Document 44Enj61O9o1oeRVmNb7M5B3ja
ORGANIC CHEMICALS DIVISION
RES
St. Louis Research Dept, Report No, 2570
.FINAL REPORT ON
INDUSTRIAL FUNCTIONAL FLUIDS SALES APPLICATION RESEARCH
Job No, 2-02-750,01-3765
July 14, i960
Reported by L. R. Stark
Work Done by: R. E. Hatton W . S . Cl oud
/ Monsanto __VI_
DSW 622348
ST. LOUIS, MO.
STLCOPCB4096381
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MONSANTO CHEMICAL COMPANY Organic Chemicals Division St. Louis Research Department
S^. Louis Research Dept. Report No. 2570
FINAL REPORT ON
INDUSTRIAL FUNCTIONAL FLUIDS SALES APPLICATION RESEARCH
Job No. 2-02-750.01-5765
July 14, i960
Reported by L. R. Stark
Work Done by: R. E. Hatton
W. S. Cloud R. C. Cox L. R. Stark
0SMV 622349
STLCOPCB4096382
DISTRIBUTION
1. File 2. R. E. Hatton 2. M. C. Throdahl - File 4. Duplicate File 5. Central Technical Files 6. L. R. Stark 7 T. P. Sands 8. R. Davis 9. Extra 10. Extra -3,1. Extra
This report contains confidential information which is the property of the Monsanto Chemical Company and which shall be disclosed only to duly authorized persons. The recipient is held accountable for the filing and safe custody of the report which must be returned on demand.
DSW 622350
STLCOPCB4096383
TABLE OP CONTENTS
INTRODUCTION ----------------------------------------------------------------------------------------------------- 1
SUMMARY------------------------------ --------- ----------------------------------------------------------------------- 1
CONCLUSIONS ------------------------------------------------- ------------------------------ ----------------- 1
DISCUSSION
I. PYDRAUL FLUIDS
A.Pydraul A-200
1. Pydraul A-200/F-9 Mixture Use Limits ---------------------------
1
2. Thermal Stability------------------------------------------------------------------------ 4
3. Fire Resistance ---------------------------------------------------------------------------- 4
4. Electrical Properties ----------------
6
5. Drop Size For Lubricator Application----------------------------------- 6
6. Foaming and Filtration Studies ----------------------------------------------- 6
7. Oilgear Pump Test Used Fluid--------------------- ------------------------------ 8
8. Pour Point Comparison With Petroleum Oil---------------------------- 9
9. Mixtures with Pydraul F-9 and TricresylPhosphate ------------- 9
10. Compatibility --------------------------------------------- ------------------------------ ll
B. Pydraul F-9
-
1. Dayton power and Light Co., Used Fluid----------------------------------11
2. Pydraul System Sludge ---------------------------------------------------------------- 12
3. Solvent Compatibility ---------------------------------------------------------------- 12 4. Elastomer Compatibility ---------------------- -------------------------------------- 13
5. Mixtures with Pydraul A-20Q and Tricresyl Phosphate ------- 13 6. Pydraul F-9/A-200 Mixture Use Limits ----------------------------------- 13
I
C. Pydraul 150 1. Shear Stability---------------------------------------------------------------------------- 13 2. Deposit in Pipes -------------------------------------------------------------------------- 14
3. Pydraul 150/Houghto-Safe 1010Heat Test ------------------------------- 14 4. MXL-L-7808C Fluid Compatibility --------------------------------------------- 15
D. Pydraul AC 1. Viscosity-------------------- --------------------------------------------------------- --------- 15 2. Fluorescence ----------------------------------------------------------------------------------15 3. Pydraul AC/Cresyl Diphenyl Phosphate Used Mixture ---------- 15 4. Ethylene Glycol Compatibility ------------ ----------------------------------- 16 5. Drop Size ----------------------------------------------------------------------------------------16 6. Comparison with Pyrogard 55 in Compressor Application -- 16
7. Compatibility with Glycerine and Fluorochemlcal FC-101 - 17
E. Pydraul 60 1. Viscosity---------------------------------------------------------------------------------------- 17
II. Competitive Fluid Evaluation
A. Shell SFR Hydraulic Fluids -------------------------------------------
18
B. Mobil Pyrogards 43, 33 and 55 ---------------------------------------------------------18
C. Koiker Fluids A, B, C, and D -------------------------------------------
20
D. Cellulube 220-Hydrocarbon OilMixture Lubricating Properties-21
III. Miscellaneous
A. Sample Supply-------------------------- ----------------------------- ----------- ------- --------- 21
DSW 622351
..... STLCOPCB4096384
INTRODUCTION
1
The objective Of this research was to provide technical sales
information to aid in retaining Monsanto's current sales position and in acquiring new business for industrial functional fluids. This report presents the sales service application studies com pleted during the period January, 1959 through December, 1959.
