1、Designation: D 6594 08An American National StandardStandard Test Method forEvaluation of Corrosiveness of Diesel Engine Oil at 135C1This standard is issued under the fixed designation D 6594; 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 () indicates an editorial change since the last revision or reapproval.INTRODUCTIONAny properly equipped laboratory, without outside assistance, can use the procedure described int
3、his test method. However, the ASTM Test Monitoring Center (TMC)2provides reference oils and anassessment of the test results obtained on those oils by the laboratory (seeAnnexA1). By these means,the laboratory will know whether their use of the test method gives results statistically similar to thos
4、eobtained by other laboratories. Furthermore, various agencies require that a laboratory utilize the TMCservices in seeking qualification of oils against specifications. For example, the U.S. Army imposessuch a requirement in connection with several Army engine lubricating oil specifications.Accordi
5、ngly, 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 to the TMC.This test method may be modified by means of information letters issued by the TMC. In a
6、ddition,the TMC may issue supplementary memoranda related to the method (see Annex A1). For otherinformation, refer to the research report of this test method.31. Scope1.1 This test method covers testing diesel engine lubricantsto determine their tendency to corrode various metals, specifi-cally all
7、oys of lead and copper commonly used in camfollowers and bearings.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It i
8、s 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.2. Referenced Documents2.1 ASTM Standards:4D 130 Test Method for Corrosiveness to Copper fromPetroleum Products by Copper Str
9、ip TestD 5185 Test Method for Determination of Additive Ele-ments, Wear Metals, and Contaminants in Used Lubricat-ing Oils and Determination of Selected Elements in BaseOils by Inductively Coupled Plasma Atomic EmissionSpectrometry (ICP-AES)D 5844 Test Method for Evaluation of Automotive EngineOils
10、for Inhibition of Rusting (Sequence IID)5D 6557 Test Method for Evaluation of Rust PreventiveCharacteristics of Automotive Engine Oils3. Terminology3.1 Definitions:3.1.1 corrosion, nthe chemical or electrochemical reac-tion between a material, usually a metal surface, and its1This test method is und
11、er the jurisdiction 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 Oct. 15, 2008. Published November 2008. Originallyapproved in 2000. Last previous edition approved in 2006 as D 6
12、59406.2The ASTM Test Monitoring Center will update changes in this test method bymeans of Information Letters. This edition incorporates revisions contained in allInformation Letters through 07-1. Information Letters may be obtained from theASTM Test Monitoring Center, 6555 Penn Ave., Pittsburgh, PA
13、 15206-4489,Attention: Administrator.3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D021443.4For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual B
14、ook of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.5Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
15、 United States.environment that can produce a deterioration of the materialand its properties. D 58443.1.2 developer, nof an ASTM test method, the assignedASTM group, working under the supervision of its governingsubcommittee and main committee, that formats the testmethod in accordance with the For
16、m and Style for ASTMStandards, and continually refines the test method.3.1.3 developer, nof a test procedure, an individual ororganization that selects the test apparatus and operatingconditions.3.1.4 non-reference oil, nany oil other than a referenceoil; such as a research formulation, commercial o
17、il, or candi-date oil. D 58443.1.5 reference oil, nan oil of known performance char-acteristics, used as a basis for comparison. D 58443.1.5.1 DiscussionReference oils are used to calibratetesting facilities, to compare the performance of other oils, orto evaluate other materials (such as seals) tha
18、t interact withoils.3.1.6 specimen, na piece or portion of a sample used tomake a test.3.1.7 sponsor, nof an ASTM test method, an organizationthat is responsible for ensuring supply of the apparatus used inthe test procedure portion of the test method.3.1.7.1 DiscussionIn some instances, such as a t
