ISO 13741-1:2023

Plastics/rubber - Determination of residual monomers and other organic components by capillary-column gas chromatography - Part 1: Direct liquid injection method

This document specifies a method for the determination of residual monomers and other (saturated) organic components in aqueous polymer dispersions and latices as well as in related products. It makes use of capillary-column gas chromatography with direct injection of the liquid sample. Residual monomers and saturated volatiles that have been successfully determined by this method include acrylic and methacrylic esters, acrylonitrile, butadiene, styrene, vinyl acetate, vinyl chloride as well as by-products such as acetaldehyde and ethylbenzene.

Plastiques/caoutchouc — Détermination des monomères résiduels et autres constituants organiques par chromatographie en phase gazeuse sur colonne capillaire — Partie 1: Méthode d'injection liquide directe

General Information

• Status: Published
• Publication Date: 25-Jan-2023
• ICS: 83.040.10 - Latex and raw rubber
• ICS: 83.080.01 - Plastics in general
• Technical Committee: ISO/TC 61/SC 9 - Thermoplastic materials
• Drafting Committee: ISO/TC 61/SC 9/WG 14 - Polymer dispersions
• Current Stage: 6060 - International Standard published
• Start Date: 26-Jan-2023
• Due Date: 27-Sep-2022
• Completion Date: 26-Jan-2023

Relations

• Revises: ISO 13741-1:1998 - Plastics/rubber - Polymer dispersions and rubber latices (natural and synthetic) - Determination of residual monomers and other organic components by capillary-column gas chromatography - Part 1: Direct liquid injection method
• Effective Date: 23-Apr-2020

Overview

ISO 13741-1:2023 - "Plastics/rubber - Determination of residual monomers and other organic components by capillary-column gas chromatography - Part 1: Direct liquid injection method" specifies a validated analytical procedure for measuring residual monomers and saturated volatile organics in aqueous polymer dispersions and latices. The method uses capillary-column gas chromatography (GC) with direct liquid injection and flame ionization detection (FID) to quantify trace volatile compounds relevant to health, safety and regulatory compliance.

Key topics and technical requirements

• Analytes covered: acrylic and methacrylic esters (e.g. methyl acrylate, n-butyl acrylate), acrylonitrile, 1,3-butadiene, styrene, vinyl acetate, vinyl chloride, and by-products such as acetaldehyde and ethylbenzene.
• Principle: dilute sample with a water-based internal standard solution and inject ~1 µL onto a capillary GC column; separate components under linear temperature programming and detect with FID.
• Instrumentation: split injection port with a liner, capillary column (30 m, ID 0.25–0.53 mm, 1–5 µm dimethylpolysiloxane film), FID, and chromatography data system/integrator. Typical operating conditions are provided (e.g., injector 150–200 °C, detector 250 °C, initial column 50 °C, program 5 °C/min).
• Reagents and internal standard: propionitrile (recommended internal standard, 990 g/kg); solvents such as dimethylformamide (DMF) or tetrahydrofuran (THF); carrier gases (nitrogen, helium or hydrogen at high purity).
• Calibration and calculation: determine response factors by injecting known masses of analyte with the internal standard; quantify sample concentrations using the prescribed response-factor calculation.
• Performance: detection limit reported as 10 mg/kg (report values below this as <10 mg/kg). Duplicate agreement within 15 % and repeatability about 30 %. Reproducibility is not yet established.

Practical applications

• Quality control in polymer-dispersion production (paints, adhesives, coatings) to monitor residual monomers and ensure product safety and regulatory compliance.
• Regulatory testing for VOC and residual monomer limits in consumer and industrial products.
• Research & development for polymer formulation optimization and process improvements to reduce volatile residuals.
• Contract testing laboratories offering accredited GC analysis of dispersions and latices.

Who should use this standard

• Analytical chemists, QC laboratories, process engineers, test laboratories, and regulatory bodies working with aqueous polymer dispersions, latices and related products.

Related standards

• ISO 3899 (historical distillation/titration methods; ISO 13741-1 is intended where more precise GC measurement is required)
• ISO 3696 (water for analytical laboratory use - referenced for reagent water quality)
• Full list of ISO 13741 parts available on the ISO website.

Keywords: ISO 13741-1:2023, residual monomers, capillary-column gas chromatography, direct liquid injection, polymer dispersions, latices, GC-FID, propionitrile, VOC detection.

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 13741-1
Second edition
2023-01
Plastics/rubber — Determination of
residual monomers and other organic
components by capillary-column gas
chromatography —
Part 1:
Direct liquid injection method
Reference number
© ISO 2023
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
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Published in Switzerland
ii
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative reference .1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 2
6 Apparatus . 2
7 Preparation of apparatus .2
8 Calibration .3
9 Procedure .5
10 Calculation . 5
11 Precision . 7
12 Test report . 8
Bibliography . 9
iii
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
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ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
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For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to
the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see
www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 9,
Thermoplastic materials.
This second edition cancels and replaces the first edition (ISO 13741-1:1998), which has been technically
revised.
The main changes are as follows:
— the title has been modified to 3 elements from 4 elements;
— part of the Scope (1.3) has been removed;
— Clause 3, Terms and definitions, has been added and subsequent clauses have been renumbered;
— Formulae (1) and (2) have been numbered.
A list of all parts in the ISO 13741-1 series can be found on the ISO website.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.
iv
Introduction
The requirements imposed today by authorities include the assessment of the content of residual
monomers and organic saturated volatiles, for health and environmental reasons sometimes down
to minute traces. Former standards for measurement of residual volatiles based on distillation linked
with titration cannot cope with such exigences.
This document presents an advanced method for the determination, by gas chromatography, of residual
monomers and other organic components in polymer dispersions and lattices. It provides a method
that is in line with present-day requirements for analytical methods, and is intended for use instead of
ISO 3899, where precise measurements of volatile-matter content are needed, and expands their scope
to include other volatile organic components.
v
INTERNATIONAL STANDARD ISO 13741-1:2023(E)
Plastics/rubber — Determination of residual monomers
and other organic components by capillary-column gas
chromatography —
Part 1:
Direct liquid injection method
WARNING — This document does not purport to address all of the safety problems, if any,
associated with its use. It is the responsibility of the user of this document to establish
appropriate safety and health practices and determine the applicability of regulatory limitations
prior to use.
1 Scope
1.1 This document specifies a method for the determination of residual monomers and other
(saturated) organic components in aqueous polymer dispersions and latices as well as in related
products. It makes use of capillary-column gas chromatography with direct injection of the liquid
sample.
1.2 Residual monomers and saturated volatiles that have been successfully determined by this
method include acrylic and methacrylic esters, acrylonitrile, butadiene, styrene, vinyl acetate, vinyl
chloride as well as by-products such as acetaldehyde and ethylbenzene.
2 Normative reference
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 3696, Water for analytical laboratory use — Specification and test methods
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
4 Principle
A test sample is diluted with water containing an inte
...