ASTM_E_1090_-_08.pdf

Designation:E109008Standard Test Method forDicumyl Peroxide and Dicumyl Peroxide DecompositionProducts in Resins1This standard is issued under the fixed designation E1090;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.Scope*1.1 This test method covers and is applicable to the deter-mination of dicumyl peroxide2and the decomposition productsdimethylbenzyl alcohol and acetophenone in cured and un-cured polyethylene(PE)and ethylene vinyl acetate(EVA)resins.These uncured polymers normally contain from 1 to 2%dicumyl peroxide,whereas the residual peroxide level in thecured polymers is usually less than 0.1%.1.2 The values stated in SI units are to be regarded asstandard.The values given in parentheses are for informationonly.1.3 Review the current Material Safety Data Sheets(MSDS)for detailed information concerning toxicity,first aidprocedures,and safety precautions.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.Specific hazards aregiven in Section 7.2.Referenced Documents2.1 ASTM Standards:3D1193 Specification for Reagent WaterE180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals(Withdrawn 2009)4E300 Practice for Sampling Industrial ChemicalsE682 Practice for Liquid Chromatography Terms and Rela-tionshipsE685 Practice for Testing Fixed-Wavelength PhotometricDetectors Used in Liquid ChromatographyE755 Test Method for Dicumyl Peroxide,Assay(LiquidChromatography)3.Summary of Test Method3.1 Dicumyl peroxide and dimethylbenzyl alcohol are ex-tracted from a cryogenically ground sample with methylenechloride.The extract is concentrated,redissolved in methanol,and analyzed by high performance liquid chromatography(HPLC).Acetophenone is extracted from a separate samplewith methanol and analyzed directly by HPLC.The analysesare performed on a reversed phase octadecylsilane(ODS)column using acetonitrile/water as the mobile phase and anultraviolet detector at 254 nm.The concentration of eachcomponent is determined by the internal standard technique,using peak height ratios of the sample and standard chromato-grams.4.Significance and Use4.1 Knowledge of the peroxide content of uncured PE andEVA samples is required to regulate the degree of crosslinkingin the cured product.As end use applications of the curedproduct can be affected by residual amounts of the peroxide orits decomposition productsdimethylbenzyl alcohol andacetophenoneknowledge of these levels is also important.This test method provides a procedure for determining theconcentration of these compounds.A method for the HPLCassay of dicumyl peroxide is described in Test Method E755.5.Apparatus5.1 Liquid Chromatograph,equipped with a 254-nm UVdetector,injection valve,and an isocratic-solvent deliverysystem capable of operating to a gage pressure of 3000 psi.Thedetector should be equipped with an attenuator switch tochange the sensitivity range as required.(See Practices E682and E685.)5.2 Recorder,0 to 1 mv range,1 s or less full-scaledeflection,with a chart speed of 0.1 in./min or other convenient1This test method is under the jurisdiction of ASTM Committee E15 onIndustrial and Specialty Chemicals and is the direct responsibility of SubcommitteeE15.01 on General Standards.Current edition approved April 1,2008.Published May 2008.Originallyapproved in 1986.Last previous edition approved in 2002 as E1090 96(2002).DOI:10.1520/E1090-08.2Dicumyl peroxide;peroxide,bis(1-methyl-1-phenylethyl)C18H22O2;CASRegistry No.80-43-3.3For 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.4The last approved version of this historical standard is referenced onwww.astm.org.*A Summary of Changes section appears at the end of this standardCopyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 speed that will produce a satisfactory chromatogram.As analternative,an electronic data system can be used.5.3 Chromatographic Column,reversed phase C-18,from250 to 300-mm by 3.9-mm inside diameter,containing octa-decylsilane chemically bonded to microparticulate silica.5NOTE1Commercial HPLC columns may vary in physicaldimensions,degree of substrate loading,and size and type of supportmaterial.For these reasons,some modification in the operating parametersmay be required to achieve optimum separation.5.4 Guard Column,reversed phas