1、Designation: D 1662 08An American National StandardStandard Test Method forActive Sulfur in Cutting Oils1This standard is issued under the fixed designation D 1662; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last r
2、evision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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
3、 copper powder 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 un
4、its are to be 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 pr
5、actices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 130 Test Method for Corrosiveness to Copper fromPetroleum Products by Copper Strip Test3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 active sulfursulf
6、ur in a cutting 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
7、difference between 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 rea
8、ction are metaltype, 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 t
9、hat the blade 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 th
10、eglass-coated 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
11、 Diluent, sulfur-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 su
12、lfur-free white 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 ofthe bottom of the beaker and add 5 6 0.25 g of copper powderand heat to 150 6 2C (302 6 5F) while stirr
13、ing 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,1This test method is under the jurisdiction of
14、ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.L0.01 on Metal Removal Fluids and Lubricants.Current edition approved May 1, 2008. Published May 2008. Originallyapproved in 1959. Last previous edition approved in 2007 as D 166207.This test m
15、ethod was prepared under 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
16、 information, refer to the standards Document Summary page onthe ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.stop stirring and insert a copper strip p
17、repared in accordancewith Test Method D 130 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 previously stated for 10 6 0.25
18、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 3The filtration apparatus may b
19、e 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, wt % 5 A 2 Bwhere:A = weight %
20、 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%, and2.1% were run in triplicate by
21、nine laboratories to determinethe intralaboratory and interlaboratory precision of TestMethod D 1662.10.1.1 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 intervalrepresenting the criti
22、cal 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 thatmaterial; “R” is the inte
23、rval 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% probability ofbeing correct.10.
24、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 fordetermining the bias was analyzed as part of this study,therefore no statement on bias can be made at this time.11. Keywords11.1
25、 active sulfur test; cutting oils; metal removal fluids3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D021628.TABLE 1 Active Sulfur (%)Average RepeatabilityStandard DeviationReproducibilityStandard DeviationRepeatabilityLimitR
26、eproducibilityLimitMaterials 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 1.3070D1662082SUMMARY OF CHANGESSubcommittee D02.L0 has identified the location of selected changes to this standard sin
27、ce the last issue(D 166207) 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 last issue(D 166292(2007) that may impa
28、ct the use of this standard. (Approved Dec. 1, 2007.)(1) Test Method D 129 is no longer the required sulfurdetermination method. Any accepted method in accordancewith 8.1 may be used.(2) The filter paper and copper powder to be used are moreclosely defined.(3) Note 2 suggests diluting the sample if
29、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 expressly advised that determination of th
30、e 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, either reapproved or withdrawn. You
31、r comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments
32、 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. Individual reprints (single or mult
33、iple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).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 oilD1662083
