1、Designation: D4636 14D4636 17Standard Test Method forCorrosiveness and Oxidation Stability of Hydraulic Oils,Aircraft Turbine Engine Lubricants, and Other HighlyRefined Oils1This standard is issued under the fixed designation D4636; the number immediately following the designation indicates the year
2、 oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Depa
3、rtment of Defense.INTRODUCTIONThis test method is the result of combining Federal Test Methods 5307.2 and 5308.7. Features anddetails of both of these test methods are included, but the new test method is basically Method 5307.2expanded to include Method 5308.7.21. Scope*1.1 This test method covers
4、the testing of hydraulic oils, aircraft turbine engine lubricants, and other highly refined oils todetermine their resistance to oxidation and corrosion degradation and their tendency to corrode various metals. Petroleum andsynthetic fluids may be evaluated using moist or dry air with or without met
5、al test specimens.1.2 This test method consists of a standard test procedure, an alternative Procedure 1, and an alternative Procedure 2. As thereare variations possible with this test method, it will be up to the particular specification to establish the conditions required. Inaddition to temperatu
6、re, the variables to specify if other than those of the standard procedure or alternative Procedure 1 or 2 are:test time, air flow and humidity, sample frequency, test fluid quantity, and metal specimen(s).1.3 The values stated in SI units are to be regarded as standard. No other units of measuremen
7、t are included in this standard.1.3.1 ExceptionThe values in parentheses in some of the figures are provided for information only for those using oldequipment based on non-SI units.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the re
8、sponsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.1.5 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in
9、the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:3D91 Test Method for Precipitation Number of Lubricating OilsD445 Test Met
10、hod for Kinematic Viscosity of Transparent and Opaque Liquids (and Calculation of Dynamic Viscosity)D664 Test Method for Acid Number of Petroleum Products by Potentiometric TitrationD1193 Specification for Reagent WaterD3339 Test Method for Acid Number of Petroleum Products by Semi-Micro Color Indic
11、ator Titration1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.09.0D on Oxidation of Lubricants.Current edition approved July 1, 2014June 1, 2017. Published July 2014June 2017. Or
12、iginally approved in 1986. Last previous edition approved in 20092014 asD4636 09.D4636 14. DOI: 10.1520/D4636-14.10.1520/D4636-17.2 FED-STD-791D is the parent document containing both test methods. As of publication on Nov. 6, 2009, it no longer contains withdrawn Method 5307.2.3 For referencedASTM
13、standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of
14、an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as publ
15、ished by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States12.2 U.S. Federal Test Method Standards:4FED-STD-791 Testing Metho
16、d of Lubricants, Liquid Fuels, and Related ProductsMethod 5307.2 Corrosiveness and Oxidation Stability of Aircraft Turbine Engine Lubricants (Withdrawn)Method 5308.7 Corrosiveness and Oxidation Stability of Light Oils (Metal Squares)MIL-S-13282 Refined Silver (99.95) (P07015)2.3 Other Standards:5AMS
17、 4616 Silicon Iron Bronze (C65900)AMS 4908 Titanium Alloy(8 % Mn) Annealed (R56080)AMS 6490 Steel (M50) (T11350)QQ-A-671 Cadmium Anod (L01900)QQ-C-576 Copper Electrolytic Tough Pitch (ETP) (C11000)QQ-M-44 Magnesium Alloy AZ31B Condition H24 or H26 (M11311)QQ-S-698 Low-Carbon Steel 1010, CR Temper No
18、. 4 or 5 (G10100)QQ-A-250/4 Aluminum Alloy 2024 T-3 or T-4 (A92024)3. Summary of Test Method3.1 This test method consists of a standard test procedure (see 10.1), an alternative Procedure 1 (see 10.2), and an alternativeProcedure 2 (see 10.3). The standard test procedure uses washer-shaped metal spe
19、cimens stacked on the air tube, 200 mL 200 mLof test oil, 1010 L L/h h air flow rate, and periodic test oil withdrawal and evaluation.Alternative Procedure 1 uses washer-shapedmetal specimens, 165 mL 165 mL of test oil, 1010 L L/h h air flow rate, and no periodic test oil sampling. Alternative Proce
