Document reXoG2evGbd7qLZb6rVdvzZBa

~fr~ STLCOPCB4096064 MONSANTO CHEMICAL COMPANY Organic Chemicals Division St. Louis Research Department St. Louis Research Report No, 2^72 FINAL REPORT ON FUNCTIONAL FLUIDS APPLICATION RESEARCH JOB NO. 2-02-760.01-3505 (II) February l6. i960 Reported by; L. R. Stark Work done by: E. P. Cunningham R. E. Hatton H. W. Luebke L. R. Stark DSW 622034 STLCOPCB4096065 DISTRIBUTION FOR REPORT KQ, 2472 1. File 2. T. M. Patrick - R. E. Ha'-.ton 3. M. C. Throdahl - file 4. Duplicate file 5. Central Technical Files - Creve 6. L. R. Stark 7 ,, ! . 2. Klein 8. T. P. Sands - H, S. Litzslnger Extra 10. Extra This report contains confidential information which is the property of the Monsanto Chemical Company which shall be disclosed only to duly authorized persons. The recipient is held accountable for the filing and safe custody of this report which must be returned on demand. DSW 622035 STLCOPCB4096066 TABLE OP CONTENTS PAGE NO. INTRODUCTION 1 SUMMARY. 1 I. II. III. Industrial Fire Resistant Type Fluids ............ High Temperature and Fire Resistant Aviation Type Fluids ................................ Miscellaneous .............................. 1 2 2 CONCLUSIONS DISCUSSION 3 3 I. Industrial Fire Resistant Type Fluids ............... 3 A. Fire Resistant Fluid Base Stock Screening ....... 3 B. Aroclor Fluid Formulation ....................... 3 C. OS-95 Formulation ................................................. .. 5 D. Fire Resistant, Low Viscosity Hydraulic Fluid, OS-104 ................................................................ 9 E. Phosphate Ester Formulation................................. .. 15 F. Preservative Type Hydraulic Fluids...................... 15 G. Rust Inhibited Pydraul F-9 and Pydraul 625-> H. Steam Turbine Lubricant, OS-81.......... .. 19 1. Rust Inhibited OS-81.............................................. ..... 19 2. OS-81 Resistant Coatings .................... ..................... .. 19 3. Gas Turbine Lubricant Application............ 19 II. High Temperature and Fire Resistant Aircraft PlUidS 21*ogaooi>*ooaoaoaovaaei)0o*aos A. High Temperature Fluid Screening and Formulation ..................................... 21 1. General Screening ........................... 21 2. High Temperature Jet Lubricant Formulation ................................. 22 3. High Temperature Hydraulic Fluid Formulation ............... .. 23 4. Polyphenyl and Polyphenyl Ether Mixtures..... 23 5. Miscellaneous ....................................................................... .. 25 B. OS-45 Fluid Evaluation .......................... 26 1. Objective and Conclusion .................... 26 2. Discussion of Experimental Work ............. 27 DSW 622036 STLCOPCB4096067 TABLE OF CONTENTS (continued) PAGE NO. C. Skydrol 500 ... - 52 1. Reformulation to Eliminate Dermatitis.... . . 32 2. Viscosity Index Improver................ . . 33 D. Silicate Weapons Lubricant.................. ... 54 E. Skydrol 7000 - Low Temperature Viscosity.... . 35 Ill. Miscellaneous ........................................ .. 55 A. ASTM Cooperative Test Work ............ .. 35 B. Synthetic Lubricants for Refrigeration Units. .. 56 C. Low Temperature Viscosity Study............ .. ,. 56 D. Lubrication Study - Paraffinic Petroleum Oil. .. 36 E. Compressor Lubricant - Pour-Ball Wear .. 37 APPENDIX Table I Table II Table III Table IV OS-95 Physical and Functional Properties OS-104 Physical and Functional Properties OS-45 Fluid Evaluation Rust Inhibited Pydraul F-9 and Pydraul 625 ASTM Cooperative Tests Fire Resistance Lubricating Properties Stability DSW 622037 STLCOPCB4096068 INTRODUCTION The objective of this research was to provide an application program to maintain and expand our current functional fluid product lines. The scope of this work included bench scale evaluation of current fluids, evaluation of potential base stocks, and formulation of fluids with greater utility or competitive position from potential base stocks. This report presents the application studies completed during the period May, 1957 through December, 1958. SUMMARY I. Industrial Fire Resistant Type Fluids Potential fire resistant industrial type fluid base stocks screened were of the classes phosphate ester, alkylated Aroclor, chlorinated biphenyl ether, and alkylated benzene. Of these a tertiary butyl triaryl phosphate exhibited qualities which would warrant further formulation efforts. This work is continued under the succeeding Job No. 3766. Formulation work was done on an Aroclor base fluid in an effort to develop a satisfactory fluid of lower price than the current Pydrauls. Viscosity index improved versions were abandoned due to unfavorable cost or performance characteristics. This project resulted in a non-viscosity index improved, fire resistant, Aroclor base industrial type hydraulic fluid designated OS-95 and subsequently named Pydraul A-200 as a sales item. A fire resistant, low viscosity hydraulic fluid, designated OS-104, was formulated to augment Pydraul 150 in systems requiring a greater degree of thermal and shear stability. During the period of this report OS-104 was not accepted by Development pending a review of market and fluid requirements. A viscosity index improved phosphate ester fluid was formulated as a chlorine-free fire resistant fluid for the Navy and as a fire resistant, mineral oil insoluble fluid for a specific application. The project was discontinued when the fluid failed the Navy specification tests and the oil Insoluble fluid application ceased to exist. A preservative type fire resistant hydraulic fluid designated 0S-100 was formulated for use by the U.S. Navy. Rust inhibited versions of Pydraul F-9 and Pydraul 625, designated OS-101 and OS-102, respectively, were formulated for customers who experience rusting problems. Some Unsuccessful work was done to find a non-foaming, non-copper attacking rust inhibitor for OS-81. 1 DSW 622038 STLCOPCB4096069 2. Two coating materials were found which are resistant to 0S-8l Various other Information was supplied pertaining to the application of OS-81 as a fire resistant industrial gas tur bine lubricant. . II High Temperature and Fire Resistant Aircraft Type Fluids Twenty experimental materials were screened for applica tion as high temperature hydraulic fluids or lubricants. None of these base stocks appeared to be suitable for formulation to the applicable military specifications. Preliminary work was done to find low melting polyphenyl ether or polyphenyl mixtures for these applications. Again, these fluids did not possess the basic physical properties for application against existing specifications. Two formulations, one based on bis(1-methylcyclohexylmethyl) sebacate and the other on 1,l-dldodecyl-3>3-di(2-ethylhexyl)urea were formulated to meet specifications for a 450F. to 550F. high temperature fluid as outlined by a pump manufacturer's represents- tlves. Full scale functional testing of these fluids was not completed during the period of this report. . A project was completed on the evaluation of the OS-45' type fluids to provide Information on their performance and service life limits. The competitive fluids, Oronite 8515 and Oronlte 8200, were included as a basis for comparison. Reformulation of Skydrol 500 to eliminate a dermatitis causing additive resulted in an acceptable formulation subsequently adopted as Skydrol 500A. Several tests were conducted on a new process Acryloid for Skydrol 500 with negative results. Further modified Acryloid samples from Rohm and Haas were evaluated under the succeeding Job No. 5767. Formulation work on a silicate weapons lubricant to meet military specification MIL-L-14107 failed to provide a qualified product. III. Miscellaneous ASTM Cooperative tests were conducted on reference fluids supplied by an ASTM committee. Lubricating properties, fire resistance, and stability information was obtained on the fluids. A minor amount of work was done to establish the level of lubricating properties desirable for refrigeration unit lubricants. DSW 622039 STLCOPCB4096070 3. Low temperature viscosity values were obtained on Skydrol 500 to check our procedure and results against values obtained at Douglas Aircraft Company. Minor lubrication studies were conducted on iron treated petroleum oil and on compressor lubricants as a service to various individuals. CONCLUSIONS ' Appropriate application studies were conducted during the period May, 1957 through December, 1958. Future work of this nature will continue under a new job number. DISCUSSION .I. I. Industrial Fire Resistant Type Fluids A. Fire Resistant Fluid Base Stock Screening Chlorinated diphenyl ether, dodecylbenzene, and three alkylated Aroclors were evaluated on the basis of low tempera ture viscosity, flash and fire points, molten metal ignition, and ASTM slope. Three Aroclor base stocks (1242, 1248, and 1254) were subjected to the same tests as reference fluids. The chlorinated dodecylbenzene exhibited the most desirable characteristics of the fluids listed; however, its fire resistance was inferior to that of Aroclor 1242. This fluid might find application as a diluent for the more fire resistant fluids to improve their low temperature characteristics. Test results appear in ..Table I. Isopropyl triaryl phosphate (prepared by , J.D. Sullivan) was considered to be less oxidatively or thermally stable than tricresyl phosphate (TCP) and was not considered further as a fire resistant fluid base stock. Tertiary butyl trlaryl phos phate (St. L. 15407, JDS) exhibited oxidation corrosion characteristics equivalent or better than TCP. Further work on the t-butyl triaryl phosphates was done under a succeeding job number (3766). Oxidation corrosion and 4-Ball Wear data appear3n Tables II and III. B. Aroclor Fluid Formulation A project was initiated to formulate an improved fire resistant industrial fluid based on Aroclors to broaden Monsanto's participation in this market, to meet competition, and to provide fluids of more desirable characteristics. The low cost of Aroclors together with their excellent fire resistance and good stability under hydrolytic, thermal, and oxidative conditions make them excellent candidates for fire resistant fluid base stocks. This project resulted in a non-viscosity index improved, fire resistant Aroclor base industrial type hydraulic fluid designated OS-95 and subsequently named Pydraul A-200 as a sales item. DSW 622040 STLCOPCB4096071 4. Initial formulation was directed at improving the viscosity index and lubricating properties of the Aroclor base stocks. A fluid equivalent or better than Pydraul P-9 in these respects was desired. Several formulations were prepared using Acryloid type viscosity index improvers (Acrylold 710, Acrylold HF-855, Acryloid HP-825, Acryloid HP-860). This approach was later abandoned due to the relatively large quantities of viscosity index improvers required. In addition to being shear unstable, these materials added considerably to the cost. These various formulations are presented in Table IV for record purposes. Included in this table are initial viscosities and four-ball wear and loss of viscosity on shearing for a few of the blends. Another class of viscosltv index improvers, the high molecular weight Ucon lubricants (CarbideJ, were found to be very shear stable. The first of these blends were made to establish the desired additive concentration and an Aroclor base stock combination. At that time a fluid was sought with a positive viscosity index and a 100P. viscosity equivalent to 200 Saybolt Universal Seconds on an absolute basis. In addition the lubricating properties were to be equivalent to Pydraul P-9. Blends which approximated the viscosity requirements were as follows: a. Aroclor 1242 Ucon 75--H-90,000 97-5* 2.5# b. Aroclor 1242 Aroclor 1252 Ucon 75--H-90,000 67.0* 29.og 4.0# Other Ucon containing formulations appear in Table V. It was deter mined that the load carrying properties of the Ucon containing Aroclors as measured by the Almen machine were inferior to the base fluid. Considerable formulation work was done to Improve the load carrying properties without depreciating the good anti wear characteristics. Several additive combinations were found which yielded Aroclor-Ucon blends with antiwear and load carrying proper ties equivalent to Pydraul P-9 in the four-ball and Almen tests. These blends appear in Table VI. It has since been questioned whether the Almen test is a good evaluation of E.P. properties and further whether or not such superior E.P. properties are necessary in a hydraulic fluid. This should be studied in the future. DSW 622041 STLCOPCB4096072 5. A revision in the fluid requirements to include a rust inhibitor further complicates the formulation problem. At that time, too, it. was found that the Ucon viscosity index improvers created an emulsion problem and were dissolved from the Aroclor base into water. For these reasons and due to the additional cost of 2.5$ to 4$ of additive necessary, the Aroclor-Ucon blends were abandoned. It is recommended that the. Ucon type of visoosity index improvers be further evaluated if future clarification of require ments for lubricating, emulsion, additive leaching by water, and anti-rust allow the use of such materials. In addition, their superior low-shear performance would warrant looking for materials of a similar nature but without the Ucon's shortcomings. Due to the unpromising outlook for the viscosity index improved versions, a non-viscosity index improved Aroclor fluid was formulated. These blends>appear in Table VII,, The required fluid was to consist of a mixture of Aroclors as the base stock with appropriate additives as necessary to obtain the specified viscosity, lubricating properties, and anti-rust ' characteristics. The desired viscosity values were a 100F. viscosity of 200 to 300 SU3 absolute, 45F. viscosity of 4500 SUS absolute maximum, and a l60F. viscosity of 60 SUS absolute minimum. The pour point was to be less than 10F. if possible. The lubri cating properties were to be equivalent or superior to those of Pydraul F-9 and the anti-rust characteristics were to be of an acceptable level, as Judged by the ASTM D-665 Steam Turbine Oil Rust Test. All other performance values were to be equivalent to those of Pydraul F-9* The final blend representing these properties and designated OS-95 consists of 66$ Aroclor 1248, 33$ Aroclor 1242, 0.5$ Santolube 393, 0.5$ Santolube 70 and 50 ppm. D.F.C. 200 by weight. A discussion of the various 03-95 performance and physical properties follows in Section C. C. OS-95 Formulation 1. General Requirements and Final Blend An Aroclor base fire resistant, industrial type hydraulic fluid, OS-95, was formulated to meet viscosity, lubricating requirements, and antirust characteristics specified by the Sales Department. These requirements and the steps taken in formulating OS-95 appear in Section B, Aroclor Fluid Formulation. The final blend representing these properties consists of 66$ (w) Aroclor 1248, 33$ Aroclor 1242, 0.5$ Santolube 393, 0.5$ Santolube 70 and 50 ppm DCF-200. This fluid was transferred to the Develop ment 'Department.for full scale evaluation and testing in the field. Bench scale performance and physical properties for OS-95 appear in Appendix Table I and specific comments on the OS-95 characteristics appear below. DSW 622042 STLCOPCB4096073 6. 2. Viscosity and Pour Point The lower limit of the required 200 to 300 SUS absolute viscosity range was chosen as a basis for Aroclor base stock mixing. This would' represent the most severe viscosity condition. A mixture of one part of Aroclor 1242 to two parts of Aroclor 1248 by weight exhibits the desired 100F. viscosity of 200 SUS absolute. These proportions may have to be varied slightly to account for the differences in viscosities of individual Aroclor batches. This Aroclor mixture has a 45P. viscosity of about 5000 SUS absolute which is slightly greater than the specified value and a l60P. viscosity above the 60 SUS absolute minimum specified. The use of greater portions of higher Aroclors would bring the 45f. viscosity above the 45F. maximum and would result in higher pour point values. 3. Lubricating Properties Pour-ball wear tests on the Aroclor base stocks indicated wear values of 0.35 mm., 0.38 ram., and 0.82 mm. at loads of 4, 10, and 42 kilograms, respectively. These values indicated the necessity of an anti-wear additive to obtain an Aroclor fluid equivalent to Pydraul P-9- The work on the viscosity index improved version of the Aroclor fluid (Section above) indicated Santolube 393 to impart good anti-wear properties to Aroclor based fluids. A Santolube 393 concentration of 0.5# was chosen on the basis of previous work. The anti-rust agent, Santolube 70, was also incorporated before further bench scale lubricating tests were performed since such additives may adversely affect lubricating properties. Additive concentrations of 0.5# (w) Santolube 393 and 0.5# (w) Santolube 70 gave acceptable Four-Ball Wear results superior to Pydraul F-9 and Almen E.P. results equivalent to Pydraul P-9. Subsequent anti-rust tests indicated the Santolube 70 concentration could be cut from 0.5# to 0.05# to give adequate protection in the ASTM D-665 rust test. A 50 gallon blend was formulated on the 0.05# Santolube 70 basis and was found to have depreciated in Pour-Ball Wear and Almen Load characteristics. Pour-Ball Wear and Alman Load tests run on variations of the Aroclor formulation indicated that a Santolube JO concentration of 0.5# returned the blend to the expected performance level. These results are outlined in Table I of the Appendix. The lubrication proper ties appeared to be better with the two additives, Saitolube 393 and Santolube 70, together than with either alone. This apparent synergistic effect was not studied further. Since it was requested that the fluids have lubricating performance equivalent to or better than Pydraul -F-9, it was decided to submit the 0.5# Santolube 393r 0-5# Santolube 70 formulation to General Motors for their full scale pump tests. Any future work on this type fluid should include a study of the optimum Santolube 393 and Santolube 70 concentrations and the use of oillness agents and anti-rust agents other than Santolube 70. DSW 622043 STLCOPCB4096074 7. 4. Rust Inhibition . Previous work with rust Inhibitors for Pydrauls has indicated that Santolube JO Is relatively effective as an inhibitor, as measured by the ASTM D-665 rust test. The Sales Department has found indications that additions of Santolube 70 to equipment with rusting problems is effective. For these reasons, Santolube 70 was chosen as the rust inhibiting additive for the Aroclor formulation. The initial concentration of 0.5# Santolube JO was reduced to 0.05# without deterioration in anti-rust properties, as Judged by the ASTM D-665 rust test. Lubrication tests on the blend containing reduced amounts of Santolube 70 indicated a performance deterioration and the Santolube 70 concentration was increased to the original value of 0.5# by weight. Refer to Discussion, Section C above, concerning the fluid lubricating properties. The high concentration of Santolube 70 is undesirable from the standpoint of foaming tendencies and copper attack in systems where water is present. 5. Miscellaneous Properties a. Appearance OS-95 is a very light yellow liquid with a slightly hazy appearance. The haze is due to very small quanti ties of antifoamant, DCF-200. b. Foam The use of Santolube 70 in the OS-95 blend causes undesirable foaming. A concentration of 50 parts per million of Dow Corning Silicone DCF-200 - 550 cs. at 25C. was used to inhibit foaming. This concentration is based on similar anti foamant concentrations used in some of the current Pydrauls. No work was done on the determination of minimum amounts of defoamant necessary. c. Neutralization Number Unused OS-95 has a total acid number of about 0.8. This apparent high acidity is due to nature of the Santolube 595 and Santolube JO present. The initial pH of the blend is greater than J. 6. Toxicity Toxicity tests have been run on OS-95 and are reported in a memo from J.T. Garrett to R.E. Hatton of February 26, 1958. This report indicates the Oral LD50 to be 10,500 milligrams per kilogram and classifies the material as "practically non-toxic" from an oral ingestion standpoint. The skin Minimum Lethal Dose was found to be 625 to 1,250 milligrams per kilogram in rabbits which DSW 622044 STLCOPCB4096075 8. classifies the material as ''slightly toxic" by skin absorption. The compound is only a mild eye Irritant and a saturated atmosphere of OS-95 vapors is only slightly Irritating to rats exposed for six hours. In summary, "The above information Indicates that OS-95 is not a very seriously toxic product to handle and, therefore, no special handling precautions are necessary." 