CEN ISO/TS 23973:2021
(Main)Liquid chromatography at critical conditions (LCCC) - Chemical heterogeneity of polyethylene oxides (ISO/TS 23973:2020)
Liquid chromatography at critical conditions (LCCC) - Chemical heterogeneity of polyethylene oxides (ISO/TS 23973:2020)
This document establishes a valid method for separation of chemically heterogeneous polyethylene oxide (PEO) mixtures and for the determination the number and content of the chemically heterogeneous species in the overall sample.
The method presented in this document serves as a technical guideline and enables laboratories to learn the principle of "critical chromatography" on a validated system.
This method presented in this document with its stated system parameters is not applicable for other polymer classes, due to the diversity of the interactions between the polymer/mobile phase/stationary phase and the number of separation systems that are therefore available.
The evaluation of the interlaboratory testing has shown that many error sources relate to the technique of liquid chromatography in general. Possible error sources are described in Annex A.
Details on the evaluation of the interlaboratory testing are given in Annex B.
Elugrams of the participants (excerpts) are given in Annex C.
Investigations of the long-term stability of the test mixture are given in Annex D.
Flüssigchromatographie unter kritischen Bedingungen - Chemische Heterogenität von Polyethylenoxiden (ISO/TS 23973:2020)
Dieses Dokument beschreibt ein gültiges Verfahren für die Trennung von chemisch heterogenen Gemischen von Polyethylenoxid (PEO) und die Ermittlung der Anzahl sowie des Gehaltes der chemisch heterogenen Spezies in der Gesamtprobe.
Das in diesem Dokument dargestellte Verfahren dient als technischer Leitfaden und soll Laboratorien befähigen, das Prinzip der „kritischen Chromatographie“ an einem validierten System zu erlernen.
Auf Grund der Vielfalt der Wechselwirkungen Polymer/mobile Phase/stationäre Phase und der dadurch zur Verfügung stehenden Anzahl der Trennsysteme ist dieses Verfahren mit den angegebenen Systemparametern nicht allgemeingültig für andere Polymerklassen.
Die Auswertung der Ringversuche hat gezeigt, dass viele Fehlerquellen in der Technik der Flüssig-chromatographie allgemein zu suchen sind. Mögliche Fehlerquellen werden im Anhang A beschrieben.
Anhang B enthält Angaben zur Evaluierung des Ringversuchs.
Elugramme der Teilnehmer (Auszüge) sind im Anhang C enthalten.
Untersuchungen zur Langzeitstabilität des Prüfgemisches sind im Anhang D aufgeführt.
Chromatographie liquide aux conditions critiques - Hétérogénéité chimique des oxydes de polyéthylène (ISO/TS 23973:2020)
Tekočinska kromatografija pri kritičnih pogojih (LCCC) - Kemijska heterogenost polietilen oksidov (ISO/TS 23973:2020)
Ta dokument določa veljavno metodo za ločevanje kemijsko heterogenih zmesi polietilen oksida (PEO) ter za določevanje števila in vsebnosti kemijsko heterogenih vrst v celotnem vzorcu. Metoda, predstavljena v tem dokumentu, je podana kot tehnična smernica, ki laboratorijem omogoča, da uvedejo načelo »kritične kromatografije« v okviru potrjenega sistema. Metoda, predstavljena v tem dokumentu, in navedeni parametri sistema se zaradi raznolikosti interakcij med polimeri/mobilno fazo/stacionarno fazo in številom sistemov za ločevanje, ki so posledično na voljo, ne uporabljajo za druge razrede polimerov. Z vrednotenjem medlaboratorijskega preskušanja je bilo ugotovljeno, da se številni viri napak navezujejo na tehniko tekočinske kromatografije na splošno. Možni viri napak so opisani v dodatku A. Podrobnosti o vrednotenju medlaboratorijskega preskušanja so podane v dodatku B. Elugrami udeležencev (izvlečki) so podani v dodatku C. Raziskave dolgoročne stabilnosti preskusne zmesi so podane v dodatku D.