SUMMARY
Appropriate application tests were performed on the Pydraul fluids as requested by the Sales Department. Some competitive fire resistant fluids were also evaluated. Various physical properties and bench scale performance properties were determined. Results of these tests appear in the Discussion section.
CONCLUSION
Appropriate sales service application studies requested by the Sales Department were completed during the period January, 1959 through December, 1959* Future work of this nature will continue under Job No. 2-02-760.01-^010.
DISCUSSION
I. Pydraul Fluids
A. Pydraul A-200
1. Pydraul A-200/F-9 Mixture Use Limits
As Pydraul F-9 is used and decomposed, its acidity increases; whereas, Pydraul A-200 starts with a relatively high initial acidity and upon sufficient use to destroy the lubricating and anti-rust additives drops in acidity. This can lead to considerable oonfusion in determining the use limits of these fluids by acidity values especially where they are mixed.
A graph of Pydraul A-200 acidity after various treatments was prepared (Figure 1). These tests which included functional testing (anti-wear and anti-rust) indicated that when Pydraul A-200 acidity (total acid number at pH 11) drops to one-half to two-thirds of the initial value, the fluid has been exposed to too much heat, oxygen, or moisture and should be considered for replacement. It Is noted that the strong acid number (below pH 4) did not Increase appreciably for Pydraul A-200.
Various Pydraul A-200/Pydraul F-9 mixtures were thermally aged at 400F. for varying lengths of time up to 96 hours. The fluid was contained in 250 ml. watch glass covered beakers in a natural convection oven. These aged samples
DSW 622352
STLCOPCB4096385
2
were checked for Initial pH, strong acid number, total acid number, four-ball wear, and rusting by a simple rust test. Titration curves revealed no significant characteristics to indicate fluid condition. The properties determined on each of the mixtures appears in Table I.
It was suggested that future work be done on mixtures from the field in an attempt to establish Idffe limit specifications for these fluid mixtures.
The following general suggestions and conclusions were presented:
a. No positive simple method for determining Pydraul F-9/Pydraul a-200 mixture useful life limits was found. There are indications that total acid number coupled with strong acid number may give some indica tion of the flulds condition. A phosphorus content (to determine the Pydraul F-9 content) in conjunction with the acidity information would be more meaningful. In any case, if the total acid number exceeds 1.2 to 1.5 or the strong acid number exceeds 0.10 it is suggested that the fluid be considered for replace ment. Such values might be expected in mixtures of 75# to 100# Pydraul F-9 in Pydraul A-200. Pydraul A-200 rich mixtures will exhibit a sharp acidity decrease when the functional additives are decomposed. This should be the point for replacement.
b. Anti-rust properties of Pydraul A-200 are depreciated considerably when mixed with Pydraul F-9 and aged thermally. If maximum anti-rust characteristics are desired, the fluids should not be mixed. The condi tion of Pydraul A-200 is then obtained directly by total acid determination. With thermally aged Pydraul A-200/Pydraul F-9 mixtures the anti-rust characteristics are not appreciably worse than for new Pydraul F-9 except at higher strong acid values where metal attack was noticed in the rust test.
c. Anti-wear characteristics of Pydraul A-200/Pydraul F-9 mixtures are generally depreciated after 50-60 hours of thermal aging at 400F. These values tend to re vert to the values determined for unadded Aroclors and are not considered excessive. Lubricating difficulties for aged fluid would probably occur only in marginal systems.
d. The presence of Pydraul A-200 in Pydraul F-9 appears to have an Inhibiting effect since total and strong acid do not Increase as rapidly in these mixtures as in Pydraul F-9 rich mixtures.
DSW 622353
STLCOPCB4096386
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DSW 622355
STLCOPCB4096388
4
2. Thermal Stability
Pydraul A-200 and OS-81 were subjected to a 400F. static oven test to determine their suitability for a particular sales application (memo: DPS to LRS, 1-30-59). Pydraul A-200 acidity dropped to 0.1 TAN (normal 0.9 TAN) between 72 and 168 hours exposure with some sludge formation. OS-81 appeared to be more stable with a very gradual acidity increase from 0.07 to 0.24 and trace quantities of solids on the beaker sides. This would indicate that OS-81 or a straight Aroclor fluid would be preferred rather than Pydraul A-200 in a high tem perature application.
Further work was done to relate the rapid acidity drop of Pydraul A-200 to its service life limits. Antirust properties of Pydraul A-200 are not destroyed before 120 hours exposure at 4qoF., foaming tendency is not de preciated up to 232 hours, and lubricating properties are depreciated at 150 hours exposure. The rapid acidity drop occurred at 150 hours and is believed to be a good measure of fluid life for undiluted Pydraul A-200.
Table II contains acidity, foam, rust and lubricating properties for Pydraul A-200 thermally aged in glass at 400*F. for varying time Intervals.
