1、Designation: D1662 08 (Reapproved 2014)Standard Test Method forActive Sulfur in Cutting Oils1This standard is issued under the fixed designation D1662; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A nu
2、mber in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method covers the determination of activesulfur in cutting oils. This test method applies to sulfur reactivewith copper powder
3、 at a temperature of 150C (302F) incutting fluids containing both natural and added sulfur.NOTE 1It has not been established by ASTM Subcommittee D02.L0as to how the active sulfur content thus determined may relate to fieldperformance of the cutting fluid.1.2 The values stated in SI units are to be
4、regarded as thestandard. The values given in parentheses are for informationonly.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 de
5、termine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D130 Test Method for Corrosiveness to Copper from Petro-leum Products by Copper Strip Test3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 active sulfursulfur in a cutti
6、ng fluid that will reactwith metallic copper at a temperature of 150C (302F) underthe prescribed conditions.4. Summary of Test Method4.1 A portion of the sample is treated with copper powder at150C (302F). The copper powder is filtered from the mixture.Active sulfur is expressed as the difference be
7、tween the sulfurcontents of the sample, as determined before and after treat-ment with copper.5. Significance and Use5.1 This test method measures the quantity of sulfur avail-able to react with metallic surfaces to form solid lubricatingaids at the temperature of the test. Rates of reaction are met
8、altype, temperature, and time dependent.6. Apparatus6.1 Filter Paper, 2.5 m retention size.6.2 Stirrer, constructed of glass in the form of an inverted T.A flat blade, approximate length 25 mm, height 6 mm,thickness 1 mm, shall be attached to a glass rod 6 mm indiameter, in such a way that the blade
9、 is symmetrical with therod and has its flat surface in the vertical plane. Alternatively,a glass-coated magnetic stirring bar 9.5 by 34.9 6 2mm(38 by138 in.) can be used.6.3 Stirring Apparatus, electric motor capable of maintain-ing a speed of 500 6 25 rpm. Alternatively, when using theglass-coated
10、 stirring bar, a combination magnetic stirrer-hotplate is required.6.4 Hot Plate, electric, or other convenient heat sourcecapable of maintaining the sample at a temperature of 150 62C (302 6 5F).6.5 Beaker, 200-mL, tall-form of heat-resistant glass, with apour-out spout.7. Materials7.1 Diluent, sul
11、fur-free white oil, methyl lardate or dialky-lbenzene.7.2 Copper Powder, 99 %, 75 m (200 mesh).8. Procedure8.1 Determine the sulfur concentration of the sample to betested using any accepted method that has precision of60.15 % for sulfur.NOTE 2For best results, dilute the sample with sulfur-free whi
12、te oil,methyl lardate or dialkylbenzene to a sulfur content of 2 to 4 %.8.2 Place 50 6 2 g of sample or sample dilution in a200-mL tall-form beaker, lower the stirrer to within 5 mm of1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants
13、 and is the direct responsibility ofSubcommittee D02.L0.01 on Metal Removal Fluids and Lubricants.Current edition approved Jan. 1, 2014. Published February 2014. Originallyapproved in 1959. Last previous edition approved in 2008 as D166208. DOI:10.1520/D1662-08R14.This test method was prepared under
14、 the joint sponsorship of the AmericanSociety of Lubrication Engineers (ASLE) and accepted by ASLE in January 1969.2For 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 t
15、he standards Document Summary page onthe ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1the bottom of the beaker and add 5 6 0.25 g of copper powderand hea
16、t to 150 6 2C (302 6 5F) while stirring at 500 6 25rpm. If a magnetic stirrer is used, rotate the stirring bar at 5006 25 rpm. When 150 6 2C (302 6 5F) is reached, add anadditional 5 6 0.25 g copper powder. Continue stirring at 1506 2C (302 6 5F) for 30 6 1 min. At the end of this period,stop stirri
17、ng and insert a copper strip prepared in accordancewith Test Method D130 for 10 6 0.25 min. If there is anyevidence of stain on the strip, recommence stirring and add anadditional 5 6 0.25 g of copper powder. Continue stirring themixture at 150 6 2C for 30 6 1 min. Again, insert a copperstrip as pre
18、viously stated for 10 6 0.25 min. Repeat thisprocedure until the copper strip shows no stain, maintaining thetemperature of the mixture at 150 6 2C.8.3 At the end of the heating period, filter the reactionmixture through the filter paper until the filtrate is clear with novisible precipitate.NOTE 3T
19、he filtration apparatus may be placed in an oven maintainedat 100 6 1C (212 6 2F) for more rapid filtration.8.4 Determine the sulfur content of the filtered sample usingthe same method as used in 8.1.9. Calculation9.1 Calculate the active sulfur concentration of the sampleas follows:Active sulfur, w
20、t % 5 A 2 Bwhere:A = weight % sulfur of the untreated sample, andB = weight % sulfur of the treated sample.10. Precision and Bias310.1 The precision of this test method is based on aninterlaboratory study conducted in 20062007. Four fluidsamples having active sulfur levels of 0.9%, 3.6%, 0.3%, and2.
