EN ISO 16014-5:2019

Plastics - Determination of average molecular weight and molecular weight distribution of polymers using size-exclusion chromatography - Part 5: Light-scattering method (ISO 16014-5:2019)

This document specifies a general method for determining the average molecular weight and the molecular weight distribution of polymers using SEC-LS, i.e. size-exclusion chromatography coupled with light-scattering detection. The average molecular weight and the molecular weight distribution are calculated from molecular weight data and weight concentrations determined continuously with elution time. The molecular weight at each elution time is determined absolutely by combining a light-scattering detector with a concentration-sensitive detector. Therefore, SEC-LS is classified as an absolute method.
This method is applicable to linear homopolymers and to nonlinear homopolymers such as branched, star-shaped, comb-like, stereo-regular and stereo-irregular polymers. It can also be applied to heterophasic copolymers whose molecular composition cannot vary. However, SEC-LS is not applicable to block, graft or heterophasic copolymers whose molecular composition can vary. And the methods are applicable to molecular weights ranging from that of the monomer to 3 000 000, but are not intended for samples that contain > 30 % of components having a molecular weight < 1 000.

Kunststoffe - Bestimmung der durchschnittlichen Molmasse und der Molmassenverteilung von Polymeren mittels Gelpermeationschromatographie - Teil 5: Lichtstreudetektionsverfahren (ISO 16014-5:2019)

Dieses Dokument legt ein allgemeines Verfahren zum Bestimmen der durchschnittlichen Molmasse und der Molmassenverteilung von Polymeren durch GPC LS, d. h. Gelpermeationschromatographie (GPC), gekoppelt mit Messung durch Lichtstreuung (LS), fest. Die durchschnittliche Molmasse und die Molmassenverteilung werden aus den Daten für die Molmasse und die Massenkonzentrationen berechnet, die kontinuierlich mit der Elutionszeit bestimmt werden. Die Molmasse bei jeder Elutionszeit wird als Absolutwert bestimmt, indem ein Detektor für die Lichtstreuung mit einem Konzentrationsdetektor kombiniert wird. Die GPC LS wird deshalb als ein absolutes Verfahren klassifiziert.
Dieses Verfahren ist für lineare Homopolymere und für nicht-lineare Homopolymere wie verzweigte, sternförmige, kammförmige, stereoreguläre, und stereoirreguläre Polymere anwendbar. Es kann auch auf heterophasige Copolymere, deren molekulare Zusammensetzung nicht variieren kann, angewendet werden. Dennoch ist GPC-LS nicht für Block-, Pfropf- oder heterophasige Copolymere, deren molekulare Zusammensetzung variieren kann, anwendbar. Und die Verfahren sind auf Molmassen anwendbar, die im Bereich vom Monomeren bis 3 000 000 liegen, jedoch sind sie nicht gedacht für Proben, die < 30 % Copolymere mit einer Molmasse < 1 000 enthalten.

Plastiques - Détermination de la masse moléculaire moyenne et de la distribution des masses moléculaires de polymères par chromatographie d'exclusion stérique - Partie 5: Méthode par diffusion lumineuse (ISO 16014-5:2019)

Le présent document spécifie une méthode générale pour la détermination de la masse moléculaire moyenne et de la distribution des masses moléculaires de polymères à l'aide de la SEC-LS, c'est-à-dire de la chromatographie d'exclusion stérique associée à la détection par diffusion lumineuse. La masse moléculaire moyenne et la distribution des masses moléculaires sont calculées à partir des données de masse moléculaire et des concentrations en masse déterminées en continu avec le temps d'élution. La masse moléculaire à chaque temps d'élution est déterminée dans l'absolu en associant un détecteur à diffusion lumineuse à un détecteur sensible aux concentrations. La méthode SEC-LS est donc classée comme méthode absolue.
Cette méthode s'applique aux homopolymères linéaires et aux homopolymères non linéaires tels que les polymères ramifiés, en étoile, en peigne, stéréo-réguliers et stéréo-irréguliers. Elle peut également s'appliquer aux copolymères hétérophasiques dont la composition moléculaire ne peut pas varier. Toutefois, la méthode SEC-LS ne s'applique pas aux copolymères séquencés, greffés ou hétérophasiques dont la composition moléculaire peut varier. Par ailleurs, les méthodes s'appliquent aux masses moléculaires allant de celle du monomère à 3 000 000, mais ne sont pas destinées aux échantillons contenant > 30 % de composants ayant une masse moléculaire < 1 000.

