ASTM_D_5060_-_12.pdf

Designation:D506012Standard Test Method forDetermining Impurities in High-Purity Ethylbenzene by GasChromatography1This standard is issued under the fixed designation D5060;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 describes the analysis of normallyoccurring impurities in,and the purity of,ethylbenzene by gaschromatography.Impurities determined include nonaromatichydrocarbons,benzene,toluene,xylenes,cumene,and dieth-ylbenzene isomers.1.2 This test method is applicable for impurities at concen-trations from 0.001 to 1.000%and for ethylbenzene purities of99%or higher.At this level,p-xylene may not be detected.1.3 In determining the performance of the test results usingthis method to applicable specifications,results shall berounded off in accordance with the rounding-off method ofPractice E29.1.4 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.5 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.For a specifichazard statement,see Section 8.2.Referenced Documents2.1 ASTM Standards:2D3437 Practice for Sampling and Handling Liquid CyclicProductsD4307 Practice for Preparation of Liquid Blends for Use asAnalytical StandardsD6809 Guide for Quality Control and Quality AssuranceProcedures for Aromatic Hydrocarbons and Related Ma-terialsE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE355 Practice for Gas Chromatography Terms and Relation-shipsE1510 Practice for Installing Fused Silica Open TubularCapillary Columns in Gas Chromatographs2.2 Other Documents:OSHA Regulations,29 CFR paragraphs 1910.1000 and1910.120033.Summary of Test Method3.1 A known amount of internal standard is added to thesample.Agas chromatograph equipped with a flame ionizationdetector and a polar fused silica capillary column is used forthe analysis.The impurities are measured relative to theinternal standard.Ethylbenzene purity is calculated by sub-tracting the impurities found from 100.00%.4.Significance and Use4.1 The test is suitable for setting specifications on ethyl-benzene and for use as an internal quality control tool whereethylbenzene is used in manufacturing processes.It may beused in development or research work involving ethylbenzene.4.2 Purity is commonly reported by subtracting the deter-mined expected impurities from 100%.Absolute puritycannot be determined if unknown impurities are present.5.Interferences5.1 A key operational parameter for this method is theseparation of p-xylene from ethylbenzene.Care should betaken during calibration to ensure the separation of these twocomponents.If p-xylene is not separated from ethylbenzeneduring the calibration of the instrument,modify the columnflow rate slightly until separation is achieved.1This test method is under the jurisdiction of ASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct responsibility ofSubcommittee D16.07 on Styrene,Ethylbenzene and C9 and C10 AromaticHydrocarbons.Current edition approved June 1,2012.Published August 2012.Originallyapproved in 1990.Last previous edition approved in 2007 as D5060 07.DOI:10.1520/D5060-12.2For 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 U.S.Government Printing Office Superintendent of Documents,732 N.Capitol St.,NW,Mail Stop:SDE,Washington,DC 20401,http:/www.access.gpo.gov.*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 6.Apparatus6.1 Gas Chromatograph(GC),any GC built for capillarycolumn chromatography and equipped with a flame ionizationdetector(FID).The system shall have sufficient sensitivity,linearity,and range to obtain a minimum peak height responsefor 0.0010 wt%impurity of twice the height of the signalbackground noise,while not exceeding the full scale of eitherthe detector or the electronic integration for the major compo-nents.It shall have a split injection system that will notdiscriminate over the boiling range of the samples analyzed.6.2 Chromatographic Column,fused silica capillary,60 mlong,0.32-mm inside diameter,internally coated to a 0.5-mthickness with a bonded(crosslinked)polyethylene glycol.Other columns may be used after it has been established tha