ASTM D5051-06(2017) Standard Test Method for Rubber Compounding Materials—Benzothiazyl Disulfide (MBTS)—Assay.pdf

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1、Designation: D5051 06 (Reapproved 2017)Standard Test Method forRubber Compounding MaterialsBenzothiazyl Disulfide(MBTS)Assay1This standard is issued under the fixed designation D5051; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision,

2、 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.1. Scope1.1 This test method covers the determination of assay ofbenzothiazyl disulfide (MBTS). It is based on a titr

3、ation of freeiodine liberated upon reduction of MBTS, with potassiumiodide (KI) in acid medium.1.2 The assay is determined as mass percent.1.3 Free 2-mercaptobenzothiazole (MBT) content is notdetermined.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement ar

4、e included in thisstandard.1.5 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 p

5、rior to use.1.6 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization Technica

6、lBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustries3. Summary of Test Method3.1 In an acid medium, MBTS is reduced wi

7、th KI to MBTand free iodine. The free iodine is titrated with standard sodiumthiosulfate solution.3.2 MBTS is sparingly soluble in any organic solvent; whileMBT, formed during the reaction of MBTS with KI is verysoluble. Therefore after reagents are added as indicated in theprocedure, continue to st

8、ir till all MBTS has reacted.4. Significance and Use4.1 The test method is designed to assess the purity ofMBTS, which is used for rubber and latex vulcanizationacceleration. The amount of MBTS is of importance inpredicting performance in rubber compounds and for rawmaterial purchase and control.4.2

9、 This test method may be used as a quality control tooland for research and development work.5. Interferences5.1 KI-reducible contaminants interfere with the results.6. Apparatus6.1 Erlenmeyer Flask, 300 cm3.6.2 Graduated Cylinder, 5cm3.6.3 Magnetic Stirrer, with hot plate.6.4 Buret, 50-cm3capacity.

10、6.5 Analytical Balance, having a sensitivity of 60.1 mg.7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the Am

11、erican Chemical Society,where such specifications are available.3Other grades may be1This test method is under the jurisdiction of ASTM Committee D11 on Rubberand Rubber-like Materials and is the direct responsibility of Subcommittee D11.11on Chemical Analysis.Current edition approved May 1, 2017. P

12、ublished June 2017. Originallyapproved in 1990. Last previous edition approved in 2012 as D5051 06 (2012).DOI: 10.1520/D5051-06R17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume informa

13、tion, refer to the standards Document Summary page onthe ASTM website.3Reagent 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 LaboratoryChem

14、icals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was d

15、eveloped in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1used, provided

16、it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.7.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Types I, II, or III of Specification D1

17、193.7.3 Acetic Acid, 100 %, analytical reagent.7.4 Isopropanol, analytical reagent.7.5 Toluene, analytical reagent.7.6 Potassium Iodide (KI), analytical reagent.7.7 Sodium Thiosulfate (Na2S2O3) (0.1 N ).7.8 Starch Indicator SolutionSlurry2gofsoluble starchwith 10 cm3of water and dilute with 90 cm3of

18、 boiling water.7.9 Hydrochloric Acid (HCl) (2 N).7.10 Solvent: Mix 5 volumes isopropanol with 3 volumestoluene.8. Sampling8.1 Depending upon the purposes of the testing, samplingshall be at the discretion of the analyst to obtain as represen-tative a sample as possible of the lot to be tested.9. Pro

19、cedure9.1 Accurately weigh about 0.5 g of the test specimen to thenearest 0.1 mg and carefully transfer it to a 300-cm3Erlen-meyer flask.9.2 Add 50 cm3of solvent to the specimen, which may notdissolve completely.9.3 With stirring, add the reagents in the following se-quence: 50 cm3of distilled water

20、, about6gofKI,25cm3of2 N HCl, and 25 cm3of acetic acid (see 3.2). Sample will nowbe dissolved.9.4 Immediately titrate (see Note 1) the liberated iodinewith 0.1 N Na2S2O3solution. Toward the end of the titration,add5cm3of starch indicator solution. The end point proceedsfrom blue-violet to yellow to