7- Compatibility OS-95 appears to be completely miscible at all concentrations with Pydraul P-9, Cellulube 220, and Houghto-Safe 1120 at temperatures of 40P., 75-80P., and 120P. No unusual deprecia tion of lubricating properties are expected from these mixtures. Shell four-ball wear and Almen E.P. values for the mixtures were generally between the values of the component fluids. The Almen and four-bail wear values for these fluids appear In Table VIII. 8. Full Scale Performance - At the time OS-95 was being developed In the laboratory, it was learned that the General Motors Corporation Process Engineering Staff had received an appropriation to do further test work on fluids and would Include any new Monsanto fluid in their pro gram free of charge. Subsequently a 550-pound lot of OS-95 was submitted for full scale pump tests by General Motors. The General Motors test, of OS-95 was conducted using a Vickers V104-D pump at 1000 psl. A preliminary report of this test was recorded in a memo to file by R. Davis, May 15, 1958. "On May 2, 1958, Stu Litzsinger and I talked to John Panek of the GMC Tech Center on the telephone. John gave us the confidential results of his pump tests with OS-95- In summary. It looks as good as the best petroleum oil he has ever tested. "After running 200 to 400 hours, a water cooler broke, letting water enter the fluid. It was separated, the pump examined and found to be in good shape, and the test continued. At 200 hours, there were 5 milligrams of wear on the ring; at 1000 hours, there were 51 milligrams of wear on the.ring. The test will be continued to 2000 hours. "The best of the petroleum hydraulic oils have 40 to 80 milligrams of wear on the ring at 2000 hours. We would be in about that range, but the test with OS-95 is even more severe than the ones run with oil because it is run with a Vickers V-104-D pump of the old style using an 11 gallon per minute ring. This is probably the most severe test that could be run with this type of pump." DSW 622045 STLCOPCB4096076 9- On the basis of these good test results, OS-95 was placed in a Kux die casting machine at Chevrolet - Bay City Division with satisfactory results. A sample of OS-95 removed from this system was evaluated for antiwear, rusting, acidity, and viscosity. This fluid reportedly used for 260 hours, of which 14 hours were at 190P., exhibits no significant change from new OS-95 except in color. These data appear in Table IX. OS-95 was installed in a Johnson Motors Lester- Phoenix die casting machine. Development Department Call Report No. FF-414 of November 14, 1958 summarized results of this test as follows: ' "A five-month service test (1800 hours) of OS-95 at Johnson Motors has shown conclusively that this fluid will offer satisfactory performance in a high-pressure hydraulic system as used in a Lester-Phoenix die casting machine. During this period of time, there has been no evidence of anything other than satisfactory operation, and nothing abnormal has been observed. Because of the success of this test, plans are to introduce OS-95 into the plant on a limited basis by using it as make-up for two machines presently operated on Pydraul F-9. If these machines operate satisfactorily for a period of two or three months, Johnson Motors would like to discontinue the pur chase of Pydraul F-9 in favor of 0S-95-" In conjunction with this test at Johnson Motors, a request was made by them to investigate the possibility of in creasing the viscosity of OS-95 by approximately 50 SUS at 100F. Subsequent calculations indicated this could be accomplished with a mixture of higher Aroclors but that the depreciation of low temperature properties was excessive. No further work was done with such a formulation. 9- Profitability Profitability of OS-95 in comparison to Pydraul F-9 was determined by M. Dmytryszyn and reported in a memo of March 15, 1958 (MD to JHL, March 15, 1958). D. Fire Resistant, Low Viscosity Hydraulic Fluid, OS-104 1. Fluid Requirements and Final Blend Pydraul 150, a low viscosity fire resistant fluid designed for use in low temperature regulator systems, has inherent thermal and shear Instability. Introduction of a competitive fluid, Houghto-Safe 1010, having greater shear and thermal stability, has resulted in the losp of Pydraul 150 sales. This necessitated the formulation of an improved Pydraul 150 type fluid. The Houghton fluid was being sold on the basis of thermal stability, such that a system failure and consequent hydraulic line overheating would cause Pydraul 150 to solidify while their fluid remains liquid, facilitating system clean-up. A shear and thermally stable, fire resistant DSW 622046 STLCOPCB4096077 10. industrial type hydraulic fluid, designated 0S-104, was formulated to meet viscosity,, thermal stability, and lubricating requirements specified by the Sales and Development Departments. During the period covered by this report, OS-104 was not accepted by the Development Department pending, a review of OS-104 and alternate formulations by Douglas Aircraft Company. Fluid requirements were determined at a meeting of Sales, Development and Research on April 2, 1958. These require ments were specified in the memos, R. Davis to H.S. Litzsinger, April 7, 1958 and H.S. Litzsinger to E.P. Cunningham, April 11, 1958. It was agreed that the Pydraul 150 supplement would be a blend of cresyl diphenyl phosphate (Santlcizer 140) and tricresyl phosphate (TCP) and would not be V.I. improved. The general characteristics of this fluid were to be essentially those of the competitive product, Houghto-Safe 1010, and are as follows: Viscosity Pour Point Oxidation and Corrosion Resistance 50 SUS at 150 F. - Less than -25P- To be equal or better than Houghto-Safe 1010 at 250F. Thermal Stability Equal to or better than Houghto-Safe 1010 when exposed for 15 min. at 520F. Lubricating Properties Foaming Equal to or better than Houghto-Safe 1010 as evalua ted by the Shell 4-Ball, Almen, and Timken tests. To be checked and reported. Rusting To be checked and reported. Flammability To be checked by the three tests of SAE specification AMS 5150. The only advantage such a blend might have over Houghto-Safe 1010 would be its better low temperature properties Imparted by the Santlcizer 140. It was suggested that a Ucon thickened and V.I. Improved Santlcizer 140 blend be considered to further Increase the low temperature advantage. The Santlcizer 140-Ucon blend was subsequently abandoned due to emulsification problems and difficulties in obtaining adequate load carrying properties. However, anti-wear properties appear to be Improved by the Ucon additive, 75-H-90,000. DSW 622047 STLCOPCB4096078 11 It was found that the Santlcizer 140-TCP mixture was deficient in lubricating properties. An extensive formulation study indicated the following formulation to be acceptable as judged by the specified qualities outlined above. 69.49# (wt.) 29.25# 0.25# 0.1# 50 ppm. Santlcizer 140 Tricresyl Phosphate Dioleyl malate (DOM) Dilinoleic acid (RT-67-A) DCF-200 Fluid Some 270 formulations or formulation variations were prepared and tested for Almen E.P., four-ball wear, or 15 minute heat stability or each of these. Of the various additives tested, the following gave the best lubricating performance in the Santlcizer 140-TCP base stock: Santolube 593 (dithiophosphate ester) Oleic acid . Vanlube AZ (Vanderbilt Co. zinc dlamyl dithiocarbamate) Santolube 70 (Monsanto tetrapropenyl succinic anhydride-amlnefatty acid reaction product) Sarkosyl 0 (Geigy Chemical Corp. N-oleyl sarcosine) Aerolube 95-C (dithiophosphate ester) Aroclor 1232 (chlorinated biphenyl) Stan-Add 121 (barium salt of P2Ss-i3obutylene R.P.) N-30 (bis, beta, chloroethyl vinyl phosphonate dibutyl hydrogen phosphite) Alkaterge T (Commercial Solvents Corp. - weakly cationic amine) M-434 (Monsanto-experimental gear oil additive blend) RT-52-A (Dihydroabietyl malate) Dioctyl malate RT-67-A (dilinoleic acid) Most of these suffered considerable degradation in the 15 minute heat test. Several antioxidants were tried without any Improvement. A better definition of fluid requirements may Indicate that much of this work was unwarranted. It is recommended that such projects be better defined in the future and that they be assessed periodically during development to see if the proposed requirements are still realistic. 2. Viscosity and Pour Point It was desired that the Pydraul 150 supplement have a low temperature fluidity advantage over Houghto-Safe 1010. It was Askania's desire (primary use of Pydraul 150 is in Askania regulator equipment) that the fluid be shear stable, operate down to -10F. and have viscosities of 3000-4000 SUS at 0F. and 50 SUS at 150F. The 50 SUS at 150F. value was easily attained by a Santlcizer 140-TCP blend and a Santlcizer 140-Ucon VI improved blend. However, subsequent viscosity checks Indicated that the 5000-4000 SUS at 0F. value was not obtained for the Houghton fluid, Santicizerl40-TCP, or Santlcizer 140 alone. DSW 622048 STLCOPCB4096079 12. OS-104 has low temperature fluidity properties superior to Houghto-Safe 1010. The pour points and low temperature viscosities are tabulated in the Appendix Table II. 3- Lubricating Properties Santiclzer 140, the principal base stock of OS-104, was found to be deficient in its lubricating properties compared to Houghto-Safe 1010. These deficiencies were Improved only slightly by addition of TCB. It was found that the aryl phos phate esters have relatively poor lubricating properties compared with the alkyl phosphates. Lubricating data, tabulated in Table X for various phosphate esters illustrate this difference in lubricating properties. It is necessary to retain the aryl phosphates for this application due to their better thermal stability. Various additives may be compounded with the thermally stable aryl esters to impart improved lubricating characteristics. However, most of the additives examined were thermally unstable giving a very dark colored fluid on heating or giving solid decomposition products. Also, most of the more common lubricating additives used in petroleum type fluids were ineffective in the Santiclzer 140-TCP system. The objective of the formulation study wa3 to improve the antiwear properties of the base fluid while retaining or improving the load carrying (E.P.) properties consistent with acceptable thermal stability. The OS-104 formulation satisfies these objectives. Lubricating data are tabulated in Appendix Table II for OS-104 and in Table X for the non-additive treated phosphate esters and for the additives separately. As was indicated in Section 1 above, future laboratory and service correlation should yield more realistic information on the lubricating requirements of hydraulic fluids. If requirements are less severe than specified, several of the milder lubricating additives might allow better performance in the thermal stability tests. 4. Thermal Stability and Oxidation-Corrosion Characteristics The thermal stability requirement of the Pvdraul 150 supplement was prompted by a Houghton advertising "gimmick" in which the two fluids are heated in excess of 500P. for about 15 minutes. The Houghto-Safe 1010 fluid remains relatively stable with only slight color and acidity changes; whereas, Pydraul 150 decomposes leaving a dark material equivalent to one-third the original volume and containing solids having a very high acid number. DSW 622049 STLCOPCB4096080 15. A study of this thermal instability and the suggestion of a thermally stable Pydraul 150 supplement comprising Santicizer 140 and TCP is contained in a file note by R.E. Hatton dated May 6, 1958. A mixture of Santicizer 140 and TCP turns yellow or light brown on heating for 15 minutes at 520F. and has only a slight acid number increase. As stated above in the section on lubricating properties, considerable difficulty-was encountered in finding lubricating additives which were effective and would stand up in the thermal stability test. The dloleyl-malatedilinoleic acid combination satisfies these requirements. Two alternate blends which had acceptable lubricating properties and thermal stability contained Santolube 593 and Santolube JO, respectively. Oxidation-corrosion tests of these blends indicated excessive copper attack; therefore, they were abandoned. OS-104 oxidation-corrosion resistance is considered to be equivalent to that of Houghto-Safe 1010. Static thermal stability and oxidation-corrosion data for these fluids appear in Table II of the Appendix. 5- Fire Resistance Fire resistance tests run on the OS-104 blend which include flash and fire points, a molten metal ignition test and high and low pressure spray flammability tests indicate this fluid to be superior to Pydraul 150 and equivalent to Houghto-Safe 1010 in fire resistance. Hot manifold tests run on the individual phosphate ester base stocks used in the OS-104 blend are also superior to Pydraul 150, and it is believed that the minor amounts of additive (total $ 0.35$) will not decrease fire resistance in this test. 6. Miscellaneous Properties a. Appearance OS-104 is a slightly cloudy, almost colorless, oily liquid. The cloudiness is due to very small quantities of the antifoamant, DCF-200. b. Foam The use of dioleyl maleate in the 0S-104 blend causes more foaming than is desirable. A concentration of 50 parts per million of Dow Corning Silicone DCF-200 (350 cs. at 25C.) was used to inhibit foaming. This concentration is based on similar antifoamant concentrations used In some of the current Pydrauls. No work was done on the determination of minimum amounts of defoamant necessary. DSW 622050 STLCOPCB4096081 14. c. Rust An attempt was made to Include anti rust additives in this formulation but most of those tried resulted in depreciation of lubricating properties. The dilinoleic acid used in the OS-104 blend has some utility as an anti-rust agent but is not present in sufficient quantity to give a completely rust-free D-665 specimen after 24 hours. The OS-104 formulation is considered to be equivalent to Houghto-Safe 1010 in rust resistance. d. Neutralization Number The acidity of OS-104 is slightly higher than the base component acidity due to the additives present. The initial total acid number of about 0.50 decreased to 0.35 in the oxidation corrosion test and increased to about 1.3 after the static heat test of 520P. 7 Alternate Formulations Before accepting 0S-104, the Development Department requested additional information on two alternate blends. One of these was cresyl diphenyl phosphate (GDP) with Ucon 75tH-90,000 as a viscosity index improver and the other a similar viscosity index improved GDP with Santolube 70 added to improve antirust characteristics. These formulations appeared to be equivalent to or better than Houghto-Safe 1010 in viscosity, 15 minute 520F. static heat test, rust and foam. Lubricating properties and oxidation-corrosion resistance were not considered quite as good. Again water leaching of the Ucon additive and possible emulsion problems make this type of formulation less desirable. The requested information transferred to the Development Department for their decision appears in Table XI. 8. Toxicity Toxicity of 0S-104 is summarized as follows from a memo J.T. Garrett to R.E. Hatton, dated October 29, 1958: "These data indicate that OS-104 may be classified as "relatively harmless" from a single oral igestion stand point, but must be classified as "practically non-toxic" from a skin absorption standpoint. It Is important to note that the skin absorption toxicity indicates that OS-104 is somewhat more toxic by this route. This, of course, can Indicate specie variation but the important observation is that by skin absorption.in rabbits neuro toxic effects were noted that were not noted by any other route. "Based on the above data, no particular hazard should be experienced in handling 0S-104. However, excessive skin contact should be avoided." DSW 622051 STLCOPCB4096082 15. 9. Patent Status A preliminary disclosure of invention has been prepared and submitted for the OS-104 formulation. 10. Cost Estimate An economic evaluation of OS-104 was completed and reported in a memo M. Dmytryszyn to E.P. Cunningham, dated September 12, 1958. E. Phosphate Ester Formulation A project was Initiated to provide a thickened, viscosity index improved, and shear stable TCP which would be competitive with a commercial fluid, Cellulube 220. Specific applications for this fluid were use as a chlorine-free fire resistant hydraulic fluid for the Navy and as a fire resistant and mineral oil insoluble fluid for an Atomic Energy Commission (AEC) installation. The oil insoluble properties were required where changeover was to be conducted without shutting down the system. Due to the failure of Monsanto TCP and formulations containing this TCP to pass the Navy hydrolytic stability test and to the discontinuance of a need for the oil insoluble fluid for the AEC installation, this project was discontinued. Physical properties and bench scale performance data for a TCP blend containing 1.55# (w) of Ucon 75-H-90,000 are pre sented in Tables XII, XIII and XIV, for record purposes. These data indicate the fluid to be equivalent to or superior to Cellulube 220 in viscosity, viscosity index, shear stability, pour point, antiwear properties and antirust properties. The fluid is relatively insoluble in both a paraffinic and a naphthenic base mineral oil with no significant V.I. improver removal by the oils. Although the TCP blend appears to be a little less soluble in the paraffinic than the naphthenic oil, a problem of separation from the paraffinic oil may be encountered due to emulsion formation. Additional data indicate the Ucon type of V.I. improver creates a severe water emulsion which may be nearly eliminated by suitable demulsificatlon additives. F. Preservative Type Hydraulic Fluids 1. Pydraul 625, Pydraul F-9 Preservative Fluid A project was initiated to provide a specific customer (Alcoa) with preservative type hydraulic fluid based on Pydraul F-9 and Pydraul 625 for equipment storage. Before this project was completed the need for such fluids ceased to exist and the work done to that time is reported for record purposes. DSW 622052 STLCOPCB4096083 16. The Army-Navy Humidity Cabinet is used to evaluate fluid preservative properties. It was found that the steel test panels used for most of the screening work on this project did not give results consistent with other laboratories. Subsequent metallographlc examination revealed that these panels were not cold rolled steel as specified for the humidity cabinet. Although these panels gave less severe results, the results are of value in that a separation of suitable and unsuitable rust inhibitors was made. Materials giving less than 50 hours protec tion were considered poor and those giving more than 50 hours protection were considered suitable for further study. The inhibitors screened are listed in Tables XV& XVI. No specific protection times are shown since any future work must be done with suitable test panels which may give different results from those obtained. Most of the screening was done with Pydraul 625 as the base fluid. In general, 3 to 5# of Inhibitor is required for maximum protection. Materials exhibiting the best protective properties were a series of reaction products of tetrapropenylsuccinic anhydride with other materials, reaction products of maleic anhydride and various long chain fatty acids, dimer acids, and several commercial inhibitors. 2. 0S-100 Preservative Type Hydraulic Fluid The U.S. Navy Engineering Experiment Station outlined requirements for preservative type fluids compatible with or preferably based upon phosphate ester fluids and providing a minimum of 30 days protection in the humidity cabinet test. A fluid, designated 0S-100, was formulated to meet these requirements. 