Plastics - Polyamides - Determination of e-caprolactam and w-laurolactam by gas chromatography (ISO 11337:2010)

ISO 11337:2010 specifies a method for determining epsilon‑caprolactam and omega‑laurolactam in polyamides by gas chromatography. It is suitable particularly for the determination of epsilon‑caprolactam in polyamide 6 and omega‑laurolactam in polyamide 12. Bearing in mind that gas chromatography offers a wide range of possible conditions, the method specified is that shown to have been suitable in practice.
Two variants of the basic method are specified:
Method A is an extraction method with boiling methanol, and the extract is injected into a gas chromatograph.
Method B is a method using a solvent, and the solution is injected into a gas chromatograph.

Kunststoffe - Polyamide - Gaschromatographische Bestimmung von ε-Caprolactam und w-Laurolactam (ISO 11337:2010)

Diese Internationale Norm legt ein gaschromatographisches Verfahren zur Bestimmung des -Caprolactamgehaltes und des -Laurolactamgehaltes in Polyamiden fest. Es ist besonders zur Bestimmung von -Caprolactam in Polyamid 6 und von -Laurolactam in Polyamid 12 geeignet. Unter Berücksichtigung der Tatsache, dass die Gaschromatographie einen ausgedehnten Bereich von Möglichkeiten bietet, hat sich das festgelegte Verfahren in der Praxis als geeignet erwiesen.
Zwei Verfahren sind in dieser Internationalen Norm festgelegt:
Verfahren A ist ein Extraktionsverfahren unter Anwendung von siedendem Methanol, bei dem die Extrakte in einen Gaschromatographen injiziert werden;
Verfahren B ist ein Verfahren unter Anwendung eines Lösemittels, bei dem die Lösung direkt in einen Gaschromatographen injiziert wird.

Plastiques - Polyamides - Détermination du e-caprolactame et du w-laurolactame par chromatographie en phase gazeuse (ISO 11337:2010)

L'ISO 11337:2010 spécifie une méthode de dosage du epsilon-caprolactame et du omega-laurolactame dans les polyamides par chromatographie en phase gazeuse. Elle convient particulièrement au dosage du epsilon-caprolactame dans le polyamide 6 et du omega-laurolactame dans le polyamide 12. Compte tenu du fait que la chromatographie en phase gazeuse présente un large éventail de conditions possibles, la méthode spécifiée est celle qui a fait ses preuves dans la pratique.
Deux variantes de la méthode de base sont spécifiées:
Méthode A, par extraction au méthanol en ébullition, où les extraits sont injectés dans un chromatographe en phase gazeuse.
Méthode B, utilisant un solvant, où la solution est injectée directement dans un chromatographe en phase gazeuse.

Polimerni materiali - Poliamidi - Določanje e-kaprolaktama in w-laurolaktama s plinsko kromatografijo (ISO 11337:2010)

Ta mednarodni standard opredeljuje metodo za določanje ε-kaprolaktama in ω-lavrolaktama v poliamidih s plinsko kromatografijo. Primerna je zlasti za določanje ε-kaprolaktama v poliamidu 6 in ω-lavrolaktama v poliamidu 12. Z upoštevanjem, da plinska kromatografija ponuja širok razpon mogočih pogojev, je določena metoda tista, ki je bila dokazano primerna v praksi.
Določeni sta dve različici osnovne metode:
⎯ Metoda A je ekstrakcijska metoda, pri kateri se izvleček po metanolnem vrenju vbrizga v plinski kromatograf.
⎯ Metoda B je metoda, pri kateri se uporablja topilo, raztopina pa se vbrizga v plinski kromatograf.

General Information

Status
Withdrawn
Publication Date
14-Dec-2010
Withdrawal Date
31-Jan-2023
Technical Committee
Drafting Committee
Current Stage

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SLOVENSKI STANDARD
01-november-2011
1DGRPHãþD
SIST EN ISO 11337:2004
SIST EN ISO 11337:2004/AC:2009
3ROLPHUQLPDWHULDOL3ROLDPLGL'RORþDQMHHNDSURODNWDPDLQZODXURODNWDPDV
SOLQVNRNURPDWRJUDILMR ,62
Plastics - Polyamides - Determination of e-caprolactam and w-laurolactam by gas
chromatography (ISO 11337:2010)
Kunststoffe - Polyamide - Gaschromatographische Bestimmung von  -
Caprolactam und -Laurolactam (ISO 11337:2010)
Plastiques - Polyamides - Détermination du e-caprolactame et du w-laurolactame par
chromatographie en phase gazeuse (ISO 11337:2010)
Ta slovenski standard je istoveten z: EN ISO 11337:2010
ICS:
83.080.20 Plastomeri Thermoplastic materials
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EUROPEAN STANDARD
EN ISO 11337
NORME EUROPÉENNE
EUROPÄISCHE NORM
December 2010
ICS 83.080.20 Supersedes EN ISO 11337:2004
English Version
Plastics - Polyamides - Determination of e-caprolactam and w-
laurolactam by gas chromatography (ISO 11337:2010)
Plastiques - Polyamides - Détermination du e-caprolactame Kunststoffe - Polyamide - Gaschromatographische
et du w-laurolactame par chromatographie en phase Bestimmung von e-Caprolactam und w-Laurolactam (ISO
gazeuse (ISO 11337:2010) 11337:2010)
This European Standard was approved by CEN on 10 December 2010.

