1、Designation: D 5968 06An American National StandardStandard Test Method forEvaluation of Corrosiveness of Diesel Engine Oil at 121C1This standard is issued under the fixed designation D 5968; the number immediately following the designation indicates the year oforiginal adoption or, in the case of r
2、evision, 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.INTRODUCTIONThe method described in this test method is based on the gas turbine lubricant corrosion andoxid
3、ation test described in Federal Test Method Standard 791, Method 5308. Because this test methodrelates to corrosion in diesel engines rather than in gas turbines, temperatures, metal coupons, andcertain parts of the test procedure were modified to be more appropriate for heavy duty diesel engines.Th
4、e method described in this test method can be used by any properly equipped laboratory, withoutoutside assistance. However, the ASTM Test Monitoring Center (TMC)2provides reference oils andan assessment of the test results obtained on those oils by the laboratory (see Annex A1). By thesemeans, the l
5、aboratory will know whether their use of the test method gives results statistically similarto those obtained by other laboratories. Furthermore, various agencies require that a laboratory utilizethe TMC services in seeking qualification of oils against specifications. For example, the U.S. Armyimpo
6、ses such a requirement in connection with several Army engine lubricating oil specifications.Accordingly, this test method is written for use by laboratories that utilize the TMC services.Laboratories that choose not to use those services may simply ignore those portions of the test methodthat refer
7、 to the TMC.This test method may be modified by means of Information Letters issued by the TMC. In addition,the TMC may issue supplementary memoranda related to the method (see Annex A1). For otherinformation, refer to the research report on the Cummins Bench Corrosion Test.31. Scope1.1 This test me
8、thod is used to test diesel engine lubricantsto determine their tendency to corrode various metals, specifi-cally alloys of lead and copper commonly used in camfollowers and bearings. Correlation with field experience hasbeen established.41.2 The values stated in SI units are to be regarded as thest
9、andard.1.3 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 establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specifi
10、c hazardstatements are given in 5.3.1, 6.6, 6.7, 6.8, 6.9, 6.10, 6.11,7.1.1, 7.1.2, 7.1.5, and 7.4.1.2. Referenced Documents2.1 ASTM Standards:5D 130 Test Method for Detection of Copper Corrosion fromPetroleum Products by the Copper Strip Tarnish TestD 5185 Determination of Additive Elements, Wear M
11、etals,and Contaminants in Used Lubricating Oils and Determi-nation of Selected Elements in Base Oils by InductivelyCoupled Plasma Atomic Emission Spectrometry (ICP-AES)E 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method1This test method is under the juri
12、sdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.B0.02 on Heavy Duty Engine Oils.Current edition approved Nov. 1, 2006. Published November 2006. Originallyapproved in 1998. Last previous edition approved in 2004 as D 596804.2ASTM
13、Test Monitoring Center, 6555 Penn Ave., Pittsburgh, PA 15206-4489.(http:/www.astmtmc.cmu.edu/)3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D02-1322. The research report andthis test method are supplemented by Information Let
14、ters and Memoranda issued bythe ASTM Test Monitoring Center. This edition incorporates revisions contained inall information letters through No. 051. Users of this test method shall contact theASTM Test Monitoring Center to obtain the most recent of these.4Wang, J. C., and Cusano, C. M., “Developmen
15、t of A Bench Test to Detect OilsCorrosive to Engine Components,” SAE Technical Paper No. 940790, 1994.5For 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
16、Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.2.2 U.S. Federal Test Method Standards:6Federal Test Method Standard 791, Method 5308.7 Corro-siveness and Oxidation Stability of Light Oils (Me
17、talSquares)3. Summary of Test Method3.1 Four metal coupons of copper, lead, tin, and phosphorbronze are immersed in a measured amount of engine oil. Theoil, at an elevated temperature, is blown with air for a period oftime. When the test is completed, the coupons and the stressedoil are examined to
