1、Designation: D943 04a (Reapproved 2010)1BS 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 rev
2、ision, 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 Defense.1NOTEUpdated Scope with regard
3、 to SI units and added mercury caveat editorially in October 2010.1. Scope1.1 This test method covers the evaluation of the oxidationstability of inhibited steam-turbine oils in the presence ofoxygen, water, and copper and iron metals at an elevatedtemperature. This test method is limited to a maxim
4、um testingtime of 10 000 h. This test method is also used for testing otheroils, such as hydraulic oils and circulating oils having a specificgravity less than that of water and containing rust and oxidationinhibitors.1.2 The values stated in SI units are to be regarded asstandard. No other units of
5、 measurement are included in thisstandard.1.2.1 ExceptionThe values in parentheses in the figuresare provided for information for those using old equipmentbased on non-SI units.1.3 WARNINGMercury has been designated by manyregulatory agencies as a hazardous material that can causecentral nervous sys
6、tem, kidney and liver damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution should be taken when handling mercury andmercury containing products. See the applicable product Ma-terial Safety Data Sheet (MSDS) for details and EPAswebsitehttp:/www.epa.gov/mercury/f
7、aq.htmfor addi-tional information. Users should be aware that selling mercuryand/or mercury containing products into your state or countrymay be prohibited by law.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the
8、user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specificwarning statements, see Section 6.2. Referenced Documents2.1 ASTM Standards:2A510 Specification for General Requirements for WireRods and C
9、oarse Round Wire, Carbon SteelB1 Specification for Hard-Drawn Copper WireD664 Test Method for Acid Number of Petroleum Productsby Potentiometric TitrationD1193 Specification for Reagent WaterD3244 Practice for Utilization of Test Data to DetermineConformance with SpecificationsD3339 Test Method for
10、Acid Number of Petroleum Prod-ucts by Semi-Micro Color Indicator TitrationD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4310 Test Method for Determination of Sludging andCorrosion Tendencies of Inhibited Mineral OilsD5770 Test Method for Semiquantitative Micro Determina-tion
11、ofAcid Number of Lubricating Oils During OxidationTestingE1 Specification for ASTM Liquid-in-Glass Thermometers2.2 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 presenceo
12、f water and an iron-copper catalyst at 95C. The test continuesuntil the measured acid number of the oil is 2.0 mg KOH/g orabove. The number of test hours required for the oil to reach2.0 mg KOH/g is the “oxidation lifetime.”1This test method is under the jurisdiction of ASTM Committee D02 onPetroleu
13、m Products and Lubricants and is the direct responsibility of SubcommitteeD02.09.0C on Oxidation of Turbine Oils.Current edition approved Oct. 1, 2010. Published December 2010. Originallyapproved in 1947. Last previous edition approved in 2004 as D94304a.In 1976, this test method ceased to be a join
14、t ASTM-IP standard. DOI:10.1520/D0943-10.2For 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 standards Document Summary page onthe ASTM website.3Available from Ener
15、gy Institute, 61 New Cavendish St., London, W1G 7AR,United Kingdom.4Available from British Standards Institute, 389 Chiswick High Rd., London,W4 4AL, United Kingdom.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4. Significance and
16、Use4.1 This test method is widely used for specification pur-poses and is considered of value in estimating the oxidationstability of lubricants, especially those that are prone to watercontamination. It should be recognized, however, that correla-tion between results of this method and the oxidatio
17、n stabilityof a lubricant in field service may vary markedly with fieldservice conditions and with various lubricants. The precisionstatement for this method was determined on steam turbineoils.NOTE 1Furthermore, in the course of testing a lubricant by thismethod, other signs of deterioration, such
18、as sludge formation or catalystcoil corrosion, may appear that are not reflected in the calculated oxidationlifetime. The subcommittee responsible for this method is investigatingthe application of alternative criteria for evaluation of lubricants using thistest apparatus. Test Method D4310 is now a
19、vailable for sludge measure-ment.5. Apparatus5.1 Oxidation Cell, of borosilicate glass, as shown in Fig. 1,consisting of a test tube, condenser, and oxygen delivery tube.The test tube has a calibration line at 300 mL (maximum error1 mL). This calibration applies to the test tube alone at 20C.NOTE 1A
20、ll 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 20C.NOTE 3Open tube ends to be ground and fire-polished.FIG. 1 Oxidation CellD943 04a (2010)125.2 Heating Bath, thermostatically controlled, ca
