DIN EN 12868-2017 Child use and care articles - Method for determining the release of N-nitrosamines and N-nitrosatable substances from elastomer or rubber teats and soothers Germa.pdf

1、April 2017 English price group 18No 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 97.190!%c5“2649918www.din.deDIN EN

2、 12868Child use and care articles Method for determining the release of Nnitrosamines and Nnitrosatable substances from elastomer or rubber teats and soothers;English version EN 12868:2017,English translation of DIN EN 12868:2017-04Artikel fr Suglinge und Kleinkinder Verfahren zur Bestimmung der Abg

3、abe von NNitrosaminen und Nnitrosierbaren Stoffen aus Flaschen und Beruhigungssaugern aus Elastomeren oder Gummi;Englische Fassung EN 12868:2017,Englische bersetzung von DIN EN 12868:2017-04Articles de puriculture Mthode pour dterminer la libration de Nnitrosamines et de substances Nnitrosables par

4、les ttines et les sucettes en lastomre ou en caoutchouc;Version anglaise EN 12868:2017,Traduction anglaise de DIN EN 12868:2017-04SupersedesDIN EN 12868:199912www.beuth.deDocument comprises 48 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered

5、authoritative.04.17 DIN EN 12868:2017-04 2 A comma is used as the decimal marker. National foreword This standard includes safety requirements. This document (EN 12868:2017) has been prepared by Technical Committee CEN/TC 252 “Child use and care articles” (Secretariat: AFNOR, France). The responsibl

6、e German body involved in its preparation was DIN-Normenausschuss Sicherheitstechnische Grundstze (DIN Standards Committee Safety Design Principles), Working Committee NA 095-05-02 AA “Child use and care articles Feeding, drinking, sucking and similar functions”. The DIN Standard corresponding to th

7、e International Standard referred to in this document is as follows: ISO/TR 22971:2005 DIN ISO/TR 22971:2012-02 Amendments This standard differs from DIN EN 12868:1999-12 as follows: a) the sample preparation has been simplified, reducing this source of interlaboratory variation; b) the pre-boiling

8、and migration steps have been separated for the determination of N-nitrosamines and of N-nitrosatable substances, allowing use of the same vessels and avoiding the possible loss of migrated substances; c) the amount of samples has been adjusted, increasing the sample mass for the determination of N-

9、nitrosatable substances; d) standard methods for extracting N-nitrosamines from the aqueous migrates have been simplified and restricted to one method, reducing interlaboratory varability; e) a rinsing step has been introduced to avoid variability due to possible loss of analytes; f) the calculation

10、 of results has been revised taking into account state-of-the-art analytical standards; g) the results and the application of analytical tolerances have been confirmed; h) alternative methods have been taken into account and quality criteria have been included for their application. Previous edition

11、s DIN EN 12868: 1999-12 DIN EN 12868:2017-04 3 National Annex NA (informative) Bibliography DIN ISO/TR 22971:2012-02, Accuracy (trueness and precision) of measurement methods and results Practicalguidance for the use of ISO 57252:1994 in designing, implementing and statistically analysinginterlabora

12、tory repeatability and reproducibility results (ISO/TR 22971:2005) DIN EN 12868:2017-04 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 12868 January 2017 ICS 97.190 Supersedes EN 12868:1999English Version Child use and care articles - Method for determining t

13、he release of N-nitrosamines and N-nitrosatable substances from elastomer or rubber teats and soothers Articles de puriculture - Mthode pour dterminer la libration de N-nitrosamines et de substances N-nitrosables par les ttines et les sucettes en lastomre ou en caoutchouc Artikel fr Suglinge und Kle

14、inkinder - Verfahren zur Bestimmung der Abgabe von N-Nitrosaminen und N-nitrosierbaren Stoffen aus Babysaugern aus Elastomeren und Gummi This European Standard was approved by CEN on 30 October 2016. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the condit

15、ions 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

16、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 standa

17、rds bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovak

18、ia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2017 CEN All rights of exploitation in any form and by any means

19、reserved worldwide for CEN national Members. Ref. No. EN 12868:2017 EEN 12868:2017 (E) 2 Contents Page European foreword . 5 Introduction 6 1 Scope 7 2 Normative references 7 3 Terms and definitions . 7 4 Principle . 8 5 Reagents . 8 Table 1 Salts and their masses for 1 l of artificial saliva salt s

20、olution 9 6 Apparatus . 9 7 Standard Solutions of N-nitrosamines 11 7.1 General . 11 7.2 N-nitrosamines identified in teats . 11 Table 2 Names, abbreviated names and CAS numbers of N-nitrosamines relevant for this standard, and the necessary limits of quantification 11 7.3 Calibration solutions (for

21、 detector response) . 12 7.4 N-nitrosamine used as internal standard . 12 8 Procedure 12 8.1 General . 12 8.2 Sample Preparation. 13 8.3 Sample A (for determination of N-nitrosatable substances) 14 8.3.1 Preparation and pre-boiling 14 8.3.2 Preparation of Migrate A (for determining N-nitrosatable su

22、bstances) See A.2 14 8.3.3 Nitrosation of Migrate A (see A.3) and preparation of Solution A 15 8.4 Sample B (for determination of N-nitrosamines) . 15 8.4.1 Preparation and pre-boiling 15 8.4.2 Preparation of Migrate B (for determining N-nitrosamines). 15 8.4.3 Preparation of Solution B 15 8.5 Prepa