Polimerni materiali - Določevanje povprečne molekulske mase in porazdelitve molekulske mase polimerov z gelsko izključitveno kromatografijo (SEC) - 5. del: Metoda s sipanjem svetlobe (ISO 16014-5:2019)

Ta dokument določa splošno metodo za določevanje povprečne molekulske mase in porazdelitve molekulske mase polimerov z uporabo gelske izključitvene kromatografije v kombinaciji s sipanjem svetlobe (SEC-LS). Povprečna molekulska masa in porazdelitev molekulske mase se izračunata na podlagi podatkov o molekulski masi in koncentraciji mase, ki se kontinuirano določa z elucijskim časom. Molekulska masa se za posamezni elucijski čas določi absolutno s kombinacijo sipanja svetlobe in na koncentracijo občutljivega detektorja. Zato se izključitvena kromatografija v kombinaciji s sipanjem svetlobe obravnava kot absolutna metoda.
Ta metoda se uporablja za linearne homopolimere in nelinearne homopolimere, kot so razvejani, zvezdasti, glavničasti, stereoregularni in stereoneregularni polimeri. Uporabiti jo je mogoče tudi za heterofazne kopolimere, katerih molekulska sestava se ne more razlikovati. Vendar pa se metoda SEC-LS ne uporablja za blokovne, cepljene ali heterofazne kopolimere, katerih molekulska sestava se lahko razlikuje. Metode se uporabljajo za molekulske mase od mase monomera do 3.000.000, vendar niso namenjene za vzorce, ki vsebujejo > 30 % komponent z molekulsko maso < 1000.

General Information

• Status: Published
• Publication Date: 11-Jun-2019
• Withdrawal Date: 30-Dec-2019
• ICS: 83.080.01 - Plastics in general
• Technical Committee: CEN/TC 139 - Paints and varnishes
• Drafting Committee: CEN/TC 139 - Paints and varnishes
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 12-Jun-2019
• Completion Date: 12-Jun-2019
• Ref Project: SIST EN ISO 16014-5:2019 - Plastics - Determination of average molecular weight and molecular weight distribution of polymers using size-exclusion chromatography - Part 5: Light-scattering method (ISO 16014-5:2019)

Relations

• Replaces: EN ISO 16014-5:2012 - Plastics - Determination of average molecular mass and molecular mass distribution of polymers using size-exclusion chromatography - Part 5: Method using light-scattering detection (ISO 16014-5:2012)
• Effective Date: 19-Jun-2019

Standards Content (Sample)