21、pable ofmaintaining the oil sample in the oxidation cell at a tempera-ture of 95 6 0.2C, fitted with a suitable stirring device toprovide a uniform temperature throughout the bath, and largeenough to hold the desired number of oxidation cells immersedin the heating bath to a depth of 390 6 10 mm and
22、 in theheating liquid itself to a depth of 355 6 10 mm.NOTE 2Metal block heaters meeting the test method requirementsmay also be used. It is not known what types of heating baths were usedin developing the precision statement.5.2.1 Studies have suggested that direct sunlight or artificiallight may a
23、dversely influence the results of this test.5Tominimize effects of light exposure on the lubricant beingtested, light shall be excluded from the lubricant by one ormore of the following ways:5.2.1.1 Use of heated liquid baths that are designed andconstructed of metal, or combinations of metals and o
24、thersuitable opaque materials, that prevent light from entering thetest cell from the sides is preferred. If a viewing window isincluded in the design, this viewing window shall be fitted witha suitable opaque cover and be kept closed when no observa-tion is being made.5.2.1.2 If glass heating baths
25、 are used, the bath shall bewrapped with aluminum foil or other opaque material.5.2.1.3 Bright light entering the test cell from directlyoverhead can be eliminated by use of an opaque shield.5.3 Flowmeter, with a capacity of at least 3 L of oxygen/h,and an accuracy of 6 0.1 L/h.5.4 Heating Bath Ther
26、mometerASTM Solvents Distilla-tion Thermometer having a range from 72 to 126C, andconforming to the requirements for Thermometer 40C asprescribed in Specification E1, or for Thermometer 70C asprescribed in Specifications for IP Standard Thermometers.Alternatively, temperaturemeasuring devices of equ
27、al or bet-ter accuracy may be used.5.5 Oxidation Cell Thermometer,3having a range from 80to 100C, graduated in 0.1C, total length250 mm, stemdiameter6.0 to 7.0 mm, calibrated for 76-mm immersion.6,7Alternatively, temperaturemeasuring devices of equal or bet-ter accuracy may be used.5.6 Thermometer B
28、racket, for holding the oxidation cellthermometer, of 18-8 stainless steel, having the dimensionsshown in Fig. 2. The thermometer is held in the bracket by twofluoroelastomer O-rings of approximately 5 mm inside diam-eter. Alternatively, thin stainless steel wire may be used.5.7 Wire Coiling Mandrel
29、, as shown in Fig. 3.5.8 Abrasive Cloth, silicon carbide, 100-grit with clothbacking.5.9 Syringes, glass, with Luer-Lok locking connectors, 10and 50-mL capacities for sampling, and water additions,respectively.5.10 Syringe Sampling Tube, Grade 304 stainless steeltubing, 2.11 mm in outside diameter,
30、1.60 mm in insidediameter, 559 6 2 mm long, with one end finished at 90 andthe other end fitted with a Luer-Lok female connector. TheLuer-Lok connector is preferably of elastomeric material, suchas polyfluorovinylchloride to provide a good seal with thesyringe.7,85.11 Stopper, for Luer fitting of sy
31、ringe sampling tube,made of polytetrafluoroethylene or polyfluorovinylchloride.95.12 Sampling Tube Holder, for supporting the syringesampling tube, made of methyl methacrylate resin, having thedimensions shown in Fig. 4.5.13 Sampling Tube Spacer, for positioning the end of thesampling tube above the
32、 sampling tube holder, made of alength of plastic tubing polyvinyl chloride, polyethylene,polypropylene, or polytetrafluoroethylene having an insidediameter of approximately 3 mm and 51 6 1 mm length.5.14 Flexible Tubing, polyvinyl chloride approximately 6.4mm in inside diameter with a wall for deli
33、very of oxygen to theoxidation cell.6. Reagents and Materials6.1 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Type II of Specification D1193.6.2 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwi
34、se indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.10Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to per
35、mit its use without lessening the accuracy ofthe determination.6.3 Acetone, reagent grade.(WarningHealth hazard;flammable.)6.4 Catalyst Wires:6.4.1 Low-Metalloid Steel Wire,111.59 mm in diameter (No.16 Washburn and Moen Gage).6.4.2 Electrolytic Copper Wire, 1.63 mm in diameter (No.16 Imperial Standa
36、rd Wire Gage or No. 14 American WireGage), 99.9 % purity, conforming to Specification B1. Softcopper wire of an equivalent grade may also be used.5Supporting data (a summary of these results) have been filed at ASTMInternational Headquarters and may be obtained by requesting Research ReportRR:D02-13
37、65.6The sole source of supply of the Brooklyn thermometer No. 21276-RM knownto the committee at this time is the Brooklyn Thermometer Co., Farmingdale, NY.7If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful
38、 consider-ation at a meeting of the responsible technical committee,1which you may attend.8The sole source of supply of syringe needles with polychloro-trifluoroethylenehub known to the committee at this time is Hamilton Co., catalog number KF-714.9Suitable stoppers are available from suppliers of i
39、nfrared spectrometer samplecells.10Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K.