3. Fire Resistance
Fire resistance tests on Pydraul A-200 indicate this fluid to be equivalent to Pydraul F-9 in fire resistance. Values obtained for Pydraul A-200 follow:
Hot Manifold (MIL-F-7100), 1300F Does not flash or bum on tube or after leaving tube.
Low Pressure Spray Flammability (AMS 3150-F) Flame brightened but did' not increase.
High Pressure Spray Flammability (AMS 3150-B) will not ignite.
Molten Metal Ignition (molten aluminum alloy) Does not spontaneously ignite. Flashes by spark.
Flash Point (C.O.C.) 380 "F.
Fire Point (C.O.C.) bb0uF.
DSW 622356
STLCOPCB4096389
5
Pydraul A-200 Thermal Stability Glass, 400F
TABLE II
Hours Exposure
0 120
144 l6o 232
Acidity, Tan. mg.KOH/gm.
0.82 0.87
0.74 .
0.42 0..17
Foam, ASTM D-892, 75F. ,ml.
30 0
0
00
Rust, ASTM D-665, Dist. Water, 24 Hr. 10*
0STd sa/6 0.7*/dak/5 l*/d/7 2?d/7
4-Ball Wear, 167F.,600 RPM
Steel-on
10 KG
Steel
40 KG
0.29 0.26 0.43 0.48
0.26 0.60
0.44 0.73
0.38 0.65
Steel-on-Bronze
10 KG
1.40 1.36
1.41
1.26 1.22
Almen E.P. Load, # Torque> '#
48 39 41 33
39 33
26 27 25 26-
*REL M-403 Rating, 10 = Perfect
DSW 622357 STLCOPCB4096390
6
4. Electrical Properties
Electrical properties of Pydraul A-200 were obtained for sales information purposes ,, These values were reported by J. R. Kuster WGK Analytical Lab. as follows:
"We were not able to determine the dielectric constants or power factors with our equipment since the losses were too great. A rough check was made with an ohmmeter. It showed approximately 200,000 ohms at 100C, The re sistivity at 100C. was 0.09 x 10 ohm/cm. The dielectric strength at 25C. was found to be 38 K.V."
5. Drop Size for Lubricator Application
The relative drop size of Pydraul AC and Pydraul A-200 in Fluorochemical FC-101 was determined for sales service information to Air Reduction Company for use of these fluids in compressors using FC-101 in the compressor lubricant sight glass. Droplets formed on a 3.5 mm. 0.D-. by 1 mm. I.D. flat glass tip were found to be 36 drops per cc for Pydraul A-200 and 44 drops per cc for Pydraul AC.
6. Foaming and Filtration Studies
The possible depletion of Pydraul A-200 anti-rust and lubrication additives by attapulgus earth filtration prompted a filtration study. Lubrication and anti rust properties of Pydraul A-200 appear to be nearly unchanged by filtration through earth and cellulose filters; however, both these filters removed the anti foam additive, creating a potential foam problem.
Table III presents the functional properties of Pydraul A-200 after passing through various filter elements. The apparatus used for the filtration test consisted of a Tuthill gear pump, white enameled bucket reservoir, Variac controlled heater, a Briggs Z-9-1-AR-SV8 filter case, and appropriate piping. One gallon of fluid was circu lated at 130F. through the filter for two hours at 1/4 gpm (estimated 30 cycles).
Various solutions to the problem of anti-foamant removal were considered. Finer dispersions of the Dow Corning 200 fluid by first dissolving in various solvents then adding to the Pydraul A-200 blend were not effective. Also, the use of different antifoam additives was not effective to date. No further work was done on this problem during this report period pending the outcome of field tests in systems containing filters.
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The possible solutions to this problem were summarized as follows:
a. Field tests in actual equipment to determine if filters remove enough anti-foamant to cause trouble. This practical approach is being conducted by the Sales Department.
b. Dispersing the anti-foamant (DCF-200, 550 cs) in such a manner that it is not removed by the filter. This is difficult since DCF fluid adheres readily to ceramic and metal surfaces and is removed from a fluid even though the particles are much smaller
than the filter pore size.
A lab scale filter test was set up in which fritted glass filters were used. A 40-60 micron filter does not remove the DCF completely; whereas a 10-15 micron filter removed the DCF at 50 ppm concentrations. DCF 200, 1000 cs 50$ by volume with alpha pinene and
DCF 200, 60,000 cs 15$ in alpha pinene were added to Pydraul A-200 to a 50 ppm anti-foamant concentration. These too were removed by the 10-15 micron glass filter. Other DCF 200 solvents-which failed to ' disperse the anti-foamant sufficiently to prevent filtering out were tributyl phosphate, tributyl
phosphite, and Skellysolve B. TCP, Santolube 595, phenyl sulfide, dibutyl phenyl phosphate, and isopropanol were not miscible with the DCF.
c. Several different anti-foam additives other than DCF were tried ^successively. PC-1544, N-5262A, and glycerine at 100 ppm and 0.1$ were not effective anti-foamants. Other materials tried at 0.1$ without success were Ucon 75-H~90,000, Ucon 50-HB-5100, Ucon LB-1715, primary amyl alcohol, methyl amyl alcohol, n-decyl alcohol, 1,5-butanediol, triethylene glycol, hexachlorocyclopentadiene, 2,5-butanediol,
and 1,4-butanediol.
d. Reformulation of Pydraul A-200 is not being considered at this time since most of the known rust inhibitors for use in this formulation are pro-foaming.