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-marec-2022
Tekočinska kromatografija pri kritičnih pogojih (LCCC) - Kemijska heterogenost
polietilen oksidov (ISO/TS 23973:2020)
Liquid chromatography at critical conditions (LCCC) - Chemical heterogeneity of
polyethylene oxides (ISO/TS 23973:2020)
Chromatographie liquide aux conditions critiques - Hétérogénéité chimique des oxydes
de polyéthylène (ISO/TS 23973:2020)
Ta slovenski standard je istoveten z: CEN ISO/TS 23973:2021
ICS:
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
CEN ISO/TS 23973
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
December 2021
TECHNISCHE SPEZIFIKATION
ICS 71.040.50
English Version
Liquid chromatography at critical conditions (LCCC) -
Chemical heterogeneity of polyethylene oxides (ISO/TS
23973:2020)
Chromatographie liquide aux conditions critiques -
Hétérogénéité chimique des oxydes de polyéthylène
(ISO/TS 23973:2020)
This Technical Specification (CEN/TS) was approved by CEN on 5 December 2021 for provisional application.
The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to
submit their comments, particularly on the question whether the CEN/TS can be converted into a European Standard.
CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS
available promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in
parallel to the CEN/TS) until the final decision about the possible conversion of the CEN/TS into an EN is reached.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, 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
© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN ISO/TS 23973:2021 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
European foreword
The text of ISO/TS 23973:2020 has been prepared by Technical Committee ISO/TC 35 "Paints and
varnishes” of the International Organization for Standardization (ISO) and has been taken over as
which is held by DIN.
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.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to announce this Technical Specification: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the
United Kingdom.
Endorsement notice
The text of ISO/TS 23973:2020 has been approved by CEN as CEN ISO/TS 23973:2021 without any
modification.
TECHNICAL ISO/TS
SPECIFICATION 23973
First edition
2020-08
Liquid chromatography at critical
conditions (LCCC) — Chemical
heterogeneity of polyethylene oxides
Chromatographie liquide aux conditions critiques — Hétérogénéité
chimique des oxydes de polyéthylène
Reference number
ISO/TS 23973:2020(E)
©
ISO 2020
ISO/TS 23973:2020(E)
© ISO 2020
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ii © ISO 2020 – All rights reserved
ISO/TS 23973:2020(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Apparatus . 2
5.1 General . 2
5.2 Eluent supply . 3
5.3 Pump . 3
5.4 Injection system . 4
5.5 Separation columns . 4
5.6 Column temperature control . 5
5.7 Detectors . 5
5.8 Eluent . 5
5.9 Data acquisition . 5
6 Sample preparation . 5
7 Performance of the measurements . 6
7.1 Determination of the critical conditions . 6
7.2 Analysis of the validation kit . 7
8 Test report . 7
Annex A (informative) Error sources . 9
Annex B (informative) Evaluation of the interlaboratory testing .10
Annex C (informative) Elugrams of the participants (excerpts) .17
Annex D (informative) Investigations of the long-term stability of the test mixture .43
Bibliography .49
ISO/TS 23973:2020(E)
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
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 35, Paints and varnishes.
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 2020 – All rights reserved
ISO/TS 23973:2020(E)
Introduction
Since the first description of liquid chromatography at critical conditions (LCCC) in
1986 (see Reference [1]), the method has been continuously refined and has proved itself to be
indispensable for polymer characterisation. Separation is required not only for the quantitative
analysis of the individual species. It also offers the preconditions for qualitative characterisation of the
fractions by means of spectroscopic and spectrometric techniques. The key factor here is the reduction
of the polydispersity/chemical heterogeneity within a fraction, which represents a large problem for
mass-spectrometric investigations.
The method has been described extensively in professional circles over the last two decades for
different polymer systems, see References [2] to [9].
Within the framework of the Technical Committee, the extent that the method supplies consistent
results for a simple, chemically heterogeneous polymer mixture was clarified as part of interlaboratory
testing.
At this time, necessary experience relating to the selection of the system (interaction between the
polarities separation phase/eluent/sample) was not expected of any of the participating laboratories.
The interlaboratory testing has shown that, even w
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