ISO 16014-3:2019
(Main)Plastics — Determination of average molecular weight and molecular weight distribution of polymers using size-exclusion chromatography — Part 3: Low-temperature method
Plastics — Determination of average molecular weight and molecular weight distribution of polymers using size-exclusion chromatography — Part 3: Low-temperature method
This document specifies a method for determining the average molecular weight and the molecular weight distribution of polymers by size-exclusion chromatography (SEC) using an organic eluent at a temperature lower than 60 °C (see Annex A). The average molecular weight and the molecular weight distribution are calculated from a calibration curve prepared using polymer standards. Therefore, this test method is classified as a relative method (see ISO 16014-1).
Plastiques — Détermination de la masse moléculaire moyenne et de la distribution des masses moléculaires de polymères par chromatographie d'exclusion stérique — Partie 3: Mesurage aux basses températures
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INTERNATIONAL ISO
STANDARD 16014-3
Third edition
2019-05
Plastics — Determination of average
molecular weight and molecular
weight distribution of polymers using
size-exclusion chromatography —
Part 3:
Low-temperature method
Plastiques — Détermination de la masse moléculaire moyenne
et de la distribution des masses moléculaires de polymères par
chromatographie d'exclusion stérique —
Partie 3: Mesurage aux basses températures
Reference number
©
ISO 2019
© ISO 2019
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 2019 – All rights reserved
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 2
6 Apparatus . 2
7 Procedure. 3
7.1 Preparation of solutions of molecular weight standards . 3
7.2 Preparation of sample solutions . 4
7.3 Preparation of solutions for column performance evaluation . 4
7.4 Setting up the apparatus. 4
7.5 Operating parameters . 5
7.5.1 Flow rate . 5
7.5.2 Injection masses and injection volumes . 5
7.5.3 Column temperature . 5
7.5.4 Detector sensitivity . 5
7.6 Number of determinations . 5
8 Data acquisition and processing . 5
9 Expression of results . 6
10 Precision . 6
10.1 General . 6
10.2 Experimental conditions . 6
10.3 Results of interlaboratory tests . 7
11 Test report . 8
Annex A (informative) Further information on applicability of method . 9
Annex B (informative) Further information on reagents .10
Annex C (informative) Further information on interlaboratory tests .11
Bibliography .17
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 5, Physical-
chemical properties.
This third edition cancels and replaces the second edition (ISO 16014-3:2012), which has been
technically revised. The main changes compared to the previous edition are as follows:
— publication dates of references have been removed;
— molecular mass has been changed to molecular weight according to IUPAC rule.
A list of all parts in the ISO 16014 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 © ISO 2019 – All rights reserved
INTERNATIONAL STANDARD ISO 16014-3:2019(E)
Plastics — Determination of average molecular weight
and molecular weight distribution of polymers using size-
exclusion chromatography —
Part 3:
Low-temperature method
1 Scope
This document specifies a method for determining the average molecular weight and the molecular
weight distribution of polymers by size-exclusion chromatography (SEC) using an organic eluent at a
temperature lower than 60 °C (see Annex A). The average molecular weight and the molecular weight
distribution are calculated from a calibration curve prepared using polymer standards. Therefore, this
test method is classified as a relative method (see ISO 16014-1).
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 5725-1, Accuracy (trueness and precision) of measurement methods and results — Part 1: General
principles and definitions
ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results — Part 2: Basic method
for the determination of repeatability and reproducibility of a standard measurement method
ISO 16014-1, Plastics — Determination of average molecular weight and molecular weight distribution of
polymers using size-exclusion chromatography — Part 1: General principles
ISO 16014-2, Plastics — Determination of average molecular weight and molecular weight distribution of
polymers using size-exclusion chromatography — Part 2: Universal calibration method
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 472 and in ISO 16014-1 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
According to ISO 16014-1.
5 Reagents
5.1 Eluent.
For a general discussion of eluents, see ISO 16014-1.
For examples of eluents used for SEC measurements at temperatures < 60 °C, see Annex B.