The approaches of Items 2, 5, and 4 were not considered
further until the outcome of the field tests. Item 1, was
determined. No further conclusions were drawn during
the period of this report.
;
7. Oilgear Pump Test Used Fluid
Pydraul A-200' removed from an Oilgear Company pump test after 86 hours was very dark colored and had greenishyellow material rising to the top on standing. This
DSW 622360
STLCOPCB4096393
9
material was found to be a water emulsion. The water content is estimated to be 0.5$.
The contaminated fluid was replaced in the test unit and
the new fluid provided satisfactory, performance. No further work was done with the used fluid.
8. pour point Comparison with Petroleum Oil
The pour point of Texaco Regal B (petroleum-based
hydraulic fluid) was found to be 0*1?. compared to a
Pydraul A-200 pour point of +5F. The kinematic
viscosity of the Texaco fluid at QF. is equivalent
to that of pydraul A-200 at +4oF. Although the two
fluids have nearly equivalent pour points, the pump-
ability of the petroleum base fluid will be much better
at lower temperatures.
'
i
These data indicate that apparent pour points of synthetics should be used Judiciously when being compared..t,p. petroleum-based fluids for sales information purposes.
9. Mixtures with Pydraul F-9 and Tricresyl Phosphate
A Pydraul A-200 customer (Budd Co.) experienced diffi
culties with pump cavitation in systems which had been
operating satisfactorily with Pydraul F-9* It was
suggested by the Sales Department that tricresyl
phosphate (TCP) be added to the Pydraul A-200'or to
mixtures of Pydraul A-200 and pydraul F-9 to bririg the
specific gravity down to the Pydraul F-9 level. Calcu
lations were made to establish the quantities required.
Four-ball wear tests on F-9, A-200, TCP mixtures indi
cated antiwear were not as good as for Pydraul F-9
of pydraul A-200 alone; however, wear was better than
for TCP alone, in all cases wear was not considered
excessive.
-
Since this problem was solved by an alternate route no further work was done.
Speoific gravity corrections of pydraul A-200 - Pydraul F-9 mixtures by TCP additions were estimated graphically and appear below. Specification mid range values of specific gravity was used for each component. Some consideration was given to the use of gasoline grade TCP. Since little is known of its quality and perfor mance as a functional fluid, this approach was abandoned.
DSW 622361
STLCOPCB4096394
10 Sp. Gr. 25/25C
Pydraul F-9
1.275 - 1.295
Pydraul A-200
1.415 - 1.450
TCP (plasticizer grade)
1.1570 - 1.1600
TCP (gasoline grade)
1.155 - 1.160
The following table presents the percent (vol.) of TCP required in various Pydraul A-200 - Pydraul F-9 mixtures to return the specific gravity to that of pydraul F-9
Pydraul A-200 Pydraul f-9
TCP, A-ll
TCP, "G" grade
Approx. 100F Vise., cs.
100 90 70 50 30 10
0
0 To 2o 5U 70 90 TOO
55 50 44 36 25 9 0
50 47 42 34 23 8 0
. 52 53 35 38.5 44 50.5 53
Approx. 100F Vise ., cp.
41.2 42.5 45 49.5 56.5 65
68
It is noted that only the mixture of TCP and Pydraul A-200 without Pydraul F-9 would be expected to have an absolute viscosity slightly less than the Pydraul A-200 absolute viscosity- of 42.7 cp. (50 cs kineamatic).
Shell Four-Ball Wear values for some of the mixtures follow.
A-200
% Vol F-9
TCP
.
4-Ball W< 10 Kg
100
--
--
0.27
--
100
--
0.25
--
--
100
0.38
47 59-2
--
16.8
53 44
0.31 0.25
22.5
52.5
25
0.35
*620 rpm. 1 hr. l67F, steel-on -steel
DSW 622362 STLCOPCB4096395
11
10. Compatibility
The compatibility of Pydraul A-200 was checked with the competitive fluid, Pyrogard 43 (Socony Mobil) and with an ..elastomeric electrical cable covering for a potential customer.
Pydraul A-200 appeared to be completely miscible with
pyrogard 43. No separation was noted during two weeks
room temperature exposure with volume concentrations of
10, 50 and 90 percent.
