1、Designation: D4310 10 (Reapproved 2015)Standard Test Method forDetermination of Sludging and Corrosion Tendencies ofInhibited Mineral Oils1This standard is issued under the fixed designation D4310; 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.1. Scope1.1 This test method covers and is used to evaluate thetendency of inhibited mineral oil based
3、steam turbine lubri-cants and mineral oil based anti-wear hydraulic oils to corrodecopper catalyst metal and to form sludge during oxidation inthe presence of oxygen, water, and copper and iron metals at anelevated temperature. The test method is also used for testingcirculating oils having a specif
4、ic gravity less than that of waterand containing rust and oxidation inhibitors.NOTE 1During round robin testing copper and iron in the oil, waterand sludge phases were measured. However, the values for the total ironwere found to be so low (that is, below 0.8 mg), that statistical analysiswas inappr
5、opriate. The results of the cooperative test program areavailable (see Section 16).1.2 This test method is a modification of Test Method D943where the oxidation stability of the same kinds of oils isdetermined by following the acid number of oil. The number oftest hours required for the oil to reach
6、 an acid number of2.0 mg KOH/g is the oxidation lifetime.1.3 Procedure A of this test method requires the determina-tion and report of the weight of the sludge and the total amountof copper in the oil, water, and sludge phases. Procedure Brequires the sludge determination only. The acid numberdeterm
7、ination is optional for both procedures.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 WARNINGMercury has been designated by manyregulatory agencies as a hazardous material that can causecentral nervous system, kidney a
8、nd 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/faq.htmfor add
9、i-tional information. Users should be aware that selling mercuryand/or mercury containing products into your state or countrymay be prohibited by law.1.6 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
10、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 7 and X1.1.5.2. Referenced Documents2.1 ASTM Standards:2A510 Specification for General Requirements for Wire Rodsand Coa
11、rse Round Wire, Carbon SteelB1 Specification for Hard-Drawn Copper WireD664 Test Method for Acid Number of Petroleum Productsby Potentiometric TitrationD874 Test Method for Sulfated Ash from Lubricating Oilsand AdditivesD943 Test Method for Oxidation Characteristics of InhibitedMineral OilsD1193 Spe
12、cification for Reagent WaterD3339 Test Method for Acid Number of Petroleum Productsby Semi-Micro Color Indicator TitrationD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsE1 Specification for ASTM Liquid-in-Glass Thermometers2.2 Energy Institute Standard:3Specification for IP Sta
13、ndard Thermometers2.3 British Standard:4BS 1829 Reference Tables for Iron v. Constantan Thermo-couples3. Terminology3.1 Definitions:1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02
14、.09.0C on Oxidation of Turbine Oils.Current edition approved Oct. 1, 2015. Published December 2015. Originallyapproved in 1983. Last previous edition approved in 2010 as D4310 10. DOI:10.1520/D4310-10R15.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Se
15、rvice 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., London, W1G 7AR,U.K., http:/www.energyinst.org.4Available from British Standards Institution (BSI), 3
16、89 Chiswick High Rd.,London W4 4AL, U.K., http:/.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.1.1 sludgea precipitate or sediment from oxidized min-eral oil and water.4. Summary of Test Method4.1 An oil sample is contacted with o
17、xygen in the presenceof water and an iron-copper catalyst at 95 C for 1000 h. Theweight of insoluble material is determined gravimetrically byfiltration of the oxidation tube contents through 5 m pore sizefilter disks. The total amount of copper in the oil, water, andsludge phases is also determined
18、 for Procedure A. Procedure Brequires the sludge determination. The copper determination isnot required. The acid number determination is optional forboth procedures.NOTE 2Optionally, some operators may choose to: (1) assess thechange in weight of the catalyst coil, or (2 ) determine the acid number
19、 at1000 h, or both. The acid number may serve as a criterion to determine ifmeasurement of insoluble material is warranted. Normally, further testingis not recommended on a highly oxidized oil (that is an oil which hasattained an acid number 2.0 mg KOH/g). Instructions for these optionaltests are no
20、t included in this test method.5. Significance and Use5.1 Insoluble material may form in oils that are subjected tooxidizing conditions.5.2 Significant formation of oil insolubles or metal corro-sion products, or both, during this test may indicate that the oilwill form insolubles or corrode metals,
21、 or both, during fieldservice. However, no correlation with field service has beenestablished.6. Apparatus6.1 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). T
22、his calibration applies to the test tube without insertsat 20 C.6.2 Heating Bath: Liquid Bath or Metal Block, thermostati-cally controlled, capable of maintaining the oil sample in theoxidation cell at a temperature of 95 C 6 0.2 C, fitted with asuitable stirring device to provide a uniform temperat
23、urethroughout the bath, and large enough to hold the desirednumber of oxidation cells immersed in the heating bath to adepth of 390 mm 6 10 mm and in the heating liquid itself to adepth of 355 mm 6 10 mm.6.2.1 Studies have suggested that direct sunlight or artificiallight may adversely influence the
24、 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:6.2.1.1 Use of heated liquid baths that are designed andconstructed of metal, or combinations of metals and othersuitable opaque ma
25、terials, 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.6.2.1.2 If glass heating baths are used, the bath sh
26、all bewrapped with aluminum foil or other opaque material.6.2.1.3 Bright light entering the test cell from directlyoverhead can be eliminated by use of an opaque shield.6.3 Flowmeter, with a flow capacity of at least 3 L ofoxygen/hour, and an accuracy of 60.1 L h.6.4 Heating Bath ThermometerASTM Sol
27、vents Distilla-tion Thermometer having a range from 72 C 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-ter
28、accuracy may be used.6.5 Oxidation Cell Thermometer, having a range from 80 Cto 100 C, graduated in 0.1 C, total length250 mm, stemdiameter6.0 mm to 7.0 mm, calibrated for 76 mm immer-sion. Temperature measuring devices such as liquid-in-glassthermometers, thermocouples, or platinum resistance ther-
29、mometers that provide equivalent or better accuracy andprecision that cover the temperature range, may be used.6.6 Wire Coiling Mandrel, as shown in Fig. 2.6.7 Thermometer Bracket, for holding the oxidation cellthermometer, of 18-8 stainless steel, having the dimensionsshown in Fig. 3. The thermomet
30、er is held in the bracket by twofluoro-elastomer O-rings of approximately 5 mm inside diam-eter. Alternatively, thin stainless steel wire may be used.6.8 Abrasive Cloth, silicon carbide, 100-grit with clothbacking.6.9 Flexible Tubing, poly vinyl chloride approximately6.4 mm (14 in.) inside diameter
31、with a332 in. wall for deliveryof oxygen to the oxidation cell.6.10 Membrane Filters,6,7white, plain, 47 mm or 90 mm indiameter, pore size 5 m.6.11 Filter Holder,6,847 mm or 90 mm, consisting of aborosilicate glass funnel and a funnel base with a coarse grade(40 m to 60 m) fritted-glass filter suppo
32、rt or stainless steelscreen support such that the filter can be clamped between theground-glass sealing surfaces of the funnel and its base bymeans of a metal clamp.6.12 Weighing Bottle,6,9cylindrical body with ground-glassstopper; approximate inside diameter 45 mm, height of body65 mm, capacity 60
33、mL.5Supporting data (summary of the results of these studies) have been filed atASTM International Headquarters and may be obtained by requesting ResearchReport RR:D02-1365.6If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments wi
34、ll receive careful consider-ation at a meeting of the responsible technical committee,1which you may attend.7The sole source of supply of the Millipore SM membrane filters (MF-type,cellulose esters) known to the committee at this time is Millipore Filter Corp.,Bedford, MA.8The sole source of supply
35、of the Millipore Pyrex XX-10-047-00 or XX-10-047-30 filter holder known to the committee at this time is Millipore Filter Corp.,Bedford, MA.9The sole source of supply of the Fisher 3-415 weighing bottle, size G, knownto the committee at this time is Fisher Scientific Co., Pittsburgh, PA.D4310 10 (20
36、15)26.13 Vacuum Source, to provide pressure reduction to13.3 kPa 6 0.7 kPa (100 mm 6 5 mm Hg) absolute pressure.6.14 Cooling VesselA desiccator or other type of tightlycovered vessel for cooling the weighing vessels before weigh-ing. The use of a drying agent is not recommended.6.15 Drying Oven, cap
37、able of maintaining a temperature of105 C 6 2 C.6.16 Forceps, having unserrated tips.6.17 Syringe, 50 mL Luer-Lok with 12 in. needle.6.18 Separatory Funnels, with a capacity of 1000 mL.6.19 Rubber Policeman.6.20 Pipette Bulb.6.21 Syringe, glass or plastic, with Luer-Lok lockingconnector, 10 mL capac
38、ity for sampling.6.22 Syringe Sampling Tube, Grade 304 stainless steeltubing, 2.11 mm (0.083 in.) outside diameter, 1.60 mm(0.063 in.) inside diameter, 559 mm 6 2 mm (24.0 in. 60.08 in.) long, with one end finished at 90 and the other endfitted with a Luer-Lok female connector.All dimensions are in
39、millimetres (inches)NOTE 1The oxidation test tube has a calibration line at 300 mL. This calibration applies to the test tube alone at 20 C.NOTE 2Open tube ends to be ground and fire-polished.FIG. 1 Oxidation CellD4310 10 (2015)3FIG. 2 Mandrel for Winding Catalyst CoilsD4310 10 (2015)47. Reagents an
40、d Materials7.1 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.10Other grades
41、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.7.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Type II of Specifi
42、cation D1193.7.3 AcetoneReagent grade. (WarningHealth hazard,flammable.)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 LaboratoryC
43、hemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.All dimensions are in millimetres (inches).Material: 18-8 Stainless Steel. 22 Gauge (0.792 mm).FIG. 3 Thermometer BracketD4310 10 (2015)57.4 Cle
44、aning Reagent, cleaning by a 24 h soak at roomtemperature in either Nochromix6,11(WarningCorrosive,health hazard) or in Micro6,12solution.7.5 n-heptane, Reagent grade. (WarningFlammable.Harmful if inhaled.)7.6 Hydrochloric Acid (WarningToxic and corrosive.),concentrated (36 mass % (relative density
45、1.19).7.7 Isopropyl AlcoholReagent grade. (WarningFlammable.)7.8 Catalyst Wires:7.8.1 Low-Metalloid Steel Wire, 1.59 mm (0.0625 in.) indiameter (No. 16 Washburn and Moen Gauge).NOTE 3Carbon steel wire, soft bright annealed and free from rust ofGrade 1008 as described in Specification A510 is satisfa
46、ctory. Similarwire conforming to BS 1829, is also satisfactory. If these steels are notavailable, other equivalent steels may be used, provided they are found tobe satisfactory in comparative tests using this Test Method D4310.7.8.2 Electrolytic Copper Wire, 1.63 mm (0.064 in.) in di-ameter (No. 16
47、Imperial Standard Wire Gauge or No. 14American Wire Gauge), 99.9 % purity, conforming to Specifi-cation B1. Soft copper wire of an equivalent grade may also beused.NOTE 4Alternatively, suitably prepared catalyst coils may be pur-chased from a supplier.7.9 Detergent, water-soluble.6,137.10 Oxygen(War
48、ningOxygen vigorously acceleratescombustion) 99.5 % minimum purity, with pressure regulationadequate to maintain a constant flow of gas through theapparatus. The use of a two-stage pressure regulator on tankoxygen is recommended.8. Sampling8.1 Samples for this test can come from tanks, drums, smallc
49、ontainers, or even operating equipment. Therefore, use theapplicable apparatus and techniques described in PracticeD4057.8.2 For one single determination the minimum requiredsample size is 300 mL.9. Preparation of Apparatus9.1 Cleaning CatalystImmediately prior to winding acatalyst coil, clean a 3.00 m 6 0.01 m length of iron wire andan equal length of copper wire with wads of absorbent cottonwet with n-heptane and follow by abrasion with abrasive clothuntil a fresh metal surface is exposed. Then wipe with dr