SLOVENSKI STANDARD
01-september-2019
Nadomešča:
SIST EN ISO 16014-5:2012
Polimerni materiali - Določevanje povprečne molekulske mase in porazdelitve
molekulske mase polimerov z gelsko izključitveno kromatografijo (SEC) - 5. del:
Metoda s sipanjem svetlobe (ISO 16014-5:2019)
Plastics - Determination of average molecular weight and molecular weight distribution of
polymers using size-exclusion chromatography - Part 5: Light-scattering method (ISO
16014-5:2019)
Kunststoffe - Bestimmung der durchschnittlichen Molmasse und der
Molmassenverteilung von Polymeren mittels Gelpermeationschromatographie - Teil 5:
Lichtstreudetektionsverfahren (ISO 16014-5:2019)
Plastiques - Détermination de la masse moléculaire moyenne et de la distribution des
masses moléculaires de polymères par chromatographie d'exclusion stérique - Partie 5:
Méthode par diffusion lumineuse (ISO 16014-5:2019)
Ta slovenski standard je istoveten z: EN ISO 16014-5:2019
ICS:
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
83.080.01 Polimerni materiali na Plastics in general
splošno
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN ISO 16014-5
EUROPEAN STANDARD
NORME EUROPÉENNE
June 2019
EUROPÄISCHE NORM
ICS 83.080.01 Supersedes EN ISO 16014-5:2012
English Version
Plastics - Determination of average molecular weight and
molecular weight distribution of polymers using size-
exclusion chromatography - Part 5: Light-scattering
method (ISO 16014-5:2019)
Plastiques - Détermination de la masse moléculaire Kunststoffe - Bestimmung der durchschnittlichen
moyenne et de la distribution des masses moléculaires Molmasse und der Molmassenverteilung von
de polymères par chromatographie d'exclusion Polymeren mittels Gelpermeationschromatographie -
stérique - Partie 5: Méthode par diffusion lumineuse Teil 5: Lichtstreudetektionsverfahren (ISO 16014-
(ISO 16014-5:2019) 5:2019)
This European Standard was approved by CEN on 26 May 2019.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 16014-5:2019 E
worldwide for CEN national Members.

Contents Page
European foreword . 3

European foreword
This document (EN ISO 16014-5:2019) has been prepared by Technical Committee ISO/TC 61 "Plastics"
in collaboration with Technical Committee CEN/TC 139 “Paints and varnishes” the secretariat of which
is held by DIN.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by December 2019, and conflicting national standards
shall be withdrawn at the latest by December 2019.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN ISO 16014-5:2012.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Endorsement notice
The text of ISO 16014-5:2019 has been approved by CEN as EN ISO 16014-5:2019 without any
modification.
INTERNATIONAL ISO
STANDARD 16014-5
Second edition
2019-05
Plastics — Determination of average
molecular weight and molecular
weight distribution of polymers using
size-exclusion chromatography —
Part 5:
Light-scattering method
Plastiques — Détermination de la masse moléculaire moyenne
et de la distribution des masses moléculaires de polymères par
chromatographie d'exclusion stérique —
Partie 5: Méthode par diffusion lumineuse
Reference number
ISO 16014-5:2019(E)
©
ISO 2019
ISO 16014-5:2019(E)
© 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
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Published in Switzerland
ii © ISO 2019 – All rights reserved

ISO 16014-5:2019(E)
Contents Page
Foreword .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Symbols . 2
5 Principle . 2
5.1 SEC . 2
5.2 Light-scattering SEC . 2
6 Reagents . 3
7 Apparatus . 3
8 Procedure. 5
8.1 Preparation of calibration solutions . 5
8.2 Preparation of a solution for determining the L-point . 5
8.3 Preparation of sample solutions . 5
8.4 Preparation of solutions for column performance evaluation . 5
8.5 Setting up the apparatus. 5
8.6 Operating parameters . 5
8.6.1 Flow rate . 5
8.6.2 Injection masses and injection volumes . 5
8.6.3 Column temperature . 6
8.6.4 Detector sensitivity . 6
8.7 Number of determinations . 6
9 Calibration . 6
9.1 Calibration of concentration-sensitive detector and light-scattering detector . 6
9.1.1 General. 6
9.1.2 Calibration method A . 6
9.1.3 Calibration method B . 7
9.1.4 Calibration method C . 7
9.2 Determination of delay volume . 8
9.3 Normalization of detector sensitivity . 8
9.4 Determination of refractive index increment . 8
10 Data acquisition and processing . 8
10.1 Data acquisition . 8
10.2 Evaluation of data and correction of chromatograms . 8
10.3 Data processing . 8
10.3.1 Baseline determination . 8
10.3.2 Determination of calculation range . 9
10.3.3 Calculation of signal intensity . 9
10.3.4 Calculation of molecular weight . 9
10.3.5 Second virial coefficient, A . 9
11 Expression of results .10
11.1 Calibration curve .
...