'
The outer elastomeric covering (composition unknown) of an electrical Cable bundle from a potential Pydraul user (Breedbands HOogovenes, Holland) was immersed in
both pydraul A-200 and Pydraul F-9 at 100 F fdr two weeks. In both cases the material became slightly more pliable and the piece in Pydraul P-9 increased in weight 12.9# and in length 1.9#. The piece in Pydraul A-200 increased in weight 16.7# and in length 3.0#. These increases are not considered excessive and would probably be less under conditions of actual use; that is, intermittent spillage, partial immersion only on the outside, and ambient temperatures below 10QF. " No property changes on the Pydrauls were determined since such information is not applicable to the problem.
B. Pydraul F-9
1. Dayton Power and Light Co., Used Fluid
Two used Pydraul F-9 samples from Dayton Power and Light Co. Sulzer boilder units were found to be withir new fluid specification limits for acidity, specific gravity, and moisture. ASTM D-665 rust values for these fluids are equivalent to new Pydraul F-9. This would indicate that the used fluid either contains no rust inhibitor or that the inhibitor was depleted in some manner. It was reported by the Sales Department thaft recommendations were made in the past to rust inhibit this fluid; but it is not known whether or not this was done.
Acidity, specific gravity, moisture, and rust values for the two used samples of Pydraul F-9 are included.
DSW 622363
STLCOPCB4096396
12
Pydraul F-9 Spec, limits Pydraul F-9 Typical new Pydraul F-9 Used No. 4 Unit Pydraul F-9 Used No. 5 Unit Cellulube 220
Neut,, No, Sp. Gr. TAN 25/25C
Moisture %
D-665 Rust
0.15 max
1.275 to 1 - 295
0.20 max.
l/d/9'
0.15
I.2805
0.10
l/d/7
0.15
1,2792
0.09
l/d/7
--
--
--
l/d/9
Note: D-665 rust with distilled water First digit of rating in dicates extent of rusting where 10 is no rusting.
2. Pydraul System Sludge
Sludge from a Saginaw Bay Industries hydraulic system filter is believed to be something other than fluid base stock breakdown products. The principal content `of the sludge is considered to be contaminants introducted externally or by wearing of the machine.
The Saginaw Bay industries system from which the sludge sample was taken has a past history of mixtures of
Pydraul F-9 with Standoil 21 and Pydraul 625. The current fluid was reported to be principally Pydraul F-9 and pydraul A-200 with Pydraul 625 added to adjust the viscosity.
The sludge sample appears to consist of major portions of metallic or inorganic material (HC1 soluble) and what is considered to be fluid base stock (Skelly B soluble). A small amount of material resumbling a polymeric viscosity
index improver was present. This material was not Skelly B soluble, but was soluble in ethyl ether and partially soluble in acetone. Little or no NaOH soluble material was present.
5. Solvent Compatibility
Eight solvents appear to be completely miscible in all proportions with Pydraul F-9 and Pydraul A-200. It is recommended that additional functional testing be done with a particular solvent when such a solvent is chosen by a customer for flushing a Pydraul containing system.
Ten, fifty, and ninety percent (volume) mixtures of each
of the following solvents in Pydrauls F-9 and A-200 resulted
in no separation during two weeks exposure at room
temperature. ,
.
........... - ------
DSW 622364
STLCOPCB4096397
13
Perchloro ethylene o-Dichlorobenzene
Orthene Tetrachloroethane Dichloroethane 1,2,4-Trichlorobenzene Aroclor 1221 Aroclor 1252
4. Elastomer Compatibility
Refer to Section A-10 above on compatibility of Pydraul P-9 with elastomeric electrical cable covering.
5. Mixtures with Pydraul A-200 and Trlcresyl phosphate
Refer to Section A-9 above for four ball wear values of Pydraul F-9/Pydraul A-200/tricresyl phosphate mixtures.
6. Pydraul F-9/Pydraul A-200 Mixture Use Limits
Refer to Section A-l above for laboratory work done to
determine Pydraul F-9/Pydraul A-200 mixture use life
limits.
'
C. Pydraul 150
1. Shear Stability
New Pydraul 150 subjected to the diesel injector shear test incurred nearly the same.loss In viscosity as the loss reported for Pydraul 150 from an actual hydraulic system at Alcoa. This result indicates (a) the loss of viscosity of the Alcoa pydraul 150 Is considered normal and (b) the diesel Injector test yields results consistent with actual
practice..
Viscosities of Pydraul 150 after successive passes through the diesel Injector shear test are presented below with values for Pydraul 150 from an Alcoa hydraulic system.