23、ration of extraction columns for Solutions A and B . 15 8.6 Extraction of N-nitrosamines . 16 8.6.1 From Solution A 16 8.6.2 From Solution B 16 8.7 Concentration of N-nitrosamines . 16 8.7.1 In Extract A . 16 8.7.2 In Extract B . 17 8.8 Blank Test . 17 8.9 Analysis 17 8.9.1 Calibration function 17 8

24、.9.2 Determination of sample concentration . 18 9 Calculation of results 18 9.1 General . 18 9.2 Variability of results and calculation of means . 19 9.2.1 Requirements for variability . 19 9.2.2 Test for variability . 19 9.2.3 Calculation of means . 19 DIN EN 12868:2017-04 EN 12868:2017 (E) 3 9.3 A

25、mount of total N-nitrosatable substances migrating from Sample A, analysed and expressed as N-nitrosamines from Concentrate A . 20 9.4 Amount of total N-nitrosamines migrating from Sample B, analysed and expressed as N-nitrosamines from Concentrate B . 20 10 Confirmation of N-nitrosamines . 20 11 An

26、alytical tolerances . 21 11.1 General . 21 11.2 Analytical tolerances (see Annex F) . 21 12 Compliance 21 13 Test report 21 Annex A (informative) Rationales . 23 A.1 General . 23 A.2 Migration Conditions (see 8.3.2) . 23 A.3 Nitrosation conditions (see 8.3.3) 23 A.4 Weight of sample used (see 8.3.1)

27、 23 A.5 Separate migrations (see 8.3.2 and 8.3.3) . 24 A.6 Duplicate tests (see 8.1) . 24 A.7 TEA and alternative detectors . 24 A.8 Deviations (see 9.2, 9.3 and 11) 25 A.9 Main differences between this standard and EN 71-12 3 . 25 Annex B (informative) Suitable gas chromatographic method . 26 Figur

28、e B.1 GC Chromatogram of a calibration solution recorded by TEA . 27 Annex C (normative) Example of results calculation and test report . 28 C.1 General . 28 C.2 Example for variability testing and means calculation for analytical results 28 Table C.1 Example for variability testing and means calcul

29、ation for Sample A 29 Table C.2 Example for variability testing and means calculation for Sample B 29 C.3 Results calculation and results table for test report . 30 Table C.3 Example of Final results and their representation 31 C.4 Other Information for test report . 31 Annex D (informative) Alterna

30、tive Methods . 32 D.1 General . 32 D.2 Liquid Chromatography (LC) 32 Table D.1 Gradient profile for the given HPLC conditions 33 D.3 MS/MS conditions . 33 Table D.2 Suitable MRM Transitions for MS/MS conditions 34 D.4 Confirmation and quantification of detected N-nitrosamines . 34 Table D.3 Maximum

31、permitted tolerances for relative ion intensities 34 DIN EN 12868:2017-04 EN 12868:2017 (E) 4 Annex E (informative) Justification of an N-nitrosamine specific adjustment for NDiNA 36 Annex F (informative) Summary of the 2015 validation trial . 38 F.1 Outline 38 Table F.1 Sample Descriptions for Vali

32、dation Trial 38 F.2 Initial statistical analysis N-nitrosatable substances 38 Table F.2 Mean data and calculations for total N-nitrosatable substances 38 F.3 Reproducibility Limit for N-nitrosatable substances 39 Table F.3 Overall means for total N-nitrosatable substances by method . 39 Table F.4 Re

33、producibility limits for total N-nitrosatable substances by method 39 Table F.5 Reproducibility limits (mg/kg) for individual N-nitrosatable substances . 40 F.4 Consideration of the NDiNA Reproducibility limit . 40 F.5 Initial statistical analysis N-nitrosamines . 40 Table F.6 Mean data and calculat

34、ions for total N-nitrosamines . 40 F.6 Variability between Determinations 41 Table F.7 Summary of average repeatability limits for duplicate determinations of N-nitrosatable substances and N-nitrosamines 41 F.7 Summary of Conclusions and implications for EN 12868 42 Table F.8 Methods used by laborat

35、ories (after removal of outliers) . 42 Bibliography . 44 DIN EN 12868:2017-04 EN 12868:2017 (E) 5 European foreword This document (EN 12868:2017) has been prepared by Technical Committee CEN/TC 252 “Child use and care articles”, the secretariat of which is held by AFNOR. This European Standard shall

36、 be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by July 2017, and conflicting national standards shall be withdrawn at the latest by July 2017. Attention is drawn to the possibility that some of the elements of this document ma

37、y be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 12868:1999. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. Compared to EN

38、12868:1999, this document contains the following significant changes: The common practice to perform at least double determinations has been made a requirement, including the preparation of samples. Sample preparation has been defined and simplified, reducing this source of interlaboratory variation

39、. The pre-boiling and migration steps have been separated for the determination of N-nitrosamines and of N-nitrosatable substances, allowing use of the same vessels and avoiding the possible loss of migrated substances. Amounts of sample have been adjusted, increasing the sample mass for the determi

40、nation of N-nitrosatable substances. Extraction of N-nitrosamines from the aqueous migrates has been restricted to one method, reducing interlaboratory variability. A rinsing step has been introduced to avoid variability due to possible loss of analytes. The calculation of results has been revised i

41、ncluding a repeatability requirement for multiple determinations and taking into account state of the art analytical procedures. The confirmation of N-nitrosamines and application of analytical tolerances have been clarified including a N-nitrosamine specific adjustment as suggested by the validatio

42、n trial. According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, