1、Designation: D4310 09Standard 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 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 sta
8、ndard 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 WireRods and Coarse
9、 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 Inhib-ited Mineral OilsD1193 Spec
10、ification for 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 St
11、andard Thermometers2.3 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.4. Summary of Test Method4.1 An oil sample is contacted with oxygen in the presenceof water
12、and an iron-copper catalyst at 95C for 1000 h. Theweight of insoluble material is determined gravimetrically by1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.09.0C on Oxidation of Turbine Oils.
13、Current edition approved Oct. 1, 2009. Published November 2009. Originallyapproved in 1983. Last previous edition approved in 2006 as D431006b. DOI:10.1520/D4310-09.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Bo
14、ok 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 Institute (BSI), 389 Chiswick High Rd.,London W4 4AL, U.K.1*A Summary of Changes s
15、ection appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.filtration of the oxidation tube contents through 5-m pore sizefilter disks. The total amount of copper in the oil, water, andsludge phases is
16、also determined 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 t
17、he acid number 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 option
18、altests are not 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 c
19、orrode metals, or both, during fieldservice. However, no correlation with field service has beenestablished.All 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 2Open tube ends to be grou
20、nd and fire-polished.FIG. 1 Oxidation CellD4310 0926. 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 calibration applies to the test tube wi
21、thout 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 temperaturethroughout the bath, and large enough to hol
22、d 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 this test.5Tominimize effects of light ex
23、posure 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 prevent light from entering thetest cel
24、l 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 with aluminum foil or other opaque mate
25、rial.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-tion Thermometer having a range from 7
26、2 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 used.6.5 Oxidation Cell Thermometer,6,7
27、having a range from 80to 100C, 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 equivalent or better accuracy and prec
28、isionthat 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 bracket by twofluoro-elastomer O-rings of
29、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 delivery ofoxygen to the oxidation c
30、ell.6.10 Membrane Filters,8white, plain, 47 or 90 mm indiameter, pore size 5 m.6.11 Filter Holder,947 or 90 mm, consisting of a borosili-cate glass funnel and a funnel base with a coarse grade (40 to60-m) fritted-glass filter support or stainless steel screensupport such that the filter can be clamp
31、ed between theground-glass sealing surfaces of the funnel and its base bymeans of a metal clamp.6.12 Weighing Bottle,10cylindrical body with ground-glassstopper; approximate inside diameter 45 mm, height of body65 mm, capacity 60 mL.6.13 Vacuum Source, to provide pressure reduction to 13.36 0.7 kPa
32、(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 of105 6 2C.6.16 Forceps, having unserrated t
33、ips.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 locking con-nector, 10-mL capacity for sampling.6.22 Syringe Sampling Tube, Grade 304 stainless steeltubing, 2
34、.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 shall beused in all tests. Unless oth
35、erwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.11Other grades may be used,5Supporting data (summary of the results of these studies) have been filed atASTM
36、International Headquarters and may be obtained by requesting ResearchReport D02-1365.6The sole source of supply of the Brooklyn Thermometer No. 21276-RM knownto the committee at this time is Brooklyn Thermometer Co., Farmingdale, NY.7If you are aware of alternative suppliers, please provide this inf
37、ormation toASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee,1which you may attend.8The sole source of supply of the Millipore SM membrane filters (MF-type,cellulose esters) known to the committee at this time is Mi
38、llipore Filter Corp.,Bedford, MA.9The 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.10The sole source of supply of the Fisher 3-415 weighing bottle, size G, knownto the committee at th
39、is time is Fisher Scientific Co., Pittsburgh, PA.11Reagent 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., Poo
40、le, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D4310 093FIG. 2 Mandrel for Winding Catalyst CoilsD4310 094provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without le
41、ssening 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,flammable.)7.4 Cleaning Reagent, cleaning by a 24-h soak at
42、 roomtemperature in either Nochromix12(WarningCorrosive,health hazard) or in Micro13solution.7.5 n-heptane, Reagent grade. (WarningFlammable.Harmful if inhaled.)7.6 Hydrochloric Acid (WarningToxic and corrosive.),concentrated (36 mass % (relative density 1.19).7.7 Isopropyl AlcoholReagent grade. (Wa
43、rningFlammable.)7.8 Catalyst Wires:7.8.1 Low-Metalloid Steel Wire, 1.59 mm (0.0625 in.) indiameter (No. 16 Washburn and Moen Gage).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 a
44、lso 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 D4310.12The sole source of supply of Nochromix known to the committee at this timeis Godax Laboratories, Inc., 720-B Erie Ave
45、nue, Takoma Park, MD 20912.13The sole source of supply of Micro known to the committee 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 Gage (0.792 mm).FIG. 3 Thermometer BracketD4310 0957.8.2
46、 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 4Alternatively, suitably prepared catalyst coils may be pur-chased
47、from a supplier.7.9 Detergent, water-soluble.147.10 Oxygen(WarningOxygen 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. Sampli
48、ng8.1 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 Ca
49、talystImmediately prior to winding acatalyst 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 cloth untila fresh metal surface is exposed. Then wipe with dry absorbentcotton until all loose particles of metal and abrasive have beenremoved. In subsequent operations handle the catalyst wireswith clean gloves (cotton, rubber, or plastic) to prevent contactwith the skin.9.2 Preparation of Catalyst CoilTwist the iron and coppe
