ASTM D7884-24
(Test Method)Standard Test Method for Determination of 4-Carboxybenzaldehyde and p-Toluic Acid in Purified Terephthalic Acid by Reverse Phase High Performance Liquid Chromatography
Standard Test Method for Determination of 4-Carboxybenzaldehyde and <emph type="bdit" >p</emph>-Toluic Acid in Purified Terephthalic Acid by Reverse Phase High Performance Liquid Chromatography
SIGNIFICANCE AND USE
4.1 The presence of 4-CBA and p-TOL in PTA used for the production of polyester is undesirable because they can affect the PET quality (such as contribute to fiber breaks), the polymerization process, and 4-CBA imparts coloration to the polymer due to thermal instability.
4.2 Determining the amount of 4-CBA and p-TOL remaining from the manufacture of PTA is often required. This test method is suitable for setting specifications and for use as an internal quality control tool where these products are produced or are used.
SCOPE
1.1 This test method covers the determination of the 4-Carboxybenzaldehyde (4-CBA) and p-Toluic acid (p-TOL) in purified terephthalic acid (PTA) by reverse phase high performance liquid chromatography (HPLC). This method is applicable for 4-CBA and p- TOL with an upper limit of 500 mg/kg, respectively, but may be applicable to a wider range.
1.2 In determining the conformance of the test results using this method to applicable specification, 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 7.
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.
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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: D7884 − 24
Standard Test Method for
Determination of 4-Carboxybenzaldehyde and p-Toluic Acid
in Purified Terephthalic Acid by Reverse Phase High
1
Performance Liquid Chromatography
This standard is issued under the fixed designation D7884; 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 determination of the
terials
4-Carboxybenzaldehyde (4-CBA) and p-Toluic acid (p-TOL)
E29 Practice for Using Significant Digits in Test Data to
in purified terephthalic acid (PTA) by reverse phase high
Determine Conformance with Specifications
performance liquid chromatography (HPLC). This method is
E691 Practice for Conducting an Interlaboratory Study to
applicable for 4-CBA and p- TOL with an upper limit of
Determine the Precision of a Test Method
500 mg ⁄kg, respectively, but may be applicable to a wider
3
2.2 ISO Document:
range.
EN ISO 8213 Chemical products for industrial use—
1.2 In determining the conformance of the test results using
Sampling techniques—Solid chemical products in the
this method to applicable specification, results shall be rounded
form of particles varying from powders to coarse lumps
off in accordance with the rounding-off method of Practice
4
2.3 Other Document:
E29.
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
1.3 The values stated in SI units are to be regarded as
1910.1200
standard. No other units of measurement are included in this
3. Summary of Test Method
standard.
1.4 This standard does not purport to address all of the 3.1 Reverse Phase HPLC Method—PTA sample is dissolved
safety concerns, if any, associated with its use. It is the in ammonium hydroxide solution, and a fixed volume of this
responsibility of the user of this standard to establish appro- solution is injected into a high performance liquid chromato-
priate safety, health, and environmental practices and deter- graph equipped with a UV detector. A C18 chemically bonded
mine the applicability of regulatory limitations prior to use.For column is used to separate the impurities 4-CBA and p-TOL
specific hazard statements, see Section 7. from PTA. The external standard calibration is used for
1.5 This international standard was developed in accor- quantification.
dance with internationally recognized principles on standard-
4. Significance and Use
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
4.1 The presence of 4-CBA and p-TOL in PTA used for the
mendations issued by the World Trade Organization Technical
production of polyester is undesirable because they can affect
Barriers to Trade (TBT) Committee.
the PET quality (such as contribute to fiber breaks), the
polymerization process, and 4-CBA imparts coloration to the
2. Referenced Documents
polymer due to thermal instability.
2
2.1 ASTM Standards:
4.2 Determining the amount of 4-CBA and p-TOL remain-
D1193 Specification for Reagent Water
ing from the manufacture of PTA is often required. This test
method is suitable for setting specifications and for use as an
1
This test method is under the jurisdiction of ASTM Committee D16 on
internal quality control tool where these products are produced
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi-
or are used.
bility of Subcommittee D16.02 on Oxygenated Aromatics.
Current edition approved March 1, 2024. Published March 2024. Originally
approved in 2013. Last previous edition approved in 2023 as D7884 – 23. DOI:
3
10.1520/D7884-24. Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 4th Floor, New York, NY 10036, http://www.ansi.org.
4
contact ASTM Customer Service at service@astm.org. 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
1
---------------------- Page: 1 ----------------------
D7884 − 24
5. Apparatus
...
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: D7884 − 23 D7884 − 24
Standard Test Method for
Determination of 4-Carboxybenzaldehyde and p-Toluic Acid
in Purified Terephthalic Acid by Reverse Phase High
1
Performance Liquid Chromatography
This standard is issued under the fixed designation D7884; 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*
1.1 This test method covers the determination of the 4-Carboxybenzaldehyde (4-CBA) and p-Toluic acid (p-TOL) in purified
terephthalic acid (PTA) by reverse phase high performance liquid chromatography (HPLC). This method is applicable for 4-CBA
and p- TOL with an upper limit of 500 mg ⁄kg, respectively, but may be applicable to a wider range.
1.2 In determining the conformance of the test results using this method to applicable specification, 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 7.
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
2.1 ASTM Standards:
D1193 Specification for Reagent Water
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
3
2.2 ISO Document:
EN ISO 8213 Chemical products for industrial use—Sampling techniques—Solid chemical products in the form of particles
varying from powders to coarse lumps
1
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, 2023March 1, 2024. Published March 2024. Originally approved in 2013. Last previous edition approved in 20202023 as
D7884 – 20.D7884 – 23. DOI: 10.1520/D7884-23.10.1520/D7884-24.
2
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 the ASTM website.
3
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
*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
1
---------------------- Page: 1 ----------------------
D7884 − 24
4
2.3 Other Document:
OSHA Regulations, 29 CFR paragraphs 1910.1000 and 1910.1200
3. Summary of Test Method
3.1 Reverse Phase HPLC Method—PTA sample is dissolved in ammonium hydroxide solution, and a fixed volume of this solution
is injected into a high performance liquid chromatograph equipped with a UV detector. A C18 chemically bonded column is used
to separate the impurities 4-CBA and p-TOL from PTA. The external standard calibration is used for quantification.
4. Significance and Use
4.1 The presence of 4-CBA and p-TOL in PTA used for the production of polyester is undesirable because they can affect the PET
quality (such as contribute to fiber breaks), the polymerization process, and 4-CBA imparts coloration to the polymer due to
thermal instability.
4.2 Determining the amount of 4-CBA and p-TOL remaining from the manufacture of PTA is often required. This test method is
suitable for setting specifications and for use as an internal quality control tool where these products are produced or are used.
5. Apparatus
5.1 High
...
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