1、Designation: D5310 101Standard 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 last revision
2、. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEThe title of Figure 3 was corrected editorially in February 2010.1. Scope*1.1 This test method covers the quantitative determinationof phe
3、nol and certain homologues of phenol in tar acid andcresylic 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 ionizationd
4、etector.1.2 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 E29.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are inclu
5、ded in thisstandard.1.4 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
6、 use. For specific hazardstatements, see Section 8.2. Referenced Documents2.1 ASTM Standards:2D3852 Practice for Sampling and Handling Phenol,Cresols, and Cresylic AcidD4790 Terminology ofAromatic Hydrocarbons and RelatedChemicalsD6809 Guide for Quality Control and Quality AssuranceProcedures for Ar
7、omatic Hydrocarbons and Related Ma-terialsE29 Practice 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 seeTerminolog
8、y D4790.4. Summary of Test Method4.1 The sample composition 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
9、a calibration sample.5. Significance and Use5.1 This 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 ChromatographA gas chromatograph compatiblew
10、ith capillary columns, equipped with inlet splitter and hightemperature flame ionization detector. Typical Operating Con-ditions 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
11、 Capillary ColumnAny column capable of resolvingall 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
12、 Calibration StandardsSamples of known compositionrepresentative 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 ap
13、proved Jan. 1, 2010. Published January 2010. Originallyapproved in 1994. Last previous edition approved in 2004 as D5310 00 (2004).DOI: 10.1520/D5310-10.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMSt
14、andards 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.1*A Summary of Changes section appears at the
15、 end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.8. Hazards8.1 Consult current OSHA regulations and suppliers mate-rial safety data sheets, and local regulations for all materialsused in this test method.9. Sampli
16、ng9.1 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 inthe unknown sample. Make sure that each component in thepreparation is of known purity. Even when purchased asrea
17、gent 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 typicalse
18、parations and retention times.10.3 Determine a response factor for each component.Choose one of the major components as the 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 Cond
19、itionsColumn Liquid Phase Diisodecyl PhthalateCyanopropyl 25 %, Phenyl 25 %,Methylpolysiloxane 50 %, Bonded PhaseDimethyl 95 %, 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
20、temperature, C 100 100 105Detector temperature, C 200275 200275 200275Injection block temperature, C 200275 200275 200275Carrier 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 flam
21、e ;10H2flow (optimize) ;10H2flow (optimize) ;10H2flow (optimize)Make up gasAN2or He N2or He N2or HeSample size, L 0.050.1 0.050.1 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 d
22、etector operations; each instrument should be optimizedaccording to manufacturers recommendations.FIG. 1 Typical Chromatogram of Cresylic Acid on Column ofDiisodecyl Phthalate on Fused SilicaFIG. 2 Typical Chromatogram of Cresylic Acid on Column of 25 %Cyanopropyl, 25 % Phenyl, 50 % Methylpolysiloxa
23、neBonded onFused SilicaFIG. 3 Typical Chromatogram of Cresylic Acid on Column of 95 %Dimethyl, 5 % Diphenyl Polysiloxane Bonded on Fused SilicaD5310 1012RFi5Ci!Ar!Ai!Cr!where:RFi= response factor for component,Ai= area of component peak,Ci= concentration of component peak, in weight per-cent,Ar= are
24、a of reference peak, andCr= concentration of reference peak, in weight percent.11. Procedure11.1 Inject a portion of the 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 componen
25、t inthe sample by calculating the corrected area for each compo-nent peak in the sample and dividing the corrected area by thesummation of all the corrected areas and multiplying by 100.Ci5RFi!Ai!(i 5 1nRFi!Ai!3 100where:Ci= concentration of the component inweight percent,RFi= response factor for co
26、mponent i calcu-lated in calibration,Ai= area of the component, i peak, and(i 5 1nRFi!Ai!= the summation of all response cor-rected areas in 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 follo
27、wing criteria should be used to judge theacceptability (95 % probability level) of the results obtained bythis test method. The criteria were derived from an interlabo-ratory study between six laboratories, using chromatographiccolumns of diisodecyl phthalate on fused silica. The data wereobtained o
28、n two days by the same operator in each laboratoryand three samples with components ranging in concentrationfrom 0.04 % to 98.5 %.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 Reproducib
29、ilityResults submitted by two laborato-ries should not be considered suspect unless they differ bymore than the amount shown in Table 3.14.2 BiasAlthough the interlaboratory study utilizedsamples prepared gravimetrically from pre-analyzed stocks ofthe highest available purity, the samples were not a
30、pproved asaccepted reference materials. Consequently, no bias is reportedfor this test method.15. Quality Guidelines15.1 Laboratories 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 gui
31、delines of standard statistical quality control practices.15.1.2 A quality control sample is a stable material isolatedfrom the production process and representative of the samplebeing analyzed.4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Resea
32、rch Report RR:D16-1013.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-cresol6 o-ethylphenol7 2,4-xylenol8 2,5-xylenol9 2,4,6-trimethylphenol10
33、 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-trimethylphenol22 3-ethyl, 5-methylphenolTABLE 3 Intermediate Precision and R
34、eproducibilityAverage 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 0.07125.27 0.262 0.262m-cresol 9.33 0.101 0.10959.46 0.177 0.24898.53 0.093 0.1
35、76o-ethylphenol 0.07 0.011 0.0150.17 0.008 0.0200.41 0.048 0.061D5310 101315.1.3 When QA/QC protocols are already established inthe testing facility, these protocols are acceptable when theyconfirm the validity of test results.15.1.4 When there are no QA/QC protocols established inthe testing facili
36、ty, use the guidelines described in GuideD6809 or similar statistical quality contol practices.16. Keywords16.1 cresols; cresylic acid; gas chromatography; phenol; taracid; xylenolsSUMMARY OF CHANGESCommittee D16 has identified the location of selected changes to this standard since the last issue(D
37、5310 - 00 (2004) that may impact the use of this standard. (Approved January 1, 2010.)(1) Added Quality Guidelines Section 15.(2) Added Guide D6809 to Referenced Documents section2.1.(3) Added a statement concerning units section 1.3.ASTM International takes no position respecting the validity of an
38、y patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to rev
39、ision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your
40、 comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyr
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