ASTM_D_4961_-_99.pdf

Designation:D 4961 99Standard Test Methods forGas Chromatographic Analysis of Major Organic Impuritiesin Phenol Produced by the Cumene Process1This standard is issued under the fixed designation D 4961;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(e)indicates an editorial change since the last revision or reapproval.1.Scope1.1 These test methods cover the determination of majororganic impurities in refined phenol manufactured by thecumene(isopropylbenzene)process.Two test methods areemployed to determine the stated major impurities.1.2 Test Method A determines the concentration of majorimpurities such as mesityl oxide,cumene,a-methylstyrene,2-methylbenzofuran,acetophenone,and dimethylbenzyl alco-hol.1.3 Test Method B determines the hydroxyacetone content.1.4 The following applies to all specified limits in thisstandard:for purposes of determining conformance with thisstandard,an observed value or a calculated value shall berounded off“to the nearest unit”in the last right-hand digitused in expressing the specification limit,in accordance withthe rounding-off method of Practice E 29.1.5 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:D 1193 Specification for Reagent Water2D 3852 Practice for Sampling and Handling Phenol andCresylic Acid3D 4790 Terminology of Aromatic Hydrocarbons and Re-lated Chemicals3E 29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications42.2Other Document:OSHA Regulations,29 CFR,paragraphs 1910.1000 and1910.120053.Terminology3.1 DefinitionsFor definitions of terms used in these testmethods,see Terminology D 4790.4.Summary of Test Methods4.1 Two test methods are used to determine the majorimpurities in phenol:4.1.1 Test Method A,Major Impurity DeterminationAknown amount of internal standard is added to the sample.Aportion of the sample is analyzed by gas chromatography.Theconcentration of each impurity is calculated relative to theknown amount of internal standard that is added.4.1.2 Test Method B,Hydroxyacetone DeterminationAmeasured amount of sample is analyzed by gas chromatogra-phy.The concentration of hydroxyacetone in the sample isdetermined by the ratio of the area of hydroxyacetone in thesample to the area in a standard sample containing a knownamount of hydroxyacetone.5.Significance and Use5.1 This test method is useful in setting specifications forrefined phenol manufactured by the cumene process and forprocess control.Test Method A is useful for individual impu-rities in the range from 10 to 100 mg/kg.Test Method B isuseful for hydroxyacetone in the range from 5 to 500 mg/kg.6.Purity of Reagents6.1 Reagent grade chemicals shall be used in all tests.Unless otherwise indicated,it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society,where suchspecifications are available.5Other grades may be used,pro-vided 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 conformingto Type IV of Specification D 1193.1These test methods are under the jurisdiction of ASTM Committee D-16 onAromatic Hydrocarbons and Related Chemicals and are the direct responsibility ofSubcommittee D16.OC on Oxygenated Aromatics.Current edition approved Jan.10,1999.Published March 1999.Originallypublished as D 4961 89.Last previous edition D 4961 93.2Annual Book of ASTM Standards,Vol 11.01.3Annual Book of ASTM Standards,Vol 06.04.4Annual Book of ASTM Standards,Vol 14.02.5Available from Superintendent of Documents,U.S.Government PrintingOffice,Washington,DC 20402.1AMERICAN SOCIETY FOR TESTING AND MATERIALS100 Barr Harbor Dr.,West Conshohocken,PA 19428Reprinted from the Annual Book of ASTM Standards.Copyright ASTM7.Hazards7.1 Consult the current OSHA regulations6,suppliers Ma-terial Safety Data Sheets and local regulations for all materialsused in these test methods.7.2 The materials used in these test methods are highly toxicand flammable.8.Sampling8.1 Sample the material in accordance with PracticeD 3852.TEST METHOD A9.Apparatus9.1 Chromatograph,equipped with an on-column injectorand flame ionization detector.9.2 Recorder,with a full scale of 1 mV and a response timeof 1 s or less.9.3 Integrating DeviceAny device capable of integratingchromatograph peak areas with a repeatability of 61%rela-tive.9.4 Chromatographic C