18、detect corrosion.3.2 An industrial reference oil is tested with each group oftests to verify test acceptability.4. Significance and Use4.1 This test method is intended to simulate the corrosionprocess of non-ferrous metals in diesel lubricants. The corro-sion process under investigation is that beli
19、eved to be inducedprimarily by inappropriate lubricant chemistry rather thanlubricant degradation or contamination. This test method hasbeen found to correlate with an extensive fleet databasecontaining corrosion-induced cam and bearing failures.5. Apparatus5.1 The main apparatus consists of the fol
20、lowing items ofstandard wall borosilicate glassware as shown in Figs. 1-6.5.1.1 Main Sample Tube, Fig. 1.5.1.2 Sample Tube Head, Fig. 2.5.1.3 Air Tube, Fig. 3.5.1.4 Thermocouple Tube, Fig. 4.5.1.5 Condenser, Allihn Type, Fig. 5.5.1.6 Assembled Apparatus, Fig. 6.5.2 Additional glassware items and ass
21、embly accessoriesneeded are:5.2.1 Spacers (for metal specimen), of borosilicate glass,standard wall, 9-mm outside diameter, 6-mm length.5.2.2 Oil Sampling Tube, Borosilicate Glass, 4-mm outsidediameter, with sampling end approximately 600 mm to reach6Available from Standardization Documents Order De
22、sk, DODSSP, Bldg. 4,Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098.FIG. 1 Sample TubeFIG. 2 Sample Tube HeadFIG. 3 Air TubeD5968062into main sample tube. Tube is bent U-shape with exit endfitted by a one-hole stopper to a 25-mL filtering flask. Exit endmay be any convenient length.5.2.3 Ad
23、apter7,8, Polytetrafluoroethylene for 10/18 joint forsealing of air tube to sample tube head.5.3 Other items and equipment are:5.3.1 Heating Bath, constant temperature control within60.5C (61F) of test temperature with an immersion depth of23 to 35 cm. Oil or aluminum baths are recommended.(WarningT
24、here are exposed hot surfaces on apparatus.Avoid skin contact by use of protective equipment.)5.3.2 Hood Ventilation, to adequately remove fumes duringheating.5.3.3 Air Supply, use air from a clean, dry source.5.3.4 Flowmeter, capable of measuring 10 6 1 L/h.5.3.5 Balance, analytical sensitivity 0.1
25、 mg.5.3.6 Balance, Laboratory, 2500-g capacity, 0.1-g sensitiv-ity.5.3.7 Microscope, with 20-diameter magnification.5.3.8 Assembly Fixture, wood slotted to hold couponssquares (assembly as shown in Fig. 7) for tying with wire.5.3.9 When air needs to be conditioned there is a need for anair drier. Th
26、e method used is optional provided the aircharacteristics of 5.3.3 are attained. For drying, a satisfactorymethod is the use of a glass column containing 8-meshanhydrous calcium sulfate with a column diameter such thatvelocity of air does not exceed 1.2 m/min.5.3.10 Oven, optional, to dry glassware
27、at elevated tempera-ture.5.3.11 Forceps, stainless steel.5.3.12 Thermocouple.5.3.13 Brush, short-bristled, stiff (old-style typewriter clean-ing brush or equivalent).6. Reagents and Materials6.1 Purity of ReagentsUse reagent grade chemicals in alltests. Unless otherwise indicated, it is intended tha
28、t all reagents7A satisfactory source for this item is Kontes Glass Co., Vineland, NJ 08360.8The sole source of supply of the apparatus known to the committee at this timeis noted in the adjoining footnote. If you are aware of alternative suppliers, pleaseprovide this information to ASTM Headquarters
29、. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend.FIG. 4 Thermocouple TubeFIG. 5 Condenser, Allihn TypeFIG. 6 Assembled ApparatusD5968063conform to the specifications of the Committee on AnalyticalReagents of the American Chemi
30、cal Society where suchspecifications are available.96.2 Metal Specimens:8,106.2.1 Coupons, 0.081 cm thick by 2.5 cm square, one each,with two drilled holes (as shown in Fig. 7), as follows:6.2.1.1 Copper (R401-A),6.2.1.2 Lead (R401-lead),6.2.1.3 Tin (R401-tin), and6.2.1.4 Phosphor Bronze (R401-LEADz
31、).6.3 Nichrome Wire, clean (for tying coupons together).6.4 Abrasive Paper, 240 grit aluminum oxide and 400 gritsilicon-carbide.11Do not use iron-containing abrasives such asnatural emery.6.5 Cotton, absorbent.6.6 Acetone (ACS), sulfur-free. (WarningFlammable.Health hazard.6.7 Degreasing Solvents, T
32、richlorotrifluorethane or 1,1,1-trichloroethane. (WarningHarmful if inhaled.)6.8 Glassware Cleaning Solution, mix 35 mL of saturatedsodium dichromate (aqueous) solution and 1000 mL of con-centrated sulfuric acid. (WarningCauses severe burns.)6.9 Carbon Remover for Glassware8,12, Oakite StripperR-8.
