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)Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS
2、, 18/04/2011 04:17, Uncontrolled Copy, (c) BSIBS EN ISO 11337:2010 BRITISH STANDARDNational forewordThis 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 It supersedes BS EN ISO 11337:2004 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee PR
3、I/21, Testing of plastics.A list of organizations represented on this committee can beobtained on request 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 83.08
4、0.20Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 January 2011.Amendments issued since publicationDate Text affectedLicensed Copy: Wang Bin, ISO/EXCHANGE CHIN
5、A STANDARDS, 18/04/2011 04:17, Uncontrolled Copy, (c) BSIEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11337 December 2010 ICS 83.080.20 Supersedes EN ISO 11337:2004English Version Plastics - Polyamides - Determination of e-caprolactam and w-laurolactam by gas chromatography (ISO 11337:20
6、10) Plastiques - Polyamides - Dtermination du e-caprolactame et du w-laurolactame par chromatographie en phase gazeuse (ISO 11337:2010) Kunststoffe - Polyamide - Gaschromatographische Bestimmung von e-Caprolactam und w-Laurolactam (ISO 11337:2010) This European Standard was approved by CEN on 10 Dec
7、ember 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 o
8、btained 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
9、 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, Luxembou
10、rg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2010 CEN All rights
11、of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 11337:2010: ELicensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 18/04/2011 04:17, Uncontrolled Copy, (c) BSIBS EN ISO 11337:2010EN ISO 11337:2010 (E) 3 Foreword This document (EN ISO 11337:2
12、010) 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 endors
13、ement, 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
14、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, De
15、nmark, 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 appr
16、oved by CEN as a EN ISO 11337:2010 without any modification. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 18/04/2011 04:17, Uncontrolled Copy, (c) BSIBS EN ISO 11337:2010ISO 11337:2010(E) ISO 2010 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Normative references1 3 Terms and
17、 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 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
18、 5.4 Preparation of internal-standard solutions.9 5.5 Procedure.10 5.6 Expression of results12 5.7 Precision 12 5.8 Test report12 Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 18/04/2011 04:17, Uncontrolled Copy, (c) BSIBS EN ISO 11337:2010ISO 11337:2010(E) iv ISO 2010 All rights reservedFo
19、reword 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 tec
20、hnical 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 o
21、f 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
22、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 fo
23、r 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 T
24、echnical Corrigendum ISO 11337:2004/Cor.1:2007. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 18/04/2011 04:17, Uncontrolled Copy, (c) BSIBS EN ISO 11337:2010INTERNATIONAL STANDARD ISO 11337:2010(E) ISO 2010 All rights reserved 1Plastics Polyamides Determination of -caprolactam and -laurola
25、ctam 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 appropri
26、ate 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 in po
27、lyamide 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 methanol
28、, 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 editio
29、n 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 purp
30、oses for this document, the terms and definitions given in ISO 472 apply. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 18/04/2011 04:17, Uncontrolled Copy, (c) BSIBS EN ISO 11337:2010ISO 11337:2010(E) 2 ISO 2010 All rights reserved4 Method A: Extraction method 4.1 Principle A test portion
31、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 reagen
32、ts of recognized analytical grade. 4.2.1 Methanol. 4.2.2 1-Dodecanol. 4.2.3 -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 prefer
33、red. 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 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 cera
34、mic 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
35、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; si
36、ntered-glass filter crucible, pore size 40 m to 50 m, capacity 30 ml; porcelain filter-plate of slightly smaller diameter than the crucible, with holes of diameter 0,4 mm. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 18/04/2011 04:17, Uncontrolled Copy, (c) BSIBS EN ISO 11337:2010ISO 11337
37、: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, or a porous ceramic thimble of similar capacity (the dimensions shall be such that the crucible or thimble c
38、an 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
39、 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), packed with acid-washed Chromosorb W1)of particle diameter 0,149 mm to 0,177 mm (80 mesh to 100 mesh) coated wit
40、h 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 obtain satisfactory separation efficiency. Other column dimensions are permissible, but only if they have been
41、 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 Carr
42、ier 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 commercially. This information is given for the convenience of users of this International Standard and does not cons
43、titute an endorsement by ISO of these products. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 18/04/2011 04:17, Uncontrolled Copy, (c) BSIBS 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 flow rates
44、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 Preparat
45、ion 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 liq
46、uid 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 mesh apertur
47、e 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 0,01 g to 0,
48、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. 4.5.2 Extrac
49、tion 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 a
