ASTM D5310-10(2014)

Standard Test Method for Tar Acid Composition by Capillary Gas Chromatography

SIGNIFICANCE AND USE
5.1 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

• Status: Historical
• Publication Date: 30-Jun-2014
• ICS: 71.080.40 - Organic acids
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.02 - Oxygenated Aromatics

Relations

• Replaces: ASTM D5310-10e1 - Standard Test Method for Tar Acid Composition by Capillary Gas Chromatography
• Effective Date: 01-Jul-2014

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D5310 − 10 (Reapproved 2014)
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 2.2 Other Documents:
OSHA Regulations, 29 CFR paragraphs 1910.1000, and
1.1 This test method covers the quantitative determination
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
5. Significance and Use
standard.
5.1 This test method is suitable for the general quantitative
1.4 This standard does not purport to address all of the
analysis of commercial tar acid mixtures. It may be used as a
safety concerns, if any, associated with its use. It is the
toolforqualitycontrolandspecificationpurposesbyproducers
responsibility of the user of this standard to establish appro-
and users.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific hazard
6. Apparatus
statements, see Section 8.
6.1 Chromatograph—Agaschromatographcompatiblewith
capillary columns, equipped with inlet splitter and high tem-
2. Referenced Documents
perature flame ionization detector. Typical Operating Condi-
2.1 ASTM Standards:
tions are given in Table 1.
D3852 Practice for Sampling and Handling Phenol, Cresols,
6.2 Peak Integrator—Electronic integration is recom-
and Cresylic Acid
D4790 Terminology ofAromatic Hydrocarbons and Related 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-
terials 6.5 Capillary Column—Any column capable of resolving
E29 Practice for Using Significant Digits in Test Data to all components of interest. Prepared columns are commercially
Determine Conformance with Specifications available from chromatography supply houses. Chromato-
grams from three columns are presented in Fig. 1, Fig. 2, and
Fig. 3. Peak identification is given in Table 2.
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 Calibration Standards—Samples of known composition
Current edition approved July 1, 2014. Published July 2014. Originally approved
ε1
in 1994. Last previous edition approved in 2010 as D5310 – 10 . DOI: 10.1520/
representative of samples to be analyzed.
D5310-10R14.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. 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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5310 − 10 (2014)
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 Dii-
sodecyl Phthalate on Fused Silica
FIG. 3 Typical Chromatogram of Cresylic Acid on Column of 95 %
Dimethyl, 5 % Diphenyl Polysiloxane Bonded on Fused Silica
10. Calibration
10.1 Prepare a sample of known composition to contain
each component in the approximate concentration expected in
the unknown sample. Make sure that each component in the
preparation is of known purity. Even when purchased as
reagent grade, it is prudent to verify impurities, including
water.
10.2 Inject an appropriate amount of the calibration sample
from 10.1 into the chromatograph and allow to run till all
FIG. 2 Typical Chromatogram of Cresylic Acid on Column of 25 %
components clear the column. Fig. 1, Fig. 2, and Fig. 3 are
Cyanopropyl, 25 % Phenyl, 50 % Meth
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: D5310 − 10 D5310 − 10 (Reapproved 2014)
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.
ε NOTE—The title of Figure 3 was corrected editorially in February 2010.
1. Scope*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.
2. Referenced Documents
2.1 ASTM Standards:
D3852 Practice for Sampling and Handling Phenol, Cresols, and Cresylic Acid
D4790 Terminology of Aromatic Hydrocarbons and Related Chemicals
D6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
2.2 Other Documents:
OSHA Regulations, 29 CFR paragraphs 1910.1000, and 1910.1200
3. Terminology
3.1 For definition of terms used in this test method see Terminology D4790.
4. Summary of Test Method
4.1 The sample composition is determined by capillary gas chromatography. The weight percent composition is calculated from
the ratio of the individual peak areas to the total area of all peaks using appropriate response factors determined for each component
by means of a calibration sample.
5. Significance and Use
5.1 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.
This test method is under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee
D16.02 on Oxygenated Aromatics.
Current edition approved Jan. 1, 2010July 1, 2014. Published January 2010July 2014. Originally approved in 1994. Last previous edition approved in 20042010 as
ε1
D5310 – 00 (2004).D5310 – 10 . DOI: 10.1520/D5310-10E01.10.1520/D5310-10R14.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available 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.
*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
D5310 − 10 (2014)
6. Apparatus
6.1 Chromatograph—A gas chromatograph compatible with capillary columns, equipped with inlet splitter and high
temperature flame ionization detector. Typical Operating Conditions are given in Table 1.
6.2 Peak Integrator—Electronic integration is recommended.
6.3 Recorder, with full scale response time of 1 s or less.
6.4 Microsyringe, capacity of 1 μL.
6.5 Capillary Column—Any column capable of resolving all components of interest. Prepared columns are commercially
available from chromatography supply houses. Chromatograms from three columns are presented in Fig. 1, Fig. 2, and Fig. 3. Peak
identification is given in Table 2.
7. Reagents and Materials
7.1 Calibration Standards—Samples of known composition representative of samples to be analyzed.
8. Hazards
8.1 Consult current OSHA regulations and suppliers’ material safety data sheets, and local regulations for all materials used in
this test method.
9. Sampling
9.1 Sample the material in accordance with Practice D3852.
10. Calibration
10.1 Prepare a sample of known composition to contain each component in the approximate concentration expected in the
unknown sample. Make sure that each component in the preparation is of known purity. Even when purchased as reagent grade,
it is prudent to verify impurities, including water.
10.2 Inject an appropriate amount of the calibration sample from 10.1 into the chromatograph and allow to run till all
components clear the column. Fig. 1, Fig. 2, and Fig. 3 are chromatograms of a cresylic acid blend illustrating typical separations
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 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
Column temperature,°C 100 100 105
Detector temperature,° C 200–275 200–275 200–275
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 ra
...