ASTM D7873-2013 0533 Standard Test Method for Determination of Oxidation Stability and Insolubles Formation of Inhibited Turbine Oils at 120° C Without the Inclusion of Water &4.pdf

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1、Designation: D7873 13Standard Test Method forDetermination of Oxidation Stability and InsolublesFormation of Inhibited Turbine Oils at 120 C Without theInclusion of Water (Dry TOST Method)1This standard is issued under the fixed designation D7873; the number immediately following the designation ind

2、icates the year oforiginal adoption or, in the case 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 is used to evaluate the

3、sludgingtendencies of steam and gas turbine lubricants during theoxidation process in the presence of oxygen and metal catalyst(copper and iron) at an elevated temperature. This test methodmay be used to evaluate industrial oils (for example, circulat-ing oils and so forth).1.2 This test method is a

4、 modification of Test MethodD4310 where the sludging and corrosion tendencies of thesame kinds of oils are determined after 1000 h at 95 C in thepresence of water. Water is omitted in this modification.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are

5、 included in thisstandard.1.3.1 ExceptionThe values in parentheses in some of thefigures are provided for information only for those using oldequipment based on non-SI units.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibil

6、ity 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.1.5 WARNINGMercury has been designated by manyregulatory agencies as a hazardous material that can causecentral nervous system, kidney and li

7、ver 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 addi-tio

8、nal information. Users should be aware that selling mercuryand/or mercury containing products into your state or countrymay be prohibited by law.2. Referenced Documents2.1 ASTM Standards:2A510M Specification for General Requirements for WireRods and Coarse Round Wire, Carbon Steel (Metric)(Withdrawn

9、 2011)3B1 Specification for Hard-Drawn Copper WireD943 Test Method for Oxidation Characteristics of InhibitedMineral OilsD1193 Specification for Reagent WaterD2272 Test Method for Oxidation Stability of Steam Tur-bine Oils by Rotating Pressure VesselD4057 Practice for Manual Sampling of Petroleum an

10、dPetroleum ProductsD4310 Test Method for Determination of Sludging andCorrosion Tendencies of Inhibited Mineral OilsE1 Specification for ASTM Liquid-in-Glass ThermometersE230 Specification and Temperature-Electromotive Force(EMF) Tables for Standardized Thermocouples2.2 Other Standards:Specification

11、 for IP Standard Thermometers4ISO 3696 Water for Analytical Laboratory UseSpecification and Test Methods53. Terminology3.1 Definitions:3.1.1 sludge, na precipitate or sediment from oxidizedmineral oil that is insoluble in n-heptane. D9434. Summary of Test Method4.1 Atotal of six to eight tubes conta

12、ining 360 mLof sampleeach are heated at 120 C with oxygen in the presence of an1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.09.0C on Oxidation of Turbine Oils.Current edition a

13、pproved Dec. 1, 2013. Published January 2014. DOI: 10.1520/D7873-13.2For 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 w

14、ebsite.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,U.K., http:/www.energyinst.org.5Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036

15、, http:/www.ansi.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1iron-copper catalyst. Each tube is removed over time and thesample is analyzed by Test Method D2272 and the insolublesare measured until the RPVOT residual ratio rea

16、ches below25 % or an agreed-upon percentage or specified time. Test runfor a specified time(s) may be run using a single tube or asmany as specified by the requestor. The mass of insolublematerial of each oil sample is determined gravimetrically byfiltration of a 100 g oil sample through a membrane

17、filter withpore size 1 m. The insoluble mass (mg/kg oil) is plottedagainst RPVOT residual ratio. The insoluble mass in milli-grams per kilogram oil at 25 % or an agreed-upon RPVOTresidual ratio or specified time is reported.5. Significance and Use5.1 Insoluble material may form in oils that are subj

18、ected 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 both, resulting invarnish formation during field service. The level of varnishformation in service will

