1、Designation: D4636 09Standard 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 oforigi
2、nal 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 Department of Def
3、ense.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. Scope1.1 This test method covers the testing of
4、 hydraulic oils,aircraft turbine engine lubricants, and other highly refined oilsto determine their resistance to oxidation and corrosion degra-dation and their tendency to corrode various metals. Petroleumand synthetic fluids may be evaluated using moist or dry airwith or without metal test specime
5、ns.1.2 This test method consists of a standard test procedure,an alternative Procedure 1, and an alternative Procedure 2. Asthere are variations possible with this test method, it will be upto the particular specification to establish the conditionsrequired. In addition to temperature, the variables
6、 to specify ifother than those of the standard procedure or alternativeProcedure 1 or 2 are: test time, air flow and humidity, samplefrequency, test fluid quantity, and metal specimen(s).1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in th
7、isstandard.1.3.1 ExceptionThe values in parentheses in some of thefigures 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 thesafety concerns, if any, associated with its use. It is theresponsibility of the user
8、 of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:3D91 Test Method for Precipitation Number of LubricatingOilsD445 Test Method for Kinematic Viscosity of Transparen
9、tand Opaque Liquids (and Calculation of Dynamic Viscos-ity)D664 Test Method for Acid Number of Petroleum Productsby Potentiometric TitrationD1193 Specification for Reagent WaterD3339 Test Method for Acid Number of Petroleum Prod-ucts by Semi-Micro Color Indicator Titration2.2 U.S. Federal Test Metho
10、d Standards:4FED-STD-791 Testing Method of Lubricants, Liquid Fuels,and Related ProductsMethod 5307.2 Corrosiveness and Oxidation Stability ofAircraft Turbine Engine Lubricants (Withdrawn)Method 5308.7 Corrosiveness and Oxidation Stability ofLight Oils (Metal Squares)MIL-S-13282 Refined Silver (99.9
11、5) (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-C-576 Copper Electrolytic Tough Pitch (ETP)(C11000)1This test method is under the jurisdiction of ASTM Committee D02 onP
12、etroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.09.0D on Oxidation of Lubricants.Current edition approved Dec. 1, 2009. Published December 2009. Originallyapproved in 1986. Last previous edition approved in 2004 as D463699(2004)1.DOI: 10.1520/D4636-09.2FED-STD-79
13、1D is the parent document containing both test methods. As ofpublication on Nov. 6, 2009, it no longer contains withdrawn Method 5307.2.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume in
14、formation, refer to the standards Document Summary page onthe ASTM website.4Available from the Standardization Document Order Desk, 700 Robbins,Avenue, Building 4D, Philadelphia PA 19111-5094 (http:/assist.daps.dla.mil).5See ASTM DS 56, Metal and Alloys in the Unified Numbering System.1Copyright AST
15、M International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.QQ-M-44 MagnesiumAlloyAZ31B 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
16、 test method consists of a standard test procedure(see 10.1), an alternative Procedure 1 (see 10.2), and analternative Procedure 2 (see 10.3). The standard test procedureuses washer-shaped metal specimens stacked on the air tube,200 mL of test oil, 10 L/h air flow rate, and periodic test oilwithdraw
17、al and evaluation. Alternative Procedure 1 useswasher-shaped metal specimens, 165 mL of test oil, 10 L/h airflow rate, and no periodic test oil sampling. AlternativeProcedure 2 uses square metal specimens tied together restingvertically in the large glass tube, 100 mL of test oil, 5 L/h airflow rate
18、, and no periodic test oil sampling.NOTE 1Flow rates other than those listed in this test method may berequired by various specifications; if they are so used, the modification tothe test method should be stated in the test report.3.2 A large glass tube containing a sample of oil and metalspecimens
