1、Designation:D529795(Reapproved 2014)Standard Test Methods forRubber Chemical AcceleratorPurity by High PerformanceLiquid Chromatography1This standard is issued under the fixed designation D5297;the number immediately following the designation indicates the year oforiginal adoption or,in the case of
2、revision,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 These test methods cover the determination of the purityof present commercially available rubber chemi
3、cal acceleratorsin the range from 80 to 100%by high performance liquidchromatography(HPLC)using ultraviolet detection and exter-nal standard calculations.1.2 Expertise in HPLC is necessary to the successful appli-cation of these test methods.1.3 The values stated in SI units are to be regarded assta
4、ndard.No other units of measurement are included in thisstandard.1.4 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
5、-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2D3853 Terminology Relating to Rubber and RubberLaticesAbbreviations for Chemicals Used in Com-poundingD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black Manufacturing
6、IndustriesD4571 Test Methods for Rubber Compounding MaterialsDetermination of Volatile MaterialD4936 Test Method for Mercaptobenzothiazole SulfenamideAssay by Reduction/Titration2.2 ISO Standard:3ISO6472 RubberCompoundingIngredientsAbbreviations3.Terminology3.1 Definitions:3.1.1 external standard ca
7、lculationa method of calculat-ing the percent composition by measuring the area of theanalyte peak,multiplying by a response factor,and dividing bythe sample concentration.All components are assumed to beresolved from the component of interest.3.1.2 lot samplea production sample representative of as
8、tandard production unit,normally referred to as the sample.3.1.3 specimenalso known as the test portion,it is theactual material used in the analysis.It must be representative ofthe lot sample.3.2 Abbreviations:3.2.1 The following abbreviations are in accordance withTerminology D3853 and ISO 6472:3.
9、2.2 MBTSBenzothiazyl disulfide.3.2.3 MBS2-(morpholinothio)benzothiazole.3.2.4 CBSN-cyclohexyl-2-benzothiazolesulfenamide.3.2.5 TBBSN-t-butyl-2-benzothiazolesulfenamide.3.2.6 DIBSN,N-diisopropyl-2-benzothiazolesulfena-mide.3.2.7 DCBSN,N-dicyclohexyl-2-benzothiazolesulfe-namide.3.2.8 DPGdiphenylguanid
10、ine.3.2.9 DOTGdi-o-tolylguanidine.4.Summary of Test Methods4.1 Aspecimen is dissolved in the appropriate solvent and afixed loop volume is analyzed by isocratic HPLC using athermostated C18 reversed phase column for materials 3.2.2 1These test methods are under the jurisdiction of ASTM Committee D11
11、 onRubber and are the direct responsibility of Subcommittee D11.11 on ChemicalAnalysis.Current edition approved Aug.1,2014.Published November 2014.Originallyapproved in 1992.Last previous edition approved in 2009 as D5297 95(2009).DOI:10.1520/D5297-95R14.2For referenced ASTM standards,visit the ASTM
12、 website,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.3Available from American National Standards Institute(ANSI),25 W.43rd St.,4th Floor,New York,NY 10036.Copyright
13、 ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 3.2.7 and a silica normal phase column for materials 3.2.8 and3.2.9,and an ultraviolet(UV)detector.Peak areas are deter-mined using a chromatographic integrator or laboratory datasystem with the amou
14、nt of analyte being determined byexternal calibration.5.Significance and Use5.1 These test methods are designed to determine the purityof rubber chemical accelerators.5.2 Since the results of these test methods are based on anintegrated peak area,it is assumed that all analytes of interestare resolv
15、ed from interfering peaks.6.Interferences6.1 Components co-eluting with the analyte of interest willcause erroneous results;thus it is required that the system becapable of providing a minimum of 10 000 theoretical plates.7.Apparatus7.1 Liquid Chromatograph,consisting of the following:7.1.1 Precisio
16、n chromatographic pump,7.1.2 Variable wavelength UV detector,7.1.3 A method for thermostating the column at 35 6 1C,for example,a column oven or water jacket,and7.1.4 A fixed loop injector with a nominal volume of 10mm3(L)or less.7.2 HPLC Column:7.2.1 A C18(ODS)reversed phase column packed withspherical,totally porous monomolecular 5-m particles ca-pable of providing 40 000 theoretical plates per metre.(Aminimum of 10 000 plates is required for this analysis.)Thiscolumn should be reserved for th