Injector Passes
Viscosity
100F
210. F
cs % Loss cs io Loss
Alcoa 0 4 8
12
25.5 31.0 24.7 23.3 22.6
24.2
--
.20.3 22.8 27.1
5.11 7.47, 5.77 5.^0 5.19
31.5
--
22.8 27.7 30.5
STLCOPCB4096398
14
2. Deposit In Pipes
The deposit in a pipe section from a German BBC turbine governor installation containing Pydraul 150 is con sidered normal for Pydraul 150 decomposed in the absence of air (Memo: R. Davis to A. T. Hinson 8/29/59).
This deposit was partially dissolved and loosened by ex posure' to either 5$ NaOH or 3$.NaOH with Ifo trisodiumphosphate at 100P. Although the deposit was very easily removed with a spatula after the caustic treatment for about 5 days, it is not known whether it would be dis lodged by normal pumping velocities through a system.. Also, the waxy nature of the deposit was such that it wasn't dissolved rapidly. Any recommendations for cleaning by this method should include circulation of warmed caustic for a sufficient interval followed by dismantling and roding out if necessary.
5. Pydraul 150/Hought-'o-Safe 1010 Heat Test
__ __
A special high temperature heat test indicates Pydraul 150 to be inferior to Houghto-Safe 1010 with respect to deposit formation. This test simulating the heating of hydraulic lines to 1200F. to 1500F. resulted in large quantities of a black granular deposit with Pydraul 150; whereas,'Houghto-Safe 1010 left only a very thin film of black deposit on the tube wall.
Test apparatus used consisted of a 12" length of 2-1/2inch standard iron pipe fitted with a cap and vent holes at the top and a reducer to a 10-inch length of 1/8-inch standard iron pipe at the bottom. The 1/8-inch pipe was capped at the bottom., Chromel-alumel thermocouples extended down in the center and nearly to the end of the l/8-inch pipe and into the upper reservoir portion of the' 2-1/2-inch pipe.
Pour hundred cc of fluid was placed in this apparatus and the lower 4 to 5 inches of the l/8-inch pipe was heated by means of gas burners until the temperature indicated by the lower couple was 1200P. to 1500F. Heating was continued at this temperature for 15 minutes. At the end of this time, the Pydraul 150 reservoir temperature was l65F. and that of the Houghto-Safe 1010 was 240P.
After being cooled, the 1/8 inch tubes were sawed in half lengthwise at the lower end revealing the deposit formation indicated above.
DSW 622366
STLCOPCB4096399
15
4. MIL-L-T8o8c Fluid Compatibility
Pydraul 150 appeared to be completely miscible at room temperature with a MIL-L-7808C fluid (Texaco Synjet 01115).
D. Pydraul AC
1. Viscosity
Viscosities of Pydraul AC determined at 70F, 100F,
and 210F. for sales information purposes are listed below.
70 F 100 F 210 F
55^ cs 87.2 cs.
3.02 cs.
2. Fluorescence
Pydraul AC exhibits negligible fluorescence under ultra violet light (believed to be 3660 Angstrom units). This is of interest in an application where a currently used petroleum base compressor lubricant is being carried over in a paper handling or processing operation and undesirable fluorescence results.
3. Pydraul AC/Cresyl Diphenyl Phosphate Used Mixture
A sample of used Pydraul AC containing 50#(v) cresyl diphenyl phosphate (CDP) from a Chemstrand Corp. (Pensacola, Florida) air compressor was found to contain extremely fine black solids and had very poor ahtiwear properties. Filtration through diatomaceous earth failed to remove all the solids and did not improve the antiwear properties. The sample was forwarded to the Analytical Laboratory for
property analysis.
Four-Ball Wear values for these mixtures follow:.
4-Ball Wear*
10 Kg. 40 Kg.
Unflltered Pydraul AC-CDP (Chemstrand used) 0.70
1.09
Filtered Pydraul AC-CDP (Chemstrand used)
0.92
-------
New Pydraul AC-CDF
0.35
0.75
*1 hour, 620 rpfi, l67F, steel-on-steel
DSW 622367
STLCOPCB4096400
16
4. Ethylene Glycol Compatibility
Pydraul AC appears to be immiscible or- sparingly soluble with ethyleneglycol at room temperature. Pydraul AC would therefore not be expected to Interfere with ethylene glycol air drying systems.
5. Drop Size
The relative drop size of pydraul AC and Pydraul A-200 in Fluorochemical FC-101 was determined for sales service Information to Ain-Reduction Company for use of. these fluids in compressors using FC-101 in the compressor lubricant sight glass. Droplets formed on a 3,5 mm. O.D. by 1 mm. I.D. flat glass tip were found to be j>6 drops per. cc for Pydraul A-200 and 44 drops per cc for Pydraul AC.
6. Comparison with pyrogard 55 in Compressor Application
Determination of fluid quantities in water - fluid emuTsions and in diatomaceous earth filter media from different air compressor systems containing Pydraul AC and Pyrogard 55 (Socony fire resistant fluid) Indicated no significant differences.