0S-100 consists of tricresyl phosphate (TCP) containing 2.37# (w) RT-67A (dilinoieic acid), 2.37# RT-53A (diamylphenylphosphoric acid), and 0.4# phenyl-alpha-naphthylamine. Formulation, physical proper ties, and bench scale performance of 0S-100 are presented in a special report (St. Louis Research Report No. 2257, March 4, 1959). G. Rust Inhibited Pydraul F-9 and Pydraul 625 1. Fluid Requirements and Final Blends Sporadic "deposit" or rust problems have been experienced by various Pydraul F-9 customers and Alcoa, specifically, has indicated marked variance In rusting tendencies of the Pydrauls as judged by the ASTM D-665 Rust Test. For purposes of customer satisfaction and Improved product quality, it was decided to include a rust inhibitor in the Pydraul F-9 and 625 formulations. Previous laboratory work and limited field experience indicated the deposit problem is alleviated by Santolube 70 Inhibition. On the basis of this lab and field experience It was decided to formulate Pydraul F-9 and Pydraul 625 with minimum quantities of Santolube 70 to give adequate rust protection. The DSW 622053 STLCOPCB4096084 17- final blend designated OS-101 consists of 99-7/6 Pydraul F-9 and 0.3$ Santolube 70 and the blend designated OS-102 consists of 99-7$ Pydraul 625 plus 0.3$ Santolube 79, and 50 ppm. DCF-200 by weight. It was concluded from the results of bench scale performance tests and physical property measurements of OS-101 and OS-102 that these fluids have superior anti-rust properties and equiva lent lubricating properties to the corresponding uninhibited Pydrauls. These tests indicate only Slight deterioration in emulsion resistance and oxidation-corrosion resistance as exhibited by slightly higher copper attack. OS-101 and OS-102 were transferred to the Development Department for limited field application. This qualified recommendation was given on the basis of the use of a surface active additive, Santolube 70. Many performance factors. Including foaming, emulsion, lubricating properties and corrosion resistance may be affected by such materials and complete characterization of such fluids by bench scale tests is difficult. It is recommended that any future work on the 0S-101 and OS-102 type fluids should include the consideration of an additive other than Santolube 70 since this material imparts undesirable foaming and emulsion forming tendencies to the fluid and results in increased copper attack especially in systems where water is present. 2. Rust Inhibition The minimum quantity of Santolube 70 required to give adequate rust protection to Pydraul F-9 and Pydraul 625 was determined to be 0.25$ and 0.01$ (wt.) respectively. These dosages were increased to 0.3$ and 0.02$ to give an additional margin of rust protection. Subsequent bench scale lubricating tests of the Pydraul 625 with 0.02$ Santolube JO indicated some deterioration in its load carrying properties. Increasing the Santolube 70 concentration to 0.3$ restored the load carrying characteristics. " 3- Lubricating Properties As indicated in the section on rust protection, it was necessary to increase the concentration of Santolube JO In Pydraul 625 in order to maintain the load carrying ability of this fluid. Almen and Timken values for 625 with 0.02$ Santolube 70, and 625 with 0.3$ Santolube 70 appearing below Illustrate this. Almen Load Timken Load Pydraul 625 Pydraul 625 + 0.02$ Sant. 70 Pydraul 625 +0.3$ Sant. 70 46 lb.-50 lb. torque 50 lb.-67 lb. torque 50 lb.-49 lb. torque 40 lb.-17,200 psi 35 lb.-13,800 psi 40 lb.-18,100 psi DSW 622054 STLCOPCB4096085 18. Shell 4-Ball Wear, Almen Wear, Almen Load and Timken Load values for 0S-101 arid OS-102 appear in Appendix Table IV. These data Indicate some wear Improvement and little change In load carrying properties upon addition of Santolube 70. 4. Fire Resistance No fire resistance testing was done on OS-101 and OS-102. Since the quantity of additive is so low, it is believed that insignificant changes in fire resistance will occur. 5- Foam and Emulsion Addition of 0.3$ (wt.) Santolube 70 to Pydraul F-9 does not affect the foaming tendency or persistence; whereas, addition of the same amount to Pydraul 625 resulted in excessive foam which did not settle readily. The incorporation of 50 parts per million of Dow Corning Fluid 200 to the Pydraul 625-Santolube 70 mixture decreased the foam to an acceptable level. The use of Dow Corning antifoam agent in the Pydraul 625 blend is necessary when Santolube 70 is used as the inhibitor. Pydraul F-9 already contains antifoamant and no further treatment is necessary' upon Santolube JO addition. The use of 0.3$ wt. Santolube 70 in Pydrauls F-9 and 625 results in only slight deterioration in emulsion forming tendencies. However, a definite emulsion layer does exist after the specified 30 minute settling period. It is not known if this amount of emulsification is enough to affect full scale operation. Foam and emulsion values for 03-101 and OS-102 appear in Appendix Table IV. 6. Oxidation and Corrosion Thermal and oxidative stability of OS-101 and OS-102 is similar to Pydrauls F-9 and 625- Copper attack is Increased slightly and the inhibited fluid exhibits a small neutraliza tion number decrease rather than the normal increase. The inclusion of Santolube JO in the Pydrauls results in a higher initial total acid number. Fluid weight loss, and viscosity change are very low and no sludge is formed. OS-101 and OS-102 become brown on exposure to the 250F. - 168 hour oxidation-corrosion conditions. These data appear in Appendix Table IV. Although no specific tests were run on 0S-101 and 0S-102, it is emphasized that Santolube JO containing fluids may result in greatly increased copper attack in systems containing water. DSW 622055 STLCOPCB4096086 19- 7. Toxicity Santolube 70 is reported by Scientific Associates (May 6, 1953) to be of relatively low order of toxicity when taken internally and to be only a mild-to-moderate eye and skin irritant. In handling OS-101 and OS-102, the same general precautions applicable to Pydraul P-9 and Pydraul 625 should be observed. H. Steam Turbine Lubricant, OS-81 1. Rust Inhibited 0S-8l Sporadic rusting has been observed on the steel catalyst coil from OS-81 steam turbine oil oxidation tests. Considerable work was done by J.D. Sullivan to find OS-81 rust Inhibitors which were non-foaming and non-copper attacking (Job Numbers 2949 and 3334 and St. Louis Research Report No. 1779). Work done under this job number Included oxidation-corrosion evaluation of OS-81 given various washing treatments, additive additions, and some tests to check test procedure variations. None of the washing treat ments or additives tried completely eliminated rusting. Also, the minor test variations and refinements were unsuccessful in eliminating rusting or allowing reproducible testa. ' The problem of test reproducibility is important since some tests with OS-81 give no rusting or only isolated rust spots; whereas, some duplicate tests resulted* in considerable rusting. Further work will be done in the future to Improve the test reproduci bility and to find appropriate inhibitors. Although no conclusive results were obtained during the period covered.by this report, the test results are presented in Table XVII. 2. OS-81 Resistant Coatings Two coating materials were checked for resistance to OS-81. Both Nycote 4/30 Protective Coating (Nycote Laboratories, Van Nuys, California) and Steelcote 220-W-100 (Steelcote Manufacturing Co., St. Louis) appear to be resistant to OS-81. Panels coated with these materials were immersed in OS-81 at 150F. for two months. The coatings were not loosened and exhibited no appreciable softening. 3- OS-81, Gas Turbine Lubricant Application During the period of this report, 0S-8l found application as an industrial gas turbine lubricant (Texas Eastern Transmission Corp.). Various Information was supplied to facilitate this application. Kinematic and Saybolt viscosities (calculated from centistoke values), determined over the range 50F to 210F.. , follow: DSW 622056 STLCOPCB4096087 20. Temperature, F. 210 100 80 60 50 K.V., centi.stoke3 3.07 33.33 88.01 340.3 838.2 Saybolt Universal ___ Seconds 36.51 142.8 407-4 1573 3872. below: Fire resistance tests run on OS-81 are presented Hot Manifold (1300F.) - Does not flash or burn on tube or after leaving tube. Low Pressure Spray - Very slight increase or brightening of flame. High Pressure Spray - Will not ignite to three feet Shell Four-Ball Wear values indicate OS-81 compares favorably with several commercial petroleum based fluids. 0S-81 Mobil DTE Medium Sonoco Solnus 200 Sonoco Sunvis 921 Texac Regal R&0 Ball Wear (l67#F., 620 rpm, 1 hr.) Steel-on-Steel 4 Kg. 10 Kg. 40 Kg. Steel-on-Bronze 4 Kg. 10 Kg. 40 Kg. 0.22 0.27 0.55 1.25 1.25 1-75 0.19 0.24 0.38 0.18 0.22 0.41 _ 1.48 -- - 1.44 -- 0.19 0.22 0.36 -- 1.91 0.39 0.46 0.58 __ -- 1.80 -- The gas turbine reservoirs were coated with a material not resistant to OS-81 (Rust-Ban 297, Esso Standard Oil Co.). It was found that OS-81 readily dissolved this coat except for the aluminum pigment. Some large soft flakes were removed which might have been difficult to filter. Sodium hydroxide solutions of 15 to 20$ concentration removed the Rust-Ban readily. Higher caustic concentra tions resulted in a gel-like coating which did not go into solution. OS-81 treated for two hours from 100F. to 150F. with 2$ of the 20$ caustic solution used for removing the Rust-Ban had a moderate increase in the 4-Ball Wear value (0.36 mm at 10 Kg. compared to the initial 0.27 mm value). Stick lubricants for plug valves were checked for OS-81 resistance. Nordstrom Valve Lubricant #555 was dissolved; whereas Nordstrom Lubricant #P-55 appeared to be OS-81 resistant at 150F. Valeo #67 (Plug Valve Lubrication Co.) also appears to be 0S-8l resistant.. DSW 622057 STLCOPCB4096088 21. This 0S-8l application work was continued under a new job number (3766). . ' . II. High Temperature and Fire Resistant Aircraft Type Fluids A. High Temperature Fluid Screening and Formulation 1. General Screening Preliminary screening tests were conducted on candidate fluids from Dayton, Lion Oil Division, St. Louis, and on competitive fluids. The fluids evaluated follow: Mixed (o,m,)bis(x-methylphenoxy)benzene, CP-30415 1.1-Di-cTocTecyl 3,3-dl-(2-ethylhexyl)urea 2.2-Dimethyl-l,3-propyl dilaurate Bis(l-methylcyclohexylmethyl)hexahydroisophthalate, CP-30417 Bis(l-methylcyclohexylmethyljsebacate Santowax OM fraction liquid at room temperature Monoisopropyl biphenyl Diisopropyl biphenyl Ethylated Santowax R Isopropyl Santowax OM Tertiary butyl Santowax OM HB-40 Ethylated HB-40 Tert. butyl HB-40 2-n-Butylamino-4-di-n-butylamino-6-piperidino-S-triazine 2-FT-n-propyl 4-N-n-butyl 6-N-n-hexyl melamine 2-N-dlethyl 4-N-dlphenyl 6-N-dlbenzyl melamine m-Tolyl- <*.,(*,x-trifluoro-m-tolyl sulfone -Chlorophenyl -nonylphenyl ether 3,4-Diphenyl chlorobenzene Synjet Oil 15 (Texaco MIL-L-7808) General Electric Versilube P-50 silicone General Electric 8l644 silicone General Electric 81717 silicone Fluorochemical PC-75 Preliminary evaluation of most of these fluids was done with the 347?-, 72-hour, MIL-L-7808C oxidation-corrosion test and by the Shell Pour-Ball Wear Test. In most cases, viscosity and an estimate of the low temperature fluidity were determined. Physical properties appear in Table XVII, oxidation-corrosion values In Table XIX, and Shell Pour-Ball Wear and Almen E.P. In Table XX. After several of the above mentioned fluids had been evaluated, their performance qualities, usable maximum bulk temperature, and field of application (Jet lube or hydraulic fluid) were reviewed. This information Is summarized in Table XXI. None of these fluids appeared to be acceptable for specifications MIL-L-7808C, 9236A, or MIL-H-8446 without additive or structural modification. Three base stocks were chosen for formulation to meet the MIL-L-9236A Jet engine lubricant specification. These included bis(l-methylcyclohexylmethyl)hexahydroisophthate, bis(1-methylcyclohexylmethyl)sebacate and the mixed (,m,)-bis(x-methylphenoxybenzene). DSW 622058 STLCOPCB4096089 22. Two fluids, mixed {o,m,jo)bis(x-methylphenoxy benzene) and 2,2-dimethyl 1,3-propyl dilaurate, were considered for formulation as high temperature hydraulic fluids. 2. High Temperature Jet Lubricant Formulation Initial high temperature fluid formulation efforts were directed toward the Jet engine lubricants. Oxidation-corrosion at 500P. for 48 hours indicated the mixed (o,m,)bis(x-methylphenoxy benzene) to be more stable than the sebacate and hexahydrolsophthalate dlesters. Both the diesters exhibit some response to antioxidant treatment although concentrations and additive types studied were not sufficient to hold acidity Increases within the MIL-L-9236A limits. Oxidation Inhibitors were chosen to include selenium and sulfur bearing compounds, a hindered phenol, and amine type inhibitors. These represented some of the more favorable compounds indicated in various government contract-reports and include phenothiazlne, phenyl mercapto benzothiazole, phenyl selenide, dilauryl selenide, 4,4'-methylene bis (2,6-di-tert.-butylphenol). Due to the time and fluid consuming nature of the oxidation-corrosion test, a simplified static oven test was attempted. Copper and steel specimens were suspended by a bent stainless steel wire in a 50 ml. watch glass covered, beaker of the fluid. Samples were removed for acidity determination at 8, 24, and 48 hours. Most of this test work was done with the dilaurate and hexahydrolsophthalate ester since the supply of the sebacate ester and bis methylphenoxy benzene were currently depleted. Although these test conditions appeared to be too severe for the particular fluids tested, phenothiazlne did exhibit some antioxidant activity. At this point in the formulation program, emphasis was shifted to high temperature hydraulic fluid formulation. No further work was done on high temperature Jet turbine lubricants utilizing the diesters or the mixed bis-methylphenoxybenzene during the report period covered by Job Number 3505- Some work done to find low melting polyphenyl and polyphenyl ether mixtures is presented in Section 4 which follows. During the course of this formulation work the MIL-L-9236 specifications were changed to require a 3.0 cs. minimum 400F viscosity rather than a 35 cs. minimum at 100F. None of the candidate materials would pass this requirement with the exception of a few higher molecular weight polyphenyls or polyphenyl ethers which also have very high melting points. There was some question as to the low temperature limitations of the 9236 specification. An engine builder (Pratt and Whitney) indicated that they would be Interested In a fluid with a relatively high pour point if It had sufficient high temperature stability and lubricating properties. In view of this, It was decided to work toward a fluid having the following characteristics. a. Thermal and oxidative stability in the 500 to 600F. range. This should be attained without the use of inhibitors. DSW 622059 STLCOPCB4096090 23. b. As wide a liquid range as possible with liquid at room temperature being a must with a pour point of 0 to 30F. acceptable. Maximum high temperature viscosity and fluidity down to -65F. are desirable. c. Lubricating ability to give adequate performance in a gas turbine engine. Additives may be necessary. In order to accomplish the objective of obtaining an appropriate candidate fluid, the following steps were to be taken: a. Select from fluids evaluated to date those which most nearly meet requirements of items 2-a and 2-b above. these fluids. b. Perform all 9236A specification tests on c. If bench scale tests Indicate gross lubricating deficiencies, improve lubricating properties by limited formulation. d. Send most promising fluids out for Ryder Gear and Bearing Fatigue testing. e. Present results of tests b and d above to engine builder for selection of candidate fluid or comments on necessary improvements. Future work will be dictated by these results. The polyphenyl ethers were chosen as the best fluid candidates for this application. Work on the evaluation and formulation of these fluids was done under Job Number 3767. 3 High Temperature Hydraulic Fluid Formulation Formulation work on a 450F. to 550F. temperature hydraulic fluid was Initiated to meet requirements outlined by a pump manufacturer's representatives (Vickers, Inc.). Two formulations of different base stocks, bis (1-methylcyclohexylmethyljsebacate and 1,1didodecyl 3,3-di(2-ethylhexyl)urea were prepared. Physical properties and bench scale performance of these fluids is presented in a special report, St. Louis Research Report No. 2335, Job No. 2-02-750.01-3505, 3767 of August 27, 1959. 4. Polyphenyl and Polyphenyl Ether Mixtures A polyphenyl and polyphenyl ether blending study was Initiated to obtain blends having improved low temperature properties for high temperature fluid and lubricant applications. This study indicated the most promising fluids to be the four or fivering all-meta ethers alone or In combination with the three-ring meta ether. The low temperature properties.of these fluids appear to be limited by viscosity rather than freezing point. Since viscosity is primarily an additive property, any further improvement would be by the addition of greater than additive quantities of a less viscous component. Currently available low viscosity materials were considered either less thermally stable or too volatile. DSW 622060 STLCOPCB4096091 24. Binary mixtures of four unsubstituted poly phenyl ethers, biphenyl stripped Santowax OM, and three fractions of Montar 9, representing mixtures thought to be principally quaterphenyls, were examined for freezing point lowering by means of a hot stage microscope fusion technique (Walter C. McCrone, Jr., "Fusion Methods in Chemical Microscopy", Interscience Publishers, Inc., 1957)- This work indicated that the only binary mixtures having liquid present at room temperature were combinations including fluids which already were liquid or had liquid present at room tempera ture. The viscous nature of these fluids at temperatures at or below room temperature resulted in supercooling to glasses and other difficulties encountered by the microscopic cold stage method necessitated a change of approach to the problem. A plot of the viscosities of the 3, 4 and 5-ring unsubstituted polyphenyl ethers indicated the viscosities of these fluids below 400F. are dependent upon the chain length. That is, all isomers; ortho, meta, para, or mixed; of equal molecular weights follow a single viscosity curve very closely. Previous experience has indicated that the "pour point" of fluids having no distinct pour point (fluids becoming glasses) as do paraffin-containing petroleum oils usually lies in a region bounded by 10,000 and 100,000 centistokes. It is also noted that this range includes the 13,000 cs. value which has been related to minimum starting ability of turbine engines. Of the polyphenyls and polyphenyl ethers, only the 4-ring and 3-ring ethers and the 3-ring polyphenyls have viscosities (extra polated in some cases) in the 10,000 to 100,000 range below 30F. The boiling point of biphenyl and diphenyl ether are considered too low for the engine lubricant application. An 18# (w) mixture of the 3-ring meta ether in the 4-ring meta-meta ether remained a viscous fluid at 0F. for three weeks. This blend was seeded with a few crystals of the 3-ring meta ether. During the three-week period the crystals appeared to neither grow nor decrease in size. This approach of mixing the 4and 3-ring meta ethers is expected to yield a fluid with a pour point in the range of 0 to -20F. The maximum allowable concentration of the 3-ring ether will be at the point that crystallization is not inhibited by the glass-like nature of the mixture. The use of terjJhenyls as diluents for the 4-ring meta ether is an alternative. However, only slightly better lower temperature properties than the 4-rlng ether alone would be expected since the terphenyls have only slightly better viscosity characteristics than the 4-ring ethers. The use of higher than the 4-ring ether or the 3-ring polyphenyl is warranted if higher boiling fluids are required. In this case the low temperature properties will also rise on the temperature scale. An attempt was made to study the temperaturesolubility characteristics of the three and four-ring meta polyphenyl ether mixture. The method used is proba&Sjfc. worthy of further consideration to find the optimum ether blend, if such a blend is reconsidered for hydraulic or less stringent lubricant applications. DSW 622061 STLCOPCB4096092 25. This method consisted of rapid agitation of the blend heavily seeded with the crystalline three-ring ether in centrifuge tubes. Periodically the tubes were removed from the constant temperature bath and were centrifuged to obtain the clear fluid. A refractive index of the fluid revealed the ether concentrations. At lower temperatures equilibrium appeared to be attained very slowly and heating during centrifuging remelted some crystals. This latter condition was Improved by cooling the centrifuge holders prior to centrifuging. Since it is believed that equilibrium conditions were not established, no specific values are reported and the method is given as a possible starting point for similar work in the future. Work on polyphenyl ether formulation was conducted under the succeeding Job No. 2-02-750.01-3767. 