19、 be dependent on many factors(turbine design, reservoir temperature, duty-cycle, for example.peaking, cycling, or base-load duty, maintenance, and so forth)and a direct correlation between results in this test and fieldvarnish formation are yet to be established.5.3 Oxidation condition at 120 C unde

20、r accelerated oxida-tion environment of Test Method D4310 and measurement ofsludge and RPVOT value could reflect a practical oil quality inactual turbine operations. Results from this test should be usedtogether with other key lubricant performance indicators (in-cluding other established oxidation

21、and corrosion tests) toindicate suitability for service.6. Apparatus6.1 Oxidation Cell, of borosilicate glass, as shown in Fig. 1,consisting of a test tube, condenser, and oxygen delivery tube.It is recommended to have a test tube with a calibration line at360 mL (maximum error 1 mL). This calibrati

22、on applies to thetest tube without inserts at 20 C.6.2 Heating Bath, thermostatically controlled, capable ofmaintaining the oil sample in the oxidation cell at a tempera-ture of 120 C 6 0.5 C, fitted with a suitable stirring device toprovide a uniform temperature throughout the bath, and largeenough

23、 to hold the desired number of oxidation cells immersedin the heating bath to a depth of 355 mm 6 10 mm. Heatedmetal block baths meeting the test method requirements mayalso be used.6.2.1 Studies have suggested that direct sunlight or artificiallight may adversely influence the results of this test.

24、 Tominimize 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 prevent

25、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 with alu

26、minum 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 Thermometer, ASTM Solvents DistillationTh

27、ermometer having a range from 98 C to 152 C andconforming to the requirements for Thermometer 41C asprescribed in Specification E1, or for Thermometer 81C asprescribed in Specifications for IP Standard Thermometers.Alternatively, temperature-measuring devices of equal or betteraccuracy and precision

28、 may be used.6.5 Oxidation Cell Thermometer, A 76 mm immersion LIGhaving a range of 110 C to 130 C, graduated in 0.1 C, totallength of 300 mm 6 5 mm, and stem diameter of 6.0 mm to 7.0mm. Alternatively, temperature-measuring devices or DCT, ofequal or better accuracy and precision may be used. Tempe

29、ra-ture of the sample shall be measured at 76 mm from the top ofthe sample. See Fig. 2 and Fig. 3.NOTE 1Temperature gradient within the sample may exist from theheating system and temperature control design.6.6 Wire Coiling Mandrel, as shown in Fig. 4.6.7 Thermometer Bracket, for holding the oxidati

30、on cellthermometer, of 18-8 stainless steel, having the dimensionsshown in Fig. 5. The thermometer 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 clo

31、thbacking.6.9 Flexible Tubing, poly vinyl chloride approximately 6.4mm (14 in.) inside diameter with a 2.4 mm (332 in.) wall fordelivery of oxygen to the oxidation cell.6.10 Membrane Filters, white, plain, 47 mm in diameter,pore size 1 m. The recommended membrane filters are PTFEand cellulose acetat

32、e plus nitrocellulose material.6.11 Filter Holder, 47 mm, consisting of a borosilicate glassfunnel and a funnel base with a coarse grade fritted-glass filtersupport with a length of 40 m to 60 m, or stainless steelscreen support such that the filter can be clamped between theground-glass sealing sur

33、faces of the funnel and its base bymeans of a metal clamp.6.12 Weighing Bottle, cylindrical body with ground-glassstopper; approximate inside diameter 65 mm, height of body45 mm , capacity 60 mL.6.13 Vacuum Source, to provide pressure reduction to13.3 kPa 6 0.7 kPa (100 mm 6 5 mm Hg) absolute pressu

34、re.6.14 Cooling Vessel, A desiccator or other type of tightlycovered vessel for cooling the weighing vessels before weigh-ing. The use of a drying agent is not recommended.D7873 132NOTE 1All dimensions are in millimetres (inches).NOTE 2The oxidation test tube has a calibration line at 360 mL. This c

