ISO 21257:2018
(Main)Plastics — Polymer polyols for use in the production of polyurethane — Determination of the residual acrylonitrile and styrene monomer content by gas chromatography
Plastics — Polymer polyols for use in the production of polyurethane — Determination of the residual acrylonitrile and styrene monomer content by gas chromatography
This document specifies a method for the determination of the residual acrylonitrile monomer and styrene monomer in polymer polyols by gas chromatography.
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INTERNATIONAL ISO
STANDARD 21257
First edition
2018-10
Plastics — Polymer polyols for use
in the production of polyurethane
— Determination of the residual
acrylonitrile and styrene monomer
content by gas chromatography
Reference number
©
ISO 2018
© ISO 2018
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2018 – All rights reserved
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents and materials . 2
6 Apparatus . 2
7 Preparation of calibration solution and sample solution . 3
7.1 General . 3
7.2 Method A for using OT column . 3
7.2.1 Preparation of internal standard solution . 3
7.2.2 Preparation of calibration solutions . 3
7.2.3 Preparation of sample solution . 4
7.3 Method B for using packed column . 4
7.3.1 Preparation of internal standard solution . 4
7.3.2 Preparation of calibration solutions . 4
7.3.3 Preparation of sample solution . 4
8 Procedure. 5
8.1 Gas chromatographic procedure . 5
8.2 Measurement of sample solutions and calibration solutions . 5
8.3 Evaluation of gas chromatographic peak . 6
9 Expression of the results . 6
9.1 Preparation of the calibration curve . 6
9.2 Calculation of results from a calibration graph . 7
9.3 Calculation of results from a single-point calibration . 8
9.4 Acceptability of results and measurement sensitivity . 9
10 Precision . 9
11 Test report . 9
Annex A (informative) Typical analytical conditions .10
Annex B (informative) Typical examples of GC chromatogram .12
Annex C (informative) Precision .14
Bibliography .15
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
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
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
constitute an endorsement.
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 12,
Thermosetting materials.
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 © ISO 2018 – All rights reserved
Introduction
Polymer polyols are defined as very fine and stable dispersions of solid, vinylic polymers (for example,
acrylonitrile/styrene copolymers are typical) in liquid polyether polyols.
Polymer polyol is used to improve the physical properties of seat cushions, especially hardness. Because
the toxicity of acrylonitrile and styrene is high, it is important to establish an analytical method to
determine residual amounts of these reactants.
The importance of residual toxicity has increased with the use of polyurethane foam, etc. which comes
in contact with food and skin. This document is intended to help manufacturers evaluate the safety of
their products.
Annexes A, B and C complement the main body of this document and not meant to be a normative part
of this document.
INTERNATIONAL STANDARD ISO 21257:2018(E)
Plastics — Polymer polyols for use in the production
of polyurethane — Determination of the residual
acrylonitrile and styrene monomer content by gas
chromatography
1 Scope
This document specifies a method for the determination of the residual acrylonitrile monomer and
styrene monomer in polymer polyols by gas chromatography.
2 Normative references
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 472, Plastics — Vocabulary
ISO 648, Laboratory glassware — Single-volume pipettes
ISO 1042, Laboratory glassware — One-mark volumetric flasks
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 472 apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https: //www .iso .org/obp
— IEC Electropedia: available at http: //www .electropedia .org/
4 Principle
The polymer polyol sample is dissolved in a suitable solvent. This sample solution is then analysed using
gas chromatography with internal standardization. The amounts of residual acrylonitrile monomer and
styrene monomer are determined from peak areas using a previously established calibration curve.
NOTE Because of the high molecular weight of substances which are part of the polymer polyol, and because
these are injected directly into the chromatograph, injector contamination can occur which will lead to erroneous
results.
Monitor the condition of the chromatographic parts and clean or replace as necessary.
An injector liner packed with glass wool has been used to improve vaporization and ease of cleaning.
5 Reagents and materials
5.1 Solvent, use analytical-grade methanol, N, N-dimethylformamide, tetrahydrofuran, dipropylene
glycol monomethyl ether or toluene.
Other solvents can also be used if suitable results are obtained for the retention time, thermal stability
and separation performance.
5.2 Internal standard, shall be selected based on the retention times of the volatile materials
contained in the polymer polyol sample and the solvent.
Recommended combinations of solvent from 5.1 and internal standard are methanol and 2-methyl-
1-propanol, N, N-dimethylformamide and ethylbenzene, dipropylene glycol monomethyl ether and
bromobenzene.
Other combinations are also possible if the retention times, thermal stability and separation
performance are suitable.
5.3 Carrier gases and fuel gases for gas chromatograph.
Use helium or nitrogen as carrier gas, hydrogen as fuel gas, dry air as supporting fuel gas.
6 Apparatus
Normal laboratory equipment and the following apparatus are required.
6.1 Gas chromatograph, with flame ionization detector and capable of employing packed or open
tubular columns with either split or splitless injector. Typical operating conditions are described in
Annex A.
6.1.1 Injection port, for liquid samples.
When using open tubular column (hereafter called an OT column), an injection port with splitter may
be applicable.
6.1.2 Column and packing material.
The column diameter and length, as well as the packing material and liquid phase, are to be selected
based on consideration of column resolution (Re) and calibration curve linearity. Both packed columns
and OT (capillary) columns (hereafter referred to as OT columns) are acceptable.
Typical columns are described in Annex A.
— OT columns: The OT column are to be selected from suitable manufacturer(s), and then shall be
conditioned sufficiently.
— Packed columns: The packed column should be packed with the liquid phase and support particles
from suitable manufacturer(s), and then conditioned sufficiently.