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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2010 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 11337:2010: E
worldwide for CEN national Members.

Contents Page
Foreword .3

Foreword
This document (EN ISO 11337:2010) has been prepared by Technical Committee ISO/TC 61 “Plastics” in
collaboration with Technical Committee CEN/TC 249 “Plastics” the secretariat of which is held by NBN.
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 June 2011, and conflicting national standards shall be withdrawn at
the latest by June 2011.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN ISO 11337:2004.
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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,
Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
Sweden, Switzerland and the United Kingdom.
Endorsement notice
The text of ISO 11337:2010 has been approved by CEN as a EN ISO 11337:2010 without any modification.

INTERNATIONAL ISO
STANDARD 11337
Second edition
2010-12-15
Plastics — Polyamides — Determination
of ε-caprolactam and ω-laurolactam by
gas chromatography
Plastiques — Polyamides — Détermination du ε-caprolactame et du
ω-laurolactame par chromatographie en phase gazeuse

Reference number
ISO 11337:2010(E)
©
ISO 2010
ISO 11337:2010(E)
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ii © ISO 2010 – All rights reserved

ISO 11337:2010(E)
Contents Page
Foreword .iv
1 Scope.1
2 Normative references.1
3 Terms and definitions .1
4 Method A: Extraction method .2
4.1 Principle .2
4.2 Reagents .2
4.3 Apparatus and materials.2
4.4 Preparation of test sample .4
4.5 Procedure.4
4.6 Expression of results.6
4.7 Precision .6
4.8 Test report.6
5 Method B: Dissolution method .7
5.1 Principle .7
5.2 Reagents .7
5.3 Apparatus.7
5.4 Preparation of internal-standard solutions.9
5.5 Procedure.10
5.6 Expression of results.12
5.7 Precision .12
5.8 Test report.12

ISO 11337:2010(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 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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
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.
ISO 11337 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical-
chemical properties.
This second edition cancels and replaces the first edition (ISO 11337:2004), which has been technically
revised. It also incorporates the Technical Corrigendum ISO 11337:2004/Cor.1:2007.

iv © ISO 2010 – All rights reserved

INTERNATIONAL STANDARD ISO 11337:2010(E)

Plastics — Polyamides — Determination of ε-caprolactam and
ω-laurolactam by gas chromatography
SAFETY STATEMENT — Persons using this document should be familiar with normal laboratory
practice, if applicable. This document does not purport to address all of the safety concerns, if any,
associated with its use. It is the responsibility of the user to establish appropriate safety and health
practices and to ensure compliance with any regulatory requirements.
1 Scope
This International Standard specifies a method for determining ε-caprolactam and ω-laurolactam in
polyamides by gas chromatography. It is suitable particularly for the determination of ε-caprolactam in
polyamide 6 and ω-laurolactam in polyamide 12. Bearing in mind that gas chromatography offers a wide range
of possible conditions, the method specified is that shown to have been suitable in practice.
Two variants of the basic method are specified:
⎯ Method A is an extraction method with boiling methanol, and the extract is injected into a gas
chromatograph.
⎯ Method B is a method using a solvent, and the solution is injected into a gas chromatograph.
2 Normative references
The following referenced documents are indispensable for the application 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 565, Test sieves — Metal wire cloth, perforated metal plate and electroformed sheet — Nominal sizes of
openings
3 Terms and definitions
For the purposes for this document, the terms and definitions given in ISO 472 apply.
ISO 11337:2010(E)
4 Method A: Extraction method
4.1 Principle
A test portion is extracted with boiling methanol and a small volume of the extract injected into a gas
chromatograph equipped with a flame-ionization detector to separate and detect the volatile components.
The extract contains 1-dodecanol as an internal standard.
4.2 Reagents
During the analysis, use only reagents of recognized analytical grade.
4.2.1 Methanol.
4.2.2 1-Dodecanol.
4.2.3 ε-Caprolactam.
4.3 Apparatus and materials
Ordinary laboratory apparatus, plus the following:
4.3.1 Mill, for reducing the sample to the required grain size.
A mill in which the sample is ground at a low temperature is preferred. Large pieces can be reduced in size
with a pair of scissors before they are fed to the mill.
4.3.2 Two sieves, with aperture sizes of 710 µm and 500 µm respectively, complying with the requirements
of ISO 565.
4.3.3 Extraction apparatus, that will accommodate an extraction crucible or porous ceramic thim
...

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