric fluids. MONS 036118 -67- HEAT TRAKSFER FLUIDS (DRM) Phenyl Ether (diphenyl oxidei With the able cooperation of the CRD catalyst group, we this month fitted out a pilot unit for the synthesis of phenyl ether by phenol dehydration on a thorla catalyst. The reactor Is a 5/8" stainless tube 18 Inches long fitted with thermowell, catalyst support screen and steady flow access leads, it Is heated to a reaction temperature (ca. 425*c) In a fluid bed thermostat. A metering pump supplies phenol to the reactor at preset flow rates. Reactor pressure is controlled by a pack pressure regulator on the reactor effluent line. Three catalyst preparations were made using three different refractory supports, namely pumice, bonded silica, and Cellte. The thorla was formed In situ by calcining the supports at 600*0 after saturating with aqueous thorium nitrate. The presence of thorium oxide was confirmed by X-ray diffraction. At this writing an Initial run at 425*0 with pumice-supported thorla haB been completed. The first 14 ml of product was liquid at room temperature, verifying that reaction did occur. The next 30 ml of product crystallized, probably Indicating low conversion of phenol. Analytical data are being collected. MONS 036119 -68- DEVELQPMENT PROJECTS Tractive Fluids (1331059-JCW)New Tractanta Substantial progress toward the development of new tractive fluids was made this month. A hydrogenated linear dimer of alpha-methylstyrene shows good traction, excellent oxidative stability and fair viscosity properties (item 1, Table i). A branched octyldecalln shows good coefficient of traction, and fair viscosity and oxidation stability (Item 2). 1 jst fr'ir iti eiar^ & JsL 0_ --2-0 <&k 2L<r F/j h l \ 1 v (0?/ i-7 ii.7 3,jir .17 <l U;/*05 no .3 7/ ,0Sb ,o ?J 3.1, */? \Yl! H,o>> iS //S 1.7 f.Y/ m 7) bti tu, 2?^ HS //./ 3L ?.u CV* ri ?f? `i--3 ^ j"3i /?,?<> x 7 f. V' 5 b! y . /n *'*~>*' , 7.1 );.o l? JF/> 5 3 00/? />/ ' i/oo, c 00 fZ/ r i '~~L.Uk. *~i PK i - J C OO eF On the other hand, a "linear" octyldecalln (Item 3) made by alkylation of naphthalene with octene-1, followed by hydro genation, had better 0 & C than the branched octyldecalln but considerably poorer traction. A dodecylcyclohexane prepared by hydrogenation of dodecylbenzene (Linear Alkylate 215) for investigation as a blending agent has good low temperature viscosity, but poor traction. The hydrogenated linear a-methylstyrene dimer compares favorably with hydrogenated dlcumyl (MCS 6l4). it la almost as good In coefficient of traction, and (surprisingly) Is as good In the 0 fc C. Its 210P viscosity Is lower, but It Is better In low temperature properties, since MCS 614 melts at about 68*P. The new material has not crystallized so far, at 0F or at -40*F. *c. 1*, i :>? - oa -o? -,0-y NUNS 036120 -69- Synthesis Linear o'-methylstyrene dimer. As reported last month, the linear rv-MS dimer is obtained by allowing rv-MS to Btand at room temperature for a long time with 0.2# Iodine. After 8 days, work-up gives the linear dimer I in 7056 yield, with 48# conversion. This procedure gives a product with 2# or less of the cyclic lndane dimer II. CH> 1 cp-c^cHx U/s r H-i -C - C//-C- - d> 1 c//t T A-W-OA. ft\T.... 1 ' H, 7i: C^( &c <{f.>-'l Same polymer Is formed. Hydrogenation of the linear dimer proceeded smoothly over Raney nickel to the fully saturated product. Running the Iodine-catalyzed dimerization at 50'c Instead of room temperature did not Increase the reaction rate, over a 3 day period. A possibly better catalyst for the dimerization Is a POCla . HsPCU mixture. This catalyst, described In an expired Dow patent, gave 68# conversion and yield of dimer in a few hours, at about 100C. However, the content of cyclic dimer Increased to about 10#. The effect of this small amount of cyclic dimer on the properties of the fluid will be