1、Designation: D943 17D943 18 BS 2000-280:1999Standard Test Method forOxidation Characteristics of Inhibited Mineral Oils1This standard is issued under the fixed designation D943; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the y
2、ear 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. Department of Defense.1. Scope*1.1 This test method covers
3、the evaluation of the oxidation stability of inhibited steam-turbine oils in the presence of oxygen,water, and copper and iron metals at an elevated temperature. This test method is limited to a maximum testing time of 10 000 h.This test method is also used for testing other oils, such as hydraulic
4、oils and circulating oils having a specific gravity less thanthat of water and containing rust and oxidation inhibitors.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.2.1 ExceptionThe values in parentheses in the figure
5、s are provided for information for those using old equipment based onnon-SI units.1.3 WARNINGMercury has been designated by many regulatory agencies as a hazardous materialsubstance that can causecentral nervous system, kidney and liver damage. serious medical issues. Mercury, or its vapor, may has
6、been demonstrated to behazardous to health and corrosive to materials. Caution should be taken Use Caution when handling mercury and mercurycontaining mercury-containing products. See the applicable product Material Safety Data Sheet (MSDS) for details and EPAswebsitehttp:/www.epa.gov/mercury/faq.ht
7、mfor additional information. Users should be aware (SDS) for additional informa-tion. The potential exists that selling mercury and/or mercury containing products into your state or country may be prohibited bylaw.or mercury-containing products, or both, is prohibited by local or national law. Users
8、 must determine legality of sales in theirlocation.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and det
9、ermine theapplicability of regulatory limitations prior to use. For specific warning statements, see Section 67.1.5 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of In
10、ternational Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2A510 Specification for General Requirements for Wire Rods and Coarse Round Wire, Carbon Steel (Metric) A0510_A0510MB1 Specifi
11、cation for Hard-Drawn Copper WireD664 Test Method for Acid Number of Petroleum Products by Potentiometric TitrationD1193 Specification for Reagent WaterD3244 Practice for Utilization of Test Data to Determine Conformance with SpecificationsD3339 Test Method for Acid Number of Petroleum Products by S
12、emi-Micro Color Indicator TitrationD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4310 Test Method for Determination of Sludging and Corrosion Tendencies of Inhibited Mineral OilsD5770 Test Method for Semiquantitative Micro Determination of Acid Number of Lubricating Oils Dur
13、ing Oxidation TestingE1 Specification for ASTM Liquid-in-Glass Thermometers1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.09.0C on Oxidation of Turbine Oils.Current edition appr
14、oved June 15, 2017Dec. 1, 2018. Published August 2017February 2019. Originally approved in 1947. Last previous edition approved in 20102017as D943 04a (2010)D943 17.1. DOI: 10.1520/D0943-17.10.1520/D0943-18.In 1976, this test method ceased to be a joint ASTM-IP standard.2 For referencedASTM standard
15、s, 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 an ASTM
16、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 published by
17、 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 States1E2877 Guide for Digital Contact Thermometers2.2 Energy Institute Standard
18、s:3Specifications for IP Standard Thermometers2.3 British Standard:4BS 18293. Terminology3.1 Definitions:3.1.1 acid number, nthe quantity of a specified base, expressed in milligrams of potassium hydroxide per gram of sample,required to titrate a sample in a specified solvent to a specified endpoint
19、 using a specified detection system.4. Summary of Test Method4.1 The oil sample is contacted with oxygen in the presence of water and an iron-copper catalyst at 95 C. The test continuesuntil the measured acid number of the oil is 2.0 mgg or above, acid number being the ratio of the mass of KOH in mi