40、, and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.11Carbon steel wire, soft bright annealed and free from rust, of Grade 1008 asdescribed in Specification A510 is satisfactory. Similar wire conforming to BS 1829is also satisfactory.
41、If these steels are not available, other equivalent steels may beused, provided they are found to be satisfactory in comparative tests using TestMethod D943.D943 04a (2010)13NOTE 3Alternatively, suitably prepared catalyst coils may be pur-chased from a supplier.6.5 Detergent, water-soluble.6.6 n-Hep
42、tane, reagent grade. (WarningFlammable.Harmful if inhaled.)6.7 Hydrochloric Acid, concentrated 36 mass % (relativedensity 1.19). (WarningToxic and corrosive.)6.8 Isopropyl Alcohol, reagent grade. (WarningFlammable.)6.9 Oxygen, 99.5 % minimum purity, with pressure regula-tion adequate to maintain a c
43、onstant flow of gas through theapparatus. The use of a two-stage pressure regulator on tankoxygen is recommended. (WarningVigorously acceleratescombustion.)6.10 Cleaning Reagent, cleaning by a 24h soak at roomtemperature either in Nochromix7,12(WarningCorrosive.Health Hazard.) or in Micro7,13solutio
44、n.7. Sampling7.1 Samples for this test can come from tanks, drums, smallcontainers, or even operating equipment. Therefore, use theapplicable apparatus and techniques described in PracticeD4057.12The sole source of supply of Nochromix known to the committee at this timeis Godax Laboratories, Inc., 7
45、20-B Erie Ave., Takoma Park, MD 20912.13The sole source of supply of the Micro solution known to the committee at thistime is International Products Corp., P.O. Box 70, Burlington, NJ 08016.NOTE 1All dimensions are in millimetres (inches).NOTE 2Material: 18-8 Stainless Steel, 22 Gage (0.792 mm).FIG.
46、 2 Thermometer BracketD943 04a (2010)14NOTEDimensions are in millimetres (inches).FIG. 3 Mandrel for Winding Catalyst CoilsD943 04a (2010)157.2 For one single determination the minimum requiredsample size is 300 mL.8. Preparation of Apparatus8.1 Cleaning CatalystImmediately prior to winding acatalys
47、t coil, clean a 3.00 6 0.01-m length of iron wire and anequal length of copper wire with wads of absorbent cotton wetwith n-Heptane and follow by abrasion with abrasive clothuntil a fresh metal surface is exposed. Then wipe with dryabsorbent cotton until all loose particles of metal and abrasivehave
48、 been removed. In subsequent operations handle thecatalyst wires with clean gloves (cotton, rubber, or plastic) toprevent contact with the skin.8.2 Preparation of Catalyst CoilTwist the iron and copperwires tightly together at one end for three turns and then windthem simultaneously alongside each o
49、ther on a threadedmandrel (Fig. 3), inserting the iron wire in the deeper thread.Remove the coil from the mandrel, twist the free ends of theiron and copper wires together for three turns, and bend thetwisted ends to conform to the shape of the spiral coil. Theoverall length of the finished coil should be 225 6 5 mm. Ifnecessary, the coil may be stretched to give the required length(Note 3 and Note 4.)NOTE 4The finished catalyst coil is a double spiral of copper and ironwire, 225 6 5 mm overall length and 15.9 to 16.5 mm inside d
