1、Designation: D5310 10 (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
2、 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. Scope1.1 This test method covers the quantitative determinationof phenol and certain homologues of phenol in tar acid andcr
3、esylic acid 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
4、 results usingthis 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
5、 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 8.2.
6、Referenced Documents2.1 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 Practic
7、e for Using Significant 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 compo
8、sition is determined by capillary 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
9、test method is suitable for 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 an
10、d high tem-perature flame ionization 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 of1sorless.6.4 Microsyringe, capacity of 1 L.6.5 Capillary ColumnAny column capable of resolvingall
11、components of interest. Prepared 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 compositionre
12、presentative of samples to be analyzed.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
13、 approvedin 1994. Last previous edition approved 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 Docume
14、nt 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.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. Un
15、ited States18. Hazards8.1 Consult current OSHA regulations and 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 con
16、taineach component in the approximate concentration expected inthe 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 samplefr
17、om 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 major components as the
18、reference peak,and calculate response factors relative to the reference peak.The response factor for the reference peak will be 1.TABLE 1 Typical Chromatographic Operating ConditionsColumn Liquid Phase Diisodecyl PhthalateCyanopropyl 25 %, Phenyl 25 %,Methylpolysiloxane 50 %, Bonded PhaseDimethyl 95
19、 %, Diphenylpolysiloxane5 %, Bonded PhaseColumn Fused Silica Fused Silica Fused SilicaColumn length, m 30 25 30Column ID, mm 0.25 0.22 0.25Film thickness, m 0.2 0.2 0.25Column temperature,C 100 100 105Detector temperature,C 200275 200275 200275Injection block temperature, C 200275 200275 200275Carri
20、er gas H2or He H2or He H2or HeCarrier flow, linear velocity, cm/s 4080 4080 4080Hydrogen flow to flame, mL/min 3040 (optimize) 3040 (optimize) 3040 (optimize)Air flow to flame ;10H2flow (optimize) ;10H2flow (optimize) ;10H2flow (optimize)Make up gasAN2or He N2or He N2or HeSample size, L 0.050.1 0.05
21、0.1 0.050.1Split ratio 100:1 to 250:1 100:1 to 250:1 100:1 to 250:1AInert gas added to hydrogen fuel gas as coolant to prevent overheating and thermal emissions for optimal detector operations; each instrument should be optimizedaccording to manufacturers recommendations.FIG. 1 Typical Chromatogram
22、of Cresylic Acid on Column of Dii-sodecyl Phthalate on Fused SilicaFIG. 2 Typical Chromatogram of Cresylic Acid on Column of 25 %Cyanopropyl, 25 % Phenyl, 50 % MethylpolysiloxaneBonded onFused SilicaFIG. 3 Typical Chromatogram of Cresylic Acid on Column of 95 %Dimethyl, 5 % Diphenyl Polysiloxane Bon
23、ded on Fused SilicaD5310 10 (2014)2RFi5Ci!Ar!Ai!Cr!where:RFi= response factor for component,Ai= area of component peak,Ci= concentration of component peak, in weight percent,Ar= area of reference peak, andCr= concentration of reference peak, in weight percent.11. Procedure11.1 Inject a portion of th
24、e unknown sample into thechromatograph, identical to that used for the standard sample,and obtain the chromatogram.12. Calculation12.1 Determine the weight percent for each component inthe sample by calculating the corrected area for each compo-nent peak in the sample and dividing the corrected area
25、 by thesummation of all the corrected areas and multiplying by 100.Ci5RFi!Ai!(i51nRFi!Ai!3100where:Ci= concentration of the component in weightpercent,RFi= response factor for component i calculated incalibration,Ai= area of the component, i peak, and(i51nRFi!Ai!= the summation of all response corre
26、cted areasin the chromatogram.13. Report13.1 Report each component to the nearest 0.01 % weight.13.2 All components should total 100 %.14. Precision and Bias414.1 The following criteria should be used to judge theacceptability (95 % probability level) of the results obtained bythis test method. The
27、criteria were derived from an interlabo-ratory study between six laboratories, using chromatographiccolumns of diisodecyl phthalate on fused silica. The data wereobtained on two days by the same operator in each laboratoryand three samples with components ranging in concentrationfrom 0.04 % to 98.5
28、%.14.1.1 Intermediate PrecisionResults in the same labora-tory should not be considered suspect unless they differ bymore than the amount shown in Table 3.14.1.2 ReproducibilityResults submitted by two laborato-ries should not be considered suspect unless they differ bymore than the amount shown in
29、Table 3.14.2 BiasAlthough the interlaboratory study utilizedsamples prepared gravimetrically from pre-analyzed stocks ofthe highest available purity, the samples were not approved asaccepted reference materials. Consequently, no bias is reportedfor this test method.15. Quality Guidelines15.1 Laborat
30、ories shall have a quality control system inplace.15.1.1 Confirm the performance of the test instrument ortest method by analyzing a quality control sample followingthe guidelines of standard statistical quality control practices.15.1.2 A quality control sample is a stable material isolatedfrom the
31、production process and representative of the samplebeing analyzed.15.1.3 When QA/QC protocols are already established inthe testing facility, these protocols are acceptable when theyconfirm the validity of test results.4Supporting data have been filed at ASTM International Headquarters and maybe obt
32、ained by requesting Research Report RR:D16-1013. ContactASTM CustomerService at serviceastm.org.TABLE 2 Compound Identification of Chromatographic Peaks inFigs. 1-3NOTE 1Compounds are listed in order of elution on diisodecylphthalate column.Number Compound1 phenol2 o-cresol3 2,6-xylenol4 p-cresol5 m
33、-cresol6 o-ethylphenol7 2,4-xylenol8 2,5-xylenol9 2,4,6-trimethylphenol10 2,3-xylenol11 p-ethylphenol12 m-ethylphenol13 3,5-xylenol14 3,4-xylenol15 4-ethyl, 2-methylphenol16 5-ethyl, 2-methylphenol17 p-isopropylphenol18 m-isopropylphenol19 3-ethyl, 2-methylphenol20 2,4,5-trimethylphenol21 2,3,5-trim
34、ethylphenol22 3-ethyl, 5-methylphenolTABLE 3 Intermediate Precision and ReproducibilityAverage WeightPercentIntermediatePrecisionReproducibilityPhenol 0.04 0.012 0.0202.41 0.054 0.06314.82 0.171 0.189o-cresol 0.16 0.026 0.0370.17 0.080 0.12582.94 0.133 0.164p-cresol 0.65 0.029 0.0385.44 0.055 0.0712
35、5.27 0.262 0.262m-cresol 9.33 0.101 0.10959.46 0.177 0.24898.53 0.093 0.176o-ethylphenol 0.07 0.011 0.0150.17 0.008 0.0200.41 0.048 0.061D5310 10 (2014)315.1.4 When there are no QA/QC protocols established inthe testing facility, use the guidelines described in GuideD6809 or similar statistical qual
36、ity control practices.16. Keywords16.1 cresols; cresylic acid; gas chromatography; phenol; taracid; xylenolsASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised t
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40、eprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 10 (2014)4
