ASTM_D_4937_-_96_2012.pdf

Designation:D493796(Reapproved 2012)Standard Test Method forp-Phenylenediamine Antidegradants Purity by GasChromatography1This standard is issued under the fixed designation D4937;the number immediately following the designation indicates the year oforiginal adoption or,in the case of 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 This test method covers the determination of the purityof Class I,II,and III p-phenylenediamine(PPD)antidegradantsas described in Classification D4676 by gas chromatography(GC)detection and area normalization for data reduction.1.2 The values stated in SI units 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 practices and determine the applica-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 ManufacturingIndustriesD4676 Classification for Rubber Compounding MaterialsAntidegradantsE260 Practice for Packed Column Gas Chromatography2.2 ISO Standard:3ISO6472 RubberCompoundingIngredientsAbbreviations3.Terminology3.1 Definitions:3.1.1 area normalization,na method of calculating thepercent composition by measuring the area of each observedpeak and dividing each peak area by the total area.Thisassumes that all peaks are eluted and that each component hasthe same detector response.3.1.2 lot sample,na production sample representative of astandard production unit,normally referred to as the sample.3.1.3 specimen,nthe actual material used in the analysis.It must be representative of the lot sample.3.2 AbbreviationsThe following abbreviations are in ac-cordance with Terminology D3853 and ISO 6472:3.2.1 77PDN,Nbis-(1,4-dimethylpentyl)-p-phenylenedi-amine.3.2.2 DTPDN,N-ditolyl-p-phenylenediamine.3.2.3 IPPDN-isopropyl-N-phenyl-p-phenylenediamine.3.2.4 PPDp-phenylenediamine.3.2.5 6PPDN-(1,3dimethylbutyl)-N-phenyl-p-phenylenediamine.4.Summary of Test Method4.1 The analysis is performed by temperature programmedGC utilizing either a packed column(Procedure A)or acapillary column(Procedure B).Quantification is achieved byarea normalization using a peak integrator or laboratory datasystem.5.Significance and Use5.1 This test method is designed to assess the relative purityof production PPDs.These additives are primarily used asantiozonants for tires and other rubber or polymeric products.5.2 Since the results of this test method are based on areanormalization,it assumes that all components are eluted fromthe column and each component has the same detector re-sponse.Although this is not strictly true,the errors introducedare relatively small and much the same for all samples;thus,they can be ignored since the intent of the test method is toestablish relative purity.5.3 Although trace amounts of“low boilers”are present inproduction samples,they are disguised by the solvent peakwhen using packed columns(Procedure A).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 May 1,2012.Published July 2012.Originally approvedin 1989.Last previous edition approved in 2006 as D4937 96(2006)1.DOI:10.1520/D4937-96R12.2For 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 the standards Document Summary page onthe ASTM website.3Available from the American National Standards Institute,25 W.43rd St.,4thFloor,New York,NY 10036.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.Interferences6.1 Utilizing the chromatographic conditions prescribedthere are no significant co-eluting peaks;however,degradationof column performance could result in interference problems.Thus,when using the packed column it is essential that thetotal system be capable of 5000 theoretical plates before beingused for this analysis.The evaluation of system efficiency isdescribed in 7.4.7.Apparatus7.1 Gas Chromatograph:7.1.1 Procedure A:Packed ColumnAny high-quality tem-perature programmed gas chromatograph equipped with athermal conductivity detector(see Note 1)is sufficient for thisanalysis.Refer to Practice E260 for general gas chromatogra-phy practices.NOTE1Although a thermal conductivity detector is recommended,aflame ionization detector can be used if appropriate adjustment is made forflow rate and specimen size.Since this p