5- Miscellaneous Two samples of Santowax OM removed from Republic Aviation's high temperature hydraulic test systems exhibited only moderate change in viscosity from an unused sample. Sample No. 1 was taken from the test unit after being subjected to the following: Room temperature to 310F. - 30 minutes 310P. to 700P. - 50 minutes . Pressure: 2000-3000 psi Linear 0 rings (Viton H) Linear X way - 1 Back-up Rings 0 Viton A - Asbestos and Sample No. 2: Room temperature to 350P. 350P- to 700F. 700P. to 780F. 30 minutes 50 minutes 15 minutes Pressure: 1000-2000 psi Linear Viton 0 - rings PRP Viton 0 - rings Duriod 5600 - Back-up The viscosities determined for these samples are as follows: Santowax 0M, No. 1 Santowax 0M, No. 2 Santowax OM, S-55 100P. 16.79 cs. 23-00 18.03 210P. 2.39 cs. 2.65 2.41 DSW 622062 STLCOPCB4096093 26. B. OS-45 Fluid Evaluation 1. Objective and Conclusions The OS-45 high temperature hydraulic fluids, Type III (-65 to 400F.) and Type IV (-65 to 550F.), were Introduced in 1951 and 1952, respectively. Since then, conflicting and inadequate information has been gained on the performance and service life of these fluids. For this reason, the project was Initiated to augment current information on performance and service life. Similar competitive fluids, Oronite 8200 and Oronite 8515, were included as a basis for comparison. These fluids were evaluated for static thermal stability, oxidation and corrosion characteristics, shear stability, and bench scale lubricating properties. Additionally, several samples of used OS-45 type fluids from high temperature pump tests were checked for lubricating properties. Chemical and physical properties were also determined in an attempt to correlate performance and service life factors. These included viscosity, acidity, specific gravity, refractive index, evaporation loss, foam, flash point, fire point, wear and load carrying ability, and attack of copper, steel, aluminum and silver. Conclusions drawn from this evaluation follow: . a. Lubricating Properties OS-45 type fluids have better antiwear properties than the Oronite fluids, 8515 and 8200, as indicated by the Shell Pour-Ball Wear test and the Almen Wear test. This statement pertains to both new fluids and fluids subjected to oxidative and thermal aging. All four fluids exhibit a slight increase in wear with aging. E.P. or load carrying properties of all four fluids, as measured by the Almen and Timken machines, are very low and approximately equal. It is to be noted that the lubricating tests used in this evaluation represent a limited number of wearing surface configurations, do not take into account atmospheres other than air, and do not control temperature except In the Pour-Ball test. b. Thermal and Oxidative Stability Thermal and oxidative treatment of OS-45 type fluids result in greater acidity increases than for the Oronite fluids, 8515 and 8200. Viscosity decrease was less for the OS-45 fluids than for the Oronite fluids In thermal and oxidative tests and about equal for all fluids In the shear test. Thermal and oxidative treatment of OS-45 Type IV results in the formation of a solid, believed to be selenium, which is very corrosive to silver and copper. Evaporation loss at 400P. for OS-45 Type III Is excessive and loss for OS-45 Type IV approaches the same high value on thermal aging. DSW 622063 STLCOPCB4096094 c. Service Life 27- Changes in acidity and viscosity of the OS-45 type fluids are probably the best indication of fluid condition for service life recommendations. No practical limits were established. 2. Discussion of Experimental Work a. Lubricating Properties Each of the unaged fluids, OS-45 Types III and IV, Oronite 8200, and Oronlte 8515, were subjected to bench scale tests which included the Shell Pour-Ball Wear test, Almen Wear, Almen Load, and Timken Passing Load. The fluids subjected to static thermal aging and the oxidation-corrosion test were checked for PourBall Wear values, as indicated in Section b below. In addition, Almen Wear and Load and Pour-Ball Wear values were obtained on used OS-45 Type IV from Hamilton Standard and Vickers pump tests, and OS-45 Type III from an Eastern Industries system. Lubricating test data for the new and used fluids appear in Appendix Table III-A and values for the thermally aged and oxidation-corrosion samples appear in Appendix Tables III-B and III-C, respectively. Standard accepted test procedures were used for each of the bench scale tests. Determination of anti-wear properties by the Four-Ball Wear tester indicate that new OS-45 type fluids are somewhat better than the Oronite fluids, 8515 and 8200, In the steelon-steel test. These values appearing in Appendix Table III-A also Indicate that the Oronite fluids have better wear properties in the steel-on-bronze test. Wear values for two used OS-45 fluid samples from actual pump systems are nearly equivalent to those for new Oronite 8515> All four fluids subjected to the no air, no catalyst, 400F. thermal aging exhibited only slight increase in steel-on-steel wear properties. This thermal aging improved the OS-45 steel-on-bronze values and depreciated the Oronite steel-on-bronze values. Four-Ball Wear values on the fluid subjected to the MIL-H-8446 oxidation-corrosion test indicate a small deterioration in antiwear properties for all four fluids with the OS-45 fluids still equal or better than the Oronite fluids. Wear tests conducted on the Almen machine gave relatively low wear values, but were variable. In general, 0S-45 Type IV gave the best wear values at the highest loads with Oronite 8200, Oronite 8515, and OS-45 Type III following In the above order. It Is significant that none of the fluids would complete the standard Almen Wear test of 4000 psi load for 20 minutes without seizure and welding of the specimens. In all cases, lower loads were required to complete the.test. Values obtained for used OS-45 Type IV are considered to be equivalent to those for new fluid. DSW 622064 STLCOPCB4096095 28. Extreme pressure tests conducted on the Almen machine and the Timken machine indicate the OS-45 fluids to be somewhat superior to the Oronite fluids in load carrying ability. However, all values were low, indicating the fluids have only mild E.P. action. It is to;be noted that all the bench scale lubricating tests used involve several configurations of sliding metal surfaces. The test which gave the most Inconsistent and severe results was the Almen Wear test where the sliding surface is a relatively large area rather than a point or line contact. This type of configuration might lead to very thin films of a non-rviscou3 lubricant or a lubricant starved condition where the abrasive or welding effect of very small wear particles would be more pronounced. Such a condition would be even more aggravated by lack of E.P. properties of the fluid. A rolling type of test, such as would occur in a ball bearing, might give different results where fatigue failure resulting from low viscosity lubricants would be more pronounced. Another factor not studied is the effect of atmospheres other than air, such as might be encountered in an enclosed hydraulic system. b. Thermal and Oxidative Stability OS-45 Types III and IV, Oronite 8200 and Oronite 8515 were thermally aged for varying time intervals up to 480 hours at 4009F. in sealed glass tubes with a nitrogen atmosphere and no metal catalysts. The glass containers consisted of 12-inch lengths of one-inch diameter pyrex gauge glass tubing sealed at one end and with a 5-inch length of one-half inch diameter gauge glass tubing on the other end. The volume of this container is approximately 90 cc, and only 70 cc of fluid was placed In each tube to allow sufficient vapor space for expansion. The tubes were cleaned with chromic acid, solvents, and distilled water and thoroughly dried before the fluid was introduced. The filled tubes were evacuated and then purged with nitrogen five to six times andthen corked with a nitrogen atmosphere. After the tube was sealed off with a glass blowing torch, it was placed into a length of 1-1/2 inch electrical conduit with a wire across each end to keep the tube from sliding out. The schedule for placing the tubes into the oven was arranged so that each sample was introduced at such a time that all could be removed from the oven at one time. This was done so that they could be cooled in the oven to eliminate the shock of contacting room temperature and eliminate the handling of high temperature tubes which might have very high pressures. Each tube was placed in a 200F. oven for about an hour before being placed in the 400F. oven, a forced convection oven, to decrease the possibilities of thermal shock breakage. All heated tubes and tubes following thermal aging were handled within the metal conduit and with gloves and face shield until they were unsealed. Time intervals of 24, 48, 120, 192, 288 and 480 hours were chosen. . DSW 622065 STLCOPCB4096096 29.. The tubes were opened by applying a torch to the small sealed end. In all cases, there was a slight negative pressure in the tubes of the fluids tested. Each fluid was evaluated at the successive aging Interval for appearance, in specific gravity, refractive index, neutralization number, evaporation los3 (ASTM D-972, 400P., 6-1/2 hours), viscosity (100P., 210F.), foam (Microscale, 1/10 ASTM D-892), flash and fire points with a rerun of flash after the fire point, and Shell Four-Ball Wear. The values obtained appear in Table II. The oxidation-corrosion test was conducted according to the procedure of military specification MIL-H-8446A. Apparatus for this test is described in Federal Test Method Standard No. 791, method 5508, and consists of a long glass tube fitted with an inlet tube and a reflux condenser. Temperature was maintained at 400F. by means of a heated aluminum block bath, using Wood's metal as the heat transfer fluid. Dry air (water pumped breathing air) was passed into 100 ml. of the test fluid at a rate of 5 liters per hour for 72 hours at the test temperature of 400F. The metal catalyst pieces of steel, aluminum, alloy and copper were tied in the form of a triangle and the silver specimen was suspended separately by means of a glass holder. After the test, the metal specimens were brushed and washed in solvents in a manner analogous to the procedure outlined in Federal Test Method Standard No. 791, method 3457. In addition to the determination of the weight change and appearance of the metals, acidity change, viscosity change, and fluid appearance, aged fluids were checked for evaporation loss, foam, and Shell Four-Ball Wear. Values for these tests appear in Appendix Table III-C. The,most significant changes occurring from the static thermal aging were in acidity, evaporation loss, viscosity and, in the case of OS-45 Type IV, the appearance of a solid material. Only slight changes were noted in specific gravity, refractive index, foaming tendency, flash point, and fire point. The total acid number of the OS-45 fluids increased from about 0.1 to 0.4 with the greatest increases occurring during the first 100 hours at 400F. The Oronite fluids exhibited little acidity increase. Thermal aging had little effect on the evaporation loss for the Oronite fluids. OS-45 Type IV exhibited increased evaporation losses after about 100 hours of exposure, and OS-45 Type III had a very high evaporation loss of 40 to 45$ at all stages of exposure. This abnormally high loss as compared to previously published results (21.23$, WADC Technical Report 55-89, Part I) led to an evaporation loss check at several different tempera tures. A plot of the evaporation loss versus temperature. Figure 1, indicates a break at about 365?- Below this value the loss is DSW 622066 STLCOPCB4096097 30. probably due primarily to evaporation, and above is probably due to increased decomposition as well as evaporation. An extension of the lower portion to 400F. would give an evaporation loss nearly equivalent to the WADC result. It is not known whether this difference in result is due to a difference in fluid stability or some characteristics of the respective evaporation loss equipment used by each laboratory. The viscosity at -100F and 210P. of the OS-45 fluids decreased less than 10# and the Oronlte fluids decreased froja 30 to 50# in viscosity when subjected to the same 480 hour exposure at 400P. Static thermal aging of OS-45 Type IV resulted In the formation of dark sediment and grey-black, needle-like crystals one to three inches long. The solids began appearing at about 48 hours of exposure at 400P. Similarly, the oxidation-corrosion test of OS-45 Type IV resulted in grey-black granular solids. In the first case the solids are believed to be selenium from the inhibitor, and in the second they are believed to be silver selenides since the silver catalyst was severely attacked. In summary, these tests indicate that the oxidative and thermal decomposition products of the 0S-45 type fluids are more volatile and have higher acidities than those from the Oronlte fluids. The OS-45 fluids suffer less viscosity decrease than the Oronlte fluids. The Four-Ball Wear of all fluids is Increased only slightly from new fluid. The Inhibitor used in OS-45 Type IV modifies the thermal and oxidative degradation, but results in a solid product and increased corrosion of copper and silver. c. Service Life Limits Several physical properties of the fluids were checked In an effort to find some property which would serve as a measure of the OS-45 type fluid useful life limit. Of these properties, acidity and viscosity are probably the most significant. The change In evaporation loss for OS-45 Type IV would Indicate depletion of inhibitor. Changes in refractive index, specific gravity, foaming, wear and E.P. properties, flash points and fire points appear to be of little value due to the small amounts of change with thermal or oxidative exposure. Viscosity changes for the 0S-45 fluids were not excessive; however, any decrease of an already low viscosity fluid might result in lubrication and control difficulties In a hydraulic system. The shear tests illustrate that the fluids may decrease in viscosity without thermal or oxidative degradation. Acidity increase of the OS-45 fluids is relatively large, especially under the oxidative conditions. This acidity, a total aaid number of about six for the OS-45 fluids, does not result in excessive attack of catalyst metals used in the MIL-H8446a oxidation-corrosion test. DSW 622067 STLCOPCB4096098 S E M I-L O G A R IT H M 1C 3 5 9 * 7 1 KCUFTTL & ES9LK CO. MACKIN U.I.A. DSW 622068 STLCOPCB4096099 31. Practical limits of viscosity and acidity were not established in this project and will be dependent on the requirements of an individual system. d. Shear Stability The two OS-45 type fluids and two Oronite fluids were subjected to ten passes through a diesel injector shear machine (General Motors Injector No. 5226710 operated at 1800 cycles per minute). Viscosities at 100P. and 210P. were measured on successive .passes through the machine to determine the viscosity decrease profile for each fluid. Values for this test appear in Appendix Table III-D. e. Miscellaneous Viscosities at -65P. and -40F. for the OS-45 base stock, OS-59 (tetra(2-ethylhexyl)silicate), were run on .two samples representing different sources of the OS-59 raw material, tetraethyl orthosilicate (TEOS). Cannon-Fensky viscosimeter tubes were used in a bath of controlled temperature. The low temperature viscosities for the two OS-59 samples prepared from John P. Queeny manufactured TEOS and Inorganic Division TEOS are listed below. -40 -65 OS-59 - John P. Queeny TEOS (A-189, Ba. #47)* 313.12 cs. 1383.3 cs. OS-59 - Everett TEOS (NBP 194) 313.75 cs. 1322.7 cs. * This material became slightly hazy on being cooled below +30P. Evaporation loss tests (ASTM D-972) were run on the OS-45 and Oronite fluids at 400F. for 6-1/2 hours. Since values for OS-45 Type III differed considerably from results published by Wrig'ht Air Development Center (WADC Technical Report 55-89, Parts I, III and IV), additional tests were run at temperatures from 340F. to 4l5P. with the OS-45 Type III fluid and at 350P. for the other fluids. These data are listed in Appendix Table III-E and OS-45 Type III data are illustrated graphically in Figure 1 of the discussion section. Oxidation-corrosion tests were completed on samples of unused OS-45, Lot Z-163, and OS-45-1, Lot Z-487, which were returned from Wright Field where abnormally high copper attack by these two lots had been observed. Oxidation-corrosion results indicate that the copper weight loss of OS-45, Lot Z-I63, Is greater than for Lot A-414 which has been evaluated previously, but both are within the specification limits. Copper and silver weight loss for OS-45-1, Lot Z-487, are much greater than specification allowances but are equivalent to a previously evaluated lot, A-312. DSW 622069 STLCOPCB4096100 32. C. Skydrol 500 1. Reformulation to Eliminate Dermatitis A severe dermatitis problem appeared with certain persons handling Skvdrol 500. This was traced to the additive, phenyl glycldyl ether (POE). Removal of POE from the formulation resulted In pump corrosion. Both Douglas and Monsanto then embarked on an active program for screening replacement additives. The 250F., l68 hour oxidation-corrosion test was used In screening additives. Tests were run for purposes of correlation with Douglas, for determining the mechanism of the corrosion or the component responsible, and for general screening of additives. It was thought that the best indicators of additive activity were attack of copper, magnesium, and cadmium and changes in acidity. Viscosity and attack of aluminum and steel was not affected appreciably. Correlation tests with Douglas stemmed from differences in results with a formulation containing the inhibitor, Ortholeum 500. These differences were never completely resolved for this formulation. Correlation work included the evaluation of a batch of FH-135 (base stock with VI improver) both at this laboratory and at Douglas. In addition, metal specimens were supplied by Douglas for our use. At the time this work was being done, we were reusing the best metal specimens. Recycle of the Douglas specimens Indicated no appreciable changes on reusing. It was concluded that our oxidationcorrosion tests were essentially equivalent to Douglas' and that discrepancies with the Ortholeum formulation were due to the nature of this additive at the particular concentration used. Oxidationcorrosion test correlation results appear in Table XXII. During this correlation work, it was found that differences existed between the two lots of FH-87 (Ba. 15-16 and Ba. 25-26) in the oxidation-corrosion test. This difference was traced to water-soluble salts. FH-87, Ba. 15-16, with 40 ppm water-soluble gave abnormally high metal attack; whereas, Ba. 25-26 with 8 ppm water-soluble salts gave normal results. Skydrol 500 prepared from either of these two FH-87 batches gave good oxidation-corrosion results with the Ba. 25-26 performing slightly better. Several tests were run to determine the mechanism of, or the component responsible for, metal attack in the Skydrol 500 oxidation-corrosion tests. In addition to the corrosion contributed by FH-87 with high water-soluble salts indicated above. It was found that the Acryloid viscosity index improvers with higher than normal acidity contributed substantially to this attack. A run was made in which adsorption alumina was used with the poor FH-87 (Ba. 15-16) as well as high acidity Acryloid. DSW 622070 STLCOPCB4096101 2Mo <E-i w MK*J 3 g ioon oP g oo Ww <EpHeq CwO Eh O O SE I o o< p .=j- 2 < (X) oo rn -- vo vo m CM Os rn m -=J- CM CM VO a\ m OJ rH Eh m CM rH in m rH CM CM i--1 CM ->P *ri oiH o CVI vo vo VO m m rH m m rH oo oo o o ooo o < o oo o o ooo o O o av r>- LoOs o Os O c-- o OS m o -=J" o o\ CM vo m CM vo o o rH CM CM O rH rH rH oo o oo o o oo O o bO o voo mo o VO vo t-- vo -=* rH t-o c-- ov ov m CM 00 oO o CM CM o rH m rH o rH in rH o os in o o o oo o o oo o o -p p < in ov ca K\ o t- VO -p in a) s -=1" rH as ON av rH CM m vo CM CM rH CO rH vo vo d- VO in rd vo vo r--1 OJ d d CM rH rH rH 03 03 o o rH 1--1 cd 4-> -p m 4) <D BE o p o o om >R CM a o jto i--i o -apJ < p S V ' i) e O o s < p It o o < p O a < P T3 4) CQ 3 <o o X a\ Os -p vo vo VO VO vo vo vo VO vo OV OS os rH rH rH rH CM rH rH CM CM VO VO OO o voo VO O voo 1| in in 1 1 1111 1 in in in in in in in CM CM CM CM CM rH rH rH rH CM rH rH CM CM II I i PQ pq CM pq pq A A A A A A A A in in in in in in m i--i m rH m m mi--i cCO 00 t00 00 o- ' t- 00 00 cCO ot-o- or-o~ iI i 1 111 1 111 Xto nto wto xto Xto X to EC to X to EC to X iw to .to X to X to EC to -=* VO i o IM 2H i H P M H HM to (U Eh O O < P O u vol oo oo < m< < p CM P P I o CM o o < p o o < p 1--1 rH 11 in CO rH rH CM -=f in in .vo o1 I 00 1i o> 00 OS CM CM CM CM CM DSW 622071 STLCOPCB4096102 33. Relatively low metal attacks and acidity increases were encountered indicating initial acidity or acidity contributed by base stock and viscosity index improver decomposition were the prime offenders. Acid scavenging type of inhibitors were thought to be desirable. These oxidation-corrosion test results appear in Table XXIII. A large number of potential inhibitors were screened in FH-135- Those showing some promise Included tetraphenyl tin, tetrabutyl tin, triphenylstlbine, and epoxy 2-ethylhexyl tallate. This latter additive appeared to be the most effective both at a 1.0# concentration alone or in combination with 0-5# FH-132 (bis(1,2-phenylmercapto)ethane) which Is normally used in the Skydrol 500 formulation. Several commercially available epoxldized fatty acid esters widely used as plasticizer stabilizers were evaluated with equivalent good results. Paraplex G-62 (Rohm and Haas) reported to be epoxldized soya oil was chosen for further evaluation based on Its availability and reported low toxicity, being approved for use in food wrapping products. Concentration studies with Paraplex G-62 indicate slightly increased copper attack with decreasing amounts below 1.0#. The use of FH-132 with the Paraplex G-62 had little effect except at lower concentrations of the epoxldized inhibitor. At 0.2# G-62 and 0.5$ FH-132, magnesium is attacked more than with G-62 alone. Oxidation-corrosion test results for the promising inhibitors and the variations of the Paraplex G-62 formulation appear in Table XXIV and additives of little promise are tabulated in Table XXV. Both the Ortholeum 300 (2.0$) containing formula tion, 0S-105, and the Paraplex G-62 (1.0#) version without FH-132 appeared to be non-irritating or skin sensitizing. On the basis of full scale pump tests at Douglas, it was decided to include 0-5# FH-132 in the formulation. This Faraplex G-62, FH-132 inhibited fluid was subsequently adopted as Skydrol 500A. Further work on this project was done under the new Job number 3767. 