determined. CRD Investigated the hydrogenated cyclic dimer as a tractant. It Is more viscous at low temperatures (.54,000 cs at 0F) and oxidatively less stable than the linear material. Also to be deteimined Is whether the crude rv-MS from Chocolate Bayou can be used as raw material. If so. It will lead to a very low raw material cost. Possible difficulty here may be the effect on hydrogenation of the small amounts of sulfur compounds In the crude tv-MS. Octyldecallns. Alkylation of naphthalene with octene-1 using 7.6# AlCla and 7.8# nltromethane In heptane solvent led to the Isolation of an octylnaphthalene mixture In 52/ yield. MONS 036121 I -70- c^a^)sc//=chk -9 c* IoomerB, formed by migration of the double bond along the chain, are also formed. Hydrogenation over Raney nickel gave the "linear" octyldecalln, item 3, Table I. This had good oxidative stability and low temperature viscosity, but rather poor traction. Alkylation of naphthalene with the highly branched octene diisobutylene gave a t-octylnaphthane fraction, and also t-butylnaphthalene, and higher t-alkyl products. This type of reorganization is a well-recognized hazard in alkylation of aromatics with poly(iso-olefins). Using naphthalene and diisobutylene at 2:1 mole ratio, with 3.956 each AlCla and nitromethane (on naphthalene) gave 4i# yield of t-octyl naphthalene and 355 t-butylnaphthalene. Hydrogenation of the octylnaphthalene over nickel gave the branched octyl decalln (item 2, Table I). This is a good tractant, with ihir 0 & C and viscosity properties. In another experiment, using about four times as much nitromethane, and working up the reaction 1/2 hour after olefin addition was complete, 29# t-butyl, and 55# t-octyl was obtained. However, it is suspected that the "t-octyl" fraction contains material of longer chain length; characterization of this product is not yet complete. Spectroscopic evidence indicates that an alkyldecalln is a major constituent of the Sun toric fluid. Judging from the two examples so far prepared, this type compound appears of less Interest than the linear c-MS dimer. Both have low raw material costB. The o'-MS dimerization is simpler, however, and the properties of the fluid are better. MCS 998. a -4oF fluid for Lycoming, is a 70:30 blend of MCS 757 with dlisodecyl adipate, with 1# dioctyldlphenylamlne as additional oxidation inhibitor. Although MCS 757 does not foam, the blend did, but foaming was controlled with 20 ppm of DC 200 silicone. Properties of this fluid are given in another section of the summary. The first two gallons of MCS 998 sent to Lycoming were lost in shipment; a second two gallons were blended and shipped. Used MCS 9612 - A sample of used MCS 9612 from Gates Rubber Co. in Denver was received. It had run for 25 hours at POO275 *F, and for 1 hour at 330F bulk oil temperature. The oil contained a fine black sludge, which was found to be metallic wear debris. Viscosity and composition (by VPC) of the oil were essentially unchanged; acid number was 0.49. HONS 036122 -71- Naphthenlc Oils - An attempt to relate differences In traction coefficient among QMR 1204, Solnus 55# and Paratex 75, all naphthenic oils, to differences In degree of unsaturation showed no observable correlation. NMR and 1R spectra were similar - there is no aromatic unsaturation. No unsaturation toward bromine was detected In the Paratex 75; the other two gave turbidities with bromine, probably due to reaction with additives. MCS 998 (RLQ) The -'10 F tmotive fit'.id, MCS 998, wan tented for vlscosl fcy, l'oiv.i, arul 4-.lull wear before shipment to Lyoonln/;. The result:: are: Viscosity at --J10J*` 100? 