ASTM_D_6142_-_12.pdf

Designation:D614212Standard Test Method forAnalysis of Phenol by Capillary Gas Chromatography1This standard is issued under the fixed designation D6142;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 the determination of knownimpurities in phenol by gas chromatography(GC).It isgenerally meant for the analysis of phenol of 99.9%or greaterpurity.1.2 This test method has been found applicable over impu-rity concentrations of 15 to 70 mg/kg.Users of this methodbelieve it is linear over a wider range.1.3 In determining the conformance 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 specific hazardstatements,see Section 9.2.Referenced Documents2.1 ASTM Standards:2D3852 Practice for Sampling and Handling Phenol,Cresols,and Cresylic AcidD4307 Practice for Preparation of Liquid Blends for Use asAnalytical StandardsD4790 Terminology of Aromatic Hydrocarbons and RelatedChemicalsD6809 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-shipsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE1510 Practice for Installing Fused Silica Open TubularCapillary Columns in Gas Chromatographs2.2 Other Document:OSHA Regulations,29 CFR paragraphs 1910.1000 and1910.120033.Terminology3.1 See Terminology D4790 for definition of terms used inthis test method.4.Summary of Test Method4.1 A known amount of an internal standard is added to asample of phenol.The prepared sample is mixed and analyzedby a gas chromatograph equipped with a flame ionizationdetector(FID).The peak area of each impurity and the internalstandard is measured.The amount of each impurity is calcu-lated from the ratio of the peak area of the internal standardversus the peak area of the impurity.Results are reported inmilligrams per kilogram.5.Significance and Use5.1 This test method is suitable for setting specifications onphenol and for use as an internal quality control tool wherephenol is produced or is used in a manufacturing process.Itmay also be used in development or research work involvingphenol.It is generally applied to determining those commonlyoccurring impurities such as mesityl oxide,cumene,hydroxyacetone,acetone,alpha-methylstyrene,2-methylbenzofuran,and acetophenone.5.2 Purity is commonly reported by subtracting the deter-mined expected impurities from 100.00.However,a gaschromatographic analysis cannot determine absolute purity if1This test method is under the jurisdiction of ASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct responsibility ofSubcommittee D16.02 on Oxygenated Aromatics.Current edition approved June 1,2012.Published June 2012.Originallyapproved in 1997.Last previous edition approved in 2008 as D6142 08.DOI:10.1520/D6142-12.2For 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 water is present or unknown components are contained withinthe material being examined.6.Interferences6.1 The internal standard chosen must be sufficiently re-solved from any impurity and the phenol peak.6.2 Any solvent used must also be sufficiently resolved fromany impurity,the internal standard,and the phenol peak.7.Apparatus7.1 Gas ChromatographAny chromatograph having aflame ionization detector that can be operated at the conditionsgiven in Table 1.The system should have sufficient sensitivityto obtain a minimum peak height response for a 2 mg/kgimpurity twice the height of the signal background noise.7.2 ColumnsThe choice of column is based on resolutionrequirements.Any column may be used that is ca