This work was done to answer specific questions concerning a problem of apparent air compressor over lubrication.
Presented below are findings and comments on this problem concerning a Pydraul AC sales application at Pratt and Whitney's East Hartford, Connecticut Research Center. V. A. Parent's memo of July 29, 1959 indicated a problem of air compressor over lubrication with subsequent carry through of fluid to end use stations.
Answers to his specific question are:
a. Extraction of the diatomaceous earth-filter samples (1/8 inch to 1/4 inch diameter clay-like particles) containing Pydraul AC and Pyrogard 55 re vealed 22.1# (wt.) and 20.5# (wt.) of these fluids re spectively. This is not considered to be a significant difference.
b. The water-fluid emulsion separated from the compressed air streams contained 10.6# (vol.) and 7.9$ (vol.) of Pydraul AC and Pyroguard 55 respectively. Again, this difference may not be significan depending upon the time and conditions of sampling. There is no way to tell whether this quantity of fluid indicates over lubrication without knowing ambient conditions of Intake air and compressor capacity.
DSW 622368
STLCOPCB4096401
17
At our analysis, the water and fluids were well separated with the water layer remaining somewhat turbid. Both the Pydraul AC and Pyrogard 55 layer's were free flowing although the Pyrogard 55 was considerably darker brown in color than new fluid.
Quantity of fluid as well as dispersed fluid droplet size can change the consistency of emulsions. Specific characteristics of Pydraul AC and pyrogard 55 water emulsions are not known. However, all other things being equal, the Pyrogard 55 system might be expected to be less viscous at lower temperatures since it is less viscous than Pydraul AC at temperatures below about
80F.
c. We have no simple procedure to check the Sova beads for loss of drying efficiency by Pydraul AC con tamination.
The writer does not recommend the scheme of passing the fluid laden air stream through the Sova bead (be-__ lieved to be Socony Vacuum silica gel) drier before going through the diatomaceous earth filter.. The drying mechanism of silica gel is due to its porous nature. * Relatively nonvolatile impurities or components of a \gas stream tend to coat and fill the silica gel decreas ing efficiency.
The best answer to this problem appears to be the reduction of lubrication to as low a rate as possible or acceptable by all concerned.. If this rate is then not sufficient to eliminate the lubricant carry-through, then more efficient separation or filtration will be necessary.
7. Compatibility with Glycerine and Fluorchemical FC-101
Pydraul AC appears to be immiscible or sparingly soluble with ethyleneglycol in concentrations of 10$, 50$, and 90$ by volume at room temperature. This work was done to answer a sales service request concerning the use of Pydraul AC by Los Angeles power and Light Company in an air compressor system followed by an ethylene glycol drying system. Pydraul AC should have no adverse effect on such a system's drying efficiency and should be readily separated by simple decantation if desired.
E. Pydraul 60
1. Viscosity
Viscosities of Pydraul 6o determined from -4oF. to 210F. for sales information purposes follow:
DSW 622369
STLCOPCB4096402
18
210 F 100F
0F -30 F -4oF
2.44 cs
9.95 cs 268. OS 2110. CS 5240. cs
II. Competitive Fluid Evaluation
A. Shell SFR Hydraulic Fluids
Viscosity values were determined for Shell Oil Co. SFR
Hydraulic Fluids B and c. It is noted that viscosity values
for these fluids correspond to values for Cellulube fluids 150 and 220 respectively. These values are presented below.
Fluid
Viscosity cs at 100f cs-at 210F
Shell SFR Hydraulic Fluid B
Shell SFR Hydraulic Fluid c
Cellulube 150
Cullulube 220
52.4
45.2 52.1 47.3
4.25
4.97 4.4 5.04
No further work was done with the Shell fluids during this report period.
B. Mobil Pyrogards 45, 55 and 55
Mobil Pyrogards 45, 53, and 55 (Socony Mobil Oil Co.) have been examined for phosphorus and chlorine content, viscosity, specific gravity, rusting tendency, and foaming tendency. This information indicated Pyrogard 45 to be a phosphate ester - Aroclor type of mixture (equivalent to 56$ Aroclor 1242 and 44# Cellulube 220) and Pyrogards 53 and 55 to be phosphate -ester fluids. Pyrogard 53 has physical and chemical characteristics very similar to Cellulube 220; whereas Pyrogard 55 has a higher viscosity and density similar to a mixture of 47# Cellulube 220 and 53# Cellulube 1000.
Pyrogards 45 and 53 have good antirust characteristics indicating the possible use of inhibitors. No foaming was observed with Pyrogards 45 and 55; however, Pyrogard 53 had a moderate foaming tendency and persistence.
Presented below are physical, chemical, and functional properties obtained for the Pyrogard fluids. Some Cellulube 220 properties are included as a comparison.
