ASTM_D_3160_-_16.pdf

Designation:D316016Standard Test Method forPhenol Content of Cumene(Isopropylbenzene)or AMS(Methylstyrene)1This standard is issued under the fixed designation D3160;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 phenol inrefinedcumene(isopropylbenzene)orAMS(methylstyrene).1.2 This test method has been found applicable in the rangefrom 5 to 50 mg/kg of phenol in refined cumene(isopropyl-benzene)or AMS(methylstyrene).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 7.2.Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD3437 Practice for Sampling and Handling Liquid CyclicProductsD6809 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 SpecificationsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 Other Document:OSHA Regulations,29 CFR paragraphs 1910.000 and 1910,120033.Summary of Test Method3.1 The phenol content of cumene orAMS is determined bythe color development of phenol with 4-aminoantipyrine.Thesample absorbance is compared to phenol standards at 472 nmon a spectrophotometer.4.Significance and Use4.1 This test method is useful in determining phenol in therange from 5 to 50 mg/kg in commercially available cumene orAMS.4.2 Phenol will inhibit certain reactions involving cumeneor AMS.5.Apparatus5.1 BalanceAny balance capable of measuring weights tothe nearest 0.001 g.5.2 SpectrophotometerAny spectrophotometer that canmeasure 0 to 2 absorbance units at 472 nm with a wavelengthrepeatability of 5 nm.5.3 Spectrophotometer Cells,2 cm.5.4 Filter Paper.6.Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused.Unless otherwise indicated,it is intended that all reagentsshall conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society,where1This 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 1,2016.Published June 2016.Originallyapproved in 1991.Last previous edition approved in 2012 as D3160 12.DOI:10.1520/D3160-16.2For 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 such specifications are available.4Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.6.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent water as definedby Type I or II of Specification D1193.Type I is the highestpurity with a maximum conductivity of 0.056 S/cm.Type IIwater requires distillation.Type III water has a maximumconductivity of 0.25 S/cm and there are significant quantitiesof other impurities.Type IV water has a maximum conductiv-ity of 5 S/cm and unlimited quantities of TOC and silica.6.3 Cumene or AMSWash 1 L of cumene or AMS with5%aqueous sodium hydroxide in a 2 L separatory funnel.Discard the aqueous sodium hydroxide phase and filter thehydrocarbon through dry filter paper.Store the hydrocarbonunder a nitrogen blanket.The previous steps are taken to ensurethat the hydrocarbon will not contain phenol or peroxides.6.4 Solution of 4-Amino-AntipyrineDissolve 3.00 g ofamino-antipyrine in distilled water and dilute to volume in adark amber 100-mL volumetric flask.This should be stable fortwo weeks.Alternate volumes of solutions may be p