19、estmethod for chemical analysis, an ASTM working group can bethe sponsor of a test method. In other instances, a companywith a self-interest may or may not be the developer of the testprocedure used within the test method, but is the sponsor of thetest method.3.1.8 test oil, nany oil subjected to ev
20、aluation in anestablished procedure. D 65574. Summary of Test Method4.1 Four metal specimens 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 copper spe
21、cimen and thestressed oil are examined to detect corrosion and corrosionproducts, respectively.4.2 A reference oil is tested with each group of tests toverify test acceptability.5. Significance and Use5.1 This test method is intended to simulate the corrosionprocess of non-ferrous metals in diesel l
22、ubricants. The corro-sion process under investigation is that believed 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 beari
23、ng failures.36. Apparatus6.1 The main apparatus consists of the following items ofstandard wall borosilicate glassware as shown in Figs. 1-6.6.1.1 Main Sample Tube, Fig. 1.6.1.2 Sample Tube Head, Fig. 2.6.1.3 Air Tube, Fig. 3.6.1.4 Thermocouple Tube, Fig. 4.6.1.5 Condenser, Allihn Type, Fig. 5.6.1.6
24、 Assembled Apparatus, Fig. 6.6.2 Additional glassware items and assembly accessoriesneeded are:6.2.1 Hanger (for metal specimens), of stainless steel, hav-ing the dimensions listed in Fig. 7.FIG. 1 Sample TubeFIG. 2 Sample Tube HeadD65940826.2.2 Adapter, polytetrafluoroethylene for 10/18 joint forse
25、aling of the air tube to the sample tube head.6.3 Other items and equipment are:6.3.1 Heating bath, with constant temperature control within60.5C of test temperature with an immersion depth of 23 to35 cm. Oil baths are recommended. (WarningThere areexposed hot surfaces on apparatus.Avoid skin contac
26、t by use ofprotective equipment.)6.3.2 Ventilation, to adequately remove fumes during heat-ing.6.3.3 Air Supply, use air from a clean, dry source.6.3.3.1 An air drier is required when air needs to beconditioned. The method used is optional provided the aircharacteristics of 6.3.3 are attained. For d
27、rying, 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.6.3.4 Flowmeter, capable of measuring 10 6 1 L/h.FIG. 3 Air TubeFIG. 4 Thermocouple TubeFIG. 5 Condenser, Allihn TypeFIG. 6 As
28、sembled ApparatusD65940836.3.5 Syringe, capable of accurately measuring out 100 mLof liquid.6.3.6 Oven, optional, to dry glassware at elevated tempera-ture.6.3.7 Forceps, stainless steel; or gloves (powder free).6.3.8 Thermocouple, or equivalent. Use sheathed thermo-couple when the thermocouple is i
29、n direct contact with oil.When a thermocouple well is used, use a sheathed or un-sheathed thermocouple in the well to control sample tempera-ture; fill thermocouple well with a heat transfer medium.6.3.9 Sanding Block and Holder, for specimen preparation.7. Reagents and Materials7.1 Purity of Reagen
30、tsUse reagent grade chemicals in alltests. Unless otherwise indicated, it is intended that all reagentsconform to the specifications maintained by the Committee onAnalytical Reagents of the American Chemical Society.67.2 Metal Specimens7,87.2.1 Specimens are 0.081 cm thick by 2.5 cm square,except th
31、at lead specimen that is 0.178 cm thick. One specimenfrom each of the following metal types, each with two drilledholes, is required:7.2.1.1 Copper (R401-A),7.2.1.2 Lead (R401-lead),7.2.1.3 Tin (R401-tin), and7.2.1.4 Phosphor Bronze (R401-PBz).7.3 Abrasive Paper,9240-grit aluminum oxide and 400-grit
32、silicon carbide. Do not use iron-containing abrasives such asnatural emery.7.4 Cotton, 100 %.7.5 Acetone (ACS), sulfur free. (WarningFlammable.Health hazard.)7.6 Glassware Cleaning Solution, NOCHROMIX.8,10(WarningCauses severe burns.)7.7 Heptane.(WarningFlammable. Health hazard.)7.8 Cleaning Solvent
33、Cyclohexane or heptane, industrialgrade. (WarningBoth are flammable and health hazards.)7.9 Reference Oil.28. Preparation of Apparatus8.1 Cleaning:8.1.1 Rinse all items and the air tube adapter with cleaningsolvent to remove residual oil, and air-dry.8.1.2 Wash all glassware items and the air tube a
34、dapter withdetergent. Rinse with tap water, distilled water, and dry.8.1.3 The following more thorough glassware cleaningprocedure can be used, if it is required for a given situation:8.1.3.1 Fill and immerse all glassware items with glasswarecleaning solution (see 7.6) and soak for 3 to 16 h. (Warn
