1、Designation: D 943 04aAn American National StandardBS 2000-280:1999Standard Test Method forOxidation Characteristics of Inhibited Mineral Oils1This standard is issued under the fixed designation D 943; the number immediately following the designation indicates the year oforiginal adoption or, in the
2、 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 approved for use by agencies of the Department of Defense.1. Scope*1.1 This
3、 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 maximum testingtime of 10 000 h. This test method is also used for testing otheroils, s
4、uch 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 as thestandard. The values given in parentheses are for informationonly.1.3 This standard does not purport to a
5、ddress all of thesafety concerns, if any, associated with its use. It is theresponsibility of the 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. Refe
6、renced Documents2.1 ASTM Standards:2A 510 Specification for General Requirements for WireRods and Coarse Round Wire, Carbon SteelB 1 Specification for Hard-Drawn Copper WireD 664 Test Method forAcid Number of Petroleum Productsby Potentiometric TitrationD 1193 Specification for Reagent WaterD 3244 P
7、ractice for Utilization of Test Data to DetermineConformance with SpecificationsD 3339 Test Method for Acid Number of Petroleum Prod-ucts by Semi-Micro Color Indicator TitrationD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4310 Test Method for Determination of the Sludging
8、andCorrosion Tendencies of Inhibited Mineral OilsD 5770 Test Method for Semi-Quantitative Micro Determi-nation of Acid Number of Lubricating Oils During Oxida-tion TestingE 1 Specification for ASTM Liquid-in-Glass Thermometers2.2 Energy Institute Standards:3Specifications for IP Standard Thermometer
9、s2.3 British Standard:4BS 18293. Summary of Test Method3.1 The oil sample is contacted with oxygen in the presenceof 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.
10、0 mg KOH/g is the “oxidation lifetime.”4. Significance and 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 c
11、orrela-tion between results of this method and the oxidation 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 l
12、ubricant by thismethod, other signs of deterioration, such 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 lubr
13、icants using thistest apparatus. Test Method D 4310 is now available 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.1This test method is under the jurisdiction of ASTM Committee D02 onPe
14、troleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.09 on Oxidation.Current edition approved Nov. 1, 2004. Published November 2004. Originallyapproved in 1947. Last previous edition approved in 2004 as D 94304.In 1976, this test method ceased to be a joint ASTM-IP sta
15、ndard.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 Energy Institute, 61 New Cavendish St.,
16、 London, W1G 7AR,United Kingdom.4Available from British Standards Institute, 389 Chiswick High Rd., London,W4 4AL, United Kingdom.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, Uni
17、ted States.The test tube has a calibration line at 300 mL (maximum error1 mL). This calibration applies to the test tube alone at 20C.5.2 Heating Bath, thermostatically controlled, capable ofmaintaining the oil sample in the oxidation cell at a tempera-ture of 95 6 0.2C, fitted with a suitable stirr
18、ing 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 in theheating liquid itself to a depth of 355 6 10 mm.NOTE 2Metal block heaters meeting the test method requirements
19、may 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 adversely influence the results of this test.5Tominimize effects of light exposure on the lubricant beingtested, light
20、 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 other5Supporting data (a summary of these results) have been filed at ASTMInternational Headquarters and may be obtain
21、ed by requesting Research ReportRR:D02-1365.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 20C.NOTE 3Open tube ends to be ground and fire-polished.FIG. 1 Oxidation CellD 943 04a2suita
22、ble 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 are used
23、, 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 ThermometerAS
24、TM 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 equal or bet
25、-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 Bracket, f
26、or 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, as show
27、n in Fig. 3.6The 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 receiv
28、e careful consider-ation at a meeting of the responsible technical committee,1which you may attend.NOTE 1All dimensions are in millimetres (inches).NOTE 2Material: 18-8 Stainless Steel, 22 Gage (0.792 mm).FIG. 2 Thermometer BracketD 943 04a3NOTEDimensions are in millimetres (inches).FIG. 3 Mandrel f
29、or Winding Catalyst CoilsD 943 04a45.8 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 (0.083
30、in.) in outside diameter, 1.60 mm(0.063 in.) in inside diameter, 559 6 2 mm (24.0 6 0.08 in.)long, with one end finished at 90 and the other end fitted witha Luer-Lok female connector. The Luer-Lok connector ispreferably of elastomeric material, such as polyfluorovinyl-chloride to provide a good sea
31、l with the syringe.7,85.11 Stopper, for Luer fitting of syringe 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 Spa
32、cer, for positioning the end of thesampling tube above the sampling tube holder, made of alength of plastic tubing polyvinyl chloride, polyethylene,polypropylene, or polytetrafluoroethylene having an insidediameter of approximately 3 mm (18 in.) and 51 6 1 mm (2.06 0.04 in.) length.5.14 Flexible Tub
33、ing, polyvinyl chloride approximately 6.4mm (14 in.) in inside diameter with a (332-in.) wall for deliveryof oxygen to the oxidation 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 Speci
34、fication D 1193.6.2 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.10Other gr
35、ades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit 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 (0.0625 in.) i
36、ndiameter (No. 16 Washburn and Moen Gage).6.4.2 Electrolytic Copper Wire, 1.63 mm (0.064 in.) indiameter (No. 16 Imperial Standard Wire Gage or No. 14American Wire Gage), 99.9 % purity, conforming to Specifi-cation B1. Soft copper wire of an equivalent grade may also beused.NOTE 3Alternatively, suit
37、ably prepared catalyst coils may be pur-chased from a supplier.6.5 Detergent, water-soluble.6.6 n-Heptane, 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. (Wa
38、rningFlammable.)6.9 Oxygen, 99.5 % minimum purity, with pressure regula-tion adequate to maintain a constant flow of gas through the8The 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
39、stoppers are available from suppliers of infrared 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 Laborato
40、ryChemicals, BDH Ltd., Poole, Dorset, U.K., 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 SpecificationA 510 is satisfactory. Similar wire c
41、onforming to BS 1829is also satisfactory. If these steels are not available, other equivalent steels may beused, provided they are found to be satisfactory in comparative tests using TestMethod D 943.Table of Dimensionsmm in.Dimension Tolerance Dimension ToleranceA 2.4 0.1 0.09375 0.005B 7.5 0.1 0.2
42、96875 0.005C 12.7 0.25 0.50 0.01D 38.1 0.50 1.50 0.02E 6.4 0.50 0.25 0.02F 25.4 0.25 1.00 0.01G 38.1 0.50 1.50 0.02H 9.5 0.50 0.375 0.02I 76.2 0.50 3.00 0.02FIG. 4 Sampling Tube HolderD 943 04a5apparatus. The use of a two-stage pressure regulator on tankoxygen is recommended. (WarningVigorously acce
43、leratescombustion.)6.10 Cleaning Reagent, cleaning by a 24h soak at roomtemperature either in Nochromix7,12(WarningCorrosive.Health Hazard.) or in Micro7,13solution.7. Sampling7.1 Samples for this test can come from tanks, drums, smallcontainers, or even operating equipment. Therefore, use theapplic
44、able apparatus and techniques described in PracticeD 4057.7.2 For one single determination the minimum requiredsample size is 300 mL.8. Preparation of Apparatus8.1 Cleaning CatalystImmediately prior to winding acatalyst coil, clean a 3.00 6 0.01-m length of iron wire and anequal length of copper wir
45、e 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 been removed. In subsequent operations handle thecatalyst wires with clean gloves
46、 (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 other on a threadedmandrel (Fig. 3), inserting the iron wire in the deeper thread.R
47、emove 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 (8.96 0.2 in.). If necessary, the coil may be stretched to give
48、therequired length (Note 3 and Note 4.)NOTE 4The finished catalyst coil is a double spiral of copper and ironwire, 225 6 5 mm (8.9 6 0.2 in.) overall length and 15.9 to 16.5 mm(0.625 to 0.650 in.) inside diameter. The turns of wire are evenly spaced,and two consecutive turns of the same wire are 3.9
49、6 to 4.22 mm (0.156 to0.166 in.) apart, center to center. The mandrel shown in Fig. 3 is designedto produce such a coil. Using this mandrel, the iron wire is wound on athread of 14.98-mm (0.590-in.) diameter, while the copper wire is woundon a thread of 15.9-mm (0.625-in.) diameter. The smaller diameter is toallow for springback of the steel wire after winding, so as to give 15.9-mmconsistent inside diameter. Use of a very soft annealed steel wire mayallow use of identical thread diameters for the two wires.Any arrangementthat leads to the