20、dure2 uses square metal specimens tied together resting vertically in the large glass tube, 100 mL 100 mL of test oil, 55 L L/h h airflow rate, and no periodic test oil sampling.NOTE 1Flow rates other than those listed in this test method may be required by various specifications; if they are so use
21、d, the modification to thetest method should be stated in the test report.3.2 A large glass tube containing a sample of oil and metal specimens is placed in a constant temperature bath and heated forthe specified number of hours while air is passed through the oil to provide agitation and a source o
22、f oxygen. Typically,temperatures of the bath used are from 100C100 C to 360C.360 C. Weighed metal specimens are placed in the tube during thetest. Corrosiveness of the oil is determined by loss in metal mass, and microscopic examination of the sample metal surface(s).Oil samples are withdrawn from t
23、he test oil and checked for changes in viscosity and acid number as a result of the oxidationreactions.3.3 Metals used in the basic test and alternative Procedure 1 are titanium, magnesium, steel (two types), bronze, silver, andaluminum. Metals used in alternative Procedure 2 are copper, steel, alum
24、inum, magnesium, and cadmium. Other metals may bespecified.3.4 Sampling of the oil for analysis is done periodically throughout the test. Alternatively, no periodic samples are taken anda final viscosity and acid number are determined for comparison with those of the original untested oil.3.5 At the
25、 end of the test, the amount of sludge present in the oil remaining in the same tube is determined by centrifugation.Also, the quantity of oil lost during the test is determined gravimetrically.3.6 Air is used dry in the standard test. A humidifier may be used to provide controlled moist air, if req
26、uired.4. Significance and Use4.1 This test method simulates the environment encountered by fully formulated lubricating fluids in actual service and uses anaccelerated oxidation rate to permit measurable results to be obtained in a reasonable time. The use of metals provides catalyticreactive surfac
27、es of those materials commonly found in real systems. The high temperature and air agitation help accelerate theoxidation reactions that are expected to occur. Moisture in the air adds another realistic condition that encourages oil breakdownby facilitating acid formation.4.2 Interpretation of resul
28、ts should be done by comparison with data from oils of known field performance. The acceleratedconditions likely will cause one or more of the following measurable effects: mass change and corroded appearance of somemetals; change of viscosity; increase in acid number; measurable reaction products i
29、n the form of sludge; and mass loss of oil dueto evaporation.4.3 This test method is most suitable for oils containing oxidation and corrosion inhibitors. Without such ingredient(s), thesevere test conditions will yield rather drastic changes to the oil.4 Available from the Standardization Document
30、Order Desk, 700 Robbins, Avenue, Building 4D, Philadelphia PA 19111-5094 (http:/assist.daps.dla.mil).5 See ASTM DS 56, Metal and Alloys in the Unified Numbering System.D4636 1725. Apparatus5.1 The main apparatus consists of the following items of standard wall borosilicate glassware as shown in Figs
31、. 1-5:5.1.1 Main Sample Tube (Fig. 1).5.1.2 Sample Tube Head (Fig. 2).FIG. 1 Sample TubeD4636 1735.1.3 Air Tube (Note 2, Fig. 3).NOTE 2An 800 mm air tube may be used for alternate Procedure 1 or 2 when using the condenser as opposed to the sample tube head in the standardprocedure.5.1.4 Condenser, A
32、llihn Type (Fig. 4).5.1.5 Condenser, Allihn Type, Fig. 4 with 71/60 joint.5.1.6 Assembled Apparatus (Fig. 5).5.2 Additional glassware items and assembly accessories needed are:5.2.1 Spacers (for Metal Specimen), of borosilicate glass, standard wall, 9-mm9 mm outside diameter, 6-mm6 mm length.5.2.2 O
33、il Sampling Tube, Borosilicate Glass, 4-mm4 mm outside diameter, with sampling end approximately 600 mm 600 mmto reach into the main sample tube. The tube is bent U-shape with exit end fitted by a one-hole stopper to a 25-mL25 mL filteringflask. The exit end may be any convenient length.5.2.3 Adapte
34、r, polytetrafluoroethylene for 10/18 joint for sealing of air tube to sample tube head.5.3 Other items and equipment are:5.3.1 Heating Bath, constant temperature within 60.5C60.5 C of test temperature with an immersion depth of 250250 mm6 20 mm. 20 mm. Oil baths or aluminum block baths are recommend