35、ingCorrosive, causes severe burns.)8.1.3.2 Remove glassware from cleaning solution; rinseseveral times with tap water, followed by distilled water, andoven-dry.6Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of re
36、agents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.7Obtain metal specimens from Test Engineering, Inc. (TEI)
37、, 12718 CimarronPath, San Antonio, TX 78249-3423.8The 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 International Headquarters. Your comments willreceive
38、careful consideration at a meeting of the responsible technical committee,which you may attend.9Suitable abrasive paper meeting these specifications is included with the metalspecimens when the specimens are ordered.10Obtain NOCHROMIX from Godax Laboratories, Inc., 720-B Erie Avenue,Takoma Park, MD
39、20912.NOTEAll dimensions in mm.FIG. 7 Specimen HangerD65940848.1.3.3 This more thorough glass cleaning procedure isnecessary in a referee situation, unless an alternative glasswarecleaning solution is available which is satisfactory to all partiesinvolved.8.2 Assembled Apparatus, shown in Fig. 6.8.3
40、 Preparation of Metal Specimens:8.3.1 In all succeeding steps, handle the specimens onlywith stainless steel forceps or powder-free gloves until the finalweighing. If large defects or particles are present on the metalspecimens, remove them first using coarse sandpaper, followedby polishing with the
41、 240 and 400-grit abrasive papers, asdescribed in 8.3.2.8.3.2 Remove any burrs from the drilled holes with a116-in.drill bit. Using a sanding block with a specimen holder, removeall surface blemishes from both sides and all four edges of eachspecimen with 240-grit abrasive paper. Finish polishing wi
42、th400-grit paper wetted by acetone to remove marks fromprevious polishing.8.3.2.1 A good technique is to rub the specimen withlongitudinal strokes in a direction perpendicular to that usedwith 240-grit paper. Use a different sheet of paper for eachmetal type.8.3.2.2 Make sure that the specimen edges
43、 are polished inthe same manner as the surfaces. Carry out this procedureusing normal room lighting and without magnification of thespecimen surface. Do not scribe or otherwise mark the sur-faces.8.3.3 Store the polished metal specimens in acetone.8.3.4 Just prior to a test start, remove each specim
44、en fromthe acetone, and clean all metal dust from the specimen using100 % cotton. Rub with a light-to-medium touch to removeparticles but do not polish the specimen further.8.3.5 Wash specimens in acetone, and allow them to dry ina desiccator.9. Procedure9.1 Add 100 6 1 mL of oil to the sample tube
45、by syringe.9.2 Place the specimen hanger onto the air tube, and hangtest specimens on their respective hooks.9.2.1 Arrange the specimens on the hanger in the sequence:lead, copper, tin, and phosphor bronze.9.3 Insert the air tube with the attached specimens into thesample tube so that the air tube r
46、ests on the bottom of thesample tube.9.4 Place the sample tube head on the sample tube.9.5 Place the assembled sample tube and condenser into thebath so that the sample tube is submerged 23 to 35 cm in thebath with the test oil temperature set at 135 6 0.5C.9.6 Start the flow of the cooling water th
47、rough the con-denser jacket.9.7 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.Use a calibrated flow meter in setting airflow rates.9.8 End of TestAfter 168 h at 135C, shut off the airflowand disassemble.9.8.1 Remove air supply
48、 and disconnect condenser.9.8.2 Remove sample tube from the bath, and allow it tocool to room temperature.10. Test Results10.1 Remove the air tube with the attached specimens fromthe sample tube. Do not touch the specimens with hands.Retain the sample tube and test oil for further examination.10.2 U
49、sing forceps, wash the copper specimen in heptane,and discard the other specimens.10.3 Rate the copper specimen for tarnish according to theStrip Examination, Interpretation, and Report sections of TestMethod D 130.10.4 Immediately after calibration of the ICP-AES instru-ment (as specified in Test Method D 5185), use Test MethodD 5185 to determine the concentration of copper, lead, and tinin both the new and used oil.10.5 CalculationsChange in metal concentration in theused test oil:D C 5 C22 C1(1)where:D C = change in metal concentration before and after
