ASTM D5310-23

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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 31-Mar-2023
• ICS: 71.080.40 - Organic acids
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.02 - Oxygenated Aromatics

Relations

• Refers: ASTM D3852-20 - Standard Practice for Sampling and Handling Phenol, Cresols, and Cresylic Acid
• Effective Date: 01-Jun-2020
• Refers: ASTM D6809-02(2016) - Standard Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
• Effective Date: 01-Nov-2016
• Refers: ASTM D3852-16 - Standard Practice for Sampling and Handling Phenol, Cresols, and Cresylic Acid
• Effective Date: 01-Jun-2016
• Refers: ASTM D4790-14 - Standard Terminology of Aromatic Hydrocarbons and Related Chemicals
• Effective Date: 01-Jul-2014
• Refers: ASTM E691-13 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-May-2013
• Refers: ASTM D3852-07(2012) - Standard Practice for Sampling and Handling Phenol, Cresols, and Cresylic Acid
• Effective Date: 01-Jun-2012
• Refers: ASTM E691-11 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Nov-2011
• Refers: ASTM D4790-11 - Standard Terminology of Aromatic Hydrocarbons and Related Chemicals
• Effective Date: 01-Feb-2011
• Refers: ASTM E29-08 - Standard Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
• Effective Date: 01-Oct-2008
• Refers: ASTM E691-08 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Oct-2008
• Refers: ASTM D4790-07 - Standard Terminology of Aromatic Hydrocarbons and Related Chemicals
• Effective Date: 15-Jul-2007
• Refers: ASTM D6809-02(2007) - Standard Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
• Effective Date: 01-Jun-2007
• Refers: ASTM D3852-07 - Standard Practice for Sampling and Handling Phenol, Cresols, and Cresylic Acid
• Effective Date: 01-Jan-2007
• Refers: ASTM E29-06b - Standard Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
• Effective Date: 15-Nov-2006
• Refers: ASTM E29-06a - Standard Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
• Effective Date: 15-Sep-2006

Overview

ASTM D5310-23: Standard Test Method for Tar Acid Composition by Capillary Gas Chromatography is a key standard for the quantitative analysis of phenol and its homologues in commercial tar acid and cresylic acid mixtures. Developed by ASTM International, this test method utilizes capillary gas chromatography to determine the homolog distribution within these mixtures, offering significant value for both producers and users concerned with quality control and specification conformance.

This standard is applicable for analyzing tar acid mixtures in industrial and specialty chemical contexts, providing normalized data for key constituents such as phenol, cresols, and xylenols. The method is widely adopted for routine quality assurance, regulatory compliance, and process optimization in sectors handling aromatic hydrocarbons.

Key Topics

• Test Method Scope

  • Covers quantitative determination of phenol and various homologues (including cresols and xylenols) in tar acid and cresylic acid mixtures.
  • Does not provide an absolute assay; the method normalizes detected components and excludes water and other compounds not sensed by the flame ionization detector.

• Analytical Procedure

  • Utilizes capillary gas chromatography with an appropriate column and detector, typically a flame ionization detector (FID).
  • Involves calibration using standards of known composition to determine response factors.
  • Sample analysis calculates mass percent composition from individual chromatographic peak areas.

• Precision and Quality Control

  • Specifies criteria for intermediate precision and interlaboratory reproducibility, ensuring reliability of results.
  • Encourages regular use of quality assurance and quality control practices, including instrument validation and interlaboratory comparison.

• Safety and Compliance

  • Users must adhere to current OSHA regulations, material safety data sheets, and local environmental and safety practices.
  • The standard recommends performing hazard assessments according to regulatory requirements.

Applications

ASTM D5310-23 is widely used in:

• Quality Control
  Producers and users of tar acids, cresylic acids, and related aromatic chemicals rely on this standard to monitor product composition, ensuring conformance to internal and customer specifications.

• Specification Testing
  Enables suppliers and customers to verify product consistency and compliance with contractual or regulatory requirements, supporting traceability and accountability.

• Process Optimization
  Chemical production facilities use the data from this test method for product development, process monitoring, and troubleshooting within production lines that handle tar acids and phenolic mixtures.