21、colorless (milky).NOTE 1The final titration must be carried out as soon as acetic acid isadded. If allowed to stand, a reduction of free iodine will occur, giving alower MBTS assay.9.5 Obtain a blank titration by proceeding from 9.2 to 9.4.10. Calculation10.1 Calculate the percent MBTS as follows:Pe

22、rcent MBTS 5A 2 B! 3 N 30.33248!2 W3100 (1)where:A = volume of Na2S2O3(see 7.7) required for titra-tion of the sample, cm3,B = volume of Na2S2O3required for titration of theblank, cm3,N = normality of the Na2S2O3solution,W = mass of the test specimen in g, and0.33248 = millimole mass of MBTS.11. Rep

23、ort11.1 Report the following information:11.1.1 Proper identification of the sample and11.1.2 Results obtained from two individual determinationsand their average, reported to the nearest 0.1 %.12. Precision and Bias412.1 This precision and bias section has been prepared inaccordance with Practice D

24、4483. Please refer to this practicefor terminology and other statistical calculation details.12.2 The precision results in this precision and bias sectiongiven an estimate of the precision of this test method with thematerials (rubbers, etc.) used in the particular interlaboratoryprogram as describe

25、d below. The precision parameters shouldnot be used for acceptance or rejection testing or any group ofmaterials without documentation that the parameters are appli-cable to the particular group of materials and the specifictesting protocols of the test method.12.3 A Type 1 interlaboratory test prog

26、ram (ITP) wasconducted in 1997 on a sample of IRM-MBTS. Six laborato-ries participated in the ITP conducting duplicate tests on eachof 2 successive test days. A test result for the assay is the valueobtained from one analysis operation. The database generatedby this ITP was divided into two parts; P

27、art 1 used the first ofthe duplicates on each day and Part 2 used the second of theduplicates. A complete statistical analysis according to D4483was conducted for each part. The analysis results of each partwhere then combined (averaged) for the final values as given inthis section. Thus the precisi

28、on results pertain to between daysingle determinations for the assay values for MBTS.12.4 The D4483 analysis revealed that one of the laborato-ries had excessive within-laboratory variation (high k-value)and the results from this laboratory were deleted. The precisionis therefore based on a five lab

29、oratory ITP.12.5 RepeatabilityThe repeatability r, of this test methodhas been established as the value tabulated in Table 1.Twosingle test results, obtained under normal test methodprocedures, that differ by more than this tabulated r (for anygiven level) must be considered as derived from differen

30、t ornon-identical sample populations.4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D11-1083.TABLE 1 Precision for MBTS AssayAMean Within-LaboratoryBBetween LaboratoryMaterial Value (a) Sr r (r) SR R (R)IRM-MBTS 96.79 0.134 0.3

31、80 0.39 0.397 1.12 1.16APrecision results for 5 laboratories, mean value in percent assay for MBTS.BSr = repeatability standard deviationr = repeatability, in measurement units(r) = repeatability (relative) in percentSR = reproducibility standard deviationR = reproducibility, in measurement units(R)

32、 = reproducibility (relative) in percentD5051 06 (2017)212.6 ReproducibilityThe reproducibility R, of this testmethod has been established as the value tabulated in Table 1.Two single test results obtained in two different laboratories,under normal test method procedures, that differ by more thanthe

33、 tabulated R must be considered to have come from differentor non-identical sample populations.12.7 BiasIn test method terminology, bias is the differencebetween an average test value and the reference (or true) testproperty value. Reference values do not exist for this testmethod since the value (o

34、f the test property) is exclusivelydefined by the test method. Bias cannot therefore be deter-mined.13. Keywords13.1 mercaptobenzothiazole; mercaptobenzothiazole disul-fideASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned

35、in this standard. Users of this standard are expressly 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 m

36、ust be reviewed every five years andif not revised, either reapproved or withdrawn. Your 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 t

37、heresponsible technical committee, which you may attend. 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 C7

38、00, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple 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). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 06 (2017)3