ASTM_D_5666_-_95_2014.pdf

Designation:D566695(Reapproved 2014)Standard Test Method forRubber Chemical AntidegradantsPurity of p-Phenylenediamine(PPD)Antidegradants by HighPerformance Liquid Chromatography1This standard is issued under the fixed designation D5666;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 purity of Type I,II,and IIIp-phenylenediamine(PPD)antidegradants as described inClassification D4676 by high performance liquid chromatog-raphy(HPLC)using ultraviolet detection and external standardcalculations.1.2 Expertise in HPLC is necessary to the successful appli-cation of this test method.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,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 MaterialsAntidegradants2.2 ISO Standards:3ISO 5725 Precision of Test MethodsISO 6472 RubberCompoundingIngredientsAbbreviations3.Terminology3.1 Definitions:3.1.1 external standard calculationa 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 astandard production unit,normally referred to as the sample.3.1.3 specimenthe actual material used in the analysis,also known as the test portion.It must be representative of thelot sample.3.2 Abbreviations:3.2.1 The following abbreviations are in accordance withTerminology D3853 and ISO 6472:3.2.2 77PDN,N bis-(1,4-dimethylpentyl)-p-phenylene-diamine.3.2.3 DTPDN,N-ditolyl-p-phenylenediamine.3.2.4 IPPDN-isopropyl-N-phenyl-p-phenylenediamine.3.2.5 PPDp-phenylenediamine.3.2.6 6PPDN-(1,3 dimethylbutyl)-N-phenyl-p-phenyl-enediamine.4.Summary of Test Method4.1 A specimen is dissolved in acetonitrile and a fixed loopvolume is analyzed by isocratic HPLC using a thermostatedC18 reversed phase column and an ultraviolet(UV)detector.Peak areas are determined using a chromatographic integratoror laboratory data system with the amount of analyte beingdetermined by external calibration.5.Significance and Use5.1 This test method is designed to determine the purity ofp-phenylenediamine antidegradants.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 Aug.1,2014.Published November 2014.Originallyapproved in 1995.Last previous edition approved in 2009 as D5666 95(2009).DOI:10.1520/D5666-95R14.2For 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 American National Standards Institute(ANSI),25 W.43rd St.,4th Floor,New York,NY 10036.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.2 Since the results of this test method are based on anintegrated peak area as determined by HPLC,it is assumed thatall analytes of interest are resolved 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 Precision 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,7.1.4 A fixed injector made of either a 20 mm3(L)rheodyne loop or an automatic sampler.7.2 HPLC Columns,consisting of:7.2.1 A precolumn packed with C18 grafted silica withparticle size of 35 to 40 m(100 to 150 mm),and7.2.2 A column of 10-to 15-cm length packed with C18grafted silica with particle size of 3 to 5 m.7.3 Integrator/Data System,capable of determining abso-lute amounts of analyte of interest by means of integration ofdetector output versus time.7.4 Analytical Balance,capable of measuring within 60.01mg.7.5 Shaking Machine,or ultrasonic tank.7.6 Volu