1、Designation: D 665 06Designation: 135/93An American National StandardStandard Test Method forRust-Preventing Characteristics of Inhibited Mineral Oil inthe Presence of Water1This standard is issued under the fixed designation D 665; the number immediately following the designation indicates the year
2、 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 (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Departme
3、nt of Defense.1. Scope1.1 This test method covers the evaluation of the ability ofinhibited mineral oils, particularly steam-turbine oils, to aid inpreventing the rusting of ferrous parts should water becomemixed with the oil. This test method is also used for testingother oils, such as hydraulic oi
4、ls and circulating oils. Provisionis made in the procedure for testing heavier-than-water fluids.NOTE 1For synthetic fluids, such as phosphate ester types, the plasticholder and beaker cover should be made of a chemically resistant material,such as polytetrafluoroethylene (PTFE).1.2 This standard do
5、es 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. For specificwarning statements, se
6、e 6.4-6.6.2. Referenced Documents2.1 ASTM Standards:2A 108 Specification for Steel Bar, Carbon and Alloy, Cold-FinishedA 240/A 240M Specification for Chromium andChromium-Nickel Stainless Steel Plate, Sheet, and Stripfor Pressure Vessels and for General ApplicationsD91 Test Method for Precipitation
7、Number of LubricatingOilsD 1193 Specification for Reagent WaterD 2422 Classification of Industrial Fluid Lubricants byViscosity SystemD 3603 Test Method for Rust-Preventing Characteristics ofSteam Turbine Oil in the Presence of Water (HorizontalDisk Method)D 4057 Practice for Manual Sampling of Petr
8、oleum andPetroleum ProductsE1 Specification for ASTM Liquid-in-Glass Thermometers2.2 Other Documents:Motor Fuels, Section I, Annex A2, Table 32, ReferenceMaterials and Blending Accessories3Specifications-IP Standard Thermometers, Vol 2, AppendixA4Specifications for IP Standard Reference Liquids, App
9、endixB4SAE Standard J405 Chemical Composition of SAEWrought Stainless Steels5BS 871 Specification for abrasive papers and cloths4BS 970 Part 1: Carbon and Carbon Manganese SteelsIncluding Free Cutting Steels43. Summary of Test Method3.1 A mixture of 300 mL of the oil under test is stirred with30 mL
10、of distilled water or synthetic sea water, as required, ata temperature of 60 6 1C (140 6 2F) with a cylindrical steeltest rod completely immersed therein. It is recommended to runthe test for 4 h; however, the test period may, at the discretionof the contracting parties, be for a shorter or longer
11、period. Thetest rod is observed for signs of rusting and, if desired, degreeof rusting.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.C0 on Turbine Oils.Current edition approved May 1, 2006. Pu
12、blished May 2006. Originallyapproved in 1942. Last previous edition approved in 2003 as D 66503.In the IP, this test method is under the jurisdiction of the StandardizationCommittee. This test method was adopted as a joint ASTMIP standard in 1964.2For referenced ASTM standards, visit the ASTM websit
13、e, 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 website.3See 1996 Annual Book of ASTM Standards, Vol 05.04.4Annual Book of IP Standard Methods for Analysis and Testing of
14、 Petroleum andRelated Products, Vol 2. Available from Energy Institute, 61 New Cavendish St.,London, WIG 7AR, U.K.51995 SAE Handbook, Vol 1. Available from Society of Automotive Engineers(SAE), 400 Commonwealth Dr., Warrendale, PA 15096-0001.1Copyright ASTM International, 100 Barr Harbor Drive, PO B
15、ox C700, West Conshohocken, PA 19428-2959, United States.NOTE 2Until 1999 it was customary to run the test for 24 h. A roundrobin with comparisons of different test times showed that no statisticallysignificant differences in rating were found for any sample, between the 4and 24 h results.64. Signif
16、icance and Use4.1 In many instances, such as in the gears of a steamturbine, water can become mixed with the lubricant, andrusting of ferrous parts can occur. This test indicates how wellinhibited mineral oils aid in preventing this type of rusting.This test method is also used for testing hydraulic
17、 andcirculating oils, including heavier-than-water fluids. It is usedfor specification of new oils and monitoring of in-service oils.NOTE 3This test method was used as a basis for Test Method D 3603.Test Method D 3603 is used to test the oil on separate horizontal andvertical test rod surfaces, and
18、can provide a more discriminating evalua-tion.5. Apparatus5.1 Oil BathA thermostatically controlled liquid bathcapable of maintaining the test sample at a temperature of 606 1C (140 6 2F) (see Note 4). An oil having a viscosity ofapproximately ISO VG 32 (see Classification D 2422)issuitable for the
