1、Designation: D 4636 99 (Reapproved 2004)e1An American National StandardStandard Test Method forCorrosiveness and Oxidation Stability of Hydraulic Oils,Aircraft Turbine Engine Lubricants, and Other HighlyRefined Oils1This standard is issued under the fixed designation D 4636; the number immediately f
2、ollowing the designation indicates the year 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 (e) indicates an editorial change since the last revision or reapproval.This standard has been a
3、pproved for use by agencies of the Department of Defense.e1NOTEWarning notes were editorially moved into the standard text in May 2004.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 t
4、he new test method is basically Method 5307.2expanded to include Method 5308.7.1. Scope1.1 This test method covers the testing of hydraulic oils,aircraft turbine engine lubricants, and other highly refined oilsto determine their resistance to oxidation and corrosion degra-dation and their tendency t
5、o corrode various metals. Petroleumand synthetic fluids may be evaluated using moist or dry airwith or without metal test specimens.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 me
6、thod, it will be upto the particular specification to establish the conditionsrequired. In addition to temperature, the variables 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 me
7、tal specimen(s).1.3 The values stated in SI units are to be regarded asstandard. The values in parentheses are for information only.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 of this standard to establ
8、ish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D91 Test Method for Precipitation Number of LubricatingOilsD 445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (the C
9、alculation of Dynamic Viscos-ity)D 664 Test Method forAcid Number of Petroleum Productsby Potentiometric TitrationD 1193 Specification for Reagent WaterD 3339 Test Method for Acid Number of Petroleum Prod-ucts by Semi-Micro Color Indicator Titration2.2 U.S. Federal Test Method Standards:3Method 5307
10、.2 Corrosiveness and Oxidation Stability ofAircraft Turbine Engine LubricantsMethod 5308.7 Corrosiveness and Oxidation Stability ofLight Oils (Metal Squares)MIL-S-13282 Refined Silver (99.95) (P07015)2.3 Other Standards:4AMS 4616 Silicon Iron Bronze (C65900)AMS 4908 Titanium Alloy(8 % Mn) Annealed (
11、R56080)AMS 6490 Steel (M50) (T11350)1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.09.0D on Oxidation of Lubricants.Current edition approved May 17, 2004. Published May 2004. Originallyapproved
12、 in 1986. Withdrawn 1994 and reinstated January 1997. Last previousedition approved in 1999 as D 4636 99.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standar
13、ds Document Summary page onthe ASTM website.3Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.4See ASTM DS 56, Metal and Alloys in the Unified Numbering System.1Copyright ASTM International, 100 Barr Harbor Drive, PO Bo
14、x C700, West Conshohocken, PA 19428-2959, United States.QQ-A-671 Cadmium Anod (L01900)QQ-C-576 Copper Electrolytic Tough Pitch (ETP)(C11000)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 (A
15、92024)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 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 f
16、low rate, and periodic test oilwithdrawal 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,
17、 100 mL of test oil, 5 L/h airflow rate, 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 contain
18、ing a sample of oil and metalspecimens 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 (212F) to 360C(680F). Weighed metal specim
19、ens are placed in the tubeduring the test. Corrosiveness of the oil is determined by lossin metal mass, and microscopic examination of the samplemetal surface(s). Oil samples are withdrawn from the test oiland checked for changes in viscosity and acid number as aresult of the oxidation reactions.3.3
20、 Metals used in the basic test and alternative Procedure 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 peri
21、odicallythroughout the test. Alternatively, no periodic 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-
22、gation. Also, the quantity of oil lost during the test 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 lubric
23、ating fluids in actual service and usesan accelerated 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 oxid
24、ation reactions that are expected to occur.Moisture in 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 wil
25、l cause one or more of the followingmeasurable effects: 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 containing
26、oxidation and corrosion inhibitors. Without such ingredient(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
27、Sample Tube Head (Fig. 2).FIG. 1 Sample TubeD 4636 99 (2004)e125.1.3 Air Tube5(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 M
28、etal Specimen), of borosilicate glass,standard wall, 9-mm outside 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
29、 25-mL filtering flask. Theexit end may be any convenient length.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(61F) of test temperature with an immersion depth
30、of 250 620 mm. Oil baths or aluminum block baths are recommended,but above 220C (428F), use aluminum block bath or othersimilar non-oil-type heating medium. (WarningThere areexposed hot surfaces on apparatus.Avoid contact with exposedskin by use of protective equipment as required.)5.3.2 Hood, venti
31、lation to adequately remove fumes duringheating.5.3.3 Air Supply, free of reactive contaminants. For dry air,dew point is 68C (90F) maximum; for moist air, moistureis 10 6 1 mg water/L air, standard conditions of 21C(70F)/105 kPa (1 atm).5.3.4 Flowmeter, capable of measuring 10 6 1 L/h at samestanda
32、rd conditions as in 5.3.3.5.3.5 Balance, analytical, sensitivity 0.1 mg.5.3.6 Balance, Laboratory, 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,100 mL
33、.5.3.9 Microscope, with 20-diameter magnification.5An 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 HeadD 4636 99 (2004)e135.3.10 Assembly Fixture, wood (slotted to hold metalsquares
34、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 or humidifier.
