ASTM D5310-10
(Test Method)Standard Test Method for Tar Acid Composition by Capillary Gas Chromatography
Standard Test Method for Tar Acid Composition by Capillary Gas Chromatography
SIGNIFICANCE AND USE
This test method is suitable for the general quantitative analysis of commercial tar acid mixtures. It may be used as a tool for quality control and specification purposes by producers and users.
SCOPE
1.1 This test method covers the quantitative determination of phenol and certain homologues of phenol in tar acid and cresylic acid mixtures using capillary gas chromatography. It is a normalization test method that determines homolog distribution but is not an absolute assay since it does not account for water or other compounds not detected by a flame ionization detector.
1.2 In determining the conformance of the test results using this method to applicable specifications, results shall be rounded off in accordance with the rounding-off method of Practice E29.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D5310 – 10
Standard Test Method for
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Tar Acid Composition by Capillary Gas Chromatography
This standard is issued under the fixed designation D5310; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope* 2.2 Other Documents:
OSHA Regulations, 29 CFR paragraphs 1910.1000, and
1.1 This test method covers the quantitative determination
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1910.1200
of phenol and certain homologues of phenol in tar acid and
cresylic acid mixtures using capillary gas chromatography. It is
3. Terminology
a normalization test method that determines homolog distribu-
3.1 For definition of terms used in this test method see
tion but is not an absolute assay since it does not account for
Terminology D4790.
water or other compounds not detected by a flame ionization
detector.
4. Summary of Test Method
1.2 In determining the conformance of the test results using
4.1 The sample composition is determined by capillary gas
this method to applicable specifications, results shall be
chromatography. The weight percent composition is calculated
rounded off in accordance with the rounding-off method of
from the ratio of the individual peak areas to the total area of
Practice E29.
all peaks using appropriate response factors determined for
1.3 The values stated in SI units are to be regarded as
each component by means of a calibration sample.
standard. No other units of measurement are included in this
standard.
5. Significance and Use
1.4 This standard does not purport to address all of the
5.1 This test method is suitable for the general quantitative
safety concerns, if any, associated with its use. It is the
analysis of commercial tar acid mixtures. It may be used as a
responsibility of the user of this standard to establish appro-
toolforqualitycontrolandspecificationpurposesbyproducers
priate safety and health practices and determine the applica-
and users.
bility of regulatory limitations prior to use. For specific hazard
statements, see Section 8.
6. Apparatus
6.1 Chromatograph—A gas chromatograph compatible
2. Referenced Documents
with capillary columns, equipped with inlet splitter and high
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2.1 ASTM Standards:
temperature flame ionization detector. Typical Operating Con-
D3852 Practice for Sampling and Handling Phenol,
ditions are given in Table 1.
Cresols, and Cresylic Acid
6.2 Peak Integrator—Electronic integration is recom-
D4790 TerminologyofAromaticHydrocarbonsandRelated
mended.
Chemicals
6.3 Recorder, with full scale response time of1sor less.
D6809 Guide for Quality Control and Quality Assurance
6.4 Microsyringe, capacity of 1 µL.
Procedures for Aromatic Hydrocarbons and Related Ma-
6.5 Capillary Column—Any column capable of resolving
terials
all components of interest. Prepared columns are commercially
E29 Practice for Using Significant Digits in Test Data to
available from chromatography supply houses. Chromato-
Determine Conformance with Specifications
grams from three columns are presented in Fig. 1, Fig. 2, and
Fig. 3. Peak identification is given in Table 2.
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This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of 7. Reagents and Materials
Subcommittee D16.02 on Oxygenated Aromatics.
7.1 CalibrationStandards—Samplesofknowncomposition
Current edition approved Jan. 1, 2010. Published January 2010. Originally
representative of samples to be analyzed.
approved in 1994. Last previous edition approved in 2004 as D5310 – 00 (2004).
DOI: 10.1520/D5310-10.
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or
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contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
Standards volume information, refer to the standard’s Document Summary page on 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
the ASTM website. www.access.gpo.gov.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D5310 – 10
TABLE 1 Typical Chromatographic Operating Conditions
Cyanopropyl 25 %, Phenyl 25 %, Dimethyl 95 %, Diphenylpolysiloxane
Column Liquid Phase Diisodecyl Phthalate
Methylpolysiloxane 50 %, Bonded Phase 5 %, Bonded Phase
Column Fused Silica Fused Silica Fused Silica
Column length, m 30 25 30
Column ID, mm 0.25 0.22 0.25
Film thickness,µ m 0.2 0.2 0.25
Column temperature,° C 100 100 105
Detector temperature,° C 200–275 200–275 2
...
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