21、1% were run in triplicate by nine laboratories to determinethe intralaboratory and interlaboratory precision of TestMethod D1662.10.1.1 RepeatabilityTwo test results obtained within onelaboratory shall be judged not equivalent if they differ by morethan the “r” value for that material; “r” is the in
22、tervalrepresenting the critical difference between two test results forthe same material, obtained by the same operator using thesame equipment on the same day in the same laboratory.10.1.2 ReproducibilityTwo test results should be judgednot equivalent if they differ by more than the “R” value for t
23、hatmaterial; “R” is the interval representing the difference be-tween two test results for the same material, obtained bydifferent operators using different equipment in different labo-ratories.10.1.3 Any judgment in accordance with the statements in10.1.1 or 10.1.2 would have an approximate 95% pro
24、bability ofbeing correct.10.1.4 Results from the interlaboratory study are summa-rized in Table 1 and Table 2 and are available as a researchreport.10.2 BiasNo accepted reference material suitable for de-termining the bias was analyzed as part of this study, thereforeno statement on bias can be made
25、 at this time.11. Keywords11.1 active sulfur test; cutting oils; metal removal fluids3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1628.TABLE 1 Active Sulfur (%)Average RepeatabilityStandard DeviationReproducibilityStandar
26、d DeviationRepeatabilityLimitReproducibilityLimitMaterials Xbar Sr SR r RA 0.9454 0.0348 0.0706 0.0974 0.1976B 3.3687 0.1022 0.5787 0.2862 1.6205C 0.3902 0.082 0.2969 0.2296 0.8312D 1.9643 0.1551 0.4668 0.4343 1.3070D1662 08 (2014)2SUMMARY OF CHANGESSubcommittee D02.L0 has identified the location of
27、 selected changes to this standard since the last issue(D166207) that may impact the use of this standard. (Approved May 1, 2008.)(1) Added Precision and Bias information and accompanyingresearch report.Subcommittee D02.L0 has identified the location of selected changes to this standard since the la
28、st issue(D166292(2007) that may impact the use of this standard. (Approved Dec. 1, 2007.)(1) Test Method D129 is no longer the required sulfur deter-mination method.Any accepted method in accordance with 8.1may be used.(2) The filter paper and copper powder to be used are moreclosely defined.(3) Not
29、e 2 suggests diluting the sample if total sulfur is high.(4) 8.3 requires that the filterate have no visible precipitate.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expres
30、sly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised,
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32、tend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States.
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34、ured from the ASTM website (www.astm.org/COPYRIGHT/).TABLE 2 Material DescriptionA Fluid 1 1% total, 0.9% active sulfur source A in paraffinic mineral oilB Fluid 2 4% total, 3.6% active sulfur source A in paraffinic mineral oilC Fluid 3 1% total, 0.3% active sulfur source B in paraffinic mineral oilD Fluid 4 4% total, 2.1% active sulfur source A+B in paraffinic mineral oilD1662 08 (2014)3