NOTE Water is often used for SEC measurements on water-soluble polymers at temperatures < 60 °C, but it
is not suitable for use in this method.
5.2 Reagent for column evaluation, according to ISO 16014-1.
There are several low molecular weight compounds that can be used, for example ethylbenzene when
tetrahydrofuran is used as eluent or diethylene glycol when N,N-dimethylformamide is used as eluent
(see Annex B).
5.3 Molecular weight standards, according to ISO 16014-1.
Some examples of commercially available molecular weight standards are given in ISO 16014-1:2019,
Annex B.
5.4 Reagent for flow rate marker (internal standard), according to ISO 16014-1.
It is often very difficult to find a low molecular weight compound suitable for use as a flow rate marker
because it should not co-elute with the polymer peak, the system peak or the solvent peak.
Examples of compounds suitable for use as a flow rate marker are sulfur when tetrahydrofuran is used
as eluent and ethylbenzene when N,N-dimethylformamide is used as eluent.
5.5 Additives.
LiBr or LiCl, for example, is used as an additive in N,N-dimethylformamide to avoid aggregation of
polyacrylonitrile, and sodium trifluoroacetate is added to 1,1,1,3,3,3-hexafluoroisopropanol for SEC
measurements on polyamide.
6 Apparatus
6.1 General
A schematic diagram of an SEC system is shown in ISO 16014-1.
Either commercially available or assembled SEC systems may be used, provided they meet the component
requirements specified and have the capability to maintain a constant column temperature < 60 °C.
6.2 Eluent reservoir, according to ISO 16014-1.
It is not necessary to keep the reservoir at the same temperature as the columns.
6.3 Pumping system, according to ISO 16014-1.
In order to maintain the flow rate accurate to within ±0,3 %, the pumping system shall be kept at
a controlled temperature. It is, however, not necessary to keep the pumping system at the same
temperature as the columns.
2 © ISO 2019 – All rights reserved
6.4 Injector, according to ISO 16014-1.
In order to maintain an accurately known flow rate, the injector temperature-control equipment shall
be capable of keeping the injector at within ±1 K of the temperature set. It is not necessary to keep the
injector at the same temperature as the columns.
6.5 Columns, according to ISO 16014-1.
Organic or inorganic packing materials may be used. There are no limitations on particle size or shape.
The set of columns used shall have a total theoretical plate number > 15 000, and the resolution factor R
shall be > 1,5 close to the polymer peak. The asymmetry factor shall be within the range 1,
...
INTERNATIONAL ISO
STANDARD 16014-3
Third edition
2019-05
Plastics — Determination of average
molecular weight and molecular
weight distribution of polymers using
size-exclusion chromatography —
Part 3:
Low-temperature method
Plastiques — Détermination de la masse moléculaire moyenne
et de la distribution des masses moléculaires de polymères par
chromatographie d'exclusion stérique —
Partie 3: Mesurage aux basses températures
Reference number
©
ISO 2019
© ISO 2019
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 2019 – All rights reserved
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 2
6 Apparatus . 2
7 Procedure. 3
7.1 Preparation of solutions of molecular weight standards . 3
7.2 Preparation of sample solutions . 4
7.3 Preparation of solutions for column performance evaluation . 4
7.4 Setting up the apparatus. 4
7.5 Operating parameters . 5
7.5.1 Flow rate . 5
7.5.2 Injection masses and injection volumes . 5
7.5.3 Column temperature . 5
7.5.4 Detector sensitivity . 5
7.6 Number of determinations . 5
8 Data acquisition and processing . 5
9 Expression of results . 6
10 Precision . 6
10.1 General . 6
10.2 Experimental conditions . 6
10.3 Results of interlaboratory tests . 7
11 Test report . 8
Annex A (informative) Further information on applicability of method . 9
Annex B (informative) Further information on reagents .10
Annex C (informative) Further information on interlaboratory tests .11
Bibliography .17
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 5, Physical-
chemical properties.
This third edition cancels and replaces the second edition (ISO 16014-3:2012), which has been
technically revised. The main changes compared to the previous edition are as follows:
— publication dates of references have been removed;
— molecular mass has been changed to molecular weight according to IUPAC rule.
