1、Designation: D943 04a (Reapproved 2010)1D943 17 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 cas
2、e 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. Department of Defense.1 NOTEUpdated Sco
3、pe with regard to SI units and added mercury caveat editorially in October 2010.1. Scope Scope*1.1 This test method covers 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 metho
4、d is limited to a maximum testing time of 10 000h. 10 000 h. This test method is also used for testing other oils, such as hydraulic oils and circulating oils having a specific gravityless than that of water and containing rust and oxidation inhibitors.1.2 The values stated in SI units are to be reg
5、arded as standard. No other units of measurement are included in this standard.1.2.1 ExceptionThe values in parentheses in the figures 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 mat
6、erial that can cause centralnervous system, kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Cautionshould be taken when handling mercury and mercury containing products. See the applicable product Material Safety Data Sheet(MSDS) for details and
7、 EPAs websitehttp:/www.epa.gov/mercury/faq.htmfor additional information. Users should be awarethat selling mercury and/or mercury containing products into your state or country may be prohibited by law.1.4 This standard does not purport to address all of the safety concerns, if any, associated with
8、 its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. For specific warning statements, see Section 6.1.5 This international standard was developed in accordance with i
9、nternationally recognized principles on standardizationestablished in 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:2A51
10、0 Specification for General Requirements for Wire Rods and Coarse Round Wire, Carbon SteelB1 Specification 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 D
11、etermine Conformance with SpecificationsD3339 Test Method for Acid Number of Petroleum Products by Semi-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 O
12、ilsD5770 Test Method for Semiquantitative Micro Determination of Acid Number of Lubricating Oils During Oxidation TestingE1 Specification for ASTM Liquid-in-Glass ThermometersE2877 Guide for Digital Contact Thermometers1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Pr
13、oducts, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.09.0C on Oxidation of Turbine Oils.Current edition approved Oct. 1, 2010June 15, 2017. Published December 2010August 2017. Originally approved in 1947. Last previous edition approved in 20042010as D943D943 04a (
14、2010)104a. . DOI: 10.1520/D0943-17.In 1976, this test method ceased to be a joint ASTM-IP standard. DOI: 10.1520/D0943-10.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refe
15、r 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 standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all cha
16、nges 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 International, 100 Ba
17、rr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States12.2 Energy Institute Standards:3Specifications for IP Standard Thermometers2.3 British Standard:4BS 18293. Summary of Test Method3.1 The oil sample is contacted with oxygen in the presence of water and an iron-copper catal
18、yst at 95C.95 C. The testcontinues until the measured acid number of the oil is 2.02.0 mg mg KOH/g or above. g or above, acid number being the ratioof the mass of KOH in milligrams to the mass of the oil sample in grams. The number of test hours required for the oil to reach2.0 mg KOH/g the measured
19、 acid number of 2.0 mgg is the “oxidation lifetime.”4. Significance and Use4.1 This test method is widely used for specification purposes and is considered of value in estimating the oxidation stabilityof lubricants, especially those that are prone to water contamination. It should be recognized, ho
20、wever, that correlation betweenresults of this method and the oxidation stability of a lubricant in field service may vary markedly with field service conditionsand with various lubricants. The precision statement for this method was determined on steam turbine oils.NOTE 1Furthermore, in the course