• Regulatory Compliance
  Laboratories reference this standard in documentation and reporting for regulatory submissions, helping to meet international trade and safety guidelines.

Related Standards

The ASTM D5310-23 test method references several related standards and practices, enhancing laboratory methodologies and compliance:

• ASTM D3852 - Practice for Sampling and Handling Phenol, Cresols, and Cresylic Acid
• ASTM D4790 - Terminology of Aromatic Hydrocarbons and Related Chemicals
• ASTM D6809 - Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
• ASTM E29 - Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
• ASTM E691 - Practice for Conducting an Interlaboratory Study to Determine Precision of a Test Method

Keywords

tar acid, capillary gas chromatography, phenol, cresol, xylenols, cresylic acid, commercial tar acids, quality control, specification testing, ASTM D5310, aromatic chemicals, laboratory testing standards, chemical analysis, industrial chemicals.

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By following ASTM D5310-23, laboratories and chemical producers can achieve consistent, accurate, and regulatory-compliant analysis of tar acid compositions, supporting both operational efficiency and product quality assurance.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D5310 − 23
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* D6809 Guide for Quality Control and Quality Assurance
Procedures for Aromatic Hydrocarbons and Related Ma-
1.1 This test method covers the quantitative determination
terials
of phenol and certain homologues of phenol in tar acid and
E29 Practice for Using Significant Digits in Test Data to
cresylic acid mixtures using capillary gas chromatography. It is
Determine Conformance with Specifications
a normalization test method that determines homolog distribu-
E691 Practice for Conducting an Interlaboratory Study to
tion but is not an absolute assay since it does not account for
Determine the Precision of a Test Method
water or other compounds not detected by a flame ionization
detector. 2.2 Other Documents:
OSHA Regulations, 29 CFR paragraphs 1910.1000, and
1.2 In determining the conformance of the test results using
1910.1200 Air contaminants – table of exposure limits
this method to applicable specifications, results shall be
and hazard communication
rounded off in accordance with the rounding-off method of
Practice E29.
3. Terminology
1.3 The values stated in SI units are to be regarded as
3.1 For definitions of terms used in this test method see
standard. No other units of measurement are included in this
Terminology D4790.
standard.
1.4 This standard does not purport to address all of the
4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
4.1 The sample composition is determined by capillary gas
responsibility of the user of this standard to establish appro-
chromatography. The mass percent composition is calculated
priate safety, health, and environmental practices and deter-
from the ratio of the individual peak areas to the total area of
mine the applicability of regulatory limitations prior to use.
all peaks using appropriate response factors determined for
For specific hazard statements, see Section 8.
each component by means of a calibration sample.
1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard-
5. Significance and Use
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
5.1 This test method is suitable for the general quantitative
mendations issued by the World Trade Organization Technical
analysis of commercial tar acid mixtures. It may be used as a
Barriers to Trade (TBT) Committee.
tool for quality control and specification purposes by producers
and users.
2. Referenced Documents
2.1 ASTM Standards:
6. Apparatus
D3852 Practice for Sampling and Handling Phenol, Cresols,
6.1 Chromatograph—A gas chromatograph compatible with
and Cresylic Acid
capillary columns, equipped with inlet splitter and high tem-
D4790 Terminology of Aromatic Hydrocarbons and Related
perature flame ionization detector. Typical Operating Condi-
Chemicals
tions are given in Table 1.
1 6.2 Peak Integrator—Electronic integration is the minimum
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi-
requirement.
bility of Subcommittee D16.02 on Oxygenated Aromatics.
6.3 Microsyringe, capacity of 1 μL.
Current edition approved April 1, 2023. Published June 2023. Originally
approved in 1994. Last previous edition approved in 2018 as D5310 – 10 (2018).
DOI: 10.1520/D5310-23.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Available from U.S. Government Printing Office Superintendent of Documents,
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
D5310 − 23
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 is required for optimal performance of the FID detector when used with capillary columns. 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
column temperatures are kept cooler, close to 100 °C to help keep the
DIDP phase on the column and wet samples are dried first by running it
through a drying tube filled with calcium carbonate. It is almost always a
custom product.
7. Reagents and Materials
7.1 Calibration Standards—Samples of known composition
representative of samples to be analyzed. It is typically a QA
FIG. 2 Typical Chromatogram of Cresylic Acid on Column of 25 %
sample containing compounds of interested usually found in
Cyanopropyl, 25 % Phenyl, 50 % Methylpolysiloxane—Bonded on
Table 2 that can help identify peak co-eluters, peak handling,
Fused Silica
detector response, peak identification by RT, RRT, sensitivity,
number of theoretical plates of peaks and resolution of peaks.
6.4 Capillary Column—Any column capable of resolving
7.2 Equipment setup check sample to check peak
all components of interest. Prepared columns are commercially
identification, resolution and sensitivity. Used for new column
available from chromatography supply houses. Chromato-
evaluations.
grams from three columns are presented in Fig. 1, Fig. 2, and
Fig. 3. Peak identification is given in Table 2. The Diisodecyl
8. Hazards
Phthalate column must be used in case of a dispute.
8.1 Consult current OSHA regulations and suppliers’ safety
NOTE 1—There are limited commercial sources of a stock product for
data sheets, and local regulations for all materials used in this
the DIDP capillary columns. They are a coated column instead of the
bonded/cross linked phases like DB5, OV225 or Dex325 columns. The test method.
...