A list of all parts in the ISO 16014 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 © ISO 2019 – All rights reserved
INTERNATIONAL STANDARD ISO 16014-3:2019(E)
Plastics — Determination of average molecular weight
and molecular weight distribution of polymers using size-
exclusion chromatography —
Part 3:
Low-temperature method
1 Scope
This document specifies a method for determining the average molecular weight and the molecular
weight distribution of polymers by size-exclusion chromatography (SEC) using an organic eluent at a
temperature lower than 60 °C (see Annex A). The average molecular weight and the molecular weight
distribution are calculated from a calibration curve prepared using polymer standards. Therefore, this
test method is classified as a relative method (see ISO 16014-1).
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 5725-1, Accuracy (trueness and precision) of measurement methods and results — Part 1: General
principles and definitions
ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results — Part 2: Basic method
for the determination of repeatability and reproducibility of a standard measurement method
ISO 16014-1, Plastics — Determination of average molecular weight and molecular weight distribution of
polymers using size-exclusion chromatography — Part 1: General principles
ISO 16014-2, Plastics — Determination of average molecular weight and molecular weight distribution of
polymers using size-exclusion chromatography — Part 2: Universal calibration method
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 472 and in ISO 16014-1 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
According to ISO 16014-1.
5 Reagents
5.1 Eluent.
For a general discussion of eluents, see ISO 16014-1.
For examples of eluents used for SEC measurements at temperatures < 60 °C, see Annex B.
NOTE Water is often used for SEC measurements on water-soluble polymers at temperatures < 60 °C, but it
is not suitable for use in this method.
5.2 Reagent for column evaluation, according to ISO 16014-1.
There are several low molecular weight compounds that can be used, for example ethylbenzene when
tetrahydrofuran is used as eluent or diethylene glycol when N,N-dimethylformamide is used as eluent
(see Annex B).
5.3 Molecular weight standards, according to ISO 16014-1.
Some examples of commercially available molecular weight standards are given in ISO 16014-1:2019,
Annex B.
5.4 Reagent for flow rate marker (internal standard), according to ISO 16014-1.
It is often very difficult to find a low molecular weight compound suitable for use as a flow rate marker
because it should not co-elute with the polymer peak, the system peak or the solvent peak.
Examples of compounds suitable for use as a flow rate marker are sulfur when tetrahydrofuran is used
as eluent and ethylbenzene when N,N-dimethylformamide is used as eluent.
5.5 Additives.
LiBr or LiCl, for example, is used as an additive in N,N-dimethylformamide to avoid aggregation of
polyacrylonitrile, and sodium trifluoroacetate is added to 1,1,1,3,3,3-hexafluoroisopropanol for SEC
measurements on polyamide.
6 Apparatus
6.1 General
A schematic diagram of an SEC system is shown in ISO 16014-1.
Either commercially available or assembled SEC systems may be used, provided they meet the component
requirements specified and have the capability to maintain a constant column temperature < 60 °C.
6.2 Eluent reservoir, according to ISO 16014-1.
It is not necessary to keep the reservoir at the same temperature as the columns.
6.3 Pumping system, according to ISO 16014-1.
In order to maintain the flow rate accurate to within ±0,3 %, the pumping system shall be kept at
a controlled temperature. It is, however, not necessary to keep the pumping system at the same
temperature as the columns.
2 © ISO 2019 – All rights reserved
6.4 Injector, according to ISO 16014-1.
In order to maintain an accurately known flow rate, the injector temperature-control equipment shall
be capable of keeping the injector at within ±1 K of the temperature set. It is not necessary to keep the
injector at the same temperature as the columns.
6.5 Columns, according to ISO 16014-1.
Organic or inorganic packing materials may be used. There are no limitations on particle size or shape.
The set of columns used shall have a total theoretical plate number > 15 000, and the resolution factor R
shall be > 1,5 close to the polymer peak. The asymmetry factor shall be within the range 1,
...
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