ASTM D5310-00(2004)
(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 The following applies to all specified limits in this standard: for purposes of determining conformance with this standard, an observed value or a calculated value shall be rounded off "to the nearest unit" in the last right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E29.
1.3 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 7.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 – 00 (Reapproved 2004)
Standard Test Method for
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 OSHA Regulations, 29 CFR, paragraphs 1910.1000, and
1910.1200
1.1 This test method covers the quantitative determination
of phenol and certain homologues of phenol in tar acid and
3. Terminology
cresylic acid mixtures using capillary gas chromatography. It is
3.1 For definition of terms used in this test method see
a normalization test method that determines homolog distribu-
Terminology D4790.
tion but is not an absolute assay since it does not account for
water or other compounds not detected by a flame ionization
4. Summary of Test Method
detector.
4.1 The sample composition is determined by capillary gas
1.2 The following applies to all specified limits in this
chromatography. The weight percent composition is calculated
standard: for purposes of determining conformance with this
from the ratio of the individual peak areas to the total area of
standard, an observed value or a calculated value shall be
all peaks using appropriate response factors determined for
rounded off “to the nearest unit” in the last right-hand digit
each component by means of a calibration sample.
used in expressing the specification limit, in accordance with
the rounding-off method of Practice E29.
5. Significance and Use
1.3 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
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.
E29 Practice for Using Significant Digits in Test Data to
6.4 Microsyringe, capacity of 1 µL.
Determine Conformance with Specifications
6.5 Capillary Column—Any column capable of resolving
2.2 Other Documents:
all components of interest. Prepared columns are commercially
available from chromatography supply houses. Chromato-
grams from three columns are presented in Fig. 1, Fig. 2, and
This test method is under the jurisdiction of ASTM Committee D16 on
Fig. 3. Peak identification is given in Table 2.
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
Subcommittee D16.02 on Oxygenated Aromatics.
7. Reagents and Materials
Current edition approved June 1, 2004. Published June 2004. Originally
approved in 1994. Last previous edition approved in 2000 as D5310 – 00. DOI: 7.1 CalibrationStandards—Samplesofknowncomposition
10.1520/D5310-00R04.
representative of samples to be analyzed.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
the ASTM website. 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5310 – 00 (2004)
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 200–275 200–275 200–275
Injection block temperature, °C 200–275 200–275 200–275
Carrier gas H or He H or He H or He
2 2 2
Carrier flow, linear velocity, cm/s 40–80 40–80 40–80
Hydrogen flow to flame, mL/min 30–40 (optimize) 30–40 (optimize) 30–40 (optimize)
Air flow to flame ;10·H flow (optimize) ;10·H flow (optimize) ;10·H flow (optimize)
2 2 2
A
Make up gas N or He N or He N or He
2 2 2
Sample size, µL 0.05–0.1 0.05–0.1 0.05–0.1
Split ratio 100:1 to 250:1 100:1 to 250:1 100:1 to 250:1
A
Inert gas added to hydrogen fuel gas as coolant to prevent overheating and thermal emissions for optimal detector operations; each instrument should be optimized
according to manufacturer’s recommendations.
FIG. 1 Typical Chromatogram of Cresylic Acid on Column of
Diisodecyl Phthalate on Fused Silica
FIG. 3 Typical Chromatogram of Cresylic Acid on Column of 95 %
Dimethyl, 5 % Diphenyl Polysiloxane Bonded on Fused Silica
(DB-5)
10. Calibration
10.1 Prepare a sample of known composition to contain
each component in the approximate concentration expected in
the unknown sam
...
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