210V = 22,250 cc = 17.'10 cs = 3.'19 on Foam . Blender Foam at 200F/200co/2 min Initial height of foam = 1/4 in. Time to breal: foam = 20 sec. ASTM 1)8-92-5 Rj? Tendency 15 ml Stability 0 boo Four Ball Wear 200F/1260 rpm/2 hru/52100 on 50100 Scar diameter - 0.87 mm. The pour point data on the "running" test conditions was measured and found to be between -CoF and -55UF. Dosed on there results and previous 0 : C and traction test.in;;, KCS 950 is judged to bo: 1) equivalent to F50 In traction under the slip velocity conditions seen on the Bycomint; LD 6 2) nlifhtly worse than 1-XS 757 in foam but better than Vcrsilube F50 . 3) a formulation that will cold start In the LD 6 at -40 V since it is equivalent in viscosity to MCS 757 at -20*1>' which passed our cold start pump test (memo 2/3 7./70). Three rail on:: of lie.': 998 were blended and two ).aTl<:is were rl;i|nnd to Lyrawiihg with two I'.ri.loji: ol1 II.K(U for flu: hi nr, puri'o: os. HONS 036123 -72- Tractlve Fluids The coefficient of traction on many fluids was measured by a new procedure on the twin disk test at two loads and two temperatures. The semi raw data Is being reduced to traction coefficient vs. slip velocity. Qualitatively four synthesized fluids are equivalent to MCS 460 In traction. They are DCCDC Hydrogenated linear dimer HLD Octyl Decalln (OD-3) H27D4 Hydrogenated still bottoms Viscosities, 4-Ball wear, and 0 & C were run (see JCW MS). Blends are being made to meet the 0F GM Torlc Fluid specifi cation of 2000 cs. Automotive Fluids (1338459-QET) Air conditioner lubricant candidates MCS 994 and 995 submitted last month to Ford performed exceptionally well In their Bystem except under simulated idle (low rpm) conditions. The difficulty resides In the relatively low viscosity of our products. We have reformulated a high viscosity lubri cant now designated MCS 1005. This material has the following composition and properties. MCS 1005 Composition: ~33# Carbowax 200 --673^ phenyl bls(3-hydroxyphenyl) phosphate 0.2* tolyl trlazole Viscosity: at 210 F 29.75 cs at 100 "F 775 cs *at 165"F 80 cs (extrapolated) * 80 cs at l65F desired by Ford) Pour Pt. about 5-10F Freon Insolubility: better than MCS 994 + MCS 995 Santoflush - Sewage Transfer Fluid (QET) A request by Chrysler for a safe, low density, water immis cible, high flash point, fluid to be used on shipboard sewage systems was Investigated. The best candidates appeared to be In the order DIDA > DOA > Santicizer 148 + mineral oil. Accordingly we sent Chrysler a sample of DIDA designated MCS 997. Their response was Immediately favorable and they have now placed a Z300 order for larger quantities of MCS 997. MONS 036124 -73- PIONEERINO (EOS) Rub-block on Rotating Ring Friction and Wear Teater: Following the receipt of Capital Authorization for this pro ject, it haB been placed in the hands of the Instrument Development Croup who are finalizing the design. In this they are being aided by Prof. J. Georgian of Washington U., particularly in regard to calculations of the dynamics of the tester. Completion of the device 1b expected by the end of June. This machine is to be used in the contract for Thermo Electron to measure the lubrication of thiophene/F-50 blends for the Rankine Cycle automobile engine. High-speed, High-temperature Bearing Tester: In anticipation of its use in two different projects under consideration by NASA, steps are being taken to modify the ERDCO Universal Gear and Bearing Rig. The first step will have to be the gear-box change to produce speeds up to 50,000 rpm. ERDCO now estimates delivery in less than 24 weeks. We shall try to place the order for this item as soon as possible. ERDCO has looked into the feasibility of oper ating the standard 100 mm roller bearing test head at speeds up to 50,000 rpm and has concluded that substitutes for both the Rollway test bearing and the loading/shaft-support ball bearing in the test head would have to be found to permit operation over the rated maximum speed of 10,000 rpm. They are currently preparing