2. Viscosity Index Improver A proposed change In the Rohm and Haas Acryloid R-3876X viscosity index improver prompted a project for its evaluation. In the proposed Rohm and Haas VI Improver process, the polymerization is conducted in Skydrol 500 base stock (FH-87) rather than in a solvent which Is subsequently replaced by FH-87. Oxidation-corrosion tests on this new style Acryloid in the Skydrol 500 formulation and in FH-87 displayed increased metal attack over similar blends using the current VI improver. To further clarify the cause cf the Increased metal attack, Rohm and Haas subjected FH-87 to their proposed polymerization procedure time and heat cycle, but without the presence of monomer or catalyst. A second sample was treated similarly, but with the polymerization catalyst present. These samples were subjected to the nxidation-corrosion test as is and at 12# concentration in untreated FH-87- These tests indicated increased metal attack from DSW 622072 STLCOPCB4096103 34. the polymerization treatments and especially with the sample which included the catalyst. This information was returned to Rohm and Haas for further suggestions. Further work on this project was done under Job Number 37^7 Table XXVI presents oxidation-corrostion test results for the proposed Skydrol 500 viscosity index improver and for the various batches of treated FH-87. D. Silicate Weapons Lubricant A proposed silicate weapons lubricant, OS-94 (93.8# mixed tetra(2-ethylbutyl, 2-ethylhexyl)silicate, /FH-134/, 0.2# Phenyl alpha-naphthylamine, 6.0# Na-Sul BSN), failed to meet humidity cabinet rust tests specified by MIL-L-14107 at Rock Island Arsenal (R.I.A. ). The qualification test resulted in failure at 264 hours, whereas, results at Douglas indicated the panels to be rust-free in excess of the minimum 400 hours for several batches of OS-94 and with several sets of metal specimens. Likewise, our humidity cabinet test results confirmed the results at Douglas. . After discussing the discrepancies with R.I.A., it was decided that they would repeat the test and provide us with some of their specimens for comparison with ours. Our test with their specimens confirmed their initial results. It was found that the steel panels which had been used were not cold rolled steel as specified for the humidity cabinet. After humidity cabinet failure of OS-94 was confirmed, two alternate formulations prepared by L.W. Bannister were tested. One of these, OS-94 with an additional 0.3# phenyl alpha-naphthylamine (PAN), resulted in panel protection of 287 hours to 480 hours on three panels. The other formulation consisting of 92.0# FH-134 silicate base stock, 7*5# Bray's Synphonate 28, and 0.5# PAN gave protection for 552 to 672 hours. This latter formulation, designated OS-106, was subjected to the remaining MIL-L-14107 specification tests with acceptable results. OS-106 was submitted for qualification testing but failed in the hydrolytic stability test. Since the market for lubricants of this type was diminished since the program was initiated. It was decided to terminate the project. Several other preservative additives were screened in FH-134. Materials which provided more than 400 hours protection were 5# (w) N-7797 (R.P- of tetrapropenyl succinic anhydride (TPSA) and 2-methyl 2,4-pentanedlol), 5# (w) Glegy NPA, and 5# NIrus N.P. (Synthetic Chemicals Corporation). Since this project was discontinued, no further work was done with these promising materials. Additives which did not give adequate protection in FH-134 follow: DSW 622073 STLCOPCB4096104 35. 5$ Santolube 203-C, 0-5# PAN 556 Santolube 203-C' 5$ Santolube 70, 0.5/6 PAN ... 5$6 Santolube 70 2-1/2J6 RT-53A, 2-1/256 RT-67A, 0.556 PAN 2-1/256 RT-53A, 2-1/256 RT-67A 556 Amine ODT, 0.556 PAN 556 Amine ODT 556 Alox 1724 556 Alox 350 (insoluble) 556 Alox 600 (insoluble) 556 Priminox 43 5# N,N,N',N*-tetrakls(2-hydroxypropyl)ethylenedlamine (Insoluble) Table XXVII presents MIL-L-14.107A specification test results run on 0S-106. E. Skydrol 7000 - Low Temperature Viscosity Skydrol 7000 viscosities of production lots were reported to be near the mid-range at 210P. and near the upper limit at 100P. A question arose concerning the viscosity at -40*F. Viscosities for batches 44 and 45 of Skydrol 7000 indicated values' 4 to 656 higher than the expected value of 7000 cs. This would indicate that low temperature viscosities as well as 100P. viscosities are Increased for batches with normal 210P. viscosities. -4oP Viscosity, cs. 100F. 210F. i ' Skydrol 7000, Ba 44 7302. 15-64 3-97 Skydrol 7000, Ba 45 7434. 16.17 4.01 Specification Limits ----- 15.5-16.0 3.96-4.04 III. Miscellaneous A. ASTM Cooperative Test Work Laboratory tests were conducted on ASTM reference fluids supplied by Technical Committee N on Hydraulic Fluids of ASTM Committee D-2 for cooperative testing.. These tests included Plash point. Fire point. High Pressure Spray Flammability, Low Pressure Spray Flamma bility, Hot Manifold Flammability, Four-Ball Wear, Almen E.P., D-943 Oxidation, and Oxidation--Corrosion tests. Fluids tested were designated as follows: < 1-A-l 2-B-l 3-C-l 4-D-l 5-D-l 6-E-l 7-F-l 8-G-l Petroleum oil Water base Phosphate ester Halogenated base Phosphate base Oil emulsion Silicate ester Silicone DSW 622074 STLCOPCB4096105 *! 36. Procedures and test results for these fluids appear In the Appendix. B. Synthetic Lubricants for Refrigeration Units A large potential use of synthetic lubricants In the refrigeration field prompted some preliminary work to establish the level of lubricating qualities desirable in such fluids. A series of four-ball wear tests were run on Suniso 3-G, the refrigeration compressor fluid presently in use by Hussmann Refrigerator Company. Similar test data from Mobil D.T.E. fluid and Pydraul P-9 fluid is included in the chart below. The comparative data indicates that Suniso 3-G is inferior to both Pydraul P-9 and Mobil D.T.E. in lubricating qualities. Test Conditions: 630 RPM 167P. 1 hour duration Pluid _____ Steel-on-steel_____ 4 kg 10 kg 40 kg Suniso 3-G Pydraul P-9 Mobil D.T.E. 0.38 0.22 0.18 0.62 0.28 0.24 o.6o 0.63 0.38 Steel-on-bronze " 10 kg 2.32 1.18 1.48 C. Low Temperature Viscosity Study Samples of Skydrol 500 were checked for -40F. and -65P- visoosities for comparison with results obtained at Douglas Aircraft Company on the same samples. This was done to check our low temperature viscosity procedure. Our results differed from the mean by about 0.75/6, which is within the 1.0# reproducibility limit for temperatures below 6oP., as specified by ASTM D-445. These results are tabulated below: GAC0 REL -65P. Viscosity -65F. Viscosity Skydrol 500 Old Acryloid - Lot A-2?62 New Acryloid - Lot A-2763 2,470 cs. 2,540 cs. 2,489 cs. 2,559 cs. D. Lubricating Study - Paraffinic Petroleum Oil i A paraffinic petroleum oil base stock was treated with fine iron filings for 24 hours at room temperature to determine the effects of such treatment on the oil's wear properties. It was found that this did not change the wear properties. Pour-ball wear tests were run with solvent washed balls and distilled water and Jewelers rouge cleaned balls with no significant difference. The f ( DSW 622075 STLCOPCB4096106 37 complete removal of all iron particles was found to be important since simple filtration by a filter paper left minute particles which led to gross wear. , Oil: Elk SAE 30 Base Stock, Inv. 2069. Iron: Fisher Cat. No. 1-57* about 40 mesh filings. Treatment: 250.7 gm. oil and 50.0 gm. iron stirred 24 hours at room temperature in a 1-liter round-bottom flask. 4-Ball Wear, 1250 rpm, 2 hours, l67F., steel-on-steel, 40 kg. Inv. 2069-no treatment O.91 mm. Inv. 2069-Dicalite filtered O.94 Inv. 2069-iron treated, filtered 1.05 (seizure in once through filter paper 5 seconds) Inv. 2069-iron treated, filtered through Dicalite coated filter O.93 Inv. 2069-iron treated, filtered through Dicalite coated filter O.97* * Steel balls used in this test cleaned with distilled water and Jewelers rouge and others cleaned with Skellysolve B and acetone. E. Compressor Lubricant - Four-Ball Wear Shell Four-Ball Wear values were obtained on compressor lubricants to assist in a problem at the Texas City plant which involved lubrication of the seals and rods of reciprocating compressors. This information was used by Texas City to outline a lubricant test program. No further work was done on this project. Four Ball Wear: 630 rpm, l67F., 1 hour, steel-on-bronze. Coastal Pale Oil Glycerine Humble White Oil 335 Ramol 4 kg. 0.90 mm. 0.48 0.6l 0.59 10 kg. 1.49 mm. 0.75 1.34 1.80 40 kg. 2.17 mm. 2.48 2.80 2.25 de 9-23-60 L. R. Stark R. E. 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Cd Cd rH d 1--I o o co<cooQQ22coco a|o PCOCOCOOCOCO<-P< EH Eh >da NJD tja NJa `^D Vfi <WD vrv VA vn "wfi >3n vj'v. wx vj\ V* sPs Vk V\fPs5f\5rN Crs ts 5f\ sPs. vrx. Crx Cfs Ws irVOCVJCVJCVlt^rHCVJrHCVJCVl^-rVCVJrH^rHiHrHrHrHirirH ITVCO OrHOOOOOOOOOOOOOOOOOOOOOOO P r<MTN r<M<\ r<v<> r<^ KN r<V^N I I r*>KNr<*\-4-KM*"N4-KNrA unvo ..................................................................................II......................................................................... OOOOOOOOOOOOOO I IOOOOOOOOO OO J fda 03 I d -p 0 CQ 1 3 V p > -p j p d -p p p fa 03 fa fa H > cd d fa rHI d 0 Hg C-- O 1--1 NO < 1--I o cd w -d d d bOH dd op d fa cd fa -p p d tc dd > S p bO d Cd wdd ad o x! o 4- W CO d fa d d fa PP 2 . cd fa cd fa cdfacdfacdfao CVJ KN-4- LOCO C-00 OVOOPPWKN4 IfNNO t-00 OVCJVO P P CJ KN KNKN P P P P P P P P CVJ CVJ CVJ CVJ CVJ CVJ CVJ CVJ CVJ CVJ CVJ CVJ CVJ f<M<> JA, KN KN KN ** ** DSW 622085 STLCOPCB4096116 TABLE V I (c o n tin u e d t-H * S3 fn co ia bO Pi O -=f Ov -3* -=J- oo G o -a cd i--H O < (3 C CQ 3 TJ O' G G3 OO Eh CU * *1 M . * *( *C *< i * *< M * *( *( *< * *> * * *c *1 *< C\lino\DOt-CVINOCJCVIOO ojvovo .inmio m^- aj cm c\j inmininvo inmm <n a -a cd G Jo 3Q fa V0 4--^-^-^3 O4-00C0VO4- O CVI4- O O -4--=t-.=fr^i-.=i-mi-ii-imm.=}-.3-.=i-.3-inin a G >> cd H ) * P>R aJ Ov oj X CVJ o m>fc G OJ -=J- ftrH ft o cd G O OO G O OO O ov T3 G I ra < .W cd in c- gvo c oo HOI O P =*- 33 cd ai 3 G Go O fa o o G < OO Il =t~ -=t OVOV mm pp GG > tH cd cd CO co oo ii -=J" Jd" Ov ON mm pp GG cd cd oo ii p- -=jovov mm pp Gc cd cd co co ooo in in in mmm XXX ooo rH *"i i-1 p H in in co co << < TJ >*>R T3 o o < O O 73 TJ in in m rl "rt O O oOO G '< o o oooooo o vo vo < < *> in in in in in in --> p in si vo vo oommmmmmooom p ojcuooovov ovovov o mmppojcvixxxx xxcmojcmx i i eojojooooooojojcvjo i-q i--11--i i i p i--i <--11--i r--11--i t i i i--i COWOO<<<C<<<<<<<<<< U \A W) U) VA VA VA VA VQ On On On On On On On vjn ^ On ni n On On ffC, ON ppppooooooooinminin O O O O <--t i--I i--I i--1 (--C i--I i--I i--IOOOO v 1 iH>R O Pm G OV| cd m CO m..v.o...<..-...i.n...m...<...-...i...W....4...-.m....v..o...c..o...i.n...i.o..N....o. OOOOOO IOOOOOOOOP cdPcdPcdPcdPOcdPOcdPo minmin^itn-^itn- iinnminvinovinoiionicn--icn--itn-oinomoo ionoicnr\ DSW 622086 STLCOPCB4096117 TABLE V II 03 'O fc c o o 03 O o 43 O a; rH CO -p o fe 43 o CO cd H O co *5 i--i KNVO O K\ I I O I I covo mon i i o i i H H rH I--I I I CJ I I mo [>H'-ooo ii i--I rH r--( I I CM I I a*- I I rH I o o CV1 -P 03 O 03 fc ill I I I I I I O o III I I I I I I 03 Pi O III I I I I I I *H O rH III I I I I I I > -p CM os 03 O *rH H H -P O t'- Eh -P C &< vo c-vo o t--mrHvo m o<C PI cBd v <3 o o o C'-aj- CM OMOad- O CTVrH CMCMCMCMCMCMmCVim a _i o05 fo t"00 CM CM CM o m Q M CMCMCMCMCMCMCMCMCMCM t) P> ad" ad" ad- mad" ad" mad- 43 PI CMCMCMCMCMCMCMCMCMCM 3 Pn i--I H H l--I i--IrHrHr--irHiHrH O OS o ti ti k JL, SVfa -P ooooooooooc PI i--I i--I I--I i--IrHrHi--I i--I i--I i--I Cd o o ooooooooooco oooooooooo -p tu >R >R>R>R>R>R^>R>R>R>RO s incM cm o\o OMnmcM m o ad- co cm moo h m c-- h m - o Kc m cm o H COad-COOOad-COOOad-OOOOmfr, -p ad- lAad- -=t mad- ad" mad* ad" O cd CMCMCMCMCMCMCMCMCMCM llQ rH H i--I r--I rl rH rH i--I t--I ri i--1 43 s3 3 u OOOOOOOOOOOP, o HrHrHHt--IHtHHrHH-P Q* fe ooooooocooc OOOOOOOOOOcdO PPPPPPPPPPCOO <;<<*a!j;<!a;<;<!a;c rH >R>R>R>R>R>R>R>R>R'5Rm . mcooo h o h me--coco o m rH t-VO CM 00 VO CM CO VO O C'- d o rl -P P cd 3 rH 43 3s p as o Ph rH cm mad- mvo t'-oo ovo DSW 622087 STLCOPCB4096118 fn s co W H Eh Oh O o2 t--l < MO M > cd s a XI P<P Eh E-t H XI I0H} M Eh < (X so o in on i CO o fr, o to t~vo o rH s o, X CM VO bO w X rH cd V o V =( 4J CO i--i \ i--i c cd o m I bO i rH x 3 cO o -p rH PH CO CO *c 31 T3 O cd o oO XI Ph Eh C * CO T3 T3 i--i c cb < 33 o OX Pl, o > >R TJ tH 33 r--1 &, O I I I ICO I I II II II H. i--11(11 f--I O II Il II rH I I I I rH I I CO II I IO o t^-1~-c\j oo o in.=t- rH ON ON i--l i--I i--I i--I o o KN O inmaO c- -=f mmvovovo oooooo mmoo co co -=r in in m.=i- in ooo ooo mo mc--rHvo -t inirurufun ooo o o o ONKN CM CM CM CO CM CM CM CM CM CM O O OOO O ONinmco o m CM CM CM CM m m OOO OOO ON-=i- CM rH C'-=f CM CM CM m KN m OOO O OO rH rH KMnS4-=i- =* -=4" -4" -=J- -=3" h m^i- in cm in rH^tvo c-- c-- >--i in in in in m -=r inin^M- m 00 t-co o o o jm- mm in in oo mt--o o rmmincM 00 OVO ONO o .=!--=}- m-=*- in in ON ON ON ON On III II 13c, pc, pc, pet fr, 3 33 3 P cXd cxd xcd cxd ixd *C3 *0 'O 'O 'O >> >>> pL, Pl, Pl, Ph PL, \a ya vfl ^ ominoocs. UN ox Ox OS rH CM t~-ONO ooooo CM CM CM CM CM CM CM CM CM CM p p pxt)ifl 33333 rH i--I rH rH rH 33 3 3 3 3 i--I rl H H H i--I rH i--l rH i--I 4) OOOOO XO vn VO vn XJX oITS iOnx IifnfX OoS OoS rH cm c-- ONO ooooo CM CM CM CM CM i--I rH i--I rH rH Cn <h C, C, ^ cd cd cd cd cd CO CO CO CO CO oI oI oI oI oI -P -P -P +J -P Si Si JG sx a bO to to WJ to M3o 3o M3o h3oH H3oH Hi HI HI KH HI >D VQ VP \1) oQs. ignV iOnx Uov oOn i--I CM C ON O s ^ s r, in in in in in ON ON ON ON ON iiiii co co co co co ooooo so so so so so o o inmoOS OS six OS OS O ON t-- CM h *** in in in in m ON ON ON ON ON ii i i co co co co co ooooo VP vn V.CN ~V-CN <VtO Ts 'ffs CPx nTn. oommo O ON C'- CM H H S H > in in in in in ON ON ON ON ON i ii ii co co co co co ooooo VP VP VP VP VP ogxomwxtunxogS o ONXCM H DSW 622088 STLCOPCB4096119 TABLE IX EVALUATION OF USED OS-95 Chevrolet - Bay City Division - 260 Hr*s, (14 hrs. at 190F. ) OS-95 New Viscosity 100F., cs. 210P., cs. 50.63 2.89 4-Ball Wear (630 RPM, 1 Hr., 167P.)_______________________ Steel-on-Steel 4 kg. 10kg. 40 kg. .21 .29 .43 Steel-on-Bronze 4 kg. 10 kg. 40 kg. 1.20 1.40 1.70 Neutralization Number 0.82 TAN Rust Test (REL, F-101, 10.0=Perfect)_______ 10.0 Appearance . Yellow, slight cloudy OS-95 Chev.-Bay City Div., . 260 Hr. 31.8 3.05 .20 .26 59 95 1.48 I.69 0.82 TAN 10.0 Reddlshbrown-nearly opaque DSW 622089 STLCOPCB4096120 L b s. .Lbs 6^0 rpm , s te e l-o n -s te e l, 1 h o u r, l6 7 F 5 2 0 F ., 15 m in u te s ?h h M P H m < E-i CO p a E-i <d CO W H Eh X Pm O K Pm Eh < a H Eh <O H paq a p s a o H Eh < a o Bh o4" I co o pa3 t) CM K'p O -P p en -p d Cd Eh p CO 4) 3 a w V Ea (-4 <c 0Bm 0 03 in 0 u pa id 1 1p m 1a 1 h0 ra p 0 1--f ft e ra 0 0 p Eh 1 co 4- co OJ VO 1 in 4" m 4" 1 OJ 0 0 p t1 in in OJ m -=t aj- LH o u a p abO m a u Eh OJ m 01 in 00 rH m bO -=J" in 10 in c- 10 in in 1 m 1 1 | 0 1 1 ID 0 O00 0 4^ 0 0 o3 bb =t OJ co rH CT\ m rH rH -4" =* 4- m m m 4" =t K\ m O Od0 d 0O O d 0 rH I * O CO 01 0 t- b0 =* m m m 1 m 1 o Bn odd0 1 0 1 rH 1m 1 0 V aP p aJ o aft m p a O a 6R* in in 2 ft o Eh oa Ooo p. p ctJ > c aft CQ OJ aa a P tH T3 H H Bh Pap O p po at aft 09 o aa ft s? a at aft a> o aft a p. >> a p. t4 ^ '*R. m-p o & at >> tn m rH \ o OE 3 aJ >r. OV mE p op p> * a c- t- ft I--t < s > a tp4. Cm Eh > 09 V o m> o H Eh a rH > a p wi OJ >> p a a a >t p o oo \Eh \Eh tOH a ap P o Po i a t'ovo Eh I a cc P o -4" Oi--I I CO o cu DSW 622090 STLCOPCB4096121 CO 2: oH <H 3 < > < -o=t rH I CoO HO X rH o w w ft Eh < COI o Eh O33 Po 33 iOn ft rH <\J VO'flH OJ UNCO ft UN NO E-OJNO Q i--I O ON o i--t O OJNO c o +o p ft -. >**. om o i i ONNO t-- ft O U-NO ... e2000+ <0 II II II ft 3 ["-'.0 ON E O U-NO Cd o oo ooo HHH I) S E Emm B o moiAimn OJ i--I UN i--I UN CO CXI -in UN OJ C-- UN^J-NO UNNO LPi O O O O O rH oo oj un un^j-co UN-3-no UNNONO O O O O O rH rH -P -- o3 $3 cd + o CO fQt'epR.m O UNO oo o ON O O m oj m UN t-- ONO o rH NO O UNCO OJ C-- m -=to mn=i- OJ m un on o I--I I KNhOOO OJNO-OJ CO o -r=H1-NO> un 3 rH o S 4a)3 ft 42 t--34-t------' O UN^J- OJ \ m rH o un EE cd o o o S S 6 OJ m42 . .fxt + o mo NO OJ UN * m c OJ rH rH cd E o m mm mo =t~ Cvi ONKN4- Hd- UNCO ft 42 O rH O 6+ cd . . O C2 C2 rSH i--SIi--SI <W12 4023 4TO2 O OO OO O OJ OJ OJ UN UN UN un o unno o o p- Hi-NO UN NO NO O O O O O rH H Hd- ONO O rH UN UN NO LTNNO CNJ O O O O O rH H o u g h to a fe 101 1O CO 3 cfdt Om TJ rH >> ft NO rH t t-- ON UNNO un oo moo cm t-o co oo NO > UN OJ CUONNo rH u- m rH OJ NO OJ UN oONoOoN rH ft PC Pc PC Pc< oo oo o oooo o rH UN O i--I OJ rH rH I -p cd 01 o +>3* rH 01 O O 03 rH > 42 m o m bOrH 04 O j cd o o o 3 + o o 2; X O rH cq 3 UN. OJ rH + E m a <c Eh S Nf* t o < -Eh >s 2 r mOJ rH > T3 43 rl H 42 ) 42 C2 -O O C rH U) S3 cd S3 o <d 42 cd rH < 43 33 h cd O Cd -H rH 42 43 Cd &rH 3 2: 43 ft C rl <d < H fe !3 43 CO o0a i-- rH r--l 0) %> i) s s S CO 01 01 mm o moj o t--1 rH I lilt IIII IIII ft ft ft Pc ft Pc aooooo mo mmo m NOhhOU OJ OJ P 43 cd cd o m42 3 O 42 T3 cd 3 E4h2 o o o ft OJ UNCONO mo oj UNmmNo rH O O O O O rH ft 3 ONO rH CO OOO UNUNmmco m O O O O O rH af6t o UNJ NO PH hH P*H Hh pH HM 400400 rH nd- rH-=J- oft 42 t- N NO 42 42 43 ft COI O3 ft cq cd 42 3 03 1 rH 03 1 i--i 42 42 42 42 i 43 CO 43 CO O O OJ OPh n aEft o o faO 3 Td P cd ft 42 42 fPt P cd cd 3 ft 03 O 3 ft O rH O >sO cd 3 > > 42 O 3 ON S ft i cd PHKmI Oft rH t-- 73 > 3 03 3 O 42 O O ft C2 42 O P CO 42 hO cfdt -P X 42 c O3 P 42 3 3 iH -p c o o i--DI ,0 -p D3 T--I p OJ UN DSW 622091 STLCOPCB4096122 DSW 622092 STLCOPCB4096123 RF O ai rtsi nt g ther m e th o d number number iso f and H .L. elxetet tnet F r a ig e n , of rus descr t AS1T0M=Bpuel ibe ru s t. o c Coo M X w <e le t rfe in ct , No. 0 154, = com O cto p le te ber, ru s t 1948 . oo ooo III III tII ONfA-4- =! rA o cvj o o oooo I I+ I \00 o co +o p p. Op^lT- (3-i II Po <s I TABLE XII TRICRESYL PHOSPHATE FORMULATION PHYSICAL AND FUNCTIONAL PROPERTIES Viscosity, cs 210F. 100F. Viscosity Index, ASTM Viscosity after shearing^2) cs. 210F. 100F. Pour Point, ASTM F. Shell 4-Ball Wear 630RPM, 1 Hr., 167F. Steel-on-Steel 4 Kg. 10 Kg. 40 Kg. Almen Load or E.P. Load Torque (4) Rust, ASTM D-665 1.0 hour 24 hours TCP Blend (1) 508 47.80 +15-0 5.376 47.92 -15 0.19 nun. 0.23 nun. 0.70 nun. 14 lbs. 27 lbs. O.K. 6.75 Cellulube 220, S-48 4.77 47.02 -8.1 4.70 46.52 -5 0.28 nun. 0.33 nun. 0.54 mm. (3) 27 lbs.K ' 35 lbs. O.K. 5-5 Notes; ' (1) TCP containing 1.55$ (w) Ucon 75-H-90,000 (2) 12 passes through GM #5226710 Injector operated at 1800 CPM. (3) Average of several runs ranging from 8 lb- load - 16 lb. torque to 50# load - 56# torque. (4) REL - M-400 rating; 10.0 = Perfect DSW 622093 STLCOPCB4096124 2 O tn < PS3I IS g oq PS>i WO &H CO < w A2h PHI CO o < Eh Oo2n S3 W PI P >H O CWO PEhS OS W OH Oh OS EH co S=i" o > o, a PVO 43 CM > PGI Pcd C3 C3 O C3 C"- n n p- to 4r~' 2 O >O o pn 43 vo >5 GP PG G o -p 2O cd P4 cd Q< CQ CO 43 PO Oo > VO nV.ViJ p 43 P >> G G P o o tin * f> bCO p p XI CM os H'--' oE o CO P > <P cd -=! o\ LO bO >i iG-l -P Xl fo 5 o o 03 S m Oo o 43 <0 P fa >H<OH O CM O co c^p- CO m in VO 00 00 co oo C3 o no rH OJ G O o 2 cd u cd Ph 03 N o o a\ rH -=t in =t =? VO t-- LO o co p-=t- co m LO t) p 1p Op H G gp Po <M o O <H o 08 cd rH OS p cd a cd So CO p o CO O <M 03 CM m >m Pi G O Pi Po o 2O O o ^1o in 73 vo c -G GP OG GG o p V 73 aG rOa p bO cd G G --i "0 -P cd cd p 43 O > o po o Go o co > O bO P 70 60 43 G PP P s po P cr\ ai G2 p G V o O P G 43 os ao a o po ca <H G I n 1G3 P c- o <M G 7V3 o o G 2 V to o X) P So P 73 C3 o Oo VOO CM o GG O >R. O XI n nG VO O p p G O -P G cd G G bO 2 O c cG G o a> Pi tH o > to G o O +5 o o Eh cd n u vo G P CO co S i73 cd o G Q, p o 2 < 73 m cd 4) cd n C3 V V CQ vo 43 P v co 43 73 P 73 o P P O X> O O cd G G OP O <M C H o P Ppi si a P * G O O <M co n P P I--I o pI H > 43 E GP OG o =m o P> a o O po <M <p aO oG o rH P rlO > G > G <3 > CO 73 p CO 43 SO 73 --143 V 43 P CO <M G o coI--l p p P <M P a am a -P \p > p oP G an P G oin cd co v co P <C p Eh 2g np G A, <3 DS nm 'O DSW 622094 STLCOPCB4096125 TABLE XIV TRICRESYL PHOSPHATE FORMULATION DEMULSIFIER ADDITIVE STUDY Additive in Tricresyl Phosphate Blend (1) Emulsion Test (FS791-32Q1.3) Fluid Emulsion Layer, cc. Layer, cc. Water Layer, cc. TCP Blend, neat 0 Cellulube 220 (2) Tricresyl Phosphate + 4$ Rohm 39 and Haas HF-825 (2) Neutralized isoamyl octyl acid 39- 5 phosphite (RI-150), 200 ppm. RI-150, 500 ppm. 39 40 RI-150, 0.1# RI-150, 0.2# 41 41 ^ret-o-Lite AD-9, 100 ppm. 40 Tret-o-Lite AD-9, 200 ppm. 41 Tret-o-Lite AD-9, 300 ppm. Tret-o-Lite AD-9, 500 ppm. 43 42 Tret-o-Llte AD-5, 100 ppm. Tret-o-Lite R-25, 100 ppm. 39- 5 0 Tret-o-Lite L-16445, 100 ppm. Dow Corning Fluid 200 (3) Sterox 5 (3) Sterox SE (3) Sterox SK (3) Sterox'CD (3) Sterox 110 (3) Primene 8l-R (3) 41 --- -- ---- -- 3-t-dodecylamine propionoic acid (3) Alkaterge T (Comm. Solv. Corp.)'