35、ed, but above 220C,220 C, use aluminum block bath orother similar non-oil-type heating medium. (WarningThere are exposed hot surfaces on apparatus. Avoid contact with exposedskin by use of protective equipment as required.)5.3.2 Hood, ventilation to adequately remove fumes during heating.5.3.3 Air S
36、upply, free of reactive contaminants. For dry air, dew point is 68C68 C maximum; for moist air, moisture is1010 mg 6 1 mg1 mg water water/L L air, standard conditions of 21C/105 21 CkPa.105 kPa.5.3.4 Flowmeter, capable of measuring 1010 Lh 6 11 L L/h h at same standard conditions as in 5.3.3.5.3.5 B
37、alance, analytical, sensitivity 0.1 mg.0.1 mg.FIG. 2 Sample Tube HeadD4636 174FIG. 3 Air TubeFIG. 4 Condenser, Allihn TypeFIG. 5 Assembled ApparatusD4636 1755.3.6 Balance, Laboratory, 2500-g2500 g capacity, 0.1-g0.1 g sensitivity.5.3.7 Centrifuge, capable of relative force of 840 6 40 relative centr
38、ifugal force at the tip of the tubes.5.3.8 Centrifuge Tubes, Test Method D91, cone-shaped, 100 mL.5.3.9 Microscope, with 20-diameter magnification.5.3.10 Assembly Fixture, wood (slotted to hold metal squares for tying with cord) as shown in Fig. 6.5.3.11 Cord or Wire, for tying metal squares togethe
39、r. Suitable cord should be lightweight of cleaned linen, cotton, nylon, orceramic fiber; suitable wire is nichrome or tantalum.5.3.12 When air must be conditioned, there is need for an air drier or humidifier. The method used is optional provided the aircharacteristics of 5.3.3 are attained. For dry
40、ing, a satisfactory method is the use of a glass column containing 8-mesh anhydrouscalcium sulfate with a column diameter such that velocity of air does not exceed 1.2 m/min. For humidifying, a satisfactory deviceis included in Appendix X1 to provide the required moist air.5.3.13 Oven, optional, to
41、dry glassware at elevated temperature.5.3.14 Forceps, stainless steel.5.3.15 Thermocouple, ,70 cm sheathed.70 cm sheathed. (See Note 3.)NOTE 3A resistance temperature device (RTD) is also acceptable.5.3.16 Brush, short-bristled, stiff (typewriter-cleaning brush or equivalent).6. Reagents and Materia
42、ls6.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where suchspecifications are available.6 Other grades may be
43、used provided it is first ascertained that the reagent is of sufficiently high purityto permit its use without lessening the accuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water as defined bySpecification D1193. Re
44、feree situations require Type II distilled water defined by Specification D1193.6.3 Metal Specimens:7, 86.3.1 Washer-Shaped Metal Specimens, 6.35-mm6.35 mm inside diameter by 19.05-mm19.05 mm (34-in.) in.) outside diameterby 0.81 mm 0.81 mm thick in the following metals:6 Reagent Chemicals, American
45、 Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary,
46、U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.7 The sole source of supply of the metal specimens known to the committee at this time is Metaspec Co., P.O. Box 27702, San Antonio, TX 78227-0707.8 If you are aware of alternative suppliers, please provide this information to ASTM Internatio
47、nal Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee 1, which you may attend.FIG. 6 Metal Square Dimensions and ArrangementD4636 176R56080 Titanium 8 % MnM11311 Magnesium AZ31BT11350 Steel M50G10100 Steel grade 1010C65900 Silicon-iron-
48、bronzeP07015 Silver 99.95A92024 Aluminum Alloy 2024 T-3 or T-46.3.2 Square-Shaped Metal Specimens (as shown in Fig. 6), 0.81-mm0.81 mm by 25.4-mm25.4 mm square in the followingmetals:C11000 Copper (ETP)G10100 Steel Grade 1010A92024 Aluminum Alloy 2024 T-3 or T-4M11311 Magnesium AZ31BL01900 Cadmium A
49、nod6.4 Abrasive Paper, silicon carbide of 240 and 400-grit. “Wet or dry,” “waterproof,” or iron-containing abrasives, such as naturalemery, are not satisfactory.6.4.1 Silicon-Carbide Grains, 150 mesh.6.5 Cotton, absorbent.6.6 n-Heptane. (WarningFlammable. Harmful if inhaled.)6.7 Acetone. (WarningExtremely flammable. Vapors may cause flash-fire.)6.8 Nitric Acid, concentrated. (WarningPoison. Corrosive. Strong oxidizer.)6.9 Degreasing Solvents:Solvents, n-Heptane or toluene. See Note 4.NOTE 4n-Heptane or toluene have been used in some lab
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