35、alibration applies to the test tube alone at 20 C.NOTE 3Open tube ends to be ground and fire-polished.FIG. 1 Oxidation CellD7873 1336.15 Drying Oven, capable of maintaining a temperature of70 C 6 5 C.6.16 Forceps, having unserrated tips.6.17 Rubber Policeman.6.18 Pipette Bulb.7. Reagents and Materia

36、ls7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.67.2 Reagent Wa

37、ter, Unless otherwise indicated, reference towater shall be understood to mean distilled, deionized water asdefined by Type I or Type II in Specification D1193 or Grade3 in ISO 3696.7.3 Acetone, Reagent grade. (WarningHealth hazard,flammable.)7.4 Cleaning Reagent, cleaning by a 24 h soak at roomtemp

38、erature in a free rinsing liquid acid cleaner with a pH of 2to 4.5.7.5 n-heptane, Reagent grade. (WarningFlammable.Harmful if inhaled.)7.6 Isopropyl Alcohol, Reagent grade. (WarningFlammable.)7.7 Catalyst Wires,7.7.1 Low-Metalloid Steel Wire1.59 mm (0.0625 in.) indiameter (No. 16 Washburn and Moen G

39、age).NOTE 2Carbon steel wire, soft bright annealed and free from rust ofGrade 1008 as described in Specification A510M is satisfactory. Similarwire conforming to Specification E230 is also satisfactory7.8 Electrolytic Copper Wire, 1.63 mm (0.064 in.) in diam-eter (No. 16 Imperial Standard Wire Gage

40、or No. 14 AmericanWire Gage), 99.9 % purity, conforming to Specification B1.NOTE 3Alternatively, suitably prepared steel and copper catalyst coilsmay be purchased from a supplier.7.9 Detergent, free rinsing, water-soluble, anionic detergentwith a pH of 9.5 to 11.7.10 Oxygen(WarningOxygen vigorously

41、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, smallcontainers, or even op

42、erating equipment. Therefore, use theapplicable apparatus and techniques described in PracticeD4057.8.2 For one single determination at a specified time theminimum required sample size is 360 mL. However, 6 to 8tubes will be required to develop the data points to obtain thesludge mass at 25 % or agr

43、eed-upon residual RPVOT ratio bylogarithmic interpolation. Therefore, approximately 2200 mLto 2900 mL will be required for this test.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 and6Reagent Chemicals, America

44、n Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U

45、.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.FIG. 2 Oxidation Cell with ThermometerFIG. 3 76 mm Immersion LIG ThermometerD7873 134an 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

46、. Then wipe with dryabsorbent cotton until all loose particles of metal and abrasivehave been removed. In subsequent operations, handle thecatalyst wires with clean gloves (cotton, rubber, or plastic) toprevent contact with the skin.9.2 Preparation of Catalyst CoilTwist the iron and copperwires tigh

47、tly together at one end for three turns and then windthem simultaneously alongside each other on a threadedmandrel (see Fig. 4), inserting the iron wire in the deeperthread. Remove the coil from the mandrel, twist the free endsof the iron and copper wires together for three turns, and bendthe twiste

48、d ends to conform to the shape of the spiral coil. Theoverall length of the finished coil should be 225 mm 6 5mm(8.9 in. 6 0.2 in.). If necessary, the coil may be stretched togive the required length (Note 4).NOTE 4The finished catalyst coil is a double spiral of copper and ironwire, 225 mm 6 5 mm (

49、8.9 in. 6 0.2 in.) overall length and 15.9 mm to16.5 mm (0.625 in. to 0.650 in.) inside diameter. The turns of wire areevenly spaced, and two consecutive turns of the same wire are 3.96 mm to4.22 mm (0.156 in. to 0.166 in.) apart, center to center. The mandrelshown in Fig. 4 is designed to produce such a coil. Using this mandrel, theiron wire is wound on a thread of 14.98 mm (0.590 in.) diameter, while thecopper wire is wound on a thread of 15.9 mm (0.625 in.) diameter. Thesmaller diameter is to allow for “springback” of the steel wir