SIST EN ISO 11337:2004
(Main)Plastics - Polyamides - Determination of e-caprolactam and w-laurolactam by gas chromatography (ISO 11337:2004)
Plastics - Polyamides - Determination of e-caprolactam and w-laurolactam by gas chromatography (ISO 11337:2004)
ISO 11337:2004 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.
Method A is suitable for the determination of epsilon-caprolactam and method B for epsilon-caprolactam and omega-laurolactam.
Kunststoffe - Polyamide - Gaschromatographische Bestimmung von e-Caprolactam und w-laurolactam (ISO 11337:2004)
Anwendungsbereich
Die vorliegende Internationale Norm legt ein gaschromatographisches Verfahren zur Bestimmung des e-Caprolactamgehaltes und des w-Laurolactamgehaltes in Polyamiden fest. Es ist besonders zur Bestimmung von e-Caprolactam in Polyamid 6 (Nylon) und von w-Laurolactam in Polyamid 12 geeignet. Unter Berücksichtigung der Tatsache, dass die Gaschromatographie einen ausgedehnten Bereich von Möglichkei-ten bietet, hat sich das festgelegte Verfahren in der Praxis als geeignet erwiesen.
In dieser Internationalen Norm werden zwei Verfahren beschrieben:
3 Verfahren A ist ein Extraktionsverfahren unter Anwendung von siedendem Methanol, bei dem die Extrakte in einen Gaschromatograph injiziert werden;
3 Verfahren B ist ein Verfahren unter Anwendung eines Lösungsmittels, bei dem die Lösung direkt in einen Gaschromatograph injiziert wird.
Plastiques - Polyamides - Détermination du e-caprolactame et du w-laurolactam par chromatographie en phase gazeuse (ISO 11337:2004)
L'ISO 11337:2004 spécifie une méthode par chromatographie en phase gazeuse pour le dosage de l'epsilon-caprolactame et de l'omega-laurolactame dans les polyamides. Elle convient particulièrement au dosage de l'epsilon-caprolactame dans le polyamide 6 et de l'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, méthode par extraction au méthanol en ébullition, où l'extrait est injecté dans un chromatographe en phase gazeuse.Méthode B, méthode utilisant un solvant, où la solution est injectée dans un chromatographe en phase gazeuse.
La méthode A est appropriée pour la détermination de l'epsilon-caprolactame et la méthode B pour celle de l'epsilon-caprolactame et de l'omega-laurolactame.
Polimerni materiali – Poliamidi – Določanje e-kaprolaktama in w-laurolaktama s plinsko kromatografijo (ISO 11337:2004)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 11337:2004
01-oktober-2004
3ROLPHUQLPDWHULDOL±3ROLDPLGL±'RORþDQMHHNDSURODNWDPDLQZODXURODNWDPDV
SOLQVNRNURPDWRJUDILMR ,62
Plastics - Polyamides - Determination of e-caprolactam and w-laurolactam by gas
chromatography (ISO 11337:2004)
Kunststoffe - Polyamide - Gaschromatographische Bestimmung von e-Caprolactam und
w-laurolactam (ISO 11337:2004)
Plastiques - Polyamides - Détermination du e-caprolactame et du w-laurolactam par
chromatographie en phase gazeuse (ISO 11337:2004)
Ta slovenski standard je istoveten z: EN ISO 11337:2004
ICS:
83.080.20 Plastomeri Thermoplastic materials
SIST EN ISO 11337:2004 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 11337:2004
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SIST EN ISO 11337:2004
EUROPEAN STANDARD
EN ISO 11337
NORME EUROPÉENNE
EUROPÄISCHE NORM
May 2004
ICS 83.080.20
English version
Plastics - Polyamides - Determination of e-caprolactam and w-
laurolactam by gas chromatography (ISO 11337:2004)
Plastiques - Polyamides - Détermination du e- Kunststoffe - Polyamide - Gaschromatographische
caprolactame et du w-laurolactam par chromatographie en Bestimmung von e-Caprolactam und w-laurolactam (ISO
phase gazeuse (ISO 11337:2004) 11337:2004)
This European Standard was approved by CEN on 13 May 2004.
