ASTM_D_4275_-_09.pdf

Designation:D427509Standard Test Method forDetermination of Butylated Hydroxy Toluene(BHT)inPolymers of Ethylene and EthyleneVinyl Acetate(EVA)Copolymers By Gas Chromatography1This standard is issued under the fixed designation D4275;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 describes a procedure for the determi-nation of butylated hydroxy toluene(BHT)(2,6-di-t-butyl-4-methyl-hydroxybenzene)in polymers of ethylene andethylene-vinyl acetate(EVA)copolymers by solvent extractionfollowed by gas chromatographic analysis.Detection of thecompound is achieved by flame ionization,and quantitativeanalysis is obtained by use of internal or external standards,asdescribed in Practices E260,E355,and E594.1.2The 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.Specific precau-tionary statements are given in Section 9.NOTE1There is no known ISO equivalent for this test method.2.Referenced Documents2.1 ASTM Standards:2D4968 Guide for Annual Review of Test Methods andSpecifications for PlasticsD7210 Practice for Extraction of Additives in PolyolefinPlasticsE260 Practice for Packed Column Gas ChromatographyE355 Practice for Gas Chromatography Terms and Relation-shipsE594 Practice for Testing Flame Ionization Detectors Usedin Gas or Supercritical Fluid ChromatographyE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodIEEE/ASTM SI-10 Practice for Use of the InternationalSystem of Units(SI)(the Modernized Metric System)3.Terminology3.1 DefinitionsUnits and symbols used in this test methodare those recommended in Practice IEEE/ASTM SI-10.Chro-matographic terms and relationships are as described in Prac-tice E355.3.2 Abbreviations:3.2.1 BHTButylated hydroxy toluene(2,6-di-tert-butyl-4-methyl-hydroxybenzene).3.2.2 MMMethyl myristate.3.2.3 EVAEthylene-vinyl acetate copolymers.3.2.4 LDPELow-density polyethylene.3.2.5 HDPEHigh-density polyethylene.4.Summary of Test Method4.1 The BHT from a finely ground polymer sample isextracted by shaking or refluxing with cyclohexane or isopro-panol.A known volume of this extract is injected into a gaschromatographic column packed with a liquid-coated solidsupport.Passing through this column in a stream of carrier gas,BHT is separated from the extraction solvent and othercomponents.Responses of BHT and any internal standard aremeasured by a flame ionization detector.This signal is re-corded to indicate the relative concentration and retention timeof BHT.5.Significance and Use5.1 Separation and identification of stabilizers used in themanufacture of polyethylene are necessary in order to correlateperformance properties with polymer composition.5.2 The BHT extraction procedure is made effective by theinsolubility of the polymer sample in solvents generally usedfor gas chromatographic analysis.1This test method is under the jurisdiction of ASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.70 on Analytical Methods.Current edition approved Aug.1,2009.Published August 2009.Originallyapproved in 1983.Last previous edition approved in 2002 as D4275-02.DOI:10.1520/D4275-09.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.Interferences6.1 Any material eluting at or near the BHT or MMretention times will cause erroneous results.Prior to extraction,solvent blanks shall be analyzed to confirm the absence ofinterfering peaks.7.Apparatus7.1 Reflux Extraction,consisting of 250-mL round-bottomflask with condenser and heating mantle to fit.7.2 Wiley Mill,with 10 and 20-mesh screens.7.3 Wrist-Action Shaker.7.4 Gas Chromatograph,equipped with a flame ionizationdetector.7.5 Chromatographic Column,3.2-mm outside diametertimes 1.8 m packed with 20%UCW-98 on 80/100 meshChromosorb P,a similar packed column,or an equivalentcapillary column,such as a HP-1 or DB-1.7.6 Integrator,capable of measuring the net peak area on theback side of a solvent peak.7.7 Gas Chromatographic Syringe,10 L.7.8 Analytical Balance,capable of weighing to 60.0001 g.7.9 Pressure Regulators,for all required gas cylinders.7.10 Filter-Dried Assemblies,for each required g