-'5' -- Isoamyl octyl acid phosphate (3) -- Neutralized isoamyl diiso-octyl acid phosphate (3) _ __ Neutralized isoamyl octyl acid phosphate (3) Fluorochemical FC-75 (MMM) (3) -- Fluorochemical FC-149 (MMM) (3) -- 56 0 0 1 1 2 2 6 2 2 1.5 3 46.5 2 Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Very little Yes Yes 2h 41 40.5 40 39 37 - 37 34 37 35 37-5 37-5 33.5 37 --- ----~ -- -- -- --_ __ _ -- -- (l) Tricresyl phosphate + 1.55# (wt.,) Ucon 75-H-90,000, (2) These fluids alone. (3) One ounce distilled water and one ounce TCP blend with about 100 ppm. additive shaken in a four-ounce bottle as a screening test. DSW 622095 STLCOPCB4096126 TABLE XV SUITABLE* HUMIDITY CABINET RUST INHIBITORS FOR. PYDRAUL 625 BLENDS________________________ Adol 14 ester/dimethylaminopropylimide, 66/34, lot R-677, RI-126** Alkaterge T, Commercial Solvents Corp., RI-148 Dlamyl-phenyl phosphoric acid, RT-53-A, RI-48 Dimer acid, RT-67-A, Emery M-461-R dimer acids, RI-24 Driacin, Universal Oil Products, R-lll Emery dimer acid from tall oil, RI-10 Geigy NPA, Geigy Industrial Chemicals, RI-50 Gulf Agent 178, RI-125 Ionad 17, Shell, RI-121 Isoamyl-octyl acid phosphate, RI-l4g Neutralized isoamyl-octyl acid phosphate, RI-150 Maleic anhydride/sperm oil R.P., CP-30294, RI-151 Maleic anhydride/butyl UFA R.P., CP-30295, RI-152 Maleic anhydride/oleic acid R.P. and 2-ethylhexanol, N-8412, RI-34 Na-Sul BSN, Vanderbilt Co. (barium dinonyl naphthalene sulfonate), RI-128 Nirus N.P., Synthetic Chemicals, Inc., RI-119 Oleyl 2-ethylhexylmaleate, RD-18-588, RI-27 3-(Oleyloxy)propionic acid, RI-96 Paradyne HO 2, RI-123 Santolene C, RI-47 Santolene C, kerosene free, RI-124 Santolene C in Pydraul 150 carrier, RI-156 Santolube 70, RI-49 Santolube 203-C, RI-57 Santolube 333, RI-44 See- footnotes - next page DSW 622096 __ STLCOPCB4096127 TABLE XV (continued) Santolube 536-B, Rl-46 Sarkosyl 0, Geigy Chemical Corp., RI-51 Sodium Petroleum Sulfonate, Freedom Valvoline, RI-45 Tetrapropenylsuccinic anhydrlde/3-amino-l-propanol R.P. 2/1, RI-31 N-8364 Tetrapropenylsuccinic anhydride/l,4-butanediol R.P., N-7794A, RI-54 Tetrapropenylsuccinic anhydride/butyrolactone/water R.P., l/l/l, N-8366, Rl-33 Tetrapropenylsuccinic anhydride/castor oil R.P , 3/1, RI-30 TPSA/2,5-dl-tert-amylhydroquinone, 2/1, N-8413, RI-35 TPSA/Duomeen T R.P., 2/1, RI-32 N-8365 TPSA/glycerine R.P., 2/l, N-8415, RI-37 TPSA/N-methyl pyrrolidine/water R.P., N-7796, RI-56 TPSA/2-methyl, 2,4-pentanediol R.P., N-7797, RI-52 TPSA/1,3-propanediol, 2/1, N-8414, Rl-36 TPSA/triethanolamine R.P., 3/1, N-8087, RI-29 1-(triisobutenyl)diethylenetriamine, CP-12992, RI-131 x Providing more than 50 hours rust protection, xx RI numbers are REL code numbers. DSW 622097 STLCOPCB4096128 TABLE XVI UNSUITABLE51 HUMIDITY CABINET RUST INHIBITORS _______________FOR PYDRAUL 625 BLENDS Acridine, RI-15 Adol 14 ester/dimethylaminopropylimide 7^/26, RI-lSl** Adol 14 ester/dimethylaminopropylimide 82/l8, RI-162 Adol 14 ester/dimethylaminopropylimide 91/9, RI-165 Alox 1724, Alox Corporation, RI-165 Amine ODT, Rohm and Haas, RI-89 Amine 9D-178, Rohm and Haas, RI-25 Ammonium oleate, RI-87 Ammonium Stearate, RI-86 Ar-dodecylphenyl melamine, RI-114 Armeen l60, RI-26 Armeen 2C, RI-94 Armeen 2C/di-tert.-butyl-p-cresol 50/50, RI-100 Armeen DM-18, RI-101 Armeen DMS, RI-90 Benzal SD, RI-65 Benzoic Acid, RI-78 Bis(1-2 phenylmercapto)ethane, RI-l6 Calcium Petroleum Sulfonate, "Synfonate 28", RI-45 Chlorinated propylene polymer "B" and diethylenetriamine reaction product, CP-15021, RI-132 Chlorinated propylene polymer "B" and ethylenediamine reaction product, CP-15552, RI-155 Cyclohexylamlne, RI-79 C. yc,lohexyl melamine, RI-115 DSW 622098 Cyclohexylmethylamine, RI-127 STLCOPCB4096129 TABLE XVI (contInued) UNSUITABLE34 HUMIDITY CABINET RUST INHIBITORS FOR PYDRAUL 625 BLENDS Dibenzyl disulfide, RI-70 Dicyclohexylamine, RI-80 1,7-Didodecec.enyldiethylenetriamine, CP-12685, RI-150 Di-2-ethylhexylamine, RI-97 Dihexyldithiophosphoric acid and cyclohexylamine salt, RI-115 Dihydroabietyl malate, RT-52A, RI-28 2,2'-Dipyridylamine, RI-14 2,6-Di-tert.-butyl-4-methyl phenol. Shell Ionol, RI-59 Dodecoxyguanamine, RI-116 Dodecylamine, RI-91 Duomeen C, RI-92 Duomeen T, RI-93 Ethylene bis(tolyl sulfide), RI-58 Ferroscene, RI-7 Drew FOT-W, Drew and Co., RI-120 F.O.A., No. 7, DuPont, RI-110 Hexydecyl Ketene dimer, RI-88 Hydroxyphenyl stearic acid, RI-40 Kleery concentrate. Synthetic Chemicals Inc., RI-118 Maleic anhydride/safflower oil reaction product, l/l, CP-50298, RI-155 Maleic anhydride/soybean oil R.P., l/l, CP-50296, RI-153 Maleic anhydride/soybean oil R.P., 1/5.5, CP-50297, RI-154 Maleic anhydride/triethyl phosphite R.P., CP-14569, RI-141 Menthane diamine, RI-122 2-Mercapto BenzothiazoleRI-5 DSW 622099 STLCOPCB4096130 TABLE XVI (continued) UNSUITABLE* HUMIDITY CABINET RUST INHIBITORS __________ FOR PYDRAUL 625 BLENDS Mulsor No. 3CW, Synthetic Chemicals, Inc., RI-117 Nalcamine G13, National Aluminate Corp., RI-12 Nalco SR-155, RI-104 Nalco SR-158, RI-109 Nalco 158-D, RI-106 Nalco 301, RI-107 N(anilinomethyl)succinimide, CP-13812, RI-140 N-dodecenylethylenediamine, CP-13045, RI-133 Nicotinic Acid diethylamide, RI-18 Nicotinic Acid Hexyl ester, RI-19 N,N-'-di-2-naphthyl--phenylenedlamine, RI-1 N,N'-diphenylbenzidine, RI-17 N,N'--phenylene-bis-acetamide, RI-8 N,N'(1,1,3,3-tetramethylbutylimino)dimethylene diphthalimide, CP-13891, RI-139 N-(l-tert-butyl-2-methylallyl)ethylenediamine, CP-11666, RI-129 N-triisobutenylethylenediamlne, CP-13530, RI-134 o-Aminodiphenyl, RI-15 Oxodecyl EMA Methylimide, 85/15, lot R-577, RI-157 Oxodecyl EMA ester-imide, 15/15, lot R-580, RI-15.8 Oxodecyl EMA ester-imide, 90/10, lot R-581, RI-159 Oxotridecyl EMA ester-imide, 65/35, lot R-582, RI-160 -Aminodiphenylamine, RI-11 Phenothiazine, RI-2 Phenyl-alpha-Naphthylamine, RI-3 DSW 622100 STLCOPCB4096131 TABLE XVI (continued) UNSUITABLE* HUMIDITY CABINET RUST INHIBITORS __ ____________ FOR PYDRAUL 62,5 BLENDS __________ Phenyl glycidyl ether, RI-22 Phenyl mercapto benzothiazale, RI-4 Phenyl Selenide, RI-6 p,p'-dioctyl diphenylamine, RI-9 jc-Phenoxyaniline, CP-14544, RI-142 Prlmene 8l-R, Rohm and Haas, RI-64 RD-1944-P, Armour Chemical Dlv., RI-102 ~ RD-2237-P> Armour Chemical Div., RI-98 RD-2322-P, Armour Chemical Div., RI-99 Santolene HLV, RI-42 Santolene J, RI-41 Santolube 394-C, Rl-23 Stearamide, RI-20 Stearanilide, RI-21 , 1(l-tert-butyl-2-methylallyl)tetraethylenepentamine, CP-15536, RI-157 1(l-tert-butyl-2-methylallyl)trlethylenetetramine, CP-13535* RI-136 5-tert-dodecylamino-propionic acid, RI-95 Tenameen 21, RI-108 Tenameen 22, RI-109 Triethylenetetramine/linoleic acid R.P., CP-15593-(2), RI-147 Triethylenetetramine/nonanolc acid R.P., CP-15592-(2), RI-146 Triethylenetetramine/stearic acid R.P., CP-15587-(2), RI-145 Triphenyl phosphite, RI-60 Unicor, Universal Oil Products, RI-103 DSW 622101 STLCOPCB4096132 TABLE XVI (continued) UNSUITABLE34 HUMIDITY CABINET RUST INHIBITORS FOR PYDRAUL 625 BLENDS _______________________ Universal Oil Products 176-5, RI-112 Vegetable Oleic acid monoglycerides. Distilled Products Industries, RI-85 x Providing less than 50 hours rust protection, xx RI numbers are REL code numbers. DSW 622102 STLCOPCB4096133 TABLE XVTI uu cd <d 0) 41 i--I rH rH r-1 OOOO 50 TJ 41 bO 3 HI 50 73 TJ CO P 5 41 0) il 1) O Mfn M o m o 6 ih T3 cd *o H A flj rH O rH P 4) 3 tO 4) *--I H r( se I > 10 O W ^g PP fn x x fT' cd bO bO cd ^ Fh <U *H tH 4) Fl-*t 3 rl H rl O CO 01 (d O 0) 4) 4> tOo *t0oTtJo O tl p pp to to HHHtltJ'd 09 03 co to P 3 F< OHHaj 0 CQ W D o 0) 09 03 oUh^OU ^ ^OO U U U > 41 4) <d td cd p o o 4) 4) 0) 03 cd flj H H H 0 Fn M O O O Eh E- 4) x F< 4) P p 0 73 a tGHo .O* p 4J p P xx x x 41 .M 01 c, t, . , C cd Fh U 4> P 50 50 tO 50 cd o cd cd cd ^ p H hH *rH *H 41 41 41 4) 4) Xt al UPUU mcq H CH OHO 0rH0(--*I 0(d I) 01 <d P Pj P *H acr 09 rH G 09 rH o *V 01 Vl >s Oft 4) rH *0 33Ft F* F* rH cd 41 cd 4) Cd 41 rH rH ^ 73 X P *0 *a rH H rH 0 rH OOOp r-H rH rH CO P CO CO Xto rH F m F* 41 >rl cd 4) X u o G 4h P >41 cd rH u c>d T3 a co O G\ 2G 2 H rl tO U) 09 CO 03 P PP O oo pp oo ft ft to CO 03 G rH PPP oft 4) O X p 0 pp g g CO ft ft ft CO 03 CO 41 03 CQ CO -H fl E Etj ^ g g xx to tox x h -h a o O CO a, to U) P p 'O o to .x UfJt UP o to 3 CO 03 U V p p cd cd C0 (0 41 41 ggr OrOrt ** ,ggg 03 rH Poa, Po s ft cd 0 cd ftp p p OQ Fi Fh Ft COXOX 41 41 4) to ft U) 5>>C-4-H01rH 41 'p P 0 O F< Vi HH 3 0 rl 41 41 41 4) 41 4'1 4'1 4`) 41 'I FU* U CO CO Vl h CO CO (0 KN"ffl r i m 41 n3 > CQ lAlAlTUA rH rH rH rH in inrHrH rHlAin rH rH m K\ inmvovo KN 41 4^ 41 41 vo vo \o\o .=t Fh XaI 4) at P td 5 CO Cd to 8h to Tt>J fn'SL^Sl.m _u X3 XO O 41 (0 X to H 41 CO CO CM X cd ft 4) 41 40 ft ft CO 5 to Fh P FVffl X O Cd P O rH C cd O O - CX s rH ft ft ftX Fh cd ft "gss r O CO ^ U r-i rH 4) -a% xPJ'SCOOCSOt *a O U T0 f>> t0 rH O 41 CO Cd 41 TO 'Orl'O a U o Q) U X rH>R.TR. 41 O 41 co at minx cd x aj U CM CM w m 9 p cd o cd 03 O O rH * O < pp o M T3 O P < T3 41 tH (0 41 Fh T3 73 X U 41 X X X p cd U p p P p 4) 4) 4) cd Ft rl rl rl P P P 4>3cdea<d CO 5 41 n\R>R 41 X Cd rH r-1 > m3 . rH C O O H P + + CO * fn rH rH CM rH rH 41 1 I I rH >rH Oj) ft rH r-H rHOj) Cap CO rH V) CO C0COXCO rH CO CO O T3 cd J cd O ftO a o o 4) CO O*--N 0-. Ph < < < < Oh Ph <C <3j P-t Pk 41 O C Xl Fh 41 P cd X rH ? ? o co* Fh O X p 73 41 rH X X P X 41 'c p s rH Fh 41 P G 41 C 41 to co O 41 cm m <iii rH CM ii CM CM tn^t r-H cm *n -Lilli cm cm mmm i mi voi rHi mi .=ir mi voi m i^r^4-4-4-4-4- DSW 622103 STLCOPCB4096134 TABLE X V III B o ll! P o in t P . tco * -=i- o o o co <T\ in o\ o CM O VO so o mo i fa-fa- i in P CTi CM CM OVO rH 1 o o a i fa- aj h- coco p nvo i p p p i m rH o o o rH o\ rH o sVO vo m O1 1 1 1 1 1 1 1 1 O1 S- 1 1 1 1 1 1 ( I 1 I 1 1 i 1 1 1 1 Pour P o in t, F. mi 5 ins v s 3 3avo\m s- i i kmao m cm sms 1 1 1 1 1 1 + i + i +++ 3 1 1 1 1 i fa- l l vo i 1 i 1 i in mm rH . fa-S-fa- o o Paj o o o e +5 5tdh CD O 4) 64gh1 Po td O O mr--I ion iI VcOo Km\ I cAo + I II + -=J- +CM 1 ip I KNO CM I CM O i m i o j* CM I in CM + I II !P till IIII fa 55a o O ll II CM O t--. IiiI lI lI lI lI lI lI iI o i--t CM i--I 03 O fa- ofa m .st- fa 4rlO\K\ C0 CM CO VO CM in s- mom^i-vo mmo avov cm m CM m CO . s-mcMco 1 1K\ fa-m m s- cm rH cm cm co oo-=r ovm co m vo 14OOH rH rH rH rH CM CM CM m VO CM co CM O m CM m oo ON CM fa-VO rH rH -=MO vo S-CO -=* CM O co o H fa- O ! ! ! i i s-mmav CM m h fa"-sj" rH H H f--CO m fa-CO H rH VO VQ VO CM mCM fa- CM vO m 00 VO s-a\mo\CM mcrv vo rH fa-00 OS =t rH -=r st mm^ i i i i i i fa-OV 1 fa- 1 i mfa-fa-fa- g73H 1 i1 iiii i i iiiii CO CO co CO CO co co CO 11111 111i1 co CO CO CO CO CO co o c 4) CI N4) ou o 4) 4) C Pi o C 4) n fa td 41 43 O (h td 3 . 03 &P 4J td 4) 0) X o c <H U3 --43 4) fa <0 rH H 43 rH fa farH Hafa. P4IJ TH3 4P43J r(--^p.4<3U. C0fa3 Xo 43 (MH ' fa r0-l rstf E43 rH p, K td Hi Oo-, K.f.a..K.o..\...fk.a..;43 f.a. * fa 3 43 I Cl OI 8.O 4) 4) co in c c fa- I o o I fa o o 1-3 VOVO Sic 4) i 4) H H I 4) C fH P H fa U P|Nhrirl 043 )H 3 O W fa pCOi-iC H.=r fa- 3 4) 3 faO O W4-H n 43 r-H C44 O ShVO a t* 41 I 4) C 1-1 P l P.43 fa43'D4>faKXC I XJ 0,<h O O td 4) rH rH fa C P K >COCO l mi ooocC(d(d(o 03 -m rH '--rH <d 0,4) S SCO Si n m * O o H .C O O OI 10 4) O pJrH h o O O fa l I rH H iH .O rH fa 4) faf-in O, P 4-3 (--< rH I O P O fa r-l *H C C fa CU-v farH H (d rl c fa43 td CTj P _r,m O fa fa r-l fa a; Q,rH co co 3 BH 4l.CJ3cd43J30fa > Vfap+J^u 0,0 &TJ rH I rf-al cO i rH I fa rH p td Q. fa TJ N O 43 i--l O p Sh p rH *> fa m p p p <d C I-H 1-1 t) t) O O - 4) fa 4) 4) 4> H 43 C rH rH rH rH S O, 4) H W W W 4) O|OO4)4)P0)MaO<Dfafa 4) fa fa <d U P I O .c O 43 i-Hfao-HPrttdaJO^-'KN'O 6B43EO)OOPftO i tHtH i Q, i p V) an) O (d P M P *H O, 4) rH Ch O (d td n P rlrlrIt) 'OC^QQh Oh I -H O r-l O -H O H H W +) Ch3 HHQ 0) fi fi ^ h 4)0 I I-- W --' l;|0 -W fa Q,p .=*- fa P I I i l 043 i ndi 4) O O X--'r~i CM W rH (/I CHXJO0 I 43 fn C|C0 SZf<U4CCCC3 rH > -H X rH CM ff) iH * O <H P (0 4) GQ P 4) I CQOI^OWMChH W EH CM cm cm Elofcnto'S 5 S fa 4U) 3 fUd V g 4) 03 fd rH > 4) 43 *o 4) 03 P rH (d td 6p H 0) X iS DSW 622104 STLCOPCB4096135 TABLE X IX Pew Few +12. Few Few a 0) A3 3c o Oz CQ c M Q> 4) 4> CCC ooO zzz i% l 4fa> tftj p d4l *H U) b( 3 H C rH 0) fld O >9 P o <o ed p vo o 00 o OJ o + 1+ VO H in in o o m cm O 1 1 1 m o o m cn o o O 1 t > + ++++ i+ 1 C\ VO CM rn i VO CM 1 1O + -=r m K\ VO m rH ++ CT\ m rH + CM O CM m o\ rH o o VO P- o K\ rH brH 8 GO rH o rH CM o rH O jn VO VO rH + + + +++ ++++ m in o cm m ii oo rH CM Oo CM rH VO in in mOoo o brH- rH O O o OoooooOooo CM rH 00 b- rH r-i CT\ O CM b- fa o c^o m b+ + ? vo in vo vo co in o Ov m in in 0\ -=j- in oo o VO CM rH i-iinoj-sj* in vo in m + + + ++ + + + rH rH CM kco ka\ VT K vo CT\ H+ K\ rH e cd K\ CM CM CM O CM in K CO ov CM 1* m O rH p wH c H rH VO VO* CM Jd' rH VO & b- CrHO CM rH O 00 O r-1 b- CO rH m b- o b- 00 m CM b- CM =t CrHO in vo P H cd W a in CO Jd* rH I1 co CO VO l CO b-=f OV in in ON m CM liii1 1 1 1 1 1 1 1 1 1 1 ii CO CO co CO CO in o\ bi- o\ I CO CO 1 1 4> C (0 4 4> O N Pi a> faC *3 p a> cd o o a> I& 0) P cd Pi o3 o c Xa3> e0) 4> s: rfHa 3 cd JC fa a> P (0 5 fa ISrPfal. X3 P S p x: 4i) CM p b p PH fa l?1? s rH & C 4) fa fa PC Pi 4> fa a> c faaI Si o o^-- so: TJ QJ x: C .a fam rH O rH c O cd 4> x: so fa a fai u P a pc fa farH flj fa fa fa*m o farH 0rH 0) x: (0 s: C 0) PH cd o CO pH OIO *3 O p a p x: 0) P p <l) j: ai 3 cl. \4> O TJ a p Q B s: a, wrH Oto j 0) p Pfai o ao ufa 3 0) p cd faO rH K'--' CM W P E| x: p Oi W PQ Ol w 0> 4> c c1 cd 0) c o 4i 031 PH 3 P I o I C| *3 ii 2i z i VO vO li 0 p 1 Si I o Pi o 3 rH U Pi P PH P 3 X) rH N & pH cd P tH 3 Pi FQ p P Pi Clio t CM Cl *3 il zz II OJ CM * EOh El fa p co 0 301 iH > fri o O rH CM X DSW 622105 STLCOPCB4096136 TABLE XXX (c o n tin u e Few +i Id e n tity No. a 4> rH 4) 4) 4) GGG O- O O rH z Z z o CQ c p a p <u P3 -WH) MG rH 0) (d aS js- h- -=t ooo III I I I p a o Eh < P >RJ p wH SoO o a > o O o p I p>> PO GZ 4> a I l rH OJ rH on OJ smt rH + oi oi oi rH ON k\ in K\ rH to O o o OJ 1 !P V ' I I OJ t-- H t-- KN m ON rH 1 l rH t*- ON st m t*- c- h- I OJ 11J l < ( CO CO CO CO CO cd p rH 4) 4) 35 4) CO rH O orH OoJ O oo + ++ rH O roH OJ o OoJ rH o Ooooo +i 11 G 4) m OJ on in OJ o rH o rH O OoJ o aOot o o o O o O o o o iii 1 11 in -=f rH st i 11 CO CO CO f- ON in ON Ol st in K\ St 11 1 CO CO CO CO CO 4> Co o g 4> P 8 4) 4) IO P G 4) I 3 4) G P 4> aN rH G 4) cP O o t"- rH o t- m 0 G O G 8 1 O a> rH c*- in i oo OJ rH Eh O P O f> in g p co 4) 4) PG rH ao, 4> P o w go o p rH 4) 2 p H-3 4) o& G ol m CO 5 5 3 o G 4) O P s a) aoj KP 4) 4) P CO > pr-v p r- 4> rH P a 3 P a &? <D Oi 4) POO--' P O rH O 4) OP rH fd PrH P cd P pP 4> p E* Pa P 4) S e V --rH- -O- p I CQ H El rH oj CQ <q o| iC P DSW 622106 STLCOPCB4096137 u fA H CJ rH cm 4) O > ooo o H oooooo CO , 111 Ch LA rH CT\ 11 in -=t Oi i i cm rH CM o OO l oooo 1 1+ + TABLE X II (c o n tin u e DSW 622107 STLCOPCB4096138 4) .a ss 6h in in m cm j* f- rH ri rH < o j^O H(o0i OJ ON in f- O K"N CM i o vto*- 4* rH H on vo vo odd o rH -3* TJ a *o 4) 4) 4> .=* in -=t MNN o ON in CM P H rl 43 41 4) rH o rH rH rH a <a 03 KN VO VO CT\ o\ r*- m in o rH o TABLE 50 .2 1 4) c N4) o p 43 & sC0> a P00 X> x: O s<0 cdt>O c<D O 4) a3 a> 5 X! XS rH O3 4) p 03 K rH 3 HP, P tH X5 x; 4I) T3 ,, 4-> 4> c*- 4) G XJ CM rH B rH s 4) P 0) a i rH Jd- x: *DH a Ok f?KN 4) I & a >> c < P, X3 A 4) oo TJ X3 rH **--' ca O O <0 Pi-' e'h --ol'!f$A n a, X4) --O' *> o 4> *0 0 T3 P Q 1 >i 43 OP > o t>> rfH^rH(d >* JC (0 P JC xp: 4) P a jc a 4) a rH O --' W 03 p * a uo & a o 4) I el PP .. PQ o| O je o CO i o c TJ rul 4) a a vol o C G 4) 4) xi: O rl > OI 4) 4) p X33 o Cl l sr TI3 >> >* P C c 4) al x; a Cl P00 03 o xs iO c E: C (d P rH N Wrt pm3i ppki CM i- >> rH ao p xJ>:> p a 4) Cl | T3i O O CM c P a m DSW 622108 cI |co CM CM CM STLCOPCB4096139 0) & au3 Dm o w c 4) e rH o < a) ,Q O h! J< fOCi\ Ii Ii Ii Il Ii II Il i in i i i i i i I rH I I I II I I f? O VO rH in o Pm o O O -=*- i o in in in oo H m VO VO in vo o r- oooo l -=rHt o m O 0Pm vto- m vo m m rH t- h- CVJ ViOn .=t**-- 00 o l<\ Ho2 rH o o O o o o o OJ o fc o o\ rH K\ <M t*- KN i i cvj aj m k\ u VO i i 0) rH o oooo & APh Si 4>P o C2 vroi- i i CO ii rH m i CO ov i t1- c1- 1t -SjC\1J CO CO CO CO CO TJ TABLE XX (c o n tin u e DSW 622109 STLCOPCB4096140 TABLE X X I F lu id Id e n tit; No. o rH T3 P -H *3 Pi rH *0 Peh > lA KN 0> P0) 3X) *"3 -} 0) 0) i--i <u P P. Cd P OP H Cd r-I Pi A Q) Si <D Eh a *H rH TJ 3 -H Cd 3 Pi rH T3 > 32 <D *P0-s> iO-72 o o oo oo oo t' t'-- VO VO o o VO o o VO oo in o o in o oo o o o o o o o o 0 CO 1 VO VO VO vo r- o o o o oo o o o o oo vo in m in in tl oo vo oo CC do Ho P 00 cd O T3 Pi rH Pi Xo oo a o p. aa> OJ 04 CM CM Ph Ph Ph 01 Pi 01 01 e> a a 0011 CVJ CM CM 01Pi 01 -m=ti* ian 1 v.=oi* vaO l cO a a a h=t-r a *r*i- a -O=jvi OV =ii- CO rH1 cn mi C=Mij- in ini a a a a a aaa in vo t*t- i^i aa < VKO\ CM ON 4 S POi a * o o o p CO o c0ND) C0) a> c K0 id M c0) cd H o p T3 }> 42 ctf cX t4 Qi N XI cd iH cd p <D N cd p 0) Pi p p K XHa2 P 0 J> c 0) P(D 4021 e1 >. X in r p 0 c o> f>> 42 & 01 Pi V*. a in X P <D E rH <U 42 sz > p*> p 42 42 op OP c C 0) <u 0) 42 42 > C 0> 42 a aa > Vi. VL in in T3c <u > O X c rH a 0) Ox t>> <U a rH 0i . Pl o a OP a o rH <3 o oa o ?> >* c Eh r^rH Eh t> a El 42 cd 42 QJ >R P 42 >R \R T3 Ol in m <U .p in E 42 in TO3 a oPi a o <U 42 & a rH O S rta> vo v-. (A ov -=f CO iH -=t- el g CO CM- CO (Q aa <D Co a 0 p 1 El i o Pi o p Pi p I i * >* rH 0 a 1 El DSW 622110 Pi Pi TJ O -H o o cd o a ao iii STLCOPCB4096141 0,096 0.193 O.296 2.35 15-4 PH-8 7 ( 1 ) , 1 .0 % PGE, h ig h a c id A o r y lo id 1 . 6l TAN In itia l F in a l 11 .2 2 CXJ rH t- CM K\ CO OO in 1<\ in m rH *=t 0 00 CM CO rH m oc =t 0 CD rH 00 0 0 in m in OC O 0 co K\ m -=f CM -=t* c^0 d d O 0 0 *H m CO in CM 1--1 in d rH co d m rH V > 'O O CM t'- i-1 0 K\ O rH m 0 CTC O cr\ 0 0 0 m t- tm CVi m CM CM .rH . 0 tn c-~ CM O cr\ o\ 0 CM 00 CT\ CM 0 CTi CTC O CM OO CrH 0 0 CM m < d O d d 0 0 d 0d O 0 0 0 Od 0 0 <D E T3 col 0 0 g\ M Eh M s < a H M0 H0 X Eh X CO ww CO < <m Eh Pi m O cd p P < i-H cd p3 <u O O O uT\ O K g CO TJ n-i 3 i-H Pc C'- m tO -=t* m O O0 00 -=t c-~ rH 0 =t CM CM in CM 0O oc in -=j" 0O CT\ 0 in t'~00 C- 0 0 0 d 0 0 0 1--1 0 0 m 0 d d d 0 0 0 00 -=f rH 0 CM in CM m CM CO in 0 0 rH 0 x- =t =t in cr\ CJC -=f CM 00 CM CM co f0 CO O O 0 0 0 in 0 0 d 0 d 0 d d 0 CO d 0 d 0 d CM 0 OJ 1--1 CO CM m rH oc -=t K\ oc 0 in o\ 00 m0 1--1 rH rH rH 0 m iH C- CTC -=$~ =t rH CM C- CO CM in d d d 0 0 d co CO =t rH rH m d co m CO cd CM rH in O 00 CM m -w 0 Ph Aa (0 9) Up aa m m y--s >--s * >R O 1--1 > P cd cd rH rH rH iH rH 1 X Pci aa u aa V CM CM m1--1 m rH cd cd ON m -=t P P w1 0 0 CM CO cd H O rH aa > i CM 1 ---v *--s rH -p -p rH m CM rH od OW* .W 0 H cd a 0 rH Pc a r--v r--^ N rH r--s ---s co VO CO >R >R od <=t CM =t rH rH CM in 0 u\ 0 --- 11 H in in in 0 1--1 O O0OO OO a Qi 1 rH O0O OO O r>> > ---S ^--s in in in in in in P rH rH "-- -- '----* '-- fn --" a H iH rH rH rH rH rH CM 1 K * a a. rH r--^ rH rH --- '-- '-- 0 0 0 0 0 0 in in in in in p >H p u p u m m m m m C- C- b- P- 0 TJ T3 a a TJ rH r--1 rH rH rH 00 00 co 00 CO co > > > > >* > 1 pi co X CO Pi CO PJ 00 X CO Pi 00 a Pc | a Pc, | a Pc, 1 a Pc 1 a Pc 1 a a 1 a 1 a a 1 g 1 a Pc 1 a Pc 4C-Q> * a) 0 Eh 2 mt COI 0 t--1 \1 ON 0 in CM 11 0 CD rH 1 m \ CM1 CM 1 tn 1 =t in ON 0 rH rH 11 in 00 CM 1 0 in| in co in1 m in 10 rH rH rH CM CM rH rH rH rH CM rH rH CM rH rH rH DSW 622111 STLCOPCB4096142 TABLE X X III (c o n tin u e d ) SKYDROL 5 0 0 , BASE STOCKS, ADDITIVE, a) 2d < E-i Ph >> -rpI o cd o < vo CVI o =t CVI O w <u CO o6 OTO o baO o 2bO <d -p -p < d 3 <PU o 2 i--i o o in oo <M mCM rHI a to 'O tH 3 in aj oc -p 09 (U O Eh 2 e iH O '--*H P in o, md rH O I CQ a t3 to d I vo o OtH cd 2O TOH3 >u o <t 93 cm k\ DSW 622112 STLCOPCB4096143 TABLE X X I\ (continued - - next page rH fa cd < Eh crH > p pH H X) crHd tH H-5 o rH < Hc CM-et-VO mo c- i 1 rH LO "-- crH--^^t-vCoM 1 CM.C.M .CM 11 OOO me00 CM mo oo ino NoinH4- m^joo cm vo oo moovo ooo cm o m oo oooooo o OV00 O rH CM O oo crHo cHm crHm KinV cCmM iCnM cH-- ooooooo oooooooo o CM O 00 00 vo oo oo K\ COMn o iCnrH o CwO &a<> \ X3 CoMv0in0 VoO\o rH C- rH in mo 0o0 c-in^m mh mh m CCMM m c-- o oooo o O o o * * * > O O rH o O oo o + o o o o o o o o o o o O Q< 41! o 60 2 o co mvo ovo CM t'CM O CM O Uo"\\ mrH oo CM t-- b-- com mo mo t-- VinO m o . ofa pcd p OX-CMO o o o o o o o o o o o o o o rH + M< CO H 2 O pcd o2 rH m m vo m vo m .