1、Designation: D 5310 00 (Reapproved 2004)Standard Test Method forTar Acid Composition by Capillary Gas Chromatography1This standard is issued under the fixed designation D 5310; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the ye
2、ar 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 This test method covers the quantitative determinationof phenol and certain homologues of phenol in tar acid an
3、dcresylic 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 The following applies to all specified
4、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 29.1.3
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 hazar
6、dstatements, see Section 8.2. Referenced Documents2.1 ASTM Standards:2D 3852 Practice for Sampling and Handling Phenol,Cresols, and Cresylic AcidD 4790 Terminology of Aromatic Hydrocarbons and Re-lated ChemicalsE 29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Spec
7、ifications2.2 Other Documents:OSHA Regulations, 29 CFR, paragraphs 1910.1000, and1910.120033. Terminology3.1 For definition of terms used in this test method seeTerminology D 4790.4. Summary of Test Method4.1 The sample composition is determined by capillary gaschromatography. The weight percent com
8、position 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 the general quantitativeanalysis of commercial
9、tar acid mixtures. It may be used as atool for quality control and specification purposes by producersand users.6. Apparatus6.1 ChromatographA gas chromatograph compatiblewith capillary columns, equipped with inlet splitter and hightemperature flame ionization detector. Typical Operating Con-ditions
10、 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 components of interest. Prepared columns are commerciallyavailable from chro
11、matography 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.8. Hazards8.1 Consult current OSHA re
12、gulations and suppliers mate-rial safety data sheets, and local regulations for all materialsused in this test method.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 A
13、romatics.Current edition approved June 1, 2004. Published June 2004. Originallyapproved in 1994. Last previous edition approved in 2000 as D 5310 00.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStanda
14、rds 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 20401.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Con
15、shohocken, PA 19428-2959, United States.9. Sampling9.1 Sample the material in accordance with PracticeD 3852.10. 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 thepreparat
16、ion 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 arechromatogram
17、s 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 reference peak,and calculate response factors relative to the reference peak.The response factor for the reference peak will be
18、 1.RFi5Ci!Ar!Ai!Cr!TABLE 1 Typical Chromatographic Operating ConditionsColumn 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 30
19、Column 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 200275Carrier gas H2or He H2or He H2or HeCarrier flow, linear velocity, cm/s 4080 4080 4080Hydrogen flow to flame, mL/mi
20、n 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 0.050.1 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 c
21、oolant to prevent overheating and thermal emissions for optimal detector 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
22、 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 Bonded on Fused Silica(DB-5)D 5310 00 (2004)2where:RFi= response factor for component,Ai= area of component peak,C
23、i= concentration of component peak, in weight per-cent,Ar= area 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.
24、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 by thesummation of all the corrected areas and multiplying by 100.Ci5RFi!Ai!(i 5 1nRFi!Ai!3 100where:Ci= concentration
25、 of the component inweight percent,RFi= response factor for component 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 compo
26、nents 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 criteria were derived from an interlabo-ratory study between six laboratories, using chromatographiccolumns of
27、 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 %.14.1.1 Intermediate PrecisionResults in the same labora-tory should not be considered suspect unless they di
28、ffer 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 Table 3.14.2 BiasAlthough the interlaboratory study utilizedsamples prepared gravimetrically from pre-analyzed
29、 stocks ofthe highest available purity, the samples were not approved asaccepted reference materials. Consequently, no bias is reportedfor this test method.15. Keywords15.1 cresols; cresylic acid; gas chromatography; phenol; taracid; xylenols4Supporting data are available from ASTM International Hea
30、dquarters. RequestRR: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-trimethylp
31、henol10 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 Precisio
32、n 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 0.07125.27 0.262 0.262m-cresol 9.33 0.101 0.10959.46 0.177 0.24898.53 0.
33、093 0.176o-ethylphenol 0.07 0.011 0.0150.17 0.008 0.0200.41 0.048 0.061D 5310 00 (2004)3ASTM 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 that determination of
34、 the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn.
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36、nts 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 copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (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).D 5310 00 (2004)4