an estimate of the cost of doing this. The high-speed ball bearing test head is also being considered. MAIC has been contacted regarding the practic ability of their designing a test head which is compatible with the ERDCO test drive. This will be feasible. Further more, they will probably be able to design a test head which will accept either 8o or 100 mm ball bearings, giving ub a chance to attain dN5 x 10 without having to replace the entire test head. Who is to build the new test head is not yet decided. A visit to MAIC to finalize the specifications for the test head is planned for May 11, when Alastalr Cameron will be available. NASA-Lewis will then be visited on the 12th to see what they think of our plans. NASA-Lewls Contract No, NAS5-124l8; A request for a no-cost time extension 1*0 this project is being planned and will be discussed on May 12 during the visit to NASA-Lewis. Prof. Cameron has contracted with his students who help man this project through June of >71. Type III Jet Lubes - Lubricity (FSC) New Additives - The following compounds were screened in our slow speed four ball teBt in MCS 524 (.1$). Those under lined show improved lubricity. M0NS 036125 -74- Ultraphos 12 P & 0 Additive #3 phenylboric acid trlallyl phosphate Ultraphos 12 This liquid is an anionic phosphate ester surfactant manu factured by Witoo Chemical Co. It gives an excellent friction curve on M50 steel. It haB not been run on any other metallurgy. This phosphate gives less deposits in an 0 & C test than MCS 293 but has a higher viscosity increase (8.3# vs. --456). P & 0 Additive #3 This chemical is tetraethyl perchloromethylene phosphonate (CaHgO)a- -(OCaHs)a a At 0.5S*, this phosphonate does not change the boundary friction of MCS 524 on M50 steel or on hard anodized aluminum. But it has an excellent curve on aluminum metal. ThiB is the first additive in MCS 524 which gives a curve on aluminum comparable in magnitude and general shape to Mobil Jet II. A comparison curve is shown with following graph. Phenylborlc acid This aoid did not Improve the boundary friction on M50, hard anodized aluminum, or aluminum metal. It is interest ing that many of our acid additives change the friction of steel or anodized aluminum but don't change the friction of aluminum metal. This metal will react instantaneously with acids as weak as water. And lubrication theory predicts the generation of fresh metal under boundary conditions. Per haps the additives react but don't produce lubricating soaps. Perhaps the metal is so reactive it reacts with the base stock giving metal corrosion. Trlallyl Phosphate This additive did not change the boundary friction on M50, anodized aluminum, or aluminum metal. New Base Stocks Most of the additives which we forwarded to SNECMA in MCS 524 were screened in MCS 963 base stock in the slow speed four ball. MCS 963 is HONS 036126 ____ 524 ------52>J f .1% m.'trcLpKoj 12 Jtso/Kso -V4Jl MQNS 0 3 6 1 2 7 Je+TT i Ma fx>/ + o.sy. P*G rfbU+t'ife I- -77- meta dsdsd + ortho SfStfStf + meta QfOQlsd + antifoam These tests were run to see what the additive response would be In a base stock chemically similar to 524 but with a different viscosity. Also, to obtain patent coverage. The additive friction curves In MCS 965 were very similar to those in MCS 521*. Thus: phenylphosphlnle acid: large reduction on hard anodized aluminum; large u reduction on M50 steel from 200-400"F followed by a p spike; some p reduction on aluminum metal. perfluoroglutarlc acid: worse high temp. p on M50 steel large p reduction on hard anodized aluminum. Also screened were MCS 963 + monopotassium oxalate MCS 963 + bls(chloropropyl)-2-propenephosphonate and MCS 963 + A-88 + trichloroacetic acid Only the oxalate had a different pattern In the lower vis cosity base stock. It had a significant friction lowering