19、is placed in a constant temperature bath and heatedfor the specified number of hours while air is passed throughthe 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.Corrosiven
20、ess of the oil is determined by loss in metal mass,and microscopic examination of the sample metal surface(s).Oil samples are withdrawn from the test oil and checked forchanges in viscosity and acid number as a result of theoxidation reactions.3.3 Metals used in the basic test and alternative Proced
21、ure 1are titanium, magnesium, steel (two types), bronze, silver, andaluminum. Metals used in alternative Procedure 2 are copper,steel, aluminum, magnesium, and cadmium. Other metals maybe specified.3.4 Sampling of the oil for analysis is done periodicallythroughout the test. Alternatively, no period
22、ic samples aretaken and a final viscosity and acid number are determined forcomparison with those of the original untested oil.3.5 At the end of the test, the amount of sludge present inthe oil remaining in the same tube is determined by centrifu-gation. Also, the quantity of oil lost during the tes
23、t isdetermined gravimetrically.3.6 Air is used dry in the standard test.Ahumidifier may beused to provide controlled moist air, if required.4. Significance and Use4.1 This test method simulates the environment encounteredby fully formulated lubricating fluids in actual service and usesan accelerated
24、 oxidation rate to permit measurable results to beobtained in a reasonable time. The use of metals providescatalytic reactive surfaces of those materials commonly foundin real systems. The high temperature and air agitation helpaccelerate the oxidation reactions that are expected to occur.Moisture i
25、n the air adds another realistic condition thatencourages oil breakdown by facilitating acid formation.4.2 Interpretation of results should be done by comparisonwith data from oils of known field performance. The acceler-ated conditions likely will cause one or more of the followingmeasurable effect
26、s: mass change and corroded appearance ofsome metals; change of viscosity; increase in acid number;measurable reaction products in the form of sludge; and massloss of oil due to evaporation.4.3 This test method is most suitable for oils containingoxidation and corrosion inhibitors. Without such ingr
27、edient(s),the severe test conditions will yield rather drastic changes tothe oil.5. Apparatus5.1 The main apparatus consists of the following items ofstandard 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).FIG. 1 Sample TubeD4636 092
28、5.1.3 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 accessoriesneeded are:5.2.1 Spacers (for Metal Specimen), of borosilicate glass,standard wall, 9-mm outsi
29、de diameter, 6-mm length.5.2.2 Oil Sampling Tube, Borosilicate Glass, 4-mm outsidediameter, with sampling end approximately 600 mm to reachinto the main sample tube. The tube is bent U-shape with exitend fitted by a one-hole stopper to a 25-mL filtering flask. Theexit end may be any convenient lengt
30、h.5.2.3 Adapter, polytetrafluoroethylene for 10/18 joint forsealing of air tube to sample tube head.5.3 Other items and equipment are:5.3.1 Heating Bath, constant temperature within 60.5C oftest temperature with an immersion depth of 250 6 20 mm. Oilbaths or aluminum block baths are recommended, but
31、 above220C, use aluminum block bath or other similar non-oil-typeheating medium. (WarningThere are exposed hot surfaceson apparatus. Avoid contact with exposed skin by use ofprotective equipment as required.)5.3.2 Hood, ventilation to adequately remove fumes duringheating.5.3.3 Air Supply, free of r
32、eactive contaminants. For dry air,dew point is 68C maximum; for moist air, moisture is 10 61 mg water/L air, standard conditions of 21C/105 kPa.5.3.4 Flowmeter, capable of measuring 10 6 1 L/h at samestandard conditions as in 5.3.3.5.3.5 Balance, analytical, sensitivity 0.1 mg.5.3.6 Balance, Laborat
33、ory, 2500-g capacity, 0.1-g sensitiv-ity.5.3.7 Centrifuge, capable of relative force of 840 6 40relative centrifugal force at the tip of the tubes.5.3.8 Centrifuge Tubes, Test Method D91, cone-shaped, 100mL.5.3.9 Microscope, with 20-diameter magnification.5.3.10 Assembly Fixture, wood (slotted to ho