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 Central Secretariat 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 Central Secretariat has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,
Slovenia, Spain, Sweden, Switzerland and United Kingdom.
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Management Centre: rue de Stassart, 36 B-1050 Brussels
© 2004 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 11337:2004: E
worldwide for CEN national Members.
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SIST EN ISO 11337:2004
EN ISO 11337:2004 (E)
Foreword
This document (EN ISO 11337:2004) 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 IBN.
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 November 2004, and conflicting national
standards shall be withdrawn at the latest by November 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,
Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary,
Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
Endorsement notice
The text of ISO 11337:2004 has been approved by CEN as EN ISO 11337:2004 without any
modifications.
2
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SIST EN ISO 11337:2004
INTERNATIONAL ISO
STANDARD 11337
First edition
2004-05-15
Plastics — Polyamides — Determination
of εεεε-caprolactam and ωωωω-laurolactam by
gas chromatography
Plastiques — Polyamides — Détermination du ε-caprolactame
et du ω-laurolactame par chromatographie en phase gazeuse
Reference number
ISO 11337:2004(E)
©
ISO 2004
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SIST EN ISO 11337:2004
ISO 11337:2004(E)
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ii © ISO 2004 – All rights reserved
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SIST EN ISO 11337:2004
ISO 11337:2004(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. 5
4.7 Precision . 6
4.8 Test report. 6
5 Method B: Dissolution method. 6
5.1 Principle . 6
5.2 Reagents . 7
5.3 Apparatus. 7
5.4 Preparation of internal-standard solutions . 8
5.5 Procedure. 10
5.6 Expression of results. 11
5.7 Precision . 11
5.8 Test report. 12
© ISO 2004 – All rights reserved iii
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SIST EN ISO 11337:2004
ISO 11337:2004(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.
iv © ISO 2004 – All rights reserved
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SIST EN ISO 11337:2004
INTERNATIONAL STANDARD ISO 11337:2004(E)
Plastics — Polyamides — Determination of εεεε-caprolactam and
ωω-laurolactam by gas chromatography
ωω
WARNING — This International Standard may involve hazardous chemicals, materials or operations. It
does not purport to address all of the safety problems, if any, associated with its use. It is the
responsibility of the user to establish appropriate safety and health practices and to determine the
applicability of regulatory limitations prior to use.
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.
Method A is suitable for the determination of ε-caprolactam and method B for ε-caprolactam and
ω-laurolactam.
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 2004 – All rights reserved 1
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SIST EN ISO 11337:2004
ISO 11337:2004(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 εε-Caprolactam.
εε
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.
EXAMPLE 2
250 ml extraction flask;
jacketed Soxhlet extractor;
2 © ISO 2004 – All rights reserved
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SIST EN ISO 11337:2004
ISO 11337:2004(E)
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:
a glass column (3 mm φ × 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;
a fused-silica capillary column (0,31 mm φ × 30 m), liquid phase 95 % dimethyl, 5 % diphenyl
polysiloxane, film thickness 0,25 µm;
a megabore carbowax column (0,53 mm φ × 15 m) of corresponding separation efficiency.
The method of packing is not specified but shall be such as to obtain satisfactory separation efficiency. The
capillary column is preferred.
Other column dimensions are permissible, but only if they have been proved to give the same results.
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
Carrier gas flow rate 20 ml/min
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.
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SIST EN ISO 11337:2004
ISO 11337:2004(E)
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 400 °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 the sieve with mesh aperture 710 µm (see 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
(see 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 may 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 with 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 following
procedure:
4.5.3 Preparation of internal-standard solution
Weigh out, to the nearest 0,000 2 g, 2 g of 1-dodecanol and transfer it to a 1 l volumetric flask. Dissolve in
methanol and make up to the mark with the same solvent.
4.5.4 Preparation of sample solution
Transfer the extract obtained in 4.5.2 to a 100 ml volumetric flask and add 10 ml of the internal-standard
solution prepared in 4.5.3. Rinse the extraction flask with small amount of methanol, add the rinsings to the
volumetric flask and make up to the mark with methanol.
4.5.5 Preparation of calibration sol
...
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