=rvo moo CM rH m^too mox-x-HOm O rH O O rH rH cm VmO mCM co o vo CCTMV fa o> Oh 2 0H4-0 o o o o o o o o o o o o o o fa o M E<h fa Ofa wfa > ! CH cP C -H tH H P P Xe! PH > X si rH p O CM VOI VOI p i--i a iH >i--l >>P t p p i cd p p cd i oo X! X! a> pq m CM CM VOI VOt OQ cd OQ p cd O O fcad fcad X X x> rH rH G c a a cd cd Xi o oin o fa in mi--i i fa fa C2 <D P c si a cd p pa pp <d a> fn pp p CM & O a w <--l i--l i--l OJ i--l P CM rH S> iX X! O a Si w rH Si -H rH rH aa Cd p uCd s cd cd p Jh P cd fcad foaa po cd cd rH -4" cm ai fa fa rH OQ OQ cd ^ m cd cd >R. OQ to p cd cd in cd cd X! X! fa tri cd ed m rH 4) O o fa CM O u f9a) O O m id 1 P fa fa o >> a a-a t3 CM CM o cd IIICO * *>p| > CM CM CM fa CM mmm m HHHPH i i iGi 4> I CM cu m r-H f> i XJ C cd T3 C cd X! o pc2q cd ou cd C cd C cd ^joqoq!! *VO CM I mo IX 'VO CM I mo a> iX!o *o rH O T3 < KfaSfa5f3a f0a Kfap >R\R>R2Q\Rhcd XO! ffaa P a cd W>RrH X!2200fafap o o w QOf M^ ^MfafafarlfaQrliP^ fafaWW<< >R>R>R cd>Rcd O in in in in.H in rH inmin p in p *>R. cd cd >R>R>R>R.'SR'eR. cd cd >R > O O O rH O P rH O P HHHHHHOOOfaOfaCMd t'- 00 I fa oto i fa fa fa T3 ! U uo < o .3- .=*- m^t- mm mmmmmmmmm m m < VO vo CM I min in in oo XJ rl O cd CM P CM CM CM CM CM CM CM CM CM CM CM W) rH fa P OQ ID O Eh 55 mi voi c-i.=ti- mi vo vo vo r--c vo rH rH rH CM rH mii-=r ovo\ HH mi ^i- mi vio ci ^cio hi cim mi in in tn m m in t~-1--c^- CMOJCMCMCMCMCMCMCM -i=* rHi c-- co CM CM cm m DSW 622113 STLCOPCB4096144 CO Q Q< O 2 H T<3U CHO tGGH O PS -P Oh Co o O H > Eh < s i-S g <& Eh PS o o LTV i-3 o 00 is < Eh -^rpH H O < bC si o h0 cd -P -<P cd -p 0) CM rH mcMco O 00 --1 CM i--l O ov o o o rH o o o o C- OhN m m H CM rH rH --i o o o o o ooo CM o hON CM m o mo O o ooo o o ooo -=* c-=f m oo fo o o o ooo rH =t in in rH o p- OV o\00 ooo o oo m m rH 1 PS b G H > g <o -P CD 4) O Eh 55 a) rH + p. Q, u G cm G G VO PL, Pl, i e C3 H u GX .G a> ss I--0)I -p -P v > & cd PS G T) cd + + PL, b H O o CD o o cd m m cd oco PS rH m o ftH4- G O o cGd J3 p JS -p c isS G P* G f* o _ OGOGPS.GWW CM S*J CVJ W rH ffi rH (H r<> r<"V r<>Kv '-- s-^-/ s * s ,r--> ----- CM CM CVJ CVJ CVJ 1 ' s--^' CM K\ rH KW 1 1 1 11 00 00 ov ovo\ CM CVJ CVJ CM CM G tH O cd 5 O G << VO CM m i in in oo CM rH cm m DSW 622114 STLCOPCB4096145 TABLE XXV SKYDROL 500 REFORMULATION, POOR ADDITIVES IN FH-135 Test Number 16-2 16-4 16-8 19-6 20-6 20-7 20-8 21-1 21-2 21-3 21-5 21-6 23-1 23-2 23-3 23-4 23-5 23-7 23-8 24-1 24-2 24-3 24-5 26-1 26-2 26-3 26-4 26-5 26-6 27-5 27-6 28-6 Additive In FH-135 0.5$ FH-132; 1$ Dlpentene Oxide 0.5$ FH-132, 1$ 1,2-Epoxy ethylbenzene 0.5# FH-132, 1$ Dibutyl tin Maleate 1$ Nacalmine G-13 1$ Mannlch Base (SL-13562) 1# Mannlch Base (SL-1353) 1$ Succinic Acid Amine Ester (SL-13561) 1$ Dlbutyl Tin Dilamate 1$ Morpholine 1$ Ethyl Silicate ' 1$ Kontrol 147 1$ Thermolate 31 1$ Kontrol 77 1$ Amberlite LA-1 1$ Amberlite LA-2 1$ 1-o-Tolylblguanide 1$ Butasan 0.5# FH-132, 1$ Benzal SD 1$ Tin Diethyldithiocarbonate (not very soluble) 0.5# FH-132, 1* PL-297 0.5$ FH-132, 1# R-677 0.5$ FH-132, 0.4$ Ferrocene 0.5$ FH-132, 1$ Sarbosyl 0 1$ Citric Acid 1$ N-Coco Morpholine 1$ Dibutyl Fumarate 1$ Dlbutyl Maleate 1$ Hydroxyquinaldlne 1$ Tartaric Acid 1$ Methyl Salicylate 1$<*.-Methyl tetra Hydrofurane 1$ Hexamethyl phosphianide DSW 622115 STLCOPCB4096146 V bO cd <z ox: Eh p o + -=t o o o <m o o 10- -=*" m CTv o o\ m m ^=t CM a\ CM m m 00 o VO rH i--1 rd rH b- CM b- mm rH + + + + + + + + + i+ + bo rH av m VO mm x x CM -=f xo CM o VO i--1 rH m i--1 b- rd t m co m in CM oo m rd i--1 m -=J" oo mm oo rH o crv in m r-l o o m CVJ oo o o o o o o oo o o o o t- o rH o b- o VO -=t o VO o ih co in rH O o ov CVJ oo CVJ o o o o m o o oo 6 o o o p 03 > rH o o CM rH o m rH oo in o o o o o o o oo o o o o CO 03 o o\ rH vo m t- OV CM in in in in b- m o\ ON VO -=$* b- m vo P r'l co cd > p rH cd cd o p cod p3 o p x: o o VO rH =t VO m rH VO 4K-V in rH vmo b^- rd rH rH in &o X! PP *rl *H ss v Z bO S cd CM O o rH o CM CM o CTV CM oo co O O mo o o vo rH CM CM rH d O KN o o CM O rH o o o rH 03 03 Cc oo pp pQJ S CO ty p ic a l PH CM CM oo CM CM CM -4" Oo CVJ o o o O o o O oo o o o o '--rH m b- r---S i-1 S ,--s ^--s N, 00 -=f ON 4 VO CM * ' '' rH T3 mP VO vo VO vo 1 1 CM 1 CM 1 in in in in +0 p Oo iC v4 co b- cd "-V ON VO P 4" i p rH rH CM CM & a .a .a OJ T3 oo 4-> p p rH o o cd tH H H rH rH rH co cm m o rH o rH > > pp oo << T3 a s b-4" b- bX- b4- H o H VO o rH vo CM 1 s ^ ' t-- O rH rH brH b1--1 bt--l rH 1--l 1 1 t~- b- 1 1 1 1 oo oo i f>> in in x- -=f w P O po rH CM b- brH rH .X in in <E < a 1 1 CM X rH CM rH CM rH CM i--l rH r-1 oo in in p n>i X 00 P'--' a rH X>'-- CO m rH I EC &H m i--i 1 EC Pc b oo 1 EC Pt, c- 00 1 EC Pc b- b- oo oo *i EC W fe b b~ co i EC t, b- b- b 001 00 1 oo t EC EC lx, h a XJ VO CmMI o o 03 Oo 03 CVJ (0 a> o 03 ao> oo <p p p. p a. o a T3 a) cd 03 DO fo-i op. o p, ps. o P o p p P, p. CQ 03 03 cd cd T3 cd EC cd EC a) oa o a C cd cd obo i EC Pc o os o X cm m DSW 622116 STLCOPCB4096147 56. Procedures and test results for these fluids appear in the Appendix. B. Synthetic Lubricants for Refrigeration Units A large potential use of synthetic lubricants in the refrigeration field prompted some preliminary work to establish the level of lubricating qualities desirable in such fluids. A series of four-ball wear tests were run on Suniso 3-G, the refrigeration compressor fluid presently in use by Hussmann Refrigerator Company. Similar test data from Mobil D.T.E. fluid and Pydraul P-9 fluid is included in the chart below. The comparative data indicates that Suniso 3-G is inferior to both Pydraul F-9 and Mobil D.T.E. in lubricating qualities. Test Conditions: 630 RPM l67F. 1 hour duration _____ Steel-on-steel Fluid 4 kg 10 kg 40 kg Suniso 3-G Pydraul F-9 Mobil D.T.E. 0.38 0.22 0.18 0.62 0.28 0.24 0.60 0.63 0.38 Steel-on-bronze 10 kg 2.32 1.18 1.48 C. Low Temperature Viscosity Study Samples of Skydrol 500 were checked for -40F. and -65F. viscosities for comparison with results obtained at Douglas Aircraft Company on the same samples. This was done to check our low temperature viscosity procedure. Our results differed from the mean by about 0.75 which is within the 1.0$.reproducibility limit for temperatures below 60F., as specified by ASTM D-445. These results are tabulated below: DACO REL -65F. Viscosity -65F. Viscosity Skydrol 500 Old Acryloid - Lot A-2762 New Acryloid - Lot A-2763 2,470 cs. 2,540 cs. 2,489 cs. 2,559 cs. D. Lubricating Study - Paraffinic Petroleum Oil A paraffinic petroleum oil base stock was treated with fine iron filings for 24 hours at room temperature to determine the effects of such treatment on the oil's wear properties. It was found that this did not change the wear properties. Four-ball wear tests were run with solvent washed balls and distilled water and jewelers rouge cleaned balls with no significant difference. The DSW 622117 STLCOPCB4096148 37- complete removal of all iron particles was found to be important since simple filtration by a filter paper left minute particles which led to gross wear. Oil: Elk SAE 30 Base Stock, Inv. 2069. Iron: Fisher Cat. No. 1-57, about 40 mesh filings. Treatment: 250.7 gm. oil and 50.0 gm. iron stirred 24 hours at room temperature in a 1-1iter round-bottom flask. 4-Ball Wear, 1250 rpm, 2 hours, l67F., steel-on-steel, 40 kg, Inv. 2069-no treatment 0.91 mm. Inv. 2069-Dicalite filtered 0.94 Inv. 2069-iron treated, filtered 1.05 (seizure in once through filter paper 5 seconds) Inv. 2069-iron treated, filtered through Dicalite coated filter O.93 Inv. 2069-iron treated, filtered through Dicalite coated filter O.97* * Steel balls used in this test cleaned with distilled water and jewelers rouge and others cleaned with Skellysolve B and acetone. E. Compressor Lubricant - Four-Ball Wear Shell Four-Ball Wear values were obtained on compressor lubricants to assist in a problem at the Texas City plant which involved lubrication of the seals and rods of reciprocating compressors. This information was used by Texas City to outline a lubricant test program. No further work was done on this project. Four Ball Wear: 630 rpm, l67F., 1 hour, steel-on-bronze. Coastal Pale Oil Glycerine Humble White Oil 335 Ramol 4 kg. 0.90 mm. 0.48 0.61 0.59 10 kg. 1.49 mm. 0.75 1.34 1.80 40 kg. 2.17 mm. 2.48 2.80 2.25 de 9-23-60 L. R. Stark R. E. Hatton DSW 622117,01 STLCOPCB4096149 TABLE XXVII MIL-L-14107A SILICATE WEAPONS LUBRICANT MIL-L-14107A Specification 0S-106 Flash Point, F. 525F., min. 586 Pour Point, F. -75F., max. Below -75F. Viscosity, cs. at 100F. cs. at -65P- 5.8 cs., min. 900 cs., max. 6.297 852.4 Neutralization Number Evaporation Loss 1.0 max. 5. 0$ max. 0.9 1.56$ Silica (SiOa, $) 10.7-12.8 11.8$ Oxidation Stability: Viscosity at -65F. 1200 cs., max. 821.8 cs. Neut. No. Increase 0.5, max. Volatile acids 0.5 mg. KOH/gm. fluid Copper Wt. Change mg./cm.2 Steel Wt. Change mg./cm.2 +0.2, max. +0.2, max. -0.9 0.5 +0.02 0 Fluid Appearance No gum or insol. sep. O.K. Humidity Cabinet Rust 400 hr., min. 552 hr. Hydrolytic Stability Copper Wt. Change mg./cm.2 +0.5, max. -0.19 Acid No. Increase Oil Layer Aqueous Layer Vise, change at 210F. 0.5 mg. KOH, max. 0.5 mg. KOH, max. +20$, max. 0.05 0 -2.7$ Insolubles Storage Stability at -65F. at room temperature 0.5$, max. No separation 168 hr. No separation 6 mos. 0.5$ No separation No separation Rubber Swell (Syn. L.) 15$, max. 7-8$, 9-0$, 14 DSW 622118 STLCOPCB4096150 APPENDIX TABLE I OS-95 PHYSICAL AND FUNCTIONAL PROPERTIES Appearance: Slightly cloudy. light yellow, oily liquid. Viscosity: Centlstokes Saybolt Universal Seconds at 210F. at 100F. at 40F. 2.86 30.14 1920. 35-8 142. 8500. Density: at 100F. at 60F. 1.4l6l gm./ml. 1.4305 gm./ml. Flash Point (COC): 380F. Fire Point (COC): 680F.^1) Hot Manifold (MIL-F-7100), 1300F. - Does not flash- or burn on tube or after leaving tube. ' Low Pressure Spray Flammability (AMS 3150-B) - Flame brightened, but did not Increase. High Pressure Spray Flammability (AMS 3150-B) - Will not ignite. Molten Metal Ignition (molten aluminum alloy at 1150 to 1250F.) - Does not spontaneously ignite. Flashes by spark. Pour Point: +50F. Neutralization No. mg. KOH/gm. to pH 11: 0.83^ Steam Turbine Oil Rust (ASTM D-b6~5) 10.0 at 48 hours Foam(ASTM D-892) at 75F. at 200F. at 75F- Shell Four-Ball Wear: lb7',F. , 530 RPM, 1 hr. Foam Vol. ml. 30 8 35 Collapse Time Seconds 60 60 60 Steel-on-steel 4 Kg. 10 Kg. 40 Kg. Steel-on-bronze 4 Kg. 10 Kg. 40 Kg. 0.21 mm. 0.29 0.43 1.20 1.40 1.70 DSW 622119 STLCOPCB4096151 APPENDIX TABLE I (continued) OS-95 PHYSICAL AND FUNCTIONAL PROPERTIES Almen E.P. Passing load - 48 lb. Passing torque - 4l lb. 24,000 psi. Almen Wear (wt. loss mg.): 1.3 mg. Timken Load (passing]: 50 lb., 16,340 psi film strength Steam Turbine Oil Oxidation (ASTM D-943): (1008 hours exposure) Viscosity 100F. Initial Final 210F. Initial Final Acidity Initial, TAN Final, TAN Fluid Appearance: Steel Appearance: Copper Appearance: Four-Ball Wear: 30.12 cs. 30.03 cs. 2.87 cs. 2.86 cs. 0.82 0.21 Greenish brown with greenish white deposit in tube bottom. Soft black deposit on surface. Black rough (etched) surface. Initial 10 Kg.-0.29 mm.. Final 10 Kg.-0.4l rr Oxldatlon-Corroslon: (Fed. Spec. 791 Method 550.8, 168 hrs. at 250F.) Metal Attack (wt. change mg/cm.2 Copper - 0.05 Aluminum - +0.01 Magnesium -0 Steel - +0.01 Cadmium Plate - -0.01 no etch, greenish to straw stain. clear very slight trace surface pitting clear clear Viscosity 100F. Initial Final 210F. Initial Final Acidity, TAN Initial Final 30.1 cs. 31.8 cs. 2.86 2.95 0.82 0.68 Evaporation Loss, Fluid Appearance: 0.6 Clear, light amber, no deposits. DSW 622120 1) fluid boiled over onto heater. (2) Apparent high acidity due to nature of additives present. (3) Rust rating: REL M-400, 10.0 - no rusting. STLCOPCB4096152 O ther OS-9 5 ADDITIVE STUDY APPENDIX TABLE (c o n tin u e dI S a n t. CD 3 mctp u m -=1" Oi O: CU LKT\\ 1 1 0"N0 crv m -=f >n VO -=t 0m0 -r4H- -O4- PO- 11 1 1 1 1 W|Eh <ca Bm <Ycoad xC3) M po-i mo 27 cm CVJ CVJ CVJ CVJ 11 OlO -=t -=t o am) -m=t 00 -=t" oin 0in0 11 l1 i1 P paqi wcdi S' -4- rn vo VinO 0rH0 0m0 dooo 1 imn min vpo- -m=r oooo 1 1 11 rinn o <D > P p>R P T3 T3 o o o o o o o o m m -4" o ''o o CVJ 1--1 CVJ ooo Oft ion ion ion in in mo mo oin o o o o o oo oo ooo 4(D> P u PCD a) c KV OVVlft m o o mo o rH in in in in in ooooo m in i--l ooo c01 o c- 0) C CD <D 3 P P f-i 3 WP in av m m in in rH CVJ rH <OP PO Eo.p Ccd >ft o oo vvoo rH in vo vvoo vvoo VO VO vvoo vvoo vvoo VO VO VO VO Sh CQ CO O'-- mo S p Po IP 11 CVJ rmH i E- mCVJ CVJ CVJ CVJ ipnH1 irnH| ipnH1 CinV|J irnH1 Eh Eh Eh Eh Eh mm iCn1d iCnV1J Eh Eh m iCnVJ I m iCnV|J . 111 Eh Eh VO CbOOP P 4) bmp to 3 ra cd -X Tj COD PCD o CVJ in in rH pH rH 1--1 O o 4O- ptco fO< pced >R ctv 1 CVJ Pc 4) P oo rH O mm mm mm mm mm m m rmn mm mn rmn P >a id iHp Pb f3l> oO rH 3 O' O P po cb3d X3 rH 3 rH rH o iH -=f o o o CVJ o cvi CVJ CVJ CVJ rH rH rH rH rH rH rH rH rH 1 -t =t -=t* =t -=t -4- =t p map 1 i o> Oh 1 Eh 1 1 1 1 1 l11 1 Eh Eh Eh Eh Eh Eh EH EH Eh 1 P CVJ 'r\4` DSW 622121 S a n t. A ro c lo r 1242 A ro c lo r 1248 STLCOPCB4096153 A P P E N D IX T A B L E I I No B u rn s e x tin g u is h ! n o t ig n ite . S I ig h t in c re a s e o f fla m e . - 03 r*J 03 *0 n <u p 3h p 4" o d o' O i--{ H OH UHH lO CO o t>> o PPP .d ca o bO O pE co cd CO HM O Eh oo W PL, . 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CO >i -P (D *H 2-i f*rHH cq ,a CQ Cd <D g S-. S Qp cd 1--I o h-3 STLCOPCB4096154 10.0 0 .4 /d /6 0.6/d/7 U ) 10.0 3P 0) 3P o3 3P XJ o DQ to o-=J- cd <D 3 rH P *rH H. o HOoH Jo) P 3 > E id g ra co CoO -Op p 3 rc<Hdu oCM moCoM moCoM oCM 3o 3 OQ 3 0) CD 3 P O 3P P xi cd 3<D CwHO 33 rH Eh ft ooc o cc Ph IH P < 55 O WH P <m OEh X Eh 3P>h o oI--I 3o PID 3 ID ft P03 to cd pid 3 rH oCD H 0o) rH CoD ccoid o po 3 -p 3 > rcCHdD E 03 E 03 E 03 inirunmo o -ptpo c 03 O 3 C3D 3o COD 33 fPt w P P Cd P t3o rcHd Pfht < CPo mo m pip 33 P3 m03 c3d ft c33d N P 3 c3d cod oO ft 3H -o=t f>t3PO t3Ho l Pcd t3o I CoO P 3 -h ccdn p 33 rPHh 3O P3 Iii Iii iii iii Iii iiiii -C=1M- I 0m0 I-H -=f- OVD O rH m mvo mvo cvj ooooop ion imn op oo o in rH rH S iI 6 -m=r i mt- cvj cvj mmomovinovmo o<h ooooorH o rH mm mo pm cvj s vo III iijiii III OVO rH CO O 00 m...m....m....m...o..o...m.. 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G P E E p P,60 P 3 G rH cd O cd p p cd 3 P02W<0 rH p to 2 p DSW 622124 M-403 r a tin g system , 10 = p e rfe c t STLCOPCB4096156 CO w M Eh @ Ph o cr: P, <MMI o 2; M Eh cGU <U 'S < O MM P m E cq <p I pG x3 H o Ph P 2: 2; o wH pPh Eh < 0) G < P CO P <> w in i co o to m in cm g , rH 1 l-- rH ID P o 1 rH O CM <U .3- e cd *r4 p 60 VO ON OVD w . vo ONinm Cti o o 1--1 co o o O i--l G cd to in vo m Q> . st i moo S 1 =t o O --i in cm vo m i coco rH O rH in o-mo CX\ o\vo vo o o o i--l CM O CM CO 1 VO vo O O 1--1 C"- CJNCO O 1 VO vo rH o CM m st o o 1 vo o rH O CM ON O1 1 rH 1 1 ONONONVO in c--- m <j\ o o o 1-- -^3" ON rH vo CO knon o o O rH VO INVO ON OO o vo o rH O rH p- i m ON o O rH CM =t 1 1 o 11 1| ON 1 o 1 1 Ph ao B t-ONh <u VO o VO VO Eh - rH rH rH hONS vo OVO vo rH i--1 i-- b-ot-tvo o VO VO rH rH rH C-O t-E- vo OVO vo H4-HH t~-o vo o rH -=3" tvo rH H rs. 2 2 1 CQ C -P p Gs O Ph a ce -cpo <u Eh A C\J CM i--1 i--l f--1 CM CM i-l rH CM CM H H CM CM CM oo oo inmmm CM CM vo vo rH rH o ooo in mmm CM CVJVOVO rH rH O OOO minmrn CVJ CM VO VO rH rH OOOO in in mm CM CM vovo rH rH OO in in CM CM rH rH O in CM rH coi coi coi CQi CO CO co CO COI COI COI CQI CO CO CO CO COtCiO ClO lCQ CO CO CO CO coI coI coI CQI CO CO CO CO CO co co co CO I CO m CM CQ 0) p *H 0-p0 G -cPo g3 op =frH in -p G rH P ON H 3 rHi1 O CM1 CQ CO a6J c g K ID rH CQ CQ H >rPh '----- V--r M H -0p2 nJ in o i--i o 0) <D M <U in CM a. o. P, co CO f> E-i H M 4) <u -p -p H H in in in in G O G o S1t =t =* iI QG QG CQ O CO o co CO Oo <D to cfdt -p X ID G CQ <D -OP G P o o <H <u a> co DSW 622125 STLCOPCB4096157 CO w M Eh s o Oh 0O 3 Pi P Ph H Po p 2 o oM 0 O Eh o <p O <I M M M Pi 0 N3 M tH 0 W CO m< 2 O P (D Eh H e Eh X< MP PP s w> Pfam W <m =t- co o p s 0 fa po is: O pO 3 P" 0 -P a0 3 t>- in p 0 in On s 1o PC CM p Pm X 0 0p 6 0) Pm 3 P Pi 0 0 Pm O 0 0 VO 3 X O rin- mt- ii Eo Ci--MI CM f--I Pm I I fa P p- 0f3t 0 o o\ m co in CM on m 3 OJ CU CM CM O* POm Eh 03 o o o O o o O 1 O o o O ft o o o O o o O I O o o O o o o O in o O I o o o O p" in in m m KN m i t- in p- VO 73 0 O P m t- 03 CM m c- 0 os in H 73 ON P Pm CM P 0 I 03 73 CM m O3P i I p CM 73 0 -p P p 0 fa p 0 fa VO C P 0 0 0 I CO 0 0 0 P -P -P p < o CM Oi--NI P p Pm P O 0 0 0 tJ p" CVJ VO *pl i--i in I CO CO o p 0 -P -P p 0 P0 P 0 3 p fa CO i--i i co 2 0 X ii cd e o o O o in in w 0 ox CM in in > > CO co (X) M HH H > 0 0 0M M Pp p I i I I m in in in H H in in m in in p" p p p iiii P o P O po p- p i p- p p" ii CO co CO co Pm Pm Pm co co co co co oooo oo oooooo fa .o o 0O p NOX PP- O pp O 0 0I p0 0 P 1 -H 0 iH P P 0 0 0 fa ft 0 PO E0 0 0p >Rp 0 o in O ON 73 I--I p P CM 0 in P 0 0 P 0 0 0 H ,P H ,0 Eh m o 73 i vo 0 CO P 73 0 O *> 0 p 0 i-H 0 3 0 3 <H o ftp0 t-I P 00 01 P HftP s ft p o 0 1 0 0 Ip ft 0 0 73 ft 0 p . P0 703 p 0 p p0 O0 op E 0 CO 0 73 CmM p P 0 0 O o >lrl 0p 0 P E0 co o E ip co X fa < p cm DSW 622126 STLCOPCB4096158 APPENDIX TABLE I I I - A (c o n tin u e d mg Standard wear te s t is 20 m inutes a t 4000 p s i lo a d . A ll wear values are average o f two successive te s ts a t In d ic a te d lo a d . 03 dCTM MGQ pO GPQ. P, Eh I o MOO 44 GCOQQ 3 J' c- fi E OJ bO e o i <U d i--I ID CM CO w CO PO CPQ, P p, Eh oj hO bEO P03 P03 fa o o N6 oo OJ -P 0GQ} O 0GQ) OJ NN min maj *0h o m cq MI oj tCD OJ f0a5 3 PI O in in 2 <13 M d vo OJ _Eh CM rH i-- < 1--1 H p CQ T3O CQ O P, p P <DM p P. Eh " 03 M <13 m OJ M rH p . T3 P 03 <13 b0 03 05 <d NN N 1N E NSN m <u o rH rH H I H M H p> 3 o 0) rH 0) rH 0) <U in (dkno PI o GQ CQ CQ CQ CQ GO (Q P m OQ m OJ rH m i <13 -P O E 3 PI 2 rH O< M Eh <0 <d P CM iP rH P OQ < CQ O P, d t) o p P P P p p p p <D Q)> p. Eh I <13 03 <13 <13 0) <13 03 03 0) W NNN N NNN N NNN o M M -H M rH *H rH rH rH rH rH in o 0) <13 03 <13 <i) a> a> 0) 0) a> a) p- o GQ OQ GQ OQ GQ CQ CQ CQ CQ CQ CQ CQ i p- CQ CO -P O o 3 iP p cd o iP b0 P H CQ 03 cd Oh c 0) g rH icn--tcin-r\ Ol i--I > DQ) faa> fa ' < rHinvo oj I <H CO I "2SS HH> > > MM M M *V *s ininmin pi-.pi- ^tj- i COCO C0 &J oo o o OJ I o OJ VO --oOJ--arHv-P4-5I I IO CO CO iP oinm O M <--I oj in in CD co oo <1) -p -p -p co co co ppp ooo P p cd m oj mu I <p +j -p -p cd CP GQ CQ 44 <13 0) a> CO -P 4J 44 C CQ CQ CQ O P P P 44 <13 <13 CD M 5o* Potf 5o* Ms M M -H Cd >>> >>>> MMMM k ^ 4J in in in in <n -=Ic -=tI- I 4If 4<4u CO CO cO Oj OOOO oj p d CQ OJ 0) fPa rH bo ra P P. p cd 0) ffl poo- ooo C--00 oo oo V00OID p cd o PI cq bflp Pp rH TO d o CQ p, cd Ph * ' 4*---- m in | rH co i -- co -- m m> MM tn>m1 II co CO oo OVO M OJ II co co ------------ mo MO in oj co CD <U 03 4M4 44 m cc oo PP oo DSW 622127 STLCOPCB4096159 APPENDIX TABLE III-B OS-45 EVALUATION - STATIC THERMAL AGING (400F., no metal, N2 atmosphere, glass container) Appearance OS-45, Type III (S-l4) All samples from 0 to 480 hours exposure were sediment-free with the ones exposed longest being slightly lighter in color than the initial material. OS-45, Type IV (S-15) Samples with 480, 288, and 192 hours exposure- had dark sediment and grey-black, needle-like crystals 1 to 3 inches long. Fluid slightly darker than new. Sample with 120 hours exposure had dark sediment with no crystals and was darker colored than new. Exposure for 48 hours resulted in a very small amount of sediment in the slightly darkened fluid and 24 hours exposure the same appearance as new fluid. Oronlte 8515 (S-19) When material was first removed from sample tubes, the fluid aged 120 to 480 hours had a bloom; whereas, that aged 0 to 48 hours had no bloom. After standing 24 hours, none of the samples had a bloom. No sediment was present and the samples were progressively darker in color from 0 to 192 hours with the 288 and 480 hour samples appearing slightly lighter. Oronlte 8200 (S-20) Appearance of 0-8200 samples were the same as for Oronlte 8515 above. DSW 622128 STLCOPCB4096160 APPENDIX TABLE III-B (continued) OS-45 EVALUATION - STATIC THERMAL AGING (400F , no metal, N2 atmosphere, glass container) Specific Gravity 60/60F. Hours Exposure 0 24 48 120 192 288 480 OS-45, III (S-14) 0.887 0.887 0.886 0.886 0.686 0.886 0.886 OS-45, IV . (S-15) 0.891 0.893 0.892 0.892 0.892 0.893 0.893 Oronite 8515 (S-19) . ~M 0-932 0.932 0.931 0-932 0.932 0.932 Oronite 8200 (S-20) 0.935 0.935 0.934 - ----- -- 0.932 -- Refractive Index -25C.: Hours Exposure OS-45, III (S-14) OS-45, IV (S-15) Oronite 8515 (S-19) Oronite 8200 (S-20) 0 1.4589 1.4392 1.4361 1.4337 24 1.4390 -- -- -- 48 1.4390 -- -- -- 120 1.4390 1.4392 1.4362 1-4337 192 1.4391 -- 288 1.4391 -- -- ----- - -- -- 480 1.4391 1.4390 1.4364 1.4335 Neutralization Number (potentiometric TAN): Hours Exposure 0 24 48 120 192 288 480 OS-45, III (S-14) - 0.08l 0.134 0.144 0.158 0.291 0.333 0.363 OS-45, IV (S-15) 0.104 0.155 0.233 0.326 0.375 0.442 0.465 Oronite 8515 (S-19) 0.049 0.057 0.049 0.06l 0.059 0.065 0.068 Oronite 8200 (S-20) 0.076 0.088 0.072 0.077 0.077 0.107 0.119 Evaporation Loss, 0 (ASTM D-972, 400F ., 6-1/2 hr.): Hours Exposure OS-45, III (S-14) OS-45, IV (S-15) Oronite 8515 (S-19) Oronite 8200 (S-20) 0 41.50 29-50 21.00 24 44.6 30.5 -- 21.10 -- 48 44.99 30.7 ----- . - . ----- 120 45-3 34.2 20.4 20.7 192 41.6 - 43.3 288 40.5 - - 39-6 --- DSW 622129 -- ---- 480 41.6 39-8 21.0 21.2 STLCOPCB4096161 P O oo < rCaQ T(UJ < s s i--toi ho 3 G P co o CPI -p w p3 <c Eh O o CM CO <u o -PP CM1 OG 'C--O G o ofa O P CVJ o oo CT\ 04 P in O K\ tn CMVD O N-O mvo H O 00003 t'-co i--I <--( i--I c0oWco0<h0i4n-mV4D- 4W cm o ocinm p ct\ mm CM CM CM CM P in ii--ni co PP0) oPIc GO 'c--o OG cm p coo cmt'indoificno ncm co c--c-covo in m l'- cm com oi--cicoo ion ccmr\mt-- 4CM- mCM cCMm oi--cI ci--oIci--oI ii--nI >H fa o O moctc-omocoMt'-ccoo c0o 4m- in** ipn rH CM mmmmmmm 4- i i co co -- O fa -o O P=* oOCtO--Ht--i- CCMM 4O"CCOO o CM CM P P P P O ofa cooccoo\cPo 4f-ccoo cno oco o rH mmmmmmm --4p" CM in i 4I- 'C--O- 00 o ofa OO P --O CM -4-MO t-- co t--co m p o co P Pi--I P i--I i--I O OCQ -P m m T<3v OCmJ Gm OG Oft 04-00 CM 4- OCPMCCPMT\CCC0OM04O0- p x >W ofa in c- <u n ft <0 oo C4 P e mi co m4- pc CM E rHI co m4- Pc Pc Pc eee ooo iii c PC I E -H iIii Oi--i I E op OI ooo ooo oo oo mm4- rH CM E P to E iOp in oo oo o pP pP oo o pcmPp Pp CcOootc'-occoo COmo 0p0 cc--o d) o a> c0Gco)r fa o Oi--I CM (cUa ft cd coo p :Ed E <op in o <rau mo oocooc o<u cq OOO CM CPi Oc PG E CMCQ 4 c-- cc 1--I t--I E 6 c OO pI pI E o o in oo o o t'-co co oo o oo oo o oo c-co t>- not-- p m cm .4- m p co m p am> ft G CM CM cc c c a rH tH H H H cd E E E oo ofa o o in t-- n.4- 4 I to o o rH i--I rH rH i--( OI CI OI ao oc o o o co m CVJ r<*V *H rH cvj CM CTi ooI p GE p cd E <pO o ooo o i--i poo iP--oI Pp P^5 osocoto'tp' too-cccom itn- sEh in C<O <u o <0 G G Ga o o o ooo oooooo wGO oft CPM400- CM 00 P -4- CM 00 P -4" CM CO P4 <D W cd o OQ o GO T3 rH HHM---> >H ipnn co o o cm co 2 G *4i--I fa in i in rH in i aio\ -p P rH | a; o -P CM rH I E 4- co 4- co C co C co cd O'-- O'-- o co o co o oG G Q DSW 622130 STLCOPCB4096162 APPENDIX TABLE III-B (continued) OS-45 EVALUATION - STATIC THERMAL AGING (400F., no metal, N2 atmosphere, glass container) Flash and Fire Points, C.O.C.: Fluid Hours Exposure OS-45, III (S-14) 0 192 480 OS-45, IV (S-15) 0 192 480 Oronite 8515 (S-19) 0 192 480 Oronite 8200 (S-20) 0 192 480 Flash, F. 370 340 340 390 310 305 395 415 345 405 410 405 Fire, F. 455 455 455 455 435 450 455 455. 