SIST EN ISO 11337:2011
(Main)Plastics - Polyamides - Determination of e-caprolactam and w-laurolactam by gas chromatography (ISO 11337:2010)
Plastics - Polyamides - Determination of e-caprolactam and w-laurolactam by gas chromatography (ISO 11337:2010)
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.
Kunststoffe - Polyamide - Gaschromatographische Bestimmung von <epsilon>-Caprolactam und <omega>-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
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 11337:2011
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
SIST EN ISO 11337:2011 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 11337:2011
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SIST EN ISO 11337:2011
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.
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SIST EN ISO 11337:2011
EN ISO 11337:2010 (E)
Contents Page
Foreword .3
2
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SIST EN ISO 11337:2011
EN ISO 11337:2010 (E)
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.
3
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SIST EN ISO 11337:2011
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SIST EN ISO 11337:2011
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
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SIST EN ISO 11337:2011
ISO 11337:2010(E)
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Published in Switzerland
ii © ISO 2010 – All rights reserved
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SIST EN ISO 11337:2011
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 2010 – All rights reserved iii
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SIST EN ISO 11337:2011
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
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SIST EN ISO 11337:2011
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 2010 – All rights reserved 1
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SIST EN ISO 11337:2011
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 thimble
containing the test portion.
The apparatus shall be of such a design that the crucible or thimble is heated by the rising methanol vapour or
the apparatus shall be constructed of an extraction flask with a Soxhlet-type reflux condenser.
Examples of suitable extraction apparatus designed along these lines are
EXAMPLE 1
⎯ 250 ml extraction flask;
⎯ extraction chamber to accommodate the extraction crucible so that it is enveloped on all sides by the rising methanol
vapour and the condensed methanol drips through it continuously;
⎯ glass triangle to support the crucible;
⎯ reflux condenser;
⎯ sintered-glass filter crucible, pore size 40 µm to 50 µm, capacity 30 ml;
⎯ porcelain filter-plate of slightly smaller diameter than the crucible, with holes of diameter 0,4 mm.
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SIST EN ISO 11337:2011
ISO 11337:2010(E)
EXAMPLE 2
⎯ 250 ml extraction flask;
⎯ jacketed Soxhlet extractor;
⎯ reflux condenser;
⎯ sintered-glass filter crucible, pore size 40 µm to 50 µm, capacity 30 ml, or a porous ceramic thimble of similar
capacity (the dimensions shall be such that the crucible or thimble can be satisfactorily accommodated in the Soxhlet
apparatus);
⎯ porcelain filter-plate of slightly smaller diameter than the crucible or thimble, as appropriate, with holes of diameter
0,4 mm.
4.3.4 Suitable heating device for extraction apparatus.
4.3.5 Analytical balance, accurate to 0,000 2 g.
4.3.6 Liquid nitrogen or solid carbon dioxide, if necessary.
4.3.7 Gas chromatograph, with flame-ionization detector.
a) Column
The following columns are suitable:
1)
⎯ a glass column (3 mm ∆ × 1,6 m), packed with acid-washed Chromosorb W of particle diameter
0,149 mm to 0,177 mm (80 mesh to 100 mesh) coated with 10 % (by mass) poly(ethylene glycol)
20M;
1)
⎯ a megabore Carbowax column (0,53 mm ∆ × 15 m) of corresponding separation efficiency.
The method of packing is not specified but shall be such as to obtain satisfactory separation efficiency.
Other column dimensions are permissible, but only if they have been proved to give the same results.
A capillary column may also be used.
Suggested operating conditions are shown in Table 1.
Table 1 — Operating conditions for gas chromatograph
Item Value
Column temperature 200 °C
Injector temperature 250 °C
Detector temperature 250 °C
Carrier gas Helium or nitrogen
a
Carrier gas flow rate 20 ml/min
a
This value is for the glass column. For any other type of column, a suitable flow rate will
have to be chosen.
1) Examples of suitable products available commercially. This information is given for the convenience of users of this
International Standard and does not constitute an endorsement by ISO of these products.
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SIST EN ISO 11337:2011
ISO 11337:2010(E)
b) Detector
Use a flame-ionization detector in which the hydrogen and air flow rates can be adjusted so that:
⎯ sensitivity is high;
⎯ the relationship between response and concentration is linear over the whole measurement range;
⎯ small changes in flow rate produce only insignificant effects on response and sensitivity.
4.3.8 Microsyringes, with capacities from 1 µl to 10 µl.
4.4 Preparation of test sample
Take a representative sample of the polymer and grind it in the mill (4.3.1). Grind the material in small portions
to prevent undue heat development (i.e. to avoid the temperature rising above about 40 °C), letting the mill
cool down in between portions. Solid carbon dioxide or liquid nitrogen (4.3.6) may be ground together with the
polymer to prevent heat build-up. With a large mill having a greater heat capacity, these precautions may not
be required. Collect the fraction that passes through a sieve with mesh aperture 710 µm (4.3.2), but not
through the one with mesh aperture 500 µm.
4.5 Procedure
4.5.1 Test portion
Weigh, to the nearest 0,001 g, (5 ± 0,5) g (mass m ) of the test sample into the filter crucible or porous thimble
0
(4.3.3). With low-concentration samples, it is preferable to increase the mass of the test portion so that it
contains approximately 0,01 g to 0,05 g of ε-caprolactam.
NOTE Polyamides can contain a small amount of water, forming part of the mass of the test portion (m ). This water
0
is not allowed for in the calculation of the methanol-extractable matter content since its effect is small compared the
variance of the determination.
4.5.2 Extraction
Cover the test portion (see 4.5.1) with the filter-plate, pour about 50 ml of methanol (4.2.1) into the extraction
flask, place the crucible or thimble containing the test portion in the extraction chamber and fit the condenser
to the chamber. Heat the solvent in the flask to boiling. When the apparatus described in 4.3.3, Example 1, is
used, adjust the rate of reflux to 1 to 2 drops per second and ensure that the drops fall into the crucible. When
a Soxhlet extractor as described in 4.3.3, Example 2, is used, adjust the heating so that there are five to eight
siphonings per hour.
Extract for a period of 3 h ± 5 min and then allow the extractor to cool to ambient temperature, overnight if
necessary.
Detach the extraction flask with its contents and analyse by gas chromatography, using the procedure
specified in 4.5.3 to 4.5.7.
4.5.3 Preparation of internal-standard solution
Weigh out, to the nearest 0,000 2 g, (2 ± 0,2) g of 1-dodecanol (4.2.2) and transfer it to a 1 l volumetric flask.
Dissolve in methanol and make up to the mark with the same solvent.
While 1-dodecanol is the preferred internal standard, it is also possible to use isopropanol.
4 © ISO 2010 – All rights reserved
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SIST EN ISO 11337:2011
ISO 11337:2010(E)
4.5.4 Preparation of sample solution
Transfer the e
...
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