21、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 calculated oxidation lifetime. The subcommittee responsible for this method is investigating theapplication of alternative criteria for ev
22、aluation of lubricants using this test apparatus. Test Method D4310 is now available for sludge measurement.5. Apparatus5.1 Oxidation Cell, of borosilicate glass, as shown in Fig. 1, consisting of a test tube, condenser, and oxygen delivery tube. Thetest tube has a calibration line at 300 mL (maximu
23、m error 1 mL). This calibration applies to the test tube alone at 20C.20 C.5.2 Heating Bath, thermostatically controlled, capable of maintaining the oil sample in the oxidation cell at a temperature of9595 C 6 0.2C,0.2 C, fitted with a suitable stirring device to provide a uniform temperature throug
24、hout the bath, and largeenough to hold the desired number of oxidation cells immersed in the heating bath to a depth of 390390 mm 6 10 mm 10 mmand in the heating liquid itself to a depth of 355355 mm 6 10 mm.10 mm.NOTE 2Metal block heaters meeting the test method requirements may also be used. It is
25、 not known what types of heating baths were used indeveloping the precision statement.5.2.1 Studies have suggested that direct sunlight or artificial light may adversely influence the results of this test.5 To minimizeeffects of light exposure on the lubricant being tested, light shall be excluded f
26、rom the lubricant by one or more of the followingways:5.2.1.1 Use of heated liquid baths that are designed and constructed of metal, or combinations of metals and other suitableopaque materials, that prevent light from entering the test cell from the sides is preferred. If a viewing window is includ
27、ed in thedesign, this viewing window shall be fitted with a suitable opaque cover and be kept closed when no observation is being made.5.2.1.2 If glass heating baths are used, the bath shall be wrapped with aluminum foil or other opaque material.5.2.1.3 Bright light entering the test cell from direc
28、tly overhead can be eliminated by use of an opaque shield.5.3 Flowmeter, with a capacity of at least 33 L L h of oxygen/h,oxygen, and an accuracy of 660.1 L 0.1 L/h. h.5.4 Heating Bath ThermometerASTM Solvents Distillation Thermometer having a range from 7272 C to 126C,126 C, andconforming to the re
29、quirements for Thermometer 40C as prescribed in Specification E1, or for Thermometer 70C as prescribedin Specifications for IP Standard Thermometers. Alternatively, temperaturemeasuring devices digital contact thermometers suchas PRTs (platinum resistance thermometers), thermistors, or thermocouples
30、 in accordance with Specification E2877 of equal orbetter accuracy may be used.5.5 Oxidation Cell Thermometer,3having a range from 8080 C to 100C,100 C, graduated in 0.1C,0.1 C, total length250mm, length250 mm, stem diameter6.0diameter6.0 mm to 7.0 mm, 7.0 mm, calibrated for 76-mm76 mm immersion.6,7
31、Alternatively, temperaturemeasuring devices digital contact thermometers such as PRTs, thermistors, or thermocouples inaccordance with Specification E2877 of equal or better accuracy may be used.5.6 Thermometer Bracket, for holding the oxidation cell thermometer, of 18-8 stainless steel, having the
32、dimensions shown inFig. 2. The thermometer is held in the bracket by two fluoroelastomer O-rings of approximately 5 mm 5 mm inside diameter.Alternatively, thin stainless steel wire may be used.3 Available from Energy Institute, 61 New Cavendish St., London, W1G 7AR, United Kingdom.W1G 7AR, U.K., htt
33、p:/www.energyinst.org.4 Available from British Standards Institute, Institution (BSI), 389 Chiswick High Rd., London, W4 4AL, United Kingdom.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
34、 Research Report RR:D02-1365.6 The sole source of supply of the Brooklyn thermometer No. 21276-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
35、 comments will receive careful consideration at ameeting of the responsible technical committee,1 which you may attend.D943 1725.7 Wire Coiling Mandrel, as shown in Fig. 3.5.8 Abrasive Cloth, silicon carbide, 100-grit100 grit with cloth backing.5.9 Syringes, glass, with Luer-Lok locking connectors,
