1、Designation: D 4310 06bAn American National StandardStandard Test Method forDetermination of Sludging and Corrosion Tendencies ofInhibited Mineral Oils1This standard is issued under the fixed designation D 4310; the number immediately following the designation indicates the year oforiginal adoption
2、or, in the 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.1. Scope*1.1 This test method is used to evaluate the tendency ofinhibited mineral oil b
3、ased steam turbine lubricants and min-eral oil based anti-wear hydraulic oils to corrode coppercatalyst metal and to form sludge during oxidation in thepresence of oxygen, water, and copper and iron metals at anelevated temperature. The test method is also used for testingcirculating oils having a s
4、pecific 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 i
5、nappropriate. The results of the cooperative test program areavailable (see Section 16).1.2 This test method is a modification of Test Method D 943where 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
6、 reach an acid number of 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 number
7、determination 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 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility
8、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 7 and X1.1.5.2. Referenced Documents2.1 ASTM Standards:2A 510 Specification for General Requirements
9、 for WireRods and Coarse Round Wire, Carbon SteelB1 Specification for Hard-Drawn Copper WireD 664 Test Method forAcid Number of Petroleum Productsby Potentiometric TitrationD 874 Test Method for Sulfated Ash from Lubricating Oilsand AdditivesD 943 Test Method for Oxidation Characteristics of Inhib-i
10、ted Mineral OilsD 1193 Specification for Reagent WaterD 3339 Test Method for Acid Number of Petroleum Prod-ucts by Semi-Micro Color Indicator TitrationD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsE1 Specification for ASTM Liquid-in-Glass Thermometers2.2 IP Standard:3Specific
11、ation for IP Standard 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 pr
12、esenceof water 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 o
13、f Turbine Oils.Current edition approved Dec. 1, 2006. Published January 2007. Originallyapproved in 1983. Last previous edition approved in 2006 as D 431006a.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of A
14、STMStandards 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 section
15、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 also de
16、termined 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
17、 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 optionaltests
18、 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 corrode
19、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 ground and
20、fire-polished.FIG. 1 Oxidation CellD 4310 06b26. 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 without
21、 insertsat 20C.6.2 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 stirring device toprovide a uniform temperature throughout the bath, and largeenough to hold the desired number of oxidation
22、 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.6.2.1 Studies have suggested that direct sunlight or artificiallight may adversely influence the results of this test.5Tominimize effects of light exposure on the lubricant beingtes
23、ted, 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 cell from the sides is preferred. I
24、f 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 material.6.2.1.3 Bright light enteri
25、ng 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 72 to 126C andconforming to the r
26、equirements 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,6,7having a range from 80to 100C, g
27、raduated in 0.1C, total length250 mm, stemdiameter6.0 to 7.0 mm, calibrated for 76-mm immersion.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 t
28、he 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 approximately 6.4-mm (14-in.) inside diameter with a332-in.
29、wall for delivery ofoxygen to the oxidation cell.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 sc
30、reensupport 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,10cylindrical body with ground-glassstopper; approximate inside diameter 45 mm, height of body65 mm, capacity 60 mL.6.13 Vacuum Source, to
31、 provide 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
32、 of105 6 2C.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 locking con-nector, 10-mL capacity for sampling.6.22 Syringe Samp
33、ling Tube, 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 ch
34、emicals 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.11Other grades may be used,provided it is first ascertained that
35、 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 Specification D 1193.5Supporting data (summary of the re
36、sults of these studies) have been filed atASTM International Headquarters and may be obtained by requesting ResearchReport RR: 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 awar
37、e of alternative suppliers, please provide this information 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,cellulos
38、e esters) known to the committee at this time is Millipore 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 w
39、eighing bottle, size G, knownto the committee at this 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 Anal
40、ar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D 4310 06b3FIG. 2 Mandrel for Winding Catalyst CoilsD 4310 06b47.3 AcetoneReagent grade. (WarningHealth hazard,flamm
41、able.)7.4 Cleaning Reagent, cleaning by a 24-h soak at 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
42、 density 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 Gage).NOTE 3Carbon steel wire, soft bright annealed and free from rust ofGrade 1008 as described in Specification A 510 i
43、s satisfactory. 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 D 4310.7.8.2 Electrolytic Copper Wire, 1.63 mm (0.064 in.) indiameter
44、(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 from a supplier.12The sole source of supply of Nochromix k
45、nown to the committee at this timeis Godax Laboratories, Inc., 720-B Erie Avenue, 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
46、 Stainless Steel. 22 Gage (0.792 mm).FIG. 3 Thermometer BracketD 4310 06b57.9 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
47、 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 PracticeD 4057.8.2 For one single determination the minimum requiredsampl
48、e 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 and anequal length of copper wire with wads of absorbent cotton wetwith n-heptane and follow by abrasion with abrasive cloth untila fresh metal surf
49、ace 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 copperwires tightly together at one end for three turns and then windthem simultaneously alongside each other on a threadedmandrel (see Fig. 2), inserting the iron wire in the deeperthread. Remove the coil from the mandrel, twist the free endsof t