455 450 450 450 Reflash after Fire, F. 415 410 ___ 415 . 380 420 -- 410 .--- -- 415 Shell Four-Ball Wear Fluid Hours Exposed Test; Conditions Ball Matl.(1) RPM Hrs. Temp. Wear Scar Diameter 4 Kg. 10 Kg 40 Kg OS-45, III 0 S-S 1200 2 l67F 0.41 0.59 1.07 (S-14) 96 S-S 1200 2 167 -- 0.56 1.11 480 S-S 1200 2 167 -- 0.56 1.08 0 S-S 1200 2 400 _ _ 0.79 __ 96 S-S 1200 2 400 -- 0.75 -- 480 S-S 1200 2 400 -- 0.80 -- 0 S-B 630 2 167 2.37* __ _ __ 96 S-B 630 2 167 2.85* -- -- 480 S-B 630 2 167 7.80* -- - - OS-45, IV (S-15) 0 S-S 1200 2 167 0.42 0.64 1.03 96 S-S 1200 2 167 -- 0.66 1.29 480 S-S 1200 2 167 0.62 1.15 0 S-S 1200 2 400 _ _ 0,. 87 _ _ 96 S-S 1200 2 400 -- 1.05 -- 480 S-S 1200 2 400 - - 1.00 -- DSW 622131 STLCOPCB4096163 APPENDIX TABLE III-B (continued) . OS-45 EVALUATION - STATIC THERMAL AGING (400F., no metal, N2.atmosphere, glass container) Shell Four-Ball Wear: Fluid OS-45, IV (S-15) (continued) Oronite 8515 (S-19) Oronite 8200 (S-20) Hours Exposed 0 96 480 Test Conditions Ball Ma-tl. (1) RPM Hrs - Temp. S-B 630 2 l67F S-B 630 2 167 S-B 630 2 167 Wear Scar Diameter 4 Kg. 2.19* 1.40* l.l6* 10 Kg __ _ -- 40 Kg _ __ --- 0 96 480 0 96 480 0 96 480 0 96 480 0 96 480 0 96 480 S-S S-S S-S S-S S-S S-S S-B S-B S-B S-S S-S S-S S-S S-S S-S S-B S-B S-B 1200 1200 1200 1200 1200 1200 630 630 630 1200 1200 1200 1200 1200 1200 630 630 630 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 167 167 167 400 400 400 167 167 167 167 167 167 400 400 400 167 167 167 0.45 -- -- 0.66 0.64 0.68 0.99 -- 0.99 - - 0.99 2.30* 2.29* __ -- -- 0.82 -- -- 0.95 0.87 0.96 ' __ -- -- 0.97 0.95 0.99 1.62* 1.87* 1.85* _-- -- -- 1.15 1.14 1.13 _-- --- __ --- 1.35 1.03 1.23 _____ -- -- _____ -- -- * 5 Kg. DSW 622132 STLCOPCB4096164 APPENDIX TABLE III-C OS-45 EVALUATION - OXIDATION-CORROSION (MIL-H-8446A) Oxidation-Corrosion Test Results Metal wt. change, mg./cm.2 Copper Steel Aluminum Silver OS-45, III OS-45, IV (S-14) . (S-15) Oronite 8515 /(S-19)1 -0.11 -0.20 0 0 -1.20 -0.01 0 -6.28 -0.29 +0.06 0 -0.01 Acidity, mg. TAN Initial Pinal Change KOH/gm., 0.08 5.9 +5.8 0.104 6.3 +6.2 0.049 0.86 +0.81 Viscosity, cs. 100F. Initial 100P. Final % Change at 100F. 11.81 14.36 +21.6 12.14 15.21 +250 24.24 19.27 -20.5 210F. Initial 210F. Final % Change at 210F. 3.98 3.24 -18.6 - 3.93 3.54 -9.9 8.14 505 -31.8 Fluid Evap. Loss, ^ Fluid Condition 8.6 dark si. sediment 8.0 dark solids 4.3 dark no solids Foam (Micro Scale 1/10 ASTM D-892) 75F. Sequence New After Q&C llcc 20cc llcc 23cc 79cc 68c c 210F. Sequence New After O&C 12cc 15cc . 7cc 45cc 8cc 25cc 75F- Sequence New After O&C llcc 15cc 12cc 15cc 66cc 88cc- Oronite 8200 (S-20) -0.04 -0.01 -0.01 -0.03 0.076 0.49 +0.42 32.57 25.10 -21.0 11.26 7-40 -34.2 3.96 dark no solids 79cc 90cc 6lcc 30cc 83cc lOOcc DSW 622133 STLCOPCB4096165 APPENDIX TABLE III-C (continued) OS-45 EVALUATION.- OXIDATION-CORROSION (MIL-H-8446A) Oxidation-Corrosion Test Results Oronite OS-45, III OS-45, IV. 8515 (S-14) (S-15) (S-19) Oronite 8200 (S-20) Four-Ball Wear (1250 RPM, .2 hr.,(steelon-steel ) New, l67F., 10 Kg. 40 Kg. O-C, l67F., 10 Kg. 40 Kg. New, 400F., 10 Kg. 0-C, 400F.., 10 Kg. 0.59 1.07 0.78 1.14 0.79 0.71 0.64 1.03 0.75 0.96 O.87 0.74 0.78 1.14 0.63 1.18 0.71 0.99 0.63 1.18 0.84 1.17 0-99 1.06 DSW 622134 STLCOPCB4096166 APPENDIX TABLE III-D OS-45 EVALUATION - SHEAR STABILITY Diesel Injector Shear Machine Fluid OS-45, III (S-14) OS-45, IV (S-15) Oronlte 8515 (S-19) Oronlte 8200 (S-20) ThPraosusgehs: Shear Machine! Viscosity at :I00F. at 210F. & .% CS . Decrease cs. Decrease 0 12.17 0 ' 4.00 0 1 11.95 1.81 5-92 2.00 2 11.80 5.04 5.91 2.25 4 11.66 4.19 5.87 ' 5-25 6 11.56 5.01 5.80 5-0 8 11-55 5.26 5.76 6.0 10 11.45 6.08 5-72 7.0 12 11.56 6.66 5.69 7.75 0 12.14 0 5-97 0 1 11-95 1-75 5-95 1.01 2 ll.8l 2.72 5-86 2.77 4 11.65 4.o4 5.76 5.29 6 11.57 4.70 . -- -- 8 -- -- 5.72 6.50 10 11.45 5.85 5.67 7.56 12 0 24.24 0 8.14 0 l 25-59 5.51 7-86 5.44 2 25.06 4.87 7.71 5.28 4 22.75 6.15 7-65 6.27 6 22.50 7.18 7-52 7.62 8 22.55 7.80 7.47 8.25 10 22.50 8.00 7-42 8.85 12 0 52.57 0 11.26 0 1 51.65 2.82 10.95 2-95 2 51.24 4.08 10.79 4.17 4 50.95 5-04 10.64 5-51 6 50.58 6-11 10.56 6.22 8 50.56 6.79 10.48 6.95 10 50.28 7.05 10.45 7-57 12 50.25 7.18 10.42 7.46 DSW 622135 STLCOPCB4096167 APPENDIX TABLE III-E OS-45 EVALUATION - EVAPORATION LOSS (ASTM D-97.2, 6-1/2 hours) Temperature, F. 340 345 350 358 362 365 375 385 392 400 415 OS-45, III (S-14) 5.6 6.9 8.4 9-7 10.3 12.2 19-2 29.5 37-7,. ^ 41.5'1) 65-8 Welg-ht Loss, # OS-45, IV (S-15) Oronite 8515 (S-19) Oronite 8200 (S-20) -- 8.5 -- -- -- -- -- -- 29-5 -- -- 8.5 -- -_ ` --- -- -- -- (2) 21.1 -- -- 7-9 -- -- --- 21.0^ -- (1) 21.23# WADC Technical Report 55-89, Part I. (2) 22.3# WADC Technical Report 55-89, Part IV. (3) 7-9# WADC Technical Report 55-89, Part III. DSW 622136 STLCOPCB4096168 .2 0 .2 6 See fo o tn o te s - - n e x t page o UN CM>R. rH VO KN <13-^ >'~ HO 3 W 3 -H O cd .G o GO-Hp -Cp M >3 cd O Pm co- E 6 O VO UN CM CVJ UN O OO ONC'-Un VO f-O O O rH O CM VO 1--1 O ON UN-=J- O o rH ooo rH oo oo 1--1 1--1 UN UN ou o vo un (--I I m 3< cm vo co cd G -P T3 O <D >> .J H Pm <ccc p G a (U O >H CU ON C- Pm o ^ G feKV <B H > Q Pm GO X rH O 3 rH < 3 rH I cd Cd G O CO ON C Pm -P P o I o -O -H pH H P>1 3 cd -P Pm CO X GJO O C <3 Ph ON w Pm >PHH rs G Oh c < wEh cd Mo pq H co X t| XG PH Pm rH CO rH I 3N cd Pm -P Xf O UN UN 1 CM C1 t oo CO t~! ONO 1 * O i--1 CM CM VO rH VO O -=T UN o CM O -=t" rH oo ooo 1--1 UN ooo UN=f CM t"-C0 O O rH UN UN C-rH Lf\ <J\ -=J" -3" O o VO UN ON rH OO oo i--11--i rHOO CCM CM VO OOO CO 00 1 rH CM 1 rH rH o CM UN rH o=r un=i- o .o o * LOON rH O UN O UN i--( Eh co E 33 Q, v UN 03 G VO VO I si bO to w fciO SjO bO XX Q =a- o o -=1-0 0 rH =f rH =* 03 -p co 3 X) X) Q. <u rH G N H 0) <D G * X* O -P <U 0 -P Pm CO G I1 TJ X) -P cOd XI jh djOcdbcO 0) c3dc"v^j C --- H X) CO G 0 1 G 0 1 r--I G 03 c0d )0oo 0)> 3J 3 cOd M - cdO bO-GP O C 0) G CC0 JH 3 -H X) 03 G G G rH 3 3 E3hrhH XO XO fc 1o G C" cu <13 -P <u <u -p O* C G 0) -P o 03 O' C 0) G 0) cd o G 03 E 0) 03 rH .X cd th -p E 03 H^Jcd -H cvj 3 vo CO CO E3B E Pm Eh Pm fa 0) x> O rH -p fa < < Eh co DSW 622137 STLCOPCB4096169 APPENDIX TABLE IV (c o n tin u e d m OJ vo 3 <2 m (U cs P -p >-< P-. 3<u Q, 0o <2 3 Oh ov I Cd Ph 3 o P to -a: -op 1 Ph Ph oM 3 c cd EMh m cd o p H CQ .tc| Eh CL, CO 3 in O vOoJ>tnR -- D i-H O 3 OJ 3 rH O cd .3 O P 3PP I 3P > 3 3 CO cd O Ph CO'-- in in vooj mo rH rH I 3< cd Pi P 3O >|J PH - 3<1) OO 3 OIJ o &H c I--I I--I I--I o p OoJ--I ooo rHO O O O O g <n i i i+ O, O CO P, o o o in c mm p m o oooo O OV CD rH t-- C"--VO af vo o Ainmn o m-=r + + 3 cd CD p 0 1 3 o 3 2 m i--i oj t--oo aj- mc--amt--=+t- ininrH+ aj- vo 3 cd i--CDI 0 1 2 o CD iii i i i ii i i i ii CD P O CD CO C-- VO o CVJVO tOSOVO CD r O O O O O P o' o Ov t>- I >R. pc, m <u ih 2o rH O 3 rH 3 rH I cd Si O CO 3p Po 3>>iHs pH C'-- ccod -4" C" OJ o o oo oo -=t- C-- co vo co mvo m i>n-cidn o+j in in o+i in m 3 cd CD O 3 XI lO p OH4- Cll OJ m OJ OSCO -af O O O O O P Pr OIN Ph rH CO rH I 3N cd Pi P 3tJO Ph vo o oooo p-vo at mvo cd c-- aj" vmocmo m+ mmp+ 3 cd i--IDI 0 1 2 o co movococo coc OJVOIAShOI oj O CD O O i--I i--l , l1 CD >H Ph o vCo'- oPc O in OJ eo E bO \ >4 x p 03Q). s o O 00 - 3 O J* o 2 CD p cd bO E cd ^H p cd p cd p cd CQ CQ O Ph 3 O E CL, p3 p3 Pi Cd 3 E 0 P tH 3E O P Pi M C 3 1 * Cd Q) <D rH rH *iH 3 ftp 6 E O 3 P O, bO <D 33 P ,3 cd O cd PH cd 3p 3p <2t! --I H Ph CD H pc, a) bO b0 Eh cd CD 3 3 PP * P cd t>P 3 b0 3 cd p>o&o, PO PhjcjdoPho OO O P,h cd O> osi P si b0 P ID X P P O S CO < O P C P ,3 GO O O P P cd cd <u 3 VO 2 P M Ph O O P P'^R.OlCVJ>R 3 3o H rH P CQ XO o< Ph to bO bfl ho bO bo bO & E W2 a, 3 0 0 o o o o OC p -=J- P4 H^ o m VO p ID <D IS1 N -> CD CD 3 CD CD 0 3 0 3P P 3 3 3 CQ 3I o p3 --o CQ P I1 33 o0 D 1 3 0 11 3P Pp 3 cd <d CD CD CD 3 CD CD o XP CD <D PP CD P o CO CO CO CO 3 P2 O 2 p 3 3 CD 2 O <D 2 p Ph o c O DSW 622138 STLCOPCB4096170 o in Oj'fcR. co m HO 3W 3 HO CO .3 O rH 3 -p -p I 3 H 3 CO >iS (DO PH CO --* 6 -4- in o CM rH CM in in m in m cm o mo m rH I 3< CO -. -P T>O> JO Ph oc ri ^m <u & rH O 3 3 rH CO O CO OHH-P-PO >i3 (0 Ph CO e O^C o E in cm oo rH -M" CM 00 -j- m -m=t- mt- CIT\ Ph 0rH0 rH I 3 tXl CO -< -P 3O !J PH E 4"(D O -=J" oo EH CO 01 Zcc m <u 3 H *. m TJ (D rH CQ O > ft CM -p co m h Vft rH m O CD i--l -* ' O O -P OC 3 h h Eh Ph i--I 3c C-- O <D <D I <H >j CM Ph Ph Ph CO OCo o o ----- CO -P CO CO 3 H i--( oo m o m QISOCM h --'-P E cO COO ft o OCQ H ft 3 crOH cO rOH -P O 03 P 3 CQ -rH <D O 3 -p CQ i--l O rH Ph CO 3 cO Z I CM O Ii CO i O ;i 3 h 3 (U 3 3 O 3 CQ O o in m o o CM i Ph 8 bO 3 -P CQ 3 3 O Z If o o bO 3 H p cO 3 O O 1 ft o in CM DSW 622139 STLCOPCB4096171 APPENDIX ASTM COOPERATIVE TESTS Section VI - Fire Resistance A. Flash and Fire Points 1. Procedure and Apparatus The Cleveland Open Cup method was conducted according to the procedure outlined in ASTM Standard Method D-92-52. The apparatus used was a Cleveland Open Cup, Fisher/Tag Improved Model, ASTM, electrically heated, Fisher Scientific Company No. 15-538. 2. Test Results ASTM Reference Fluid 1-A-l 2-B-l 3-C-l 4-D-l 5-D-l 6-E-l Flash Point, F. Fire Point, F 430 465 no result -- boiling and frothing 510 620 395 665 455 630 no result -- boiling and frothing B. High Pressure Spray 1. Procedure and Apparatus The procedure used is outlined in Military Specification MIL-F-7100 (December, 1950) Section 4.2.2.8,1 as follows: "Assemble equipment for applying 1,000 psi to the test fluid. A suitable arrangement shown in Figure 1 (of the specification) consists of a nitrogen bottle, a hydraulic cylinder and necessary lines, valves, and gauges. The orifice nozzle shall incorporate a clean, sharp-edged orifice approximately 0.0145 inch in diameter in metal plate or disc 0.064 inch thick and with a flat area of at least 0.38 inch in diameter on the fluid side of the ori fice. The cylinder shall be charged with the test fluid at the temperature of 15-6 to 37-8C. (60 to 100F.). Apply nitrogen pressure so that the pressure on the fluid side is 1,000 psi, and open the valve at the orifice and attempt to ignite the spray at the orifice with an oxyacetylene torch adjusted to a neutral flame and using a No. 3 Purox tip or equivalent, while maintaining Be fluid pressure at 1,000 + 50 psi. If the fluid cannot be ignited at the orifice, the test shall be repeated by applying the flame at increasing distances from the orifice up to lo Inches from the orifice. The results shall be recorded as follows: 'Will not ignite', 'Flashes with difficulty', or 'Flashes readily'. Also, the distance DSW 622140 STLCOPCB4096172 APPENDIX - ASTM COOPERATIVE TESTS Section VI Page 2 from the orifice at which ignition or flashing is carried downstream from the test flame area and whether any flashing is self-extinguishing or results in a sustained fire shalL be recorded." An aircraft type hydraulic accumulator with no diaphragm was used by this laboratory instead of the hydraulic cylinder reservoir specified. The apparatus was cleaned after each test by circulating first kerosene and then acetone, followed by air and nitrogen blowing to remove the solvents. Attempts to ignite the spray stream were made up to distances of 3 feet from the orifice instead of the specified 18 inches. 2. Test Results ASTM Reference Fluid Result 1-A-l 2-B-l 3-C-l 4-D-l 5-D-l 6-E-l Flashes and burns readily. Will not ignite. Flashes with difficulty only when the torch was about 2 feet from orifice. Self-extinguishing. Will not ignite. Will not ignite. Will not ignite. C. Low Pressure Spray Flammability 1. Procedure and Apparatus The procedure used is outlined in Aeronautical Material Specification SMS 3150B (Society of Automotive Engineers, Inc.), Revision of February 15, 1953, Section 4.9.2 as follows:' "Prepare a shallow metal pan approximately 1 ft. square with sides not over 2 inches high, into which is placed a platform or grid made from 1/8 to 1/4 inch mesh wire and spaced 1/2 inch from the bottom of the pan. Saturate 10 gm. of cotton waste with 20 gm. of Grade 1120 engine oil, roll the waste into a ball and place in the center of the grid. "Place a quantity of the test fluid in a Binks Thor No. 7 paint spray gun (0.070 inch orifice). Set line pressure to 40 psi, and adjust gun to produce a dense cone-shaped spray. "ignite the oil soaked waste and allow the fire to reach maximum Intensity. Aim spray gun on the fire as shown in Figure 6 (center of spray 1-1/2 to 3 inches above burning waste and 16 to 20 inches away) and intensify fire DSW 622141 STLCOPCB4096173 APPENDIX - ASTM COOPERATIVE TESTS Section VI Page 5 by depressing trigger slightly (air Jet only). Introduce fluid mist by fully depressing trigger in bursts.- Record the results as 'increase1,'no increase', or 'decrease1 in fire when the fluid mist is introduced into fire. Spray several ounces of liquid to be certain of results. "Use new waste for each test and Insure that the pan is approximately at room temperature." 2. Test Results ASTM Reference Fluid1 2 3 4 5 6 Result 1-A-l 2-B-l 3-C-l 4-D-l 5-D-l 6-E-l Greatly increased flame Decrease in flame No increase in flame No Increase in flame No increase in flame No increase in flame D. Hot Manifold 1. Procedure and Apparatus The similated exhaust stack section and test procedure described in Military Specification MIL-F-7100, Section 4.2.2.8.2 was followed. Two 10 ml. portions were dropped at the specified rate of 40 to 60 seconds per 10.ml. for each fluid tested. The manifold was heated to l3ooF. and the pan and shield around the manifold was cooled nearly to room temperature between each test. , 2. Test Results ASTM Reference Fluid Hot Manifold Results 1-A-l Flashing and burning on tube (mostly along bead). Does not flash or burn after leaving tube. 2-B-l Does not burn on tube. Only occasional flashing along bead (very small flames). Does not flash or burn after leaving tube. 3-C-l Does not flash or burn on tube or. after leaving tube. 4-D-l Does not flash or burn on tube or after leaving tube. 5-D-l Does not flash or burn on tube or after leaving tube. DSW 622142 STLCOPCB4096174 APPENDIX - ASTM COOPERATIVE TESTS Section VI Page 4 ASTM Reference Fluid 6-E-l 7-F-l 8-G-l Hot Manifold Results Flashes along bead. Does not flash or burn after leaving tube. i' Burns on tube. Droplets burn while falling to pan. Does not flash or burn in pan. Burns on tube and falling droplets. Does not flash or burn in pan. DSW 622143 STLCOPCB4096175 APPENDIX ASTM COOPERATIVE TESTS Section VII - Lubricating Properties A. Four-Ball Wear 1. Procedure and Apparatus The apparatus used was a Shell Four-Ball Wear Machine manufactured by Roxana Machine Works, St. Louis, Missouri, which has appropriate devices for rotating ball speed control, ball loading, temperature control and test time control. Test balls used were SKF Industries 0.5 Inch, grade 1, EP, Atlas Ball Bearings of SAE 52-100 steel and Hartford Steel on bronze at a spindle speed of 635 rpm, a temperature of l67F., and loads of 4, 10 and 40 kilo grams , for one hour. The test balls were cleaned with Skellysolve B and acetone prior to the test. The cleaned balls were chucked in the machine and the fluid introduced, the load was applied, and the fluid and balls heated to l67F. At the test temperature, the machine was started and run for 1 hour. The wear spot diameter on the three lower stationary balls was measured, averaged, and reported. 2. Test Results ASTM Reference Fluid Wear Scar Diameter, mm, l67F ., 1 hour 635 Steel-on-Steel Steel-on-Bronze 4 Kg 10 Kg 40 Kg 4. Kg 10 Kg 40 Kg 1-A-l 2-B-l 3-C-l 4-D.-1 5-D-l 6-E-l 0.21 0.49 0.27 0.32 0.21 0.52 0.24 0.63 0.37 0.32 0.24 0.59 0.57 ' 1.05 0.55 0-79 o. 66 0.70 1.52 1.15 0.60 0.8l 0.79 0.80 2.11 1.17 0.82 0.79 1.03 0.85 2.69 1.65 1.05 1.03 1.17 0.98 B. Almen Extreme Pressure Test 1. Procedure and Apparatus An Almen EP testing machine was used in which a l/4 inch diameter drill rod journal is rotated at 600 rpm between the halves of a split bushing, the complete assembly being inversed in the test oil. After a 30 second no load break-in period, two pound weights are added to the loading system at 10-second intervals until seizure occurs or 50 pounds have been added. The loading system is such that the load is applied to the bushing halves DSW 622144 STLCOPCB4096176 APPENDIX - ASTM COOPERATIVE TESTS Section VII Page 2 with each two-pound weight equivalent to 1,000 lbs. per sq. in. on the projected bearing area. The passing load for a completed 10-second interval is recorded along with the torque in pounds at the end of the interval. Duplicate runs were made and the average is reported. The test specimens (rod and split bushings) were obtained from Laboratory Equipment Company, Mooresville, Indiana. Prior to the test they are washed with Skellysolve B and acetone. 2. Test Results ASTM Reference Fluid Almen Passing Load Pounds Almen Passing Torque Pounds 1-A-l 2-B-l 3-C-l 4-D-l. 5-D-l 6-E-l 14 21 8 12 50 50 50 38 50 47 39 DSW 622145 STLCOPCB4096177 APPENDIX ASTM COOPERATIVE TESTS Section VIII - Stability A. Oxidation - D-945 1. Procedure and Apparatus The Oxidation Characteristics of Inhibited Steam-Turbine . Oils method was conducted according to the procedure outlined in ASTM Standard Method: D-945-54. A 250-ml. filter flask fitted with a stopper and glass tube extending down into the flask was added to. the oxygen inlet system between the flow meters and oxida tion tubes. Distilled water was maintained in this flask to a depth of about 5/4 inch on the center inlet tube. Oxygen bubbled through this water and passed on to the oxidation tubes resulted in slower removal of water from the oxidation tubes in the cases where the water layer is lighter than the oil layer. Neutraliza tion values were run by a potentiometric method, ASTM Designation: D-664-54, with results reported as total acid number (TAN) or total base number (TBN), mg. KOH per gm. 2. Test Results Refer to Table 1 following. B. Oxidation and Corrosion Test 1. Procedure and Apparatus The procedure and apparatus used in this test is outlined and described in Federal Test Method Standard No. 791 j Method 5308.4. 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