20、lligrams tothe mass of the oil sample in grams. KOH/g or above. The number of test hours required for the oil to reach the measured acidnumber of 2.0 mgg KOH/g is the “oxidation lifetime.”5. Significance and Use5.1 This test method is widely used for specification purposes and is considered of value
21、 in estimating the oxidation stabilityof lubricants, especially those that are prone to water contamination. It should be recognized, however, that correlation betweenresults of this method and the oxidation stability of a lubricant in field service may vary markedly with field service conditionsand
22、 with various lubricants. The precision statement for this method was determined on steam turbine oils.NOTE 1Furthermore, in the course of testing a lubricant by this method, other signs of deterioration, such as sludge formation or catalyst coilcorrosion, may appear that are not reflected in the ca
23、lculated oxidation lifetime. The subcommittee responsible for this method is investigating theapplication of alternative criteria for evaluation of lubricants using this test apparatus. Test Method D4310 is now available for sludge measurement.6. Apparatus6.1 Oxidation Cell, of borosilicate glass, a
24、s shown in Fig. 1, consisting of a test tube, condenser, and oxygen delivery tube. Thetest tube has a calibration line at 300 mL (maximum error 1 mL). This calibration applies to the test tube alone at 20 C.6.2 Heating Bath, thermostatically controlled, capable of maintaining the oil sample in the o
25、xidation cell at a temperature of95 C 6 0.2 C, fitted with a suitable stirring device to provide a uniform temperature throughout the bath, and large enough tohold the desired number of oxidation cells immersed in the heating bath to a depth of 390 mm 6 10 mm and in the heating liquiditself to a dep
26、th of 355 mm 6 10 mm.NOTE 2Metal block heaters meeting the test method requirements may also be used. It is not known what types of heating baths were used indeveloping the precision statement.6.2.1 Studies have suggested that direct sunlight or artificial light may adversely influence the results o
27、f this test.5 To minimizeeffects of light exposure on the lubricant being tested, light shall be excluded from the lubricant by one or more of the followingways:6.2.1.1 Use of heated liquid baths that are designed and constructed of metal, or combinations of metals and other suitableopaque materials
28、, that prevent light from entering the test cell from the sides is preferred. If a viewing window is included in thedesign, this viewing window shall be fitted with a suitable opaque cover and be kept closed when no observation is being made.6.2.1.2 If glass heating baths are used, the bath shall be
29、 wrapped with aluminum foil or other opaque material.6.2.1.3 Bright light entering the test cell from directly overhead can be eliminated by use of an opaque shield.6.3 Flowmeter, with a capacity of at least 3 Lh of oxygen, and an accuracy of 60.1 Lh.6.4 Heating Bath ThermometerASTM Solvents Distill
30、ation Thermometer having a range from 72 C to 126 C, andconforming to the requirements for Thermometer 40C as prescribed in Specification E1, or for Thermometer 70C as prescribedin Specifications for IP Standard Thermometers. Alternatively, digital contact thermometers such as PRTs (platinum resista
31、ncethermometers), thermistors, or thermocouples in accordance with Specification E2877 of equal or better accuracy may be used.6.5 Oxidation Cell Thermometer,3having a range from 80 C to 100 C, graduated in 0.1 C, total length250 mm, stemdiameter6.0 mm to 7.0 mm, calibrated for 76 mm immersion.6,7 A
32、lternatively, digital contact thermometers such as PRTs,thermistors, or thermocouples in accordance with Specification E2877 of equal or better accuracy may be used.3 Available from Energy Institute, 61 New Cavendish St., London, W1G 7AR, U.K., http:/www.energyinst.org.4 Available from British Stand
33、ards Institution (BSI), 389 Chiswick High Rd., London W4 4AL, U.K., http:/.5 Supporting data (a summary of these results) have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1365.6 The sole source of supply of the Brooklyn thermometer No. 21276
34、-RM known to the committee at this time is the Brooklyn Thermometer Co., Farmingdale, NY.7 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 committe