36、1010 mLand 50-mL50 mLcapacities for sampling, and water additions,respectively.NOTE 1All dimensions are in millimetres (inches).NOTE 2The oxidation test tube has a calibration line at 300 mL. 300 mL. This calibration applies to the test tube alone at 20C.20 C.NOTE 3Open tube ends to be ground and fi
37、re-polished.FIG. 1 Oxidation CellD943 1735.10 Syringe Sampling Tube, Grade 304 stainless steel tubing, 2.11 mm 2.11 mm in outside diameter, 1.60 mm 1.60 mm ininside diameter, 559559 mm 6 2 mm 2 mm long, with one end finished at 90 and the other end fitted with a Luer-Lok femaleconnector. The Luer-Lo
38、k connector is preferably of elastomeric material, such as polyfluorovinylchloride to provide a good sealwith the syringe.8,75.11 Stopper, for Luer fitting of syringe sampling tube, made of polytetrafluoroethylene or polyfluorovinylchloride.95.12 Sampling Tube Holder, for supporting the syringe samp
39、ling tube, made of methyl methacrylate resin, having thedimensions shown in Fig. 4.5.13 Sampling Tube Spacer, for positioning the end of the sampling tube above the sampling tube holder, made of a length ofplastic tubing polyvinyl chloride, polyethylene, polypropylene, or polytetrafluoroethylene hav
40、ing an inside diameter ofapproximately 3 mm 3 mm and 5151 mm 6 1 mm 1 mm length.8 The sole source of supply of syringe needles with polychloro-trifluoroethylene hub known to the committee at this time is Hamilton Co., catalog number KF-714.9 Suitable stoppers are available from suppliers of infrared
41、 spectrometer sample cells.NOTE 1All dimensions are in millimetres (inches).NOTE 2Material: 18-8 Stainless Steel, 22 Gage (0.792 mm).(0.792 mm).FIG. 2 Thermometer BracketD943 174NOTE 1Dimensions are in millimetres (inches).FIG. 3 Mandrel for Winding Catalyst CoilsD943 1755.14 Flexible Tubing, polyvi
42、nyl chloride approximately 6.4 mm in inside diameter with a wall for delivery of oxygen to theoxidation cell.6. Reagents and Materials6.1 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water as defined byType II of Specification D1193.6.2 Purity of
43、 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.10 Other grades may be used, provided
44、 it is first ascertained that the reagent is of sufficiently high purityto permit its use without lessening the accuracy of the determination.6.3 Acetone, reagent grade.(WarningHealth (WarningHealth hazard; flammable.)10 Reagent Chemicals, American Chemical Society Specifications, American Chemical
45、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, U.S. Pharmacopeial Convention, Inc. (USPC), Rockvill
46、e, MD.D943 1766.4 Catalyst Wires:6.4.1 Low-Metalloid Steel Wire,111.59 mm 1.59 mm in diameter (No. 16 Washburn and Moen Gage).6.4.2 Electrolytic Copper Wire, 1.63 mm 1.63 mm in diameter (No. 16 Imperial Standard Wire Gage or No. 14 American WireGage), 99.9 % purity, conforming to Specification B1. S
47、oft copper wire of an equivalent grade may also be used.NOTE 3Alternatively, suitably prepared catalyst coils may be purchased from a supplier.6.5 Detergent, water-soluble.6.6 n-Heptane, reagent grade. (WarningWarningFlammable.Flammable. Harmful if inhaled.)6.7 Hydrochloric Acid, concentrated 36 mas
48、s % (relative density 1.19). (WarningWarningToxicToxic and corrosive.)6.8 Isopropyl Alcohol, reagent grade. (WarningWarningFlammable.)Flammable.)6.9 Oxygen, 99.5 % minimum purity, with pressure regulation adequate to maintain a constant flow of gas through the apparatus.The use of a two-stage pressu
49、re regulator on tank oxygen is recommended. (WarningWarningVigorouslyVigorouslyaccelerates combustion.)11 Carbon steel wire, soft bright annealed and free from rust, of Grade 1008 as described in Specification A510 is satisfactory. Similar wire conforming to BS 1829 is alsosatisfactory. If these steels are not available, other equivalent steels may be used, provided they are found to be satisfactory in comparative tests using Test Method D943.Table of Dimensionsmm in.Dimension Tolerance Dimens