on M50 steel In MCS 5^4 but only a small friction lowering In MCS 963. Other additives CP 64600 - This Is Ludwig Maler*s phosphosulfide. A 500F ZTinTTeist was run on samples of MCS 524 plus 0.136 and 0.055* of this sulfide. Generally, these blendB gave reasonably clean tests with fewer deposits than MCS 293. Specifically: In the presence of copper, the formulated fluid had less black deposits at both concentrations than MCS 293. Some vapor coking was observed. In metal attack the copper corrosion was comparable to MCS 293. We Increased the silver corrosion. The viscosity Increase was 9% vs. 436 for MCS 293. HONS 036129 -78- In the absence of copper the deposits were as above. The metal attaok had increased silver corrosion. The vise. Increase was comparable to MCS 293. All In all not a bad test, considering the reactivity of the additive. SKF-NASA Report on MCS 2931 The final report on the bearing tests with MCS 2931 has been written. The authors are L. A. Peacock and W. L. Rhoads of SKF. It has some discrepancies with the Information given us by Bob Johnson. The report states that MCS 2931 ran two successful tests out of six with two runs giving fluid related spalling failures. Our call report says 2931 passed five out of six tests with one spalling failure which was not fluid related. It is Interesting that the lubricity failures in the report are surface Initiated spalling failures, l.e. fatigue failures. This mode of failure can be Initiated by water. The trichloroacetic acid additive used in MCS 2931 did contain /~1% water. We should watch water content for pos sible correlation with fatigue in any future use of this product. The authors use a dimensionless parameter h/<f~ to character ize fluid performance. This is the ratio of the film thick ness, h, to the composite surface roughness. A high value implies a good film and puts the fluid In the higher EHD region (l.e. near hydrodynamic lubrication). A value below 2 Implies lots of contact, l.e. a more boundary like EHD regime. The correlation of this parameter with bearing performance Is not too good. fc*i.uiwr cw wucat rmiE rvJl' (5) :. r.r-nv.L on ..r :;r;i, t it 2. *.v7Y;r:. s. i r-M-ir rujmosiucwi. ww. :oon nw r; ;:n:: wi-'M-v <a !:. ..o: if iso 'Oly::::::yl ithsr. *'Sc1 *;ht 2E3i;:. 7. rv:::;::ti: vr^.o '.itw.'T ::oucai/R Til cut asM". n. ;:r.ii'vY urv.TtD *TStc^. 3.C - <*.0 3-n {iriii .i/.Ti <i.s o.r <U? <JT 2/-"/ (r:i7;.-.L'.; <i.c 3,r-'..n WD Miaopr" : ,--,A.v HONS 036130 -79- Of the fluids rated equal or better than MCS 2931, only the Krytox 1**3 AB and possibly the Dow fluorosllioone could be used in air operations. Phenylphosphlnlc acid - This acid has one striking friction properry. That is, its jj- temp profile up to about 450F is very similar regardless of the metallurgy. This is shown graphically on the following figure. Perhaps this tells us something about the mechanism of lubrication by this acid. Phenyloctadecanolc acid - This material (Eastman) is a general boundary additive for MCS 524. Last month I stated that it contained no terminal phenyl group. The NMR people now say this is an error. The sample is a mixture of <MCHb)it-CO*H and CHs(CHa)N C~(CHa)is_gOaH COaH It would be interesting to see if the pure terminal acid is more effective than the mixture. Aryl Phosphate Lubricity Several additives were evaluated as steel lubricity agents for aryl phosphates. Specifically, they were tested in MCS 941 (36* CPDPP + 37* TPP + 27* CDP). Our Interest in this baBe stock has dropped since we are now making blends based on NCPDPP. However, MCS 94l is a good reference phosphate with poor steel lubricity. The screening test was the Chrysler Falex Test. This uses a hard steel (Rc 20) on a soft steel (Rb 65). The results were as follows: Additive (.1*) none Falex Test Failure Load psi 1000 2-propyl benzenephosphonite