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.
Designation: D5310 − 10 (Reapproved 2018) D5310 − 23
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 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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use. For specific hazard statements, see Section 8.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
2.2 Other Documents:
OSHA Regulations, 29 CFR paragraphs 1910.1000, and 1910.1200 paragraphs 1910.1000, and 1910.1200Air contaminants –
table of exposure limits and hazard communication
3. Terminology
3.1 For definitiondefinitions of terms used in this test method see Terminology D4790.
This test method is under the jurisdiction of ASTM Committee D16 on Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsibility of
Subcommittee D16.02 on Oxygenated Aromatics.
Current edition approved Nov. 1, 2018April 1, 2023. Published November 2018June 2023. Originally approved in 1994. Last previous edition approved in 20142018 as
D5310 – 10 (2014).(2018). DOI: 10.1520/D5310-10R18.10.1520/D5310-23.
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 − 23
4. Summary of Test Method
4.1 The sample composition is determined by capillary gas chromatography. The weightmass 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.
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.the minimum requirement.
6.3 Recorder, with full scale response time of 1 s or less.
6.3 Microsyringe, capacity of 1 μL.
6.4 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. The Diisodecyl Phthalate column must be used in case of a dispute.
NOTE 1—There are limited commercial sources of a stock product for the DIDP capillary columns. They are a coated column instead of the bonded/cross
linked phases like DB5, OV225 or Dex325 columns. The column temperatures are kept cooler, close to 100 °C to help keep the DIDP phase on the column
and wet samples are dried first by running it through a drying tube filled with calcium carbonate. It is almost always a custom product.
7. Reagents and Materials
7.1 Calibration Standards—Samples of known composition representative of samples to be analyzed. It is typically a QA sample
containing compounds of interested usually found in Table 2 that can help identify peak co-eluters, peak handling, detector
response, peak identification by RT, RRT, sensitivity, number of theoretical plates of peaks and resolution of peaks.
7.2 Equipment setup check sample to check peak identification, resolution and sensitivity. Used for new column evaluations.
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 is required for optimal performance
of the FID detector when used with capillary columns. Each instrument should be optimized according to manufacturer’s recommendations.
D5310 − 23
FIG. 1 Typical Chromatogram of Cresylic Acid on
Column of Diisodecyl Phthalate on Fused Silica
FIG. 2 Typical Chromatogram of Cresylic Acid on Column of 25 % Cyanopropyl, 25 % Phenyl, 50 % Methylpolysiloxane—Bonded on
Fused Silica
FIG. 3 Typical Chromatogram of Cresylic Acid on Column of 95 % Dimethyl, 5 % Diphenyl Polysiloxane Bonded on Fused Silica
8. Hazards
8.1 Consult current OSHA regulations and suppliers’ safety
...