DSW 622370
STLCOPCB4096403
19
Appearance
Odor
Phosphorus $ Chlorine $ Viscosity
cs at 100P cs at 210 F Specific Gravity : at 25/25C Flash point COC F Fire Point COC F A. I. T., F Foam at 75F D-665 Rust
Pyrogard 43 Pyrogard 53
Pyrogard 55
Cellulube 220
very light
yellow clear
light yellow
very slight turbid
amber slight turbid
mild Aroclor mild phosphate mild phosphate ------ester
5.45
7.24
7.29
7.76
23.79
<0.3
<0.3
0
30.1 5.47
1.2687
47.5 4.96
1.1465
96.5 6.80
1.1741
47.33 5.04
1.1468
410 490 320 44o
610 610 673 685 .
1115 None 10
1070 Yes* 10
1090 None l/d/7
' 1075
-- --
#
5 min. blow
Collapse
75F 200 F
75F
210 ml
0 48o
205 sec. 0
120 ml at 10 min.
**
10
is
rust
free,
1
is
32
rust
dots
less
than
1 mm. dlam.
Pyrogard 43 (Socony Mobil Oil Co.) reported to be suitable for use as a steam turbine lubricant was sub jected to the ASTM D-943 oxidation test. Results of this test Indicate Pyrogard 43 to be inferior to OS-81 in this test..
ASTM D-943 Steam Turbine Oil Oxidation results for Pyrogard 43 (Soeony Mobil Oil Co.) appear below. It was noted that the fluid has a relatively high acid number which is probably due to rust inhibitors believed
DSW 622371
STLCOPCB4096404
20
to be -present* Between 168 and 336 hours exposure this value dropped and at this time the fluid became con siderably darker with some carbonaceous deposits forming on the tube walls especially at the fluid - water inter face .
Test time: 1512 Hours
Acidity:
Initial N.N., TAN 0.22 Final N.N., TAN 0.88
Initial pH 4.1 Final pH 4.2
Viscosity:
100F Initial 30.1
100F Final
27.0
Change, %
-10.6
210F initial 3.47
210F Final
3-35
Change, #
-3.4
Fluid Appearance:
Dark brown, opaque, insolubles in fluid ;Insolubles: 2.5$ Metal Condition:
Steel: heavily scaled and rusted, dark rust - black color
Copper: yellow green coat, etched
Acidity change with time:
Hours
TAN
PH
Fluid
0 168 336 696
840 1200 15.12
0.22
-------------- *
0.13 0.29 0.48 0.51 0.88
4.1
--------- -----
4.0 3,9 4.8 4.2 4.2
SI. yellow clear
SI. yellow clear Dark brown with deposits Dark brown Dark brown opaque Dark brown opaque Dark brown opaque
C. Kolker Fluids A, B, C and D
Four fluids formulated by Kolker Chemical Company (memo: RD to REH, 1-2-59) were checked for viscosity, density, and pour point characteristics, it was Indicated that these
DSW 622372
STLCOPCB4096405
21
fluids are believed to be phosphate esters and chlorinated biphenyl or mixtures of theses.
Table IV contains density, viscosity, and pour point information for the four Kolker fluids designated A, B, C, and D.
D. Cellulube 220 - Hydrocarbon Oil Mixture Lubricating
Properties
~ ''
Four-Ball wear values run on a sample of hydrocarbon base oil contaminated with Cellulube 220 indicate normal wear values. Pour-Ball wear values run on the oil layer are as follows:
Steel on Steel, 6J0 rpm, l67P
10 kg, 1 hour 40 kg, 10 hours*
0.24 mm 0.64 mm
Steel on Bronze, 650 rpm, 167P, 1 hour
--
10 kg
1.57 mm
.
^Machine did not shut off after one hour. This information was provided for sales service purposes.
E. Houghto-Safe 1010/pydraul 150 Heat Test
A special heat test comparing the thermal stabilities of Houghto-Safe 1010 and pydraul 150 appears in Section C-5.
III. MISCELLANEOUS
A. Sample Supply
An .8 ounce (oil sample bottle) of pydraul P-9 was sent at the Sales Department's request to Robert T. Holmes, Shell Oil Company, Chicago 5, Illinois
DSW 622373 STLCOPCB4096406
22
Fluid
Kolker A Kolker B Kolker C Kolker D
TABLE IV
Kolker Fluids
Density, gm/ml ______
6oF
100F 100 F cs
Viscosity 210 F lO.OOOcs
cs 5f
100.000 cs 6F
Pour
Point F
1.469 1.457 129. 4.55
53
40 37
1.296 1.284 1.4257 1.401
26.2 45.3
5.25 3.44
14 33
-2 -10 21 15
- --_
1.166 125. 7.52
38
22 15
bl 11/8/60
R. E. Hatton L. R. Stark
DSW 622374 STLCOPCB4096407
O LM m 9 9 L9
^,.*5 -
DSW 622375 STLCOPCB4096408