H-1128 4250 (passes test) 3270 4250 (passes test) 2700 L-77 CP64600 --- 2100 900 The results with the first two additives are not bad at all. MONS 036131 HONS 03613*: y i.. ,3-f/ fi c.; o , Aj hcs 3TiV O. / ' * ' 0. ! */. ---------- X, 5T; , o./ % ----------- -- 4/ o.o'rr% -------- s/e-e./ I a? -8l- 2-propyl benzenephosphonite tf-P-OCaHy =------------------------------------------------- H This 1b not an acid but 1b probably easily hydrolyzed. It should be screened In the Republic Test. H-1128 - This compound Is It was obtained from the Oil Additives Qroup. L-77 (Carbide) This is a silicone-ethylene oxide block polymer. It Is advertised as a "super1' wetting agent for stainless steel, teflon, aluminum, and glass. Since this polymer probably isn't reacting at the surface, the Increased load carrying Is probably due to Increased wetting. Blends with a higher concentration will be run. CP64600 This is Ludwig Maler's phosphosulflde. Pump-Plow Properties of Aryl phosphates We are also starting to look at some flow properties of arylphosphatee such as cavitation probe, and streaming potentials. A one gallon blend of NCPDPP plus 0.04% FC-98 was made up for the streaming potential measurement. Water-011 Emulsion Lubricity Water-Olycol Lubricity One suggested approach to the lubrication of water-oil emulsions Is to minimize the Interrupted flow of two phases at the surface. My first thought to a chemical approach to minimum phase separation was to try Carbide's surfactant silicones. These are block polymers of silicone-ethylene oxides. Thus one tall of the molecule would be soluble In each phase and might tie them together. AIbo, by varying the ethylene oxide chain, the vlBcoslty of the water layer might be matched with the oil layer. I have since found a Carbide patent for water lubricants (U.S. Patent 3,457,173 issued 6-22-69). Water lubricants Include emulsions and water-glycol blends. The feature of the Invention Is the use of silicone-ethylene oxide polymers In aqueous fluids. A typical structure for such a polymer Is HONS 036133 c, H3 o 9** 5/ o The lubricity of the block polymers Is enhanced by emulsi fied polyolefins such as polymerized n-olefins. Examples are given of Improved Palex loads for emulsions. The use of these block polymers may explain the excellent pump wear properties of Carbide's Ucon Hydrolube 150 LT. We should evaluate these polymers In water blends or interest to us. Presumably Carbide has done considerable testing of these products. NASA-Lewis Research Thermal Decomposition (Tp) Runs Bill Jones asked us to rerun two Tp's in the presence of M50 steel. This was because our Td values were higher than they expected based on their experience with these fluids. He thought the metal might catalyze a lower TD. This did In fact happen with one of the samples. All of the vapor pressure and Tp curves are completed. The results have been phoned to W. Jones. He also requested copies of the curves for calculation of Arrhenius constants. Lew Fowler is preparing a graphic conversion scale so these can be read directly from the curves. This should be ready this week. MCS 460 Samples One quart samples of MCS *160 were sent to Bob Johnson at NASA-Lewls and Ward Weiner at Oeorgla Tech. I also sent them a preliminary data sheet for this compound. Film Thickness Contract MONS 036134 Work continued on the heat capacities and bulk modulus curves of the model compounds. Cameron recently has used -83hls film thlckneBB measurements to study freezing In the contact zone. He has expressed an Interest In thermodynamic measurements of glass transitions or pour points. This might be heat capacity (via DTA or DSC) or it might be density or modulus measured as a function of temp. This Is still up In the air but we may make some further physical property tests on the fluids. HONS 036135