35、e,1 which you may attend.D943 1826.6 Thermometer Bracket, for holding the oxidation cell thermometer, of 18-8 stainless steel, having the dimensions shown inFig. 2. The thermometer is held in the bracket by two fluoroelastomer O-rings of approximately 5 mm inside diameter.Alternatively, thin stainle
36、ss steel wire may be used.6.7 Wire Coiling Mandrel, as shown in Fig. 3.6.8 Abrasive Cloth, silicon carbide, 100 grit with cloth backing.NOTE 1All dimensions are in millimetres (inches).NOTE 2The oxidation test tube has a calibration line at 300 mL. This calibration applies to the test tube alone at
37、20 C.NOTE 3Open tube ends to be ground and fire-polished.FIG. 1 Oxidation CellD943 1836.9 Syringes, glass, with Luer-Lok locking connectors, 10 mL and 50 mL capacities for sampling, and water additions,respectively.6.10 Syringe Sampling Tube, Grade 304 stainless steel tubing, 2.11 mm in outside diam
38、eter, 1.60 mm in inside diameter,559 mm 6 2 mm long, with one end finished at 90 and the other end fitted with a Luer-Lok female connector. The Luer-Lokconnector is preferably of elastomeric material, such as polyfluorovinylchloride to provide a good seal with the syringe.8,76.11 Stopper, for Luer f
39、itting of syringe sampling tube, made of polytetrafluoroethylene or polyfluorovinylchloride.96.12 Sampling Tube Holder, for supporting the syringe sampling tube, made of methyl methacrylate resin, having thedimensions shown in Fig. 4.6.13 Sampling Tube Spacer, for positioning the end of the sampling
40、 tube above the sampling tube holder, made of a length ofplastic tubing polyvinyl chloride, polyethylene, polypropylene, or polytetrafluoroethylene having an inside diameter ofapproximately 3 mm and 51 mm 6 1 mm length.8 The sole source of supply of syringe needles with polychloro-trifluoroethylene
41、hub known to the committee at this time is Hamilton Co., catalog number KF-714.9 Suitable stoppers are available from suppliers of infrared spectrometer sample cells.NOTE 1All dimensions are in millimetres (inches).NOTE 2Material: 18-8 Stainless Steel, 22 Gage (0.792 mm).FIG. 2 Thermometer BracketD9
42、43 184NOTE 1Dimensions are in millimetres (inches).FIG. 3 Mandrel for Winding Catalyst CoilsD943 1856.14 Flexible Tubing, polyvinyl chloride approximately 6.4 mm in inside diameter with a wall for delivery of oxygen to theoxidation cell.7. Reagents and Materials7.1 Purity of WaterUnless otherwise in
43、dicated, references to water shall be understood to mean reagent water as defined byType II of Specification D1193.7.2 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 A
44、nalytical Reagents of the American Chemical Society where suchspecifications are available.10 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.10 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 Annual 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.NOTE 1Dimensions are in millimetres (inches).FIG. 4 Sampling Tube HolderD943 1867.3 Acetone, reagent grade. (WarningHealth hazard; flammable.)7.4 Catalyst Wires:7.4.1 Low-Metalloid Steel Wire,111.59 mm in diameter (No. 16 Washburn and Moen Ga
47、ge).7.4.2 Electrolytic Copper Wire, 1.63 mm in diameter (No. 16 Imperial Standard Wire Gage or No. 14 American Wire Gage),99.9 % purity, conforming to Specification B1. Soft copper wire of an equivalent grade may also be used.NOTE 3Alternatively, suitably prepared catalyst coils may be purchased fro
48、m a supplier.7.5 Detergent, water-soluble.7.6 n-Heptane, reagent grade. (WarningFlammable. Harmful if inhaled.)7.7 Hydrochloric Acid, concentrated 36 mass % (relative density 1.19). (WarningToxic and corrosive.)7.8 Isopropyl Alcohol, reagent grade. (WarningFlammable.)7.9 Oxygen, 99.5 % minimum purit
49、y, with pressure regulation adequate to maintain a constant flow of gas through the apparatus.The use of a two-stage pressure regulator on tank oxygen is recommended. (WarningVigorously accelerates combustion.)7.10 Cleaning Reagent, cleaning by a 24h soak at room temperature either in Nochromix12,7 (WarningCorrosive. HealthHazard.) or in Micro7,13 solution.8. Sampling8.1 Samples for this test can come from tanks, drums, small containers, or even operating equipment. Therefore, use theapplicable apparatus an
