DIN EN ISO 11337-2011 Plastics - Polyamides - Determination of -caprolactam and -laurolactam by gas chromatography (ISO 11337 2010) German version EN ISO 11337 2010《塑料 聚酰胺 用气相色谱法测定.pdf

1、April 2011 Translation by DIN-Sprachendienst.English price group 12No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS

2、83.080.20!$nb/“1756312www.din.deDDIN EN ISO 11337Plastics Polyamides Determination of -caprolactam and -laurolactam bygas chromatography (ISO 11337:2010)English translation of DIN EN ISO 11337:2011-04Kunststoffe Polyamide Gaschromatographische Bestimmung von -Caprolactam und -Laurolactam(ISO 11337:2

3、010)Englische bersetzung von DIN EN ISO 11337:2011-04Plastiques Polyamides Dtermination du -caprolactame et du -laurolactame parchromatographie en phase gazeuse (ISO 11337:2010)Traduction anglaise de DIN EN ISO 11337:2011-04SupersedesDIN EN ISO 11337:2004-09 andDIN EN ISO 11337 Corrigendum1:2009-07w

4、ww.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.2103.11eveevvDIN EN ISO 11337:2011-04 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee ISO/TC 61 “Plastics” (Secretariat:

5、 ANSI, USA) in collaboration with Technical Committee CEN/TC 249 “Plastics”, (Secretariat: NBN, Belgium). The responsible German body involved in its preparation was the Normenausschuss Kunststoffe (Plastics Standards Committee), Working Committee NA 054-01-03 AA Physikalische, rheologische und anal

6、ytische Prfungen. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 472 DIN EN ISO 472 ISO 565 DIN ISO 565 Amendments This standard differs from DIN EN ISO 11337:2004-09 and DIN EN ISO 11337 Corrigendum 1:2009-07 as follows: a) in Subclau

7、se 4.3.7, the fused-silica capillary column has been deleted from the list of suitable columns and the information that a capillary column may also be used has been added; b) in Table 1 “Operating conditions for gas chromatograph”, a footnote relating to the carrier gas flow rate has been added; c)

8、in Subclause 4.5.3, “2,0 g of 1-dodecanol” has been changed to read “(2 0,2) g of 1-dodecanol (4.2.2)”; d) in Subclause 4.5.3, it is indicated that the use of isopropanol is also possible; e) in Subclause 4.5.5, “0,05 g of -caprolactam” has been changed to read “(0,05 0,005) g of -caprolactam (4.2.3

9、)”; f) in Subclause 5.1, it is indicated that 1-dodecanol, 2-azacyclononane or 2-azacyclooctanone may also be used as the internal standard; g) in Subclause 5.2 “Reagents”, “Anhydrous methanol” (5.2.6) has been added; h) in Subclause 5.3.1, it has been stated that the use of a capillary column shoul

10、d be avoided; i) in Table 3 “Operating conditions for gas chromatograph”, the carrier gas flow rate has been changed from “35 ml/min” to “35 ml/min to 60 ml/min”; j) Subclause 5.4 “Preparation of internal-standard solutions” now includes a new Subclause 5.4.1 “General” and the following subclauses h

11、ave been renumbered; k) the equation in Subclause 5.6 “Expression of results” has been modified and the explanation of the symbols has been updated; l) the standard has been editorially revised; m) the corrigendum related to the fused-silica capillary column in Subclause 4.3.7 has been deleted, see

12、a). Previous editions DIN EN ISO 11337 Corrigendum 1: 2009-07 DIN EN ISO 11337: 2004-09 2 DIN EN ISO 11337:2011-04 National Annex NA (informative) Bibliography DIN EN ISO 472, Plastics Vocabulary DIN ISO 565, Test sieves Metal wire cloth, perforated metal plate and electroformed sheet Nominal sizes

13、of openings 3 DIN EN ISO 11337:2011-04 4 This page is intentionally blank EUROPEAN 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 v-laurolactam by gas chromatography

14、(ISO 11337:2010) Plastiques Polyamides Dtermination du e-caprolactame et du v-laurolactame par chromatographie en phase gazeuse (ISO 11337:2010) Kunststoffe Polyamide Gaschromatographische Bestimmung von e-Caprolactam und v-Laurolactam (ISO 11337:2010) This European Standard was approved by CEN on 1

15、0 December 2010. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may

16、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

17、 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, Luxem

18、bourg, 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 right

19、s of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 11337:2010: EContents 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 and materials.2

20、 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 5.7 Precision

21、12 5.8 Test report12 EN ISO 11337:2010 (E) DIN EN ISO 11337:2011-04 2Foreword 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 Standar

22、d 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 docu

23、ment 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

24、 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, Spa

25、in, 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. EN ISO 11337:2010 (E) DIN EN ISO 11337:2011-04 3SAFETY STATEMENT Persons using this document should be familiar with normal laborato

26、ry 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 Interna

27、tional Standard specifies a method for determining -caprolactam and -laurolactam in polyamides by gas chromatography. It is suitable particularly for the determination of -caprolactam in polyamide 6 and -laurolactam in polyamide 12. Bearing in mind that gas chromatography offers a wide range of poss

28、ible 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

29、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 amendment

30、s) 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. EN ISO 11337:2010 (E) DIN EN ISO 1133

31、7:2011-04 44 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 a

32、n 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 Apparatus and materials Ordinary laboratory apparatus, plus the following: 4.3.1 Mill, for reducing the sample to the required grain siz

33、e. 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 m and 500 m respectively, complying with the requirements of ISO 565. 4.3.3 Extraction

34、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

35、 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 cont

36、inuously; 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 of slightly smaller diameter than the crucible, with holes of diameter 0,4 mm. EN ISO 11337:2010 (E) DIN EN ISO 11337:2011-04 5EXAMPLE 2

37、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 can be satisfactorily accommodated in the Soxhlet

38、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 nece

39、ssary. 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 with 10 % (by mass) poly(ethylene glycol) 20M; a meg

40、abore 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 proved to give the same results. A capillary col

41、umn 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 Carrier gas flow rate 20 ml/minaaThis value is for th

42、e 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. E

43、N ISO 11337:2010 (E) DIN EN ISO 11337:2011-04 6b) 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

44、 produce only insignificant effects on response and sensitivity. 4.3.8 Microsyringes, with capacities from 1 l to 10 l. 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

45、(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 re

46、quired. Collect the fraction that passes through a sieve with mesh aperture 710 m (4.3.2), but not through the one with mesh 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

47、 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 -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 calcu

48、lation 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

49、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 all