35、The method used is optional provided theair characteristics of 5.3.3 are attained. For drying, a satisfac-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 devi
36、ce is included in Appendix X1 to provide therequired moist air.5.3.13 Oven, optional, to dry glassware at elevated tempera-ture.5.3.14 Forceps, stainless steel.5.3.15 Thermocouple6, 70 cm (27.6 in.) sheathed.5.3.16 Brush, short-bristled, stiff (typewriter-cleaning brushor equivalent).6. Reagents and
37、 Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.7Other grades ma
38、y be usedprovided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.6.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Specification D 1193.
39、 Referee situations require Type IIdistilled water defined by Specification D 1193.6.3 Metal Specimens:8, 96.3.1 Washer-Shaped Metal Specimens, 6.35-mm (14-in.)inside diameter by 19.05-mm (34-in.) outside diameter by 0.81mm (0.032 in.) thick in the following metals:R56080 Titanium 8 % MnM11311 Magne
40、sium AZ31BT11350 Steel M50G10100 Steel grade 1010C65900 Silicon-iron-bronzeP07015 Silver 99.95A92024 Aluminum Alloy 2024 T-3 or T-46A resistance temperature device (RTD) is also acceptable.7Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For su
41、ggestions 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 Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.8The sole source of supply
42、of the metal specimens known to the committee atthis time is Metaspec Co., P.O. Box 27702, San Antonio, TX 78227-0707.9If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of the r
43、esponsible technical committee1, which you may attend.FIG. 3 Air TubeFIG. 4 Condenser, Allihn TypeD 4636 99 (2004)e146.3.2 Square-Shaped Metal Specimens (as shown in Fig. 6),0.81-mm (0.032-in.) by 25.4-mm (1-in.) square in the follow-ing metals:C11000 Copper (ETP)G10100 Steel Grade 1010A92024 Alumin
44、um Alloy 2024 T-3 or T-4M11311 Magnesium AZ31BL01900 Cadmium Anod6.4 Abrasive Paper, silicon carbide, various grades, includ-ing 240 and 400-grit. Many papers, including “wet or dry,”“waterproof,” or iron-containing abrasives, such as naturalemery are not satisfactory.6.4.1 Silicon-Carbide Grains, 1
45、50 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 Acid, concentrated. (WarningPoison. Corro-sive. Strong oxidizer.)6.9 Degreasing Solvents:10n-Heptane or toluene.6.10 Carbon Remover for
46、Glassware11, 9(WarningCauses severe burns.)Mix 35 mL of saturated sodiumdichromate (aqueous) solution and 1000 mL of concentratedsulfuric acid. (WarningCorrosive.)6.11 Glassware Cleaning Solution (WarningCauses se-vere burns.)Mix 35 mL of MICRO12in water or 35 mL ofNOCHROMIX13and 1000 mL of concentr
47、ated 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 As this test method investigates the corrosive effect ofoil on metal in an artificial environment, precautions must betaken to prevent p
48、remature oxidation of metal specimens bystray chemicals during test preparations. The cleaned speci-mens shall be touched only by surfaces known to be free ofinterfering contaminants. Do not touch cleaned specimen(s)with hands. Maintain clean glassware (see Appendix X2)inadust-free cabinet; rinse ag
49、ain 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 the required number and types of specimens tobe used in the test method. Measure the diameter of eachspecimen and specimen hole to