33、(WarningCorrosive, causes severe burns.)6.10 Tetrahydrofuran.(WarningToxic and flammable.Health hazard.)6.11 Naphtha, Aromatic.(WarningFlammable. Healthhazard.)6.12 Filter Paper.6.13 Kimwipe Tissues, or similar.6.14 Industrial Reference Oil.27. Preparation of Apparatus7.1 Cleaning of Glassware from
34、Previous Run:7.1.1 Rinse all glassware items and the air tube adapter withdegreasing solvent to remove residual oil, and air dry.(WarningHarmful if inhaled.)7.1.2 Fill or immerse the sample tube, air tube, and the9-mm glass spacers in carbon remover at room temperatureuntil carbonaceous deposits are
35、 removed. Water rinse afterremoval. (WarningCorrosive, causes severe burns.)7.1.3 Wash all glassware items and the air tube adapter withdetergent.8,13Rinse with water to remove detergent, and dry.7.1.4 Store all items in a dust free cabinet until needed fortest. If stored longer than one week, rinse
36、 again with distilledwater before use, and dry.7.1.5 A more elaborate glass cleaning procedure can beused, if it is for a given situation. This cleaning procedure isnecessary in a referee situation unless a cleaning solution canbe used which is satisfactory to all parties involved. Fill andimmerse a
37、ll glassware items with glassware cleaning solutionand soak for 3 to 16 h. (WarningCorrosive, causes severeburns.)7.1.6 Remove glassware from cleaning solution, rinse sev-eral times with tap water, followed by distilled water, and ovendry.7.2 Cleaning of Glassware (New):7.2.1 Proceed as in 7.1.3 and
38、 7.1.6 in that order (omit 7.1.1,7.1.2, 7.1.4, and 7.1.5).7.3 AssemblyAssemble as shown in Fig. 6 using only thetest oil to lubricate glass joints during assembly.7.4 Preparation of Metal Specimens:7.4.1 Wash a length of the metal tying wire with tetrahy-drofuran and acetone and allow to dry. (Warni
39、ngThis andthe following preparation processes should be performed undera fume hood.)7.4.2 The metal squares are prepared as follows:7.4.2.1 Using the 240 grit abrasive paper, remove all surfaceblemishes from both sides and all four edges of each square,and any burrs from the drilled holes. Finish po
40、lishing with 400grit paper wetted by acetone to remove marks from previouspolishing. A good technique is to place abrasive paper on a flat9Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by th
41、e American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.10Satisfactory metal specimens may be obtained from: Test Engineering, Inc.(TEI
42、), 12718 Cimarron Path, San Antonio, TX 78249-3423. This is the only couponsource to be used for obtaining a valid reference run and data for certification.11Suitable abrasive paper meeting these specifications is included with the metalcoupons from the source indicated in 6.2.12Oakite Stripper R-8
43、is available from Oakite Products, Inc., 50 Valley Rd.,Berkeley Heights, NJ 07922. It has been found satisfactory for this purpose.13A detergent found satisfactory is Alconox made by Alconox, Inc., 215 ParkAve. S., New York, NY 10003.FIG. 7 Arrangement of Metal CouponsD5968064surface, then rub the s
44、pecimen with longitudinal strokes in adirection perpendicular to that used with 240 grit paper. Use adifferent sheet of paper for each metal type.7.4.2.2 In all succeeding steps, handle the squares only withtongs or filter paper until the final weighing. If large defects orparticles are present on t
45、he metal coupons, course sand papershould be used first to remove them; this is followed bypolishing with the 240 and 400 grit abrasive paper.(1) Store the polished metal coupon in tetrahydrofuran andproceed until all coupons are polished.(2) Remove each square from the tetrahydrofuran, clean allmet
46、al dust from the square by rubbing vigorously with cleanpads of absorbent cotton until a fresh pad remains unsoiled.(3) Wash squares in tetrahydrofuran and allow them to dryin a dessicator.(4) Immediately weigh each square to within 0.1 mg.(5) Arrange all squares in the wooden assembly fixture inthe
47、 pattern shown in Fig. 7. The sequence should be: lead,copper, tin, phosphor bronze.7.4.2.3 Using only forceps to handle the clean wire, tie thesquares together as shown in Fig. 7.8. Procedure8.1 Preparation for New Test Set-Up for Reference Oil andTest Oils:8.1.1 Insert the tied coupons in the test
48、 tube, positioning thesquares vertically (so that the air tube can be inserted to touchthe bottom of the test tube). Weigh the air tube, test tube, andcontents together to within 0.1 g.8.1.2 Add 100 6 1 mL of oil to the test tube, reweigh the airtube, test tubes, and contents together to within 0.1
49、g, anddetermine the weight of oil added.8.1.3 Assemble the test tube and condenser and mount theassembly so that the test tube is submerged 23 to 35 cm in thebath with the test oil temperature set at 121 6 0.5C.8.1.4 Start the flow of cooling water through the condenserjacket.8.1.5 Insert the air tube (orifice-end down) through thecondenser and into the oil sample and support it so that itsorifice is within 0.3 cm of the bottom of the tubes.8.2 To begin testing connect the source of clean, dry air (56 0.5 L/h) to the air tube and allow the air to flow for 168 h.8.3
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