1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN ISO 11337:2010Plastics Polyamides Determination of e-caprolactam and w-laurolactamby gas chromatography (ISO11337:2010)BS EN ISO 11337:2010 BRITISH STANDARDNational forewor
2、dThis British Standard is the UK implementation of EN ISO11337:2010. It supersedes BS EN ISO 11337:2004 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee PRI/21, Testing of plastics.A list of organizations represented on this committee can beobtained on r
3、equest to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2011ISBN 978 0 580 65739 9ICS 83.080.20Compliance with a British Standard cannot confer immunity fromlegal obligations.This British St
4、andard was published under the authority of theStandards Policy and Strategy Committee on 31 January 2011.Amendments issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11337 December 2010 ICS 83.080.20 Supersedes EN ISO 11337:2004English Version Plasti
5、cs - Polyamides - Determination of e-caprolactam and w-laurolactam by gas chromatography (ISO 11337:2010) Plastiques - Polyamides - Dtermination du e-caprolactame et du w-laurolactame par chromatographie en phase gazeuse (ISO 11337:2010) Kunststoffe - Polyamide - Gaschromatographische Bestimmung von
6、 e-Caprolactam und w-Laurolactam (ISO 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 a
7、lteration. 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
8、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, Es
9、tonia, 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 COMIT EUROPEN DE NORMALISATION EU
10、ROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 11337:2010: EBS EN ISO 11337:2010EN ISO 11337:2010 (E) 3 Foreword This document (EN ISO 1133
11、7:2010) 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 end
12、orsement, 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 identifyi
13、ng 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,
14、 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 a
15、pproved by CEN as a EN ISO 11337:2010 without any modification. BS EN ISO 11337:2010ISO 11337:2010(E) ISO 2010 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Normative references1 3 Terms and definitions .1 4 Method A: Extraction method 2 4.1 Principle .2 4.2 Reagents 2 4.3 Apparatus an
16、d materials.2 4.4 Preparation of test sample .4 4.5 Procedure.4 4.6 Expression of results6 4.7 Precision 6 4.8 Test report6 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 results12 5
17、.7 Precision 12 5.8 Test report12 BS EN ISO 11337:2010ISO 11337:2010(E) iv ISO 2010 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normal
18、ly 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
19、 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 I
20、nternational 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 o
21、f 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 re
22、places the first edition (ISO 11337:2004), which has been technically revised. It also incorporates the Technical Corrigendum ISO 11337:2004/Cor.1:2007. BS EN ISO 11337:2010INTERNATIONAL STANDARD ISO 11337:2010(E) ISO 2010 All rights reserved 1Plastics Polyamides Determination of -caprolactam and -l
23、aurolactam 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 ap
24、propriate safety and health practices and to ensure compliance with any regulatory requirements. 1 Scope This International Standard specifies a method for determining -caprolactam and -laurolactam in polyamides by gas chromatography. It is suitable particularly for the determination of -caprolactam
25、 in polyamide 6 and -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 me
26、thanol, 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
27、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 th
28、e purposes for this document, the terms and definitions given in ISO 472 apply. BS EN ISO 11337:2010ISO 11337:2010(E) 2 ISO 2010 All rights reserved4 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 chro
29、matograph 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 -Caprolactam. 4.3
30、 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 m
31、ill. 4.3.2 Two sieves, with aperture sizes of 710 m and 500 m 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 cru
32、cible 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 th
33、e 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 m to 50 m, capacity 30 ml; porcelain filter-plate
34、of slightly smaller diameter than the crucible, with holes of diameter 0,4 mm. BS EN ISO 11337:2010ISO 11337:2010(E) ISO 2010 All rights reserved 3EXAMPLE 2 250 ml extraction flask; jacketed Soxhlet extractor; reflux condenser; sintered-glass filter crucible, pore size 40 m to 50 m, capacity 30 ml,
35、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.
36、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 1,6 m), pack
37、ed with acid-washed Chromosorb W1)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 megabore Carbowax1)column (0,53 mm 15 m) of corresponding separation efficiency. The method of packing is not specified but shall be such as to ob
38、tain 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
39、 temperature 200 C Injector temperature 250 C Detector temperature 250 C Carrier gas Helium or nitrogen Carrier gas flow rate 20 ml/minaaThis 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 commercia
40、lly. This information is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of these products. BS EN ISO 11337:2010ISO 11337:2010(E) 4 ISO 2010 All rights reservedb) Detector Use a flame-ionization detector in which the hydrogen and air fl
41、ow 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 l to 10 l. 4.4
42、 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 dioxi
43、de 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 m (4.3.2), but not through the one with mes
44、h aperture 500 m. 4.5 Procedure 4.5.1 Test portion Weigh, to the nearest 0,001 g, (5 0,5) g (mass m0) of the test sample into the filter crucible or porous thimble (4.3.3). With low-concentration samples, it is preferable to increase the mass of the test portion so that it contains approximately 0,0
45、1 g to 0,05 g of -caprolactam. NOTE Polyamides can contain a small amount of water, forming part of the mass of the test portion (m0). This water 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
46、.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.
47、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
48、. 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 W
49、eigh 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. BS EN ISO 11337:2010ISO 11337:2010(E) ISO 2010 All rights reserved 54.5.4 Preparation of sample solution Transfer the extract obtained in 4.5.2 to a 100 ml volumetric flask and add 10 ml of the int