19、bath. The bath shall have a cover with holes toaccommodate the test beakers.NOTE 4ASTM Thermometer 9C (9F), as prescribed in SpecificationE1, or IP Thermometer 21C in accordance with IP Standard Thermom-eters, Volume 2, Appendix A, is suitable to indicate the temperature.Alternatively, calibrated th
20、ermocouples may be used.5.2 BeakerA 400-mL, Berzelius-type, tall-form heat-resistant glass beaker without pourout, as shown in Fig. 1,approximately 127 mm (5 in.) in height measured from theinside bottom center and approximately 70 mm (234 in.) ininside diameter measured at the middle.5.3 Beaker Cov
21、erA flat beaker cover of glass or poly(methyl methacrylate) (PMMA) (Note 5), kept in position bysuitable means such as a rim or groove. Two holes shall beprovided on any diameter of the cover; one for a stirrer 12 mm(1532 in.) in diameter with its center 6.4 mm (14 in.) from the6Supporting data (res
22、ults of the cooperative test program with modified testduration) have been filed at ASTM International Headquarters and may be obtainedby requesting Research Report RR: D02-1474.NOTEAll units are in millimetres, unless otherwise specified.FIG. 1 Rusting Test ApparatusD665062center of the cover; and
23、the other, on the opposite side of thecenter of the cover, for the test rod assembly (see Section 8), 18mm (4564 in.) in diameter with its center 16 mm (58 in.) fromthe center of the cover. In addition, a third hole 12 mm (1532in.) in diameter shall be provided for a temperature measuringdevice, wit
24、h its center 22.5 mm (78 in.) from the center of thecover and on a diameter of the cover at right angles to thediameter through the other two holes.NOTE 5An inverted petri dish makes a suitable cover, as the sides ofthe dish aid in keeping it in position. Fig. 2 shows a PMMA resin coverfor the beake
25、r which has been found to be suitable. An optional feature isshown, consisting of a slot, 1.6 by 27 mm (116 by 1116 in.), which iscentered on a diameter of the stirrer hole at right angles to the coverdiameter through the test rod hole and stirrer hole. This feature allowswithdrawal of the stirrer w
26、hile the beaker cover is in place. When the testmethod test is used for other fluids such as synthetics, the beaker covershould be made from chemically resistant material such as polymonochlo-rotrifluoroethylene (PCTFE).5.4 The plastic holder shall be made of PMMA resin inaccordance with the dimensi
27、ons shown in Fig. 3 (two types ofholders are illustrated). When testing synthetic fluids, theplastic holder should be made from chemically resistantmaterial such as polytetrafluoroethylene (PTFE).5.5 StirrerA stirrer constructed entirely from stainlesssteel (Note 6 and Note 7) in the form of an inve
28、rted T. A flatblade 25 by 6 by 0.6 mm (1 by 0.24 by 0.024 in.) shall beattached to a 6-mm (0.24-in.) rod in such a way that the bladeis symmetrical with the rod and has its flat surface in thevertical plane.NOTE 6A suitable material is an 18 % chromium, 8 % nickel alloysteel conforming to Type 304,
29、of Specification A 240/A 240M,orSAENo. 30304 (see SAE J405), or BS 970: Part 1: 1983: 302S31.NOTE 7If stainless steel is not obtainable, stirrers made of heat-resistant glass and having approximately the same dimensions as thestainless steel stirrers specified can be used.5.6 Stirring ApparatusAny c
30、onvenient form of stirringapparatus capable of maintaining a speed of 1000 6 50 rpm.5.7 Grinding and Polishing EquipmentA CAMI 150-grit(99-m) and a CAMI 240-grit (53.5-m) in accordance withBS 871 or its equivalent, metalworking aluminum oxide abra-sive cloth coat on a jeans backing (the correspondin
31、g Europeangrades (FEPA) are P150J and P280J, respectively), a suitablechuck (see Fig. 4) for holding the test rod, and a means ofrotating the test rod at a speed of 1700 to 1800 rpm.NOTE 8CAMI (CoatedAbrasives Manufacturers Institute) is a UnitedStates organization and FEPA (Federation of European P
32、roducers ofAbrasives) is a European organization.5.8 Oven, capable of maintaining a temperature of 65C(150F).NOTEAll units are in millimetres, unless otherwise specified.FIG. 2 Beaker CoverD665063NOTEAll units are in millimetres, unless otherwise specified.FIG. 3 Test Rod and HoldersNOTEAll units ar
33、e in millimetres, unless otherwise specified.FIG. 4 Chuck for Polishing Test RodsD6650646. Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnaly
34、tical Reagents of the American Chemical Society wheresuch specifications are available.7Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.6.2 Purity of WaterUnless otherwise in
