ASTM D3465-21

Standard Guide for Purity of Monomeric Plasticizers by Gas Chromatography

SIGNIFICANCE AND USE
5.1 Infrared techniques frequently cannot detect low-level materials. Gas chromatographic methods possess higher sensitivity and are used to extend limits of detection.  
5.2 It is expected that this guide will be suitable for specifications, manufacturing control, and research and development. An area percent method of determining concentration of the components shall be used if the area percent of the plasticizer is 99.0 % or higher. However, if the area percent of the plasticizer is less than 99.0 % or if any question were to arise about the data, an internal standard shall be used.  
5.3 Impurities potentially found in monomeric plasticizers include alcohols, dibasic acids, and monoesters.
SCOPE
1.1 This gas chromatographic guide covers a procedure for extending the range of purity determination of monomeric plasticizers beyond that now determined by other methods. Due to the need to volatilize the plasticizer, only monomeric plasticizers having definitive boiling points and a molecular weight less than 1000 Daltons, such as dioctyl phthalate, are applicable to this guide.  
1.2 The values in SI units are to be regarded as standard.  
1.3 The text of this guide references notes and footnotes that provide explanatory material. These notes and footnotes (excluding those in tables and figures) are not to be considered as requirements of this guide.  
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. Specific precautionary statements are given in Section 9.
Note 1: There is no known ISO equivalent to this standard.  
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: 30-Jun-2021
• ICS: 83.040.30 - Auxiliary materials and additives for plastics
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.70 - Analytical Methods

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: D3465 − 21
Standard Guide for
1
Purity of Monomeric Plasticizers by Gas Chromatography
This standard is issued under the fixed designation D3465; 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* D2124 Test Method forAnalysis of Components in Poly(Vi-
nyl Chloride) Compounds Using an Infrared Spectropho-
1.1 This gas chromatographic guide covers a procedure for
3
tometric Technique (Withdrawn 2020)
extending the range of purity determination of monomeric
E177 Practice for Use of the Terms Precision and Bias in
plasticizers beyond that now determined by other methods.
ASTM Test Methods
Due to the need to volatilize the plasticizer, only monomeric
E260 Practice for Packed Column Gas Chromatography
plasticizers having definitive boiling points and a molecular
E355 Practice for Gas Chromatography Terms and Relation-
weight less than 1000 Daltons, such as dioctyl phthalate, are
ships
applicable to this guide.
E594 Practice for Testing Flame Ionization Detectors Used
1.2 The values in SI units are to be regarded as standard.
in Gas or Supercritical Fluid Chromatography
1.3 Thetextofthisguidereferencesnotesandfootnotesthat E1510 Practice for Installing Fused Silica Open Tubular
Capillary Columns in Gas Chromatographs
provide explanatory material. These notes and footnotes (ex-
cluding those in tables and figures) are not to be considered as IEEE/ASTM SI-10 Practice for Use of the International
System of Units (SI), the Modernized Metric System
requirements of this guide.
1.4 This standard does not purport to address all of the
3. Terminology
safety concerns, if any, associated with its use. It is the
3.1 Definitions:
responsibility of the user of this standard to establish appro-
3.1.1 General—Definitions are in accordance with Termi-
priate safety, health, and environmental practices and deter-
nology D883 and Terminology D1600 unless otherwise indi-
mine the applicability of regulatory limitations prior to use.
cated.
Specific precautionary statements are given in Section 9.
3.1.2 All gas chromatography terms and relationships used
NOTE 1—There is no known ISO equivalent to this standard.
in this guide are consistent with, or refer to, Practice E355.
1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard-
4. Summary of Guide
ization established in the Decision on Principles for the
4.1 Atestportionoftheplasticizertobeanalyzedisinjected
Development of International Standards, Guides and Recom-
onto a gas chromatographic column and separated into its
mendations issued by the World Trade Organization Technical
components, which are sensed by the detector and quantified
Barriers to Trade (TBT) Committee.
byanelectronicdataacquisitionsystem(computer).Thepurity
is based on the percent total area response of the principal
2. Referenced Documents
peak(s). All other components are impurities.
2
2.1 ASTM Standards:
5. Significance and Use
D883 Terminology Relating to Plastics
D1600 Terminology forAbbreviatedTerms Relating to Plas-
5.1 Infrared techniques frequently cannot detect low-level
tics
materials. Gas chromatographic methods possess higher sensi-
tivity and are used to extend limits of detection.
5.2 It is expected that this guide will be suitable for
1
This guide is under the jurisdiction of ASTM Committee D20 on Plastics and
specifications, manufacturing control, and research and devel-
is the direct responsibility of Subcommittee D20.70 on Analytical Methods (Section
D20.70.02). opment. An area percent method of determining concentration
Current edition approved July 1, 2021. Published July 2021. Originally approved
of the components shall be used if the area percent of the
in 1975. Last previous edition approved in 2014 as D3465 - 14. DOI: 10.1520/
plasticizer is 99.0 % or higher. However, if the area percent of
D3465-21.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.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 ------------
...

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: D3465 − 14 D3465 − 21
Standard Test Method Guide for
1
Purity of Monomeric Plasticizers by Gas Chromatography
This standard is issued under the fixed designation D3465; 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 gas chromatographic test method covers a procedure for extending the range of purity determination of monomeric
plasticizers beyond that now determined by other methods. Due to the need to volatilize the plasticizer, only monomeric
plasticizers having definitive boiling points and a molecular weight less than 1000 Daltons, such as dioctyl phthalate, are applicable
to this test method.
1.2 The values in SI units are to be regarded as standard.
1.3 The text of this test method references notes and footnotes that provide explanatory material. These notes and footnotes
(excluding those in tables and figures) are not to be considered as requirements of this test method.
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. Specific precautionary statements are given in Section 9
NOTE 1—There is no known ISO equivalent to this standard.
2. Referenced Documents
2
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
D1600 Terminology for Abbreviated Terms Relating to Plastics
D2124 Test Method for Analysis of Components in Poly(Vinyl Chloride) Compounds Using an Infrared Spectrophotometric
3
Technique (Withdrawn 2020)
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E260 Practice for Packed Column Gas Chromatography
E355 Practice for Gas Chromatography Terms and Relationships
E594 Practice for Testing Flame Ionization Detectors Used in Gas or Supercritical Fluid Chromatography
E1510 Practice for Installing Fused Silica Open Tubular Capillary Columns in Gas Chromatographs
IEEE/ASTM SI-10 Practice for Use of the International System of Units (SI), the Modernized Metric System
1
This test method guide is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.70 on Analytical Methods
(Section D20.70.02).
Current edition approved March 1, 2014July 1, 2021. Published March 2014July 2021. Originally approved in 1975. Last previous edition approved in 20072014 as
ε1
D3465 - 00(2007)D3465 - 14. . DOI: 10.1520/D3465-14.10.1520/D3465-21.
2
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.
3
The last approved version of this historical standard is referenced on www.astm.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 ----------------------
D3465 − 21
3. Terminology
3.1 Definitions:
3.1.1 General—Definitions are in accordance with Terminology D883 and Terminology D1600 unless otherwise indicated.
3.1.2 All gas chromatography terms and relationships used in this test method are consistent with, or refer to, Practice E355.
4. Summary of Test Method
4.1 A test portion of the plasticizer to be analyzed is injected onto a gas chromatographic column and separated into its
components, which are sensed by the detector and quantified by an electronic data acquisition system (computer) or an integrator.
The purity is based on the total area response of the principal peak(s). All other components are impurities.
5. Significance and Use
5.1 Infrared techniques frequently cannot detect low-level materials. Gas chromatographic methods possess higher sensitivity, and
are used to extend limits of detection.
5.2 It is expected that this test method will be suitable for specifications, manufacturing control, and research and development.
An area percent method of determining concentration of the components shall be used if the area percent of the plasticizer is
99.0 % or higher. However, if the area percent of the plasticizer is less than 99.0 % or if
...