1、Designation: D4310 10Standard 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 case of revision, the
2、 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. Scope*1.1 This test method covers and is used to evaluate thetendency of inhibited mineral oil based steam turbine lub
3、ri-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 specific gravity less t
4、han 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 inappropriate. The resu
5、lts 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 an acid number o
6、f 2.0mg 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 numberdetermination is option
7、al 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 and liver damage.
8、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 addi-tional informat
9、ion. 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 standard to estab
10、lish 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 WireRods and Coarse Round Wire, C
11、arbon 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 Inhib-ited Mineral OilsD1193 Specification for
12、Reagent WaterD3339 Test Method for Acid Number of Petroleum Prod-ucts by 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 Standard Thermom
13、eters2.3 British Standard:4BS 1829 Reference Tables for Iron v. Constantan Thermo-couples3. Terminology3.1 Definitions:3.1.1 sludgea precipitate or sediment from oxidized min-eral oil and water.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and
14、is the direct responsibility of SubcommitteeD02.09.0C on Oxidation of Turbine Oils.Current edition approved July 1, 2010. Published July 2010. Originally approvedin 1983. Last previous edition approved in 2009 as D431009. DOI: 10.1520/D4310-10.2For referenced ASTM standards, visit the ASTM website,
15、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., London WIM, 8AR,England.4Available from British Standards Ins
16、titute (BSI), 389 Chiswick High Rd.,London W4 4AL, U.K.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, United States.4. Summary of Test Method4.1 An oil sample is contacted with oxy
17、gen in the presenceof water and an iron-copper catalyst at 95C 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 fo
18、r 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 at1
19、000 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 not in
20、cluded 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, or
21、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). This
22、calibration applies to the test tube without insertsat 20C.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 6 0.2C, fitted with asuitable stirring device to provide a uniform temperaturethrou
23、ghout the bath, and large enough to hold the desirednumber of oxidation cells immersed in the heating bath to adepth of 390 6 10 mm and in the heating liquid itself to a depthof 355 6 10 mm.6.2.1 Studies have suggested that direct sunlight or artificiallight may adversely influence the results of th
24、is 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 materials, that
25、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 shall bewrapped
26、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 Solvents Distilla
27、-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-ter accuracy may be
28、used.6.5 Oxidation Cell Thermometer, having a range from 80 to100C, graduated in 0.1C, total length250 mm, stemdiameter6.0 to 7.0 mm, calibrated for 76-mm immersion.Temperature measuring devices such as liquid-in-glass ther-mometers, thermocouples, or platinum resistance thermom-eters that provide e
29、quivalent or better accuracy and precisionthat 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 thermometer is held in the brack
30、et 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 approximately 6.4-mm (14-in.) inside diameter with a332-in. wall for
31、 delivery ofoxygen to the oxidation cell.6.10 Membrane Filters,6,7white, plain, 47 or 90 mm indiameter, pore size 5 m.6.11 Filter Holder,6,847 or 90 mm, consisting of aborosilicate glass funnel and a funnel base with a coarse grade(40 to 60-m) fritted-glass filter support or stainless steelscreen su
32、pport 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 mL.6.13 Vacuum Source, to prov
33、ide pressure reduction to 13.36 0.7 kPa (100 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, capable of maintaining a temperature of10
34、5 6 2C.6.16 Forceps, having unserrated tips.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 Int
35、ernational Headquarters. Your comments will 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
36、.,Bedford, MA.8The sole source of supply 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 Sc
37、ientific Co., Pittsburgh, PA.D4310 1026.17 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 locking con-nector, 10-mL capacity for sampling.6.22 Syringe Sampling Tube,
38、Grade 304 stainless steeltubing, 2.11 mm (0.083 in.) outside diameter, 1.60 mm (0.063in.) inside diameter, 559 6 2 mm (24.0 6 0.08 in.) long, withone end finished at 90 and the other end fitted with a Luer-Lokfemale connector.7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals sha
39、ll beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAll dimensions are in millimetres (inches)NOTE 1The oxidation test tube has a calibration line at 300 mL. This calibration applies to the test tube alone at 20C.NOTE 2
40、Open tube ends to be ground and fire-polished.FIG. 1 Oxidation CellD4310 103FIG. 2 Mandrel for Winding Catalyst CoilsD4310 104Analytical 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
41、 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 Specification D1193.7.3 AcetoneReagent grade. (WarningHealth hazard,flamma
42、ble.)7.4 Cleaning 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 % (relat
43、ive density 1.19).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., and the Unite
44、d States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.11The sole source of supply of Nochromix known to the committee at this timeis Godax Laboratories, Inc., 720-B Erie Avenue, Takoma Park, MD 20912.12The sole source of supply of Micro known to the co
45、mmittee at this time isInternational Products Corp., P.O. Box 70, Burlington, NJ 08016.All dimensions are in millimetres (inches).Material: 18-8 Stainless Steel. 22 Gauge (0.792 mm).FIG. 3 Thermometer BracketD4310 1057.7 Isopropyl AlcoholReagent grade. (WarningFlammable.)7.8 Catalyst Wires:7.8.1 Low
46、-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 satisfactory. Similarwire conforming to BS 1829, is also satisfactory. If these steels are notav
47、ailable, 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.) indiameter (No. 16 Imperial Standard Wire Gauge or No. 14American Wire Gauge), 99.9 % purity, conforming to Sp
48、ecifi-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(WarningOxygen vigorously acceleratescombustion) 99.5 % minimum purity, with pressure regulatio
49、nadequate 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, smallcontainers, 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 6 0.01-m length of iron wire