35、dicated, referencesto water shall be understood to mean reagent water as definedby Type II of Specification D 1193.6.3 The synthetic sea water shall have the following com-position:Salt g/LNaCl 24.54MgCl26H2O 11.10Na2SO44.09CaCl21.16KCl 0.69NaHCO30.20KBr 0.10H3BO30.03SrCl26H2O 0.04NaF 0.0036.3.1 The
36、 solution can be conveniently prepared as follows.This procedure avoids any precipitation in concentrated solu-tions with subsequent uncertainty of complete resolution.Using certified pure (cp) chemicals and distilled water, preparethe following stock solutions:Stock Solution No. 1:MgCl26H2O 3885 gC
37、aCl2(anhydrous) 406 gSrCl26H2O14Dissolve and dilute to 7 LStock Solution No. 2:KCl 483 gNaHCO3140 gKBr 70 gH3BO321 gNaF 2.1 gDissolve and dilute to 7 L6.3.2 To prepare the synthetic sea water, dissolve 245.4 g ofNaCl and 40.94 g of Na2SO4in a few litres of distilled water,add 200 mL of Stock Solutio
38、n No. 1 and 100 mL of StockSolution No. 2 and dilute to 10 L. Stir the 10-L batch and add0.1 N Na2CO3solution until the pH is between 7.8 and 8.2.One or two millilitres of the carbonate solution will berequired.6.4 Precipitation Naphtha, as specified in Test MethodD91.(WarningFlammable. Health hazar
39、d.)6.5 Isooctane, as specified in Motor Fuels, Section I, AnnexA2, Table 32, Reference Materials and Blending Accessories.(WarningFlammable. Health hazard.)6.6 IP 60/80 Petroleum Spirit, as specified by IP StandardReference Liquids, Appendix B. (WarningFlammable.Health hazard.)6.7 Steel Test Rod, as
40、 specified in Section 8.7. Sampling7.1 Sample for this test can come from tanks, drums, smallcontainers, or even operating equipment, and they should betruly representative of the entire quantity. Therefore, use theapplicable apparatus and techniques described in PracticeD 4057, or other comparable
41、standard practice.8. Test Rod and Its Preparation8.1 For each test oil, prepare two steel test rods. These mayeither be new or from a previous test (see Note 9) and shall beprepared in accordance with 8.2 and 8.3.8.2 The test rod assembly shall consist of a round steel testrod fitted to a plastic ho
42、lder. The round steel test rod, whennew, shall be 12.7 mm (0.5 in.) in diameter and approximately68 mm (21116 in.) in length exclusive of the threaded portionwhich screws into the plastic holder and shall be tapered at oneend as shown in Fig. 3. It shall be made of steel conforming toGrade 10180 of
43、Specification A 108 or to BS 970 Part I:1983-070M20. If these steels are not available, other equiva-lent steels may be used, provided they are found to besatisfactory by comparative test using this Test MethodD 665 IP 135.NOTE 9When making a check test, the steel test rod that showed rustshould not
44、 be reused. Test rods that repeatedly show rust in tests of variousoils can be imperfect. Such test rods should be used with oils known topass the test. If rusting occurs in repeat tests, these test rods should bediscarded.8.3 Preliminary GrindingIf the test rod has been usedpreviously and is free o
45、f rust or other irregularities, thepreliminary grinding may be omitted, and it may be subjectedonly to final polishing as prescribed in 8.4. If the test rod is newor if any part of its surface shows rust or other irregularities,clean it with ASTM precipitation naphtha or isooctane or IP60/80 petrole
46、um spirit and grind with medium 150-grit alumi-num oxide cloth to remove all irregularities, pits, and scratches,as determined by visual inspection (Note 10). Perform thegrindings by mounting the test rod in the chuck of the grindingand polishing apparatus, and turning it at a speed of 1700 to1800 r
47、pm while applying the 150-grit aluminum oxide cloth.Old 150-grit aluminum oxide cloth may be used to remove rustor major irregularities, but complete the grinding with newcloth. Proceed at once with the final polishing with 240-gritaluminum oxide cloth, or remove the test rod from the chuckand store
48、 in isooctane until needed. Discard reused test rodswhen the diameter is reduced to 9.5 mm (0.375 in.).NOTE 10Do not touch the test rods with the hands at any stage aftercleaning with naphtha or isooctane or the petroleum spirit (which precedeseither preliminary grinding or final polishing) until th
49、e test is completed.Forceps or a clean, lintless cloth may be used.8.4 Final Polishing:8.4.1 Just before the test is to be made, subject the test rodto final polishing with 240-grit aluminum oxide cloth. If thepreliminary grinding has just been completed, stop the motor7Reagent Chemicals, American 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., a
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