6.1.3 Detector, hydrogen flame ionization detector (hereafter referred to as FID).
6.2 Data processor, selected based on suitability for recording the signals from the detector and
processing the chromatograms.
6.3 Sample injection syringe, micro
...
INTERNATIONAL ISO
STANDARD 21257
First edition
2018-10
Plastics — Polymer polyols for use
in the production of polyurethane
— Determination of the residual
acrylonitrile and styrene monomer
content by gas chromatography
Reference number
©
ISO 2018
© ISO 2018
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2018 – All rights reserved
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents and materials . 2
6 Apparatus . 2
7 Preparation of calibration solution and sample solution . 3
7.1 General . 3
7.2 Method A for using OT column . 3
7.2.1 Preparation of internal standard solution . 3
7.2.2 Preparation of calibration solutions . 3
7.2.3 Preparation of sample solution . 4
7.3 Method B for using packed column . 4
7.3.1 Preparation of internal standard solution . 4
7.3.2 Preparation of calibration solutions . 4
7.3.3 Preparation of sample solution . 4
8 Procedure. 5
8.1 Gas chromatographic procedure . 5
8.2 Measurement of sample solutions and calibration solutions . 5
8.3 Evaluation of gas chromatographic peak . 6
9 Expression of the results . 6
9.1 Preparation of the calibration curve . 6
9.2 Calculation of results from a calibration graph . 7
9.3 Calculation of results from a single-point calibration . 8
9.4 Acceptability of results and measurement sensitivity . 9
10 Precision . 9
11 Test report . 9
Annex A (informative) Typical analytical conditions .10
Annex B (informative) Typical examples of GC chromatogram .12
Annex C (informative) Precision .14
Bibliography .15
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
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
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
constitute an endorsement.
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 12,
Thermosetting materials.
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 © ISO 2018 – All rights reserved
Introduction
Polymer polyols are defined as very fine and stable dispersions of solid, vinylic polymers (for example,
acrylonitrile/styrene copolymers are typical) in liquid polyether polyols.
Polymer polyol is used to improve the physical properties of seat cushions, especially hardness. Because
the toxicity of acrylonitrile and styrene is high, it is important to establish an analytical method to
determine residual amounts of these reactants.
The importance of residual toxicity has increased with the use of polyurethane foam, etc. which comes
in contact with food and skin. This document is intended to help manufacturers evaluate the safety of
their products.
Annexes A, B and C complement the main body of this document and not meant to be a normative part
of this document.
INTERNATIONAL STANDARD ISO 21257:2018(E)
Plastics — Polymer polyols for use in the production
of polyurethane — Determination of the residual
acrylonitrile and styrene monomer content by gas
chromatography
1 Scope
This document specifies a method for the determination of the residual acrylonitrile monomer and
styrene monomer in polymer polyols by gas chromatography.
2 Normative references
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 472, Plastics — Vocabulary
ISO 648, Laboratory glassware — Single-volume pipettes
ISO 1042, Laboratory glassware — One-mark volumetric flasks
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 472 apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https: //www .iso .org/obp
— IEC Electropedia: available at http: //www .electropedia .org/
4 Principle
The polymer polyol sample is dissolved in a suitable solvent. This sample solution is then analysed using
gas chromatography with internal standardization. The amounts of residual acrylonitrile monomer and
styrene monomer are determined from peak areas using a previously established calibration curve.
NOTE Because of the high molecular weight of substances which are part of the polymer polyol, and because
these are injected directly into the chromatograph, injector contamination can occur which will lead to erroneous
results.
Monitor the condition of the chromatographic parts and clean or replace as necessary.
An injector liner packed with glass wool has been used to improve vaporization and ease of cleaning.
5 Reagents and materials
5.1 Solvent, use analytical-grade methanol, N, N-dimethylformamide, tetrahydrofuran, dipropylene
glycol monomethyl ether or toluene.
Other solvents can also be used if suitable results are obtained for the retention time, thermal stability
and separation performance.
5.2 Internal standard, shall be selected based on the retention times of the volatile materials
contained in the polymer polyol sample and the solvent.
Recommended combinations of solvent from 5.1 and internal standard are methanol and 2-methyl-
1-propanol, N, N-dimethylformamide and ethylbenzene, dipropylene glycol monomethyl ether and
bromobenzene.
Other combinations are also possible if the retention times, thermal stability and separation
performance are suitable.
5.3 Carrier gases and fuel gases for gas chromatograph.
Use helium or nitrogen as carrier gas, hydrogen as fuel gas, dry air as supporting fuel gas.
6 Apparatus
Normal laboratory equipment and the following apparatus are required.
6.1 Gas chromatograph, with flame ionization detector and capable of employing packed or open
tubular columns with either split or splitless injector. Typical operating conditions are described in
Annex A.
6.1.1 Injection port, for liquid samples.
When using open tubular column (hereafter called an OT column), an injection port with splitter may
be applicable.
6.1.2 Column and packing material.
The column diameter and length, as well as the packing material and liquid phase, are to be selected
based on consideration of column resolution (Re) and calibration curve linearity. Both packed columns
and OT (capillary) columns (hereafter referred to as OT columns) are acceptable.
Typical columns are described in Annex A.
— OT columns: The OT column are to be selected from suitable manufacturer(s), and then shall be
conditioned sufficiently.
— Packed columns: The packed column should be packed with the liquid phase and support particles
from suitable manufacturer(s), and then conditioned sufficiently.
6.1.3 Detector, hydrogen flame ionization detector (hereafter referred to as FID).
6.2 Data processor, selected based on suitability for recording the signals from the detector and
processing the chromatograms.
6.3 Sample injection syringe, micro
...
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