1、Designation:D531010(Reapproved 2014)Standard Test Method forTar Acid Composition by Capillary Gas Chromatography1This standard is issued under the fixed designation D5310;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of la
2、st 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 covers the quantitative determinationof phenol and certain homologues of phenol in tar acid andcresylic acid
3、 mixtures using capillary gas chromatography.It isa normalization test method that determines homolog distribu-tion but is not an absolute assay since it does not account forwater or other compounds not detected by a flame ionizationdetector.1.2 In determining the conformance of the test results usi
4、ngthis method to applicable specifications,results shall berounded off in accordance with the rounding-off method ofPractice E29.1.3 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.4 This standard does not purport to address al
5、l 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 8.2.Referenced Documents
6、2.1 ASTM Standards:2D3852 Practice for Sampling and Handling Phenol,Cresols,and Cresylic AcidD4790 Terminology of Aromatic Hydrocarbons and RelatedChemicalsD6809 Guide for Quality Control and Quality AssuranceProcedures for Aromatic Hydrocarbons and Related Ma-terialsE29 Practice for Using Significa
7、nt Digits in Test Data toDetermine Conformance with Specifications2.2 Other Documents:OSHA Regulations,29 CFR paragraphs 1910.1000,and1910.120033.Terminology3.1 For definition of terms used in this test method seeTerminology D4790.4.Summary of Test Method4.1 The sample composition is determined by c
8、apillary gaschromatography.The weight percent composition is calculatedfrom the ratio of the individual peak areas to the total area ofall peaks using appropriate response factors determined foreach component by means of a calibration sample.5.Significance and Use5.1 This test method is suitable for
9、 the general quantitativeanalysis of commercial tar acid mixtures.It may be used as atool for quality control and specification purposes by producersand users.6.Apparatus6.1 ChromatographAgas chromatograph compatible withcapillary columns,equipped with inlet splitter and high tem-perature flame ioni
10、zation detector.Typical Operating Condi-tions are given in Table 1.6.2 Peak IntegratorElectronic integration is recom-mended.6.3 Recorder,with full scale response time of 1 s or less.6.4 Microsyringe,capacity of 1 L.6.5 Capillary ColumnAny column capable of resolvingall components of interest.Prepar
11、ed columns are commerciallyavailable from chromatography supply houses.Chromato-grams from three columns are presented in Fig.1,Fig.2,andFig.3.Peak identification is given in Table 2.7.Reagents and Materials7.1 Calibration StandardsSamples of known compositionrepresentative of samples to be analyzed
12、.1This 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 July 1,2014.Published July 2014.Originally approvedin 1994.Last previous edition ap
13、proved in 2010 as D5310 101.DOI:10.1520/D5310-10R14.2For 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 fro
14、m U.S.Government Printing Office Superintendent of Documents,732 N.Capitol St.,NW,Mail Stop:SDE,Washington,DC 20401,http:/www.access.gpo.gov.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 8.Hazards8.1 Consult current OSHA regulations and
15、 suppliers mate-rial safety data sheets,and local regulations for all materialsused in this test method.9.Sampling9.1 Sample the material in accordance with Practice D3852.10.Calibration10.1 Prepare a sample of known composition to containeach component in the approximate concentration expected inth
16、e unknown sample.Make sure that each component in thepreparation is of known purity.Even when purchased asreagent grade,it is prudent to verify impurities,includingwater.10.2 Inject an appropriate amount of the calibration samplefrom 10.1 into the chromatograph and allow to run till allcomponents clear the column.Fig.1,Fig.2,and Fig.3 arechromatograms of a cresylic acid blend illustrating typicalseparations and retention times.10.3 Determine a response factor for each component.Choose one of the