1、Designation: D4636 09D4636 14Standard 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 Scope*1.1 This test method
4、covers 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 with
5、out metal 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 te
6、mperature, 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 mea
7、surement 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
8、 the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:3D91 Test Method for Precipitation Number of Lubricating OilsD445 Test Method for Kinem
9、atic 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 Indicator Titratio
10、n2.2 U.S. Federal Test Method Standards:4FED-STD-791 Testing Method 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)1
11、 This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.09.0D on Oxidation of Lubricants.Current edition approved Dec. 1, 2009July 1, 2014. Published December 2009July 2014. Ori
12、ginally approved in 1986. Last previous edition approved in 20042009 asD463699(2004)D4636 09. 1. DOI: 10.1520/D4636-09.10.1520/D4636-14.2 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 reference
13、dASTM 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.4 Available from the Standardization Document Order Desk, 700 Robbins, Avenu
14、e, Building 4D, Philadelphia PA 19111-5094 (http:/assist.daps.dla.mil).This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depi
15、ct all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM Internation
16、al, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1MIL-S-13282 Refined Silver (99.95) (P07015)2.3 Other Standards:5AMS 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-
17、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. 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 proc
18、edure (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 specimens stacked on the air tube, 200 mL of testoil, 10 L/h air flow rate, and periodic test oil withdrawal and evaluation. Alternative Procedure 1
19、 uses washer-shaped metalspecimens, 165 mL of test oil, 10 L/h air flow rate, and no periodic test oil sampling. Alternative Procedure 2 uses square metalspecimens tied together resting vertically in the large glass tube, 100 mL of test oil, 5 L/h air flow rate, and no periodic test oilsampling.NOTE
20、 1Flow rates other than those listed in this test method may be required by various specifications; if they are so used, 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 ba
21、th and heated forthe specified number of hours while air is passed through the oil to provide agitation and a source of oxygen. Typically,temperatures of the bath used are from 100C to 360C. Weighed metal specimens are placed in the tube during the test.Corrosiveness of the oil is determined by loss
22、 in metal mass, and microscopic examination of the sample metal surface(s). Oilsamples are withdrawn from the test oil and checked for changes in viscosity and acid number as a result of the oxidation reactions.3.3 Metals used in the basic test and alternative Procedure 1 are titanium, magnesium, st
23、eel (two types), bronze, silver, andaluminum. Metals used in alternative Procedure 2 are copper, steel, aluminum, 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 fina
24、l viscosity and acid number are determined for comparison with those of the original untested oil.3.5 At the 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 gravimetricall
25、y.3.6 Air is used dry in the standard test. A humidifier may be used to provide controlled moist air, if required.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
26、 measurable results to be obtained in a reasonable time. The use of metals provides catalyticreactive surfaces 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
27、 realistic condition that encourages oil breakdownby facilitating acid formation.4.2 Interpretation of results 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 cor
28、roded appearance of somemetals; change of viscosity; increase in acid number; measurable reaction products in 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
29、 test conditions will yield rather drastic changes to the oil.5. Apparatus5.1 The main apparatus consists of the following items of standard wall borosilicate glassware as shown in Figs. 1-5:5.1.1 Main Sample Tube (Fig. 1).5.1.2 Sample Tube Head (Fig. 2).5 See ASTM DS 56, Metal and Alloys in the Uni
30、fied Numbering System.D4636 1425.1.3 Air Tube6(Fig. 3).5.1.4 Condenser, Allihn 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
31、 glass, standard wall, 9-mm outside diameter, 6-mm length.5.2.2 Oil Sampling Tube, Borosilicate Glass, 4-mm outside diameter, with sampling end approximately 600 mm to reach intothe main sample tube. The tube is bent U-shape with exit end fitted by a one-hole stopper to a 25-mL filtering flask. The
32、exit endmay be any convenient length.5.2.3 Adapter, 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 60.5C of test temperature with an immersion depth of 250 6 20 mm. Oilbaths or alum
33、inum block baths are recommended, but above 220C, use aluminum block bath or other similar non-oil-type heatingmedium. (WarningThere are exposed hot surfaces on apparatus. Avoid contact with exposed skin by use of protectiveequipment as required.)5.3.2 Hood, ventilation to adequately remove fumes du
34、ring heating.5.3.3 Air Supply, free of reactive contaminants. For dry air, dew point is 68C maximum; for moist air, moisture is 10 6 1mg water/L air, standard conditions of 21C/105 kPa.5.3.4 Flowmeter, capable of measuring 10 6 1 L/h at same standard conditions as in 5.3.3.5.3.5 Balance, analytical,
35、 sensitivity 0.1 mg.6 An 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 standard procedure.FIG. 1 Sample TubeD4636 1435.3.6 Balance, Laboratory, 2500-g capacity, 0.1-g sensitivity.5.3.7 Centrifuge, capable of relative for
36、ce of 840 6 40 relative centrifugal force at the tip of the tubes.5.3.8 Centrifuge Tubes, Test Method D91, cone-shaped, 100 mL.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 W
37、ire, for tying metal squares together. 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 aircharacteri
38、stics of 5.3.3 are attained. For drying, 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
39、moist air.5.3.13 Oven, optional, to dry glassware at elevated temperature.5.3.14 Forceps, stainless steel.5.3.15 Thermocouple7,70 cm sheathed.5.3.16 Brush, short-bristled, stiff (typewriter-cleaning brush or equivalent).6. Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall be
40、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 such7 A resistance temperature device (RTD) is also acceptable.FIG. 2 Sample Tube HeadD4636 144specifications ar
41、e available.8 Other grades may be 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
42、 defined bySpecification D1193. Referee situations require Type II distilled water defined by Specification D1193.6.3 Metal Specimens:9, 106.3.1 Washer-Shaped Metal Specimens, 6.35-mm inside diameter by 19.05-mm (34-in.) outside diameter by 0.81 mm thick inthe following metals:R56080 Titanium 8 % Mn
43、M11311 Magnesium AZ31BT11350 Steel M50G10100 Steel grade 1010C65900 Silicon-iron-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-mm by 25.4-mm square in the following metals:C11000 Copper (ETP)G10100 Steel Grade 1010A92024
44、Aluminum Alloy 2024 T-3 or T-4M11311 Magnesium AZ31BL01900 Cadmium Anod8 Reagent Chemicals, American 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
45、Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.9 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-
46、0707.10 If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee 1, which you may attend.FIG. 3 Air TubeD4636 145FIG. 4 Condenser, Allihn TypeFIG.
47、 5 Assembled ApparatusD4636 1466.4 Abrasive Paper, silicon carbide, various grades, including carbide of 240 and 400-grit. Many papers, including “wet “Wetor dry,” “waterproof,” or iron-containing abrasives, such as natural emery, are not satisfactory.6.4.1 Silicon-Carbide Grains, 150 mesh.6.5 Cotto
48、n, 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:11n-Heptane or toluene.6.10 Carbon Remover for Glassware12, 10(
49、WarningCauses severe burns.)Mix 35 mL of saturated sodium dichromate(aqueous) solution and 1000 mL of concentrated sulfuric acid. (WarningCorrosive.)6.11 Glassware Cleaning Solution (WarningCauses severe burns.)Mix 35 mL of MICRO13 in water or 35 mL ofNOCHROMIX14 and 1000 mL of concentrated sulfuric acid.6.12 Metal Cleaning SolutionMix equal parts of 15 g NaOH per litre of water and 15 g of Na3PO4 per litre of water.(WarningCorrosive.)7. Hazards7.1 As this test method investigates the corrosive effect of oil on metal in an artificial environment,