34、ld metalsquares for tying with cord) as shown in Fig. 6.5.3.11 Cord or Wire, for tying metal squares together.Suitable cord should be lightweight of cleaned linen, cotton,nylon, or ceramic fiber; suitable wire is nichrome or tantalum.5.3.12 When air must be conditioned, there is need for an airdrier
35、 or humidifier. The method used is optional provided the6An 800-mm air tube may be used for alternate Procedure 1 or 2 when using thecondenser as opposed to the sample tube head in the standard procedure.FIG. 2 Sample Tube HeadD4636 093air characteristics of 5.3.3 are attained. For drying, a satisfa
36、c-tory method is the use of a glass column containing 8-meshanhydrous calcium sulfate with a column diameter such thatvelocity of air does not exceed 1.2 m/min. For humidifying, asatisfactory device is included in Appendix X1 to provide therequired moist air.5.3.13 Oven, optional, to dry glassware a
37、t elevated tempera-ture.5.3.14 Forceps, stainless steel.5.3.15 Thermocouple7, 70 cm sheathed.5.3.16 Brush, short-bristled, stiff (typewriter-cleaning brushor equivalent).6. Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it i
38、s intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.8Other grades may be usedprovided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without
39、lessening the accuracy ofthe determination.6.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Specification D1193. Referee situations require Type IIdistilled water defined by Specification D1193.6.3 Metal Specimens:9, 106.3.1 Was
40、her-Shaped Metal Specimens, 6.35-mm inside di-ameter by 19.05-mm (34-in.) outside diameter by 0.81 mmthick in the following metals:R56080 Titanium 8 % MnM11311 Magnesium AZ31BT11350 Steel M50G10100 Steel grade 1010C65900 Silicon-iron-bronzeP07015 Silver 99.95A92024 Aluminum Alloy 2024 T-3 or T-46.3.
41、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 Aluminum Alloy 2024 T-3 or T-4M11311 Magnesium AZ31BL01900 Cadmium Anod7A resistance temperature device (RTD) is also acceptable.8Reagent Chemicals,
42、 American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National For
43、mulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.9The sole source of supply of the metal specimens known to the committee atthis time is Metaspec Co., P.O. Box 27702, San Antonio, TX 78227-0707.10If you are aware of alternative suppliers, please provide this information toASTM Intern
44、ational Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee1, which you may attend.FIG. 3 Air TubeFIG. 4 Condenser, Allihn TypeD4636 0946.4 Abrasive Paper, silicon carbide, various grades, includ-ing 240 and 400-grit. Many papers, inclu
45、ding “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 in-haled.)6.7 Acetone.(WarningExtremely flammable. Vaporsmay cause flash-fire.)6.8 Nitric A
46、cid, concentrated. (WarningPoison. Corro-sive. Strong oxidizer.)6.9 Degreasing Solvents:11n-Heptane or toluene.6.10 Carbon Remover for Glassware12, 10(WarningCauses severe burns.)Mix 35 mL of saturated sodiumdichromate (aqueous) solution and 1000 mL of concentratedsulfuric acid. (WarningCorrosive.)6
47、.11 Glassware Cleaning Solution (WarningCauses se-vere burns.)Mix 35 mL of MICRO13in water or 35 mL ofNOCHROMIX14and 1000 mL of concentrated sulfuric acid.6.12 Metal Cleaning SolutionMix equal parts of 15 gNaOH per litre of water and 15 g of Na3PO4per litre of water.(WarningCorrosive.)7. Hazards7.1
48、As this test method investigates the corrosive effect ofoil on metal in an artificial environment, precautions must betaken to prevent premature oxidation of metal specimens bystray chemicals during test preparations. The cleaned speci-mens shall be touched only by surfaces known to be free ofinterf
49、ering contaminants. Do not touch cleaned specimen(s)with hands. Maintain clean glassware (see Appendix X2)inadust-free cabinet; rinse again and dry if clean glass has beenstored unused for more than a week.7.2 Heating Bath, n-heptane, toluene, acetone, carbon re-mover, nitric and sulfuric acids, and sodium hydroxide allrequire caution in handling as detailed in 5.3.1 and 6.6-6.12.8. Sampling8.1 As this test method is performed on uniform, finishedoils, no special sampling procedure is needed for this oil.8.2 Preparation of Metal Specimens:8.2.1 Collect t
