1、Designation: D1991 05 (Reapproved 2010)Standard Test Method forRubber Chemicals2-Mercaptobenzothiazole (MBT)Assay1This standard is issued under the fixed designation D1991; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year o
2、f 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 a procedure for the assay of2-mercaptobenzothiazole (MBT). It is based on a potentiomet-ric
3、titration of MBT with sodium hydroxide.1.2 The assay is determined as percent by mass.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns, if any, associate
4、d 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.2. Referenced Documents2.1 ASTM Standards:2D4483 Practice for Evaluating Precision for Test MethodStandar
5、ds in the Rubber and Carbon Black ManufacturingIndustries3. Summary of Test Method3.1 A sample of MBT is dissolved in ethanol. The solutionis titrated potentiometrically using a solution of sodium hy-droxide as the titrant.4. Significance and Use4.1 MBT is commonly used as an accelerator for rubber
6、andlatex vulcanization. The purity of MBT may be of importancein predicting performance in rubber compounds and this testmethod is designed to assess the purity of MBT.4.2 This test method may be used as a quality control tooland for research and development work.5. Apparatus5.1 Erlenmeyer Flask, 25
7、0-cm3.5.2 Analytical Balance, having a sensitivity of 60.1 mg.5.3 Potentiograph.5.4 Glass pH Electrode, and reference electrode.5.5 Graduated Cylinder, 200-cm3.6. Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reage
8、nts shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.36.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean distilled water or water ofequal purity.6.3 Aqueous
9、 Sodium Hydroxide Solution (40 g NaOH in1dm3of solution)Standardize by accepted analytical tech-niques to ensure that the maximum error of the normalizationfactor is not more than 0.001.6.4 Ethanol, denatured with toluene (in the ratio of 100volumes ethanol to 1 volume toluene).6.5 Toluene.7. Sampli
10、ng7.1 Sampling shall be at the discretion of the analyst toobtain as representative a sample as possible, of the lot to betested.8. Procedure8.1 Weigh (to nearest 0.001 g) about5gofthespecimen,and transfer into a 250-cm3Erlenmeyer flask. Using a gradu-ated cylinder, add 125 cm3denatured ethanol (6.4
11、). Titrate thesolution potentiometrically, using a glass electrode system,with NaOH (6.3) as the titrant (A) (see Fig. 1).1This test method is under the jurisdiction of ASTM Committee D11 on Rubberand is the direct responsibility of Subcommittee D11.11 on Chemical Analysis.Current edition approved J
12、une 1, 2010. Published December 2010. Originallyapproved in 1991. Last previous edition approved in 2005 as D1991 05. DOI:10.1520/D1991-05R10.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards vol
13、ume information, 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 Annual Standards for Lab
14、oratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.9. Calculation9.1 Fro
15、m the plot of pH versus millilitres of NaOH, asillustrated in Fig. 1, the equivalence point for the potentiomet-ric titration is defined as the point of maximum slope.9.1.1 This point is identified as follows:9.1.1.1 Draw a tangent through the steepest part of thecurve. Determine the two points at w
16、hich the curve departsfrom this tangent line. The midpoint of the line segmentbetween these two points represents the equivalence point.9.2 Calculate the MBT content by the following equation:MBT content, % 5167.2 3 A 3 N 3 100W 3 1000(1)where:A = volume of sodium hydroxide to the equivalencepoint,
17、cm3,167.2 = molecular mass of MBT,W = mass g of specimen, andN = normality of titrant.10. Report10.1 Report the following information:10.1.1 Proper identification of the sample, and10.1.2 Results obtained from two individual determinationsand their average, reported to the nearest 0.1 %.11. Precisio
18、n and Bias11.1 This precision and bias section has been prepared inaccordance with Practice D4483. Refer to this practice forterminology and other statistical calculation details.11.2 The precision results in this precision and bias sectiongive an estimate of the precision of this test method with t
19、hematerials used in the particular interlaboratory programs asdescribed below. The precision parameters should not be usedfor acceptance/rejection testing of any group of materialswithout documentation that they are applicable to those par-ticular materials and the specific testing protocols that in
20、cludethis test method.11.3 A Type 1 (interlaboratory) precision was evaluated in1988. Both repeatability and reproducibility are short term. Aperiod of a few days separates replicate test results.Atest resultis the mean of the assay results.11.4 An MBT sample was analyzed in ten laboratories ontwo d
21、ifferent days.11.5 The results of the precision calculations for repeatabil-ity and reproducibility are shown in Table 1.11.6 RepeatabilityThe repeatability, r, of this test methodhas been established as the value tabulated in Table 1.Twosingle test results, obtained under normal test method proce-d
22、ures, that differ by more than the tabulated r (for any givenlevel) must be considered as derived from different or noniden-tical sample populations.11.7 ReproducibilityThe reproducibility, R, of this testmethod has been established as the value tabulated in Table 1.Two single test results obtained
23、in two different laboratories,under normal test method procedures, that differ by more thanthe tabulated R (for any given level) must be considered tohave come from different or nonidentical sample populations.11.8 Repeatability and reproducibility expressed as a per-centage of the mean level, (r) a
24、nd (R), have equivalentapplication statements as above for r and R. For the (r) and (R)statements, the difference in the two single test results isexpressed as a percentage of the arithmetic mean of the two testresults.11.9 BiasIn test method terminology, bias is the differ-ence between an average t
25、est value and the reference (or true)test property value. Reference values have not been evaluatedfor this test method. Bias therefore cannot be determined.12. Keywords12.1 accelerators; assay; mercaptobenzothiazole (MBT);thiazoleFIG. 1 Potentiometric Titration Using NaOH as the TitrantTABLE 1 MBT A
26、ssayAMaterialAverage%Within Laboratories Between LaboratoriesSr r (r) SR R (R)MBT 97.56 0.286 0.810 0.83 1.675 4.74 4.86ASr = repeatability standard deviation,r = repeatability2.83 3 the square root of the repeatability variance,(r) = repeatability (as percentage of material average),SR = reproducib
27、ility standard deviation,R = reproducibility2.83 3 the square root of the reproducibilityvariance, and(R) = reproducibility (as percentage of material average).D1991 05 (2010)2ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item menti
28、onedin 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 a
29、nd must 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
30、of theresponsible 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 Bo
31、x C700, 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 ASTM website (www.astm.org/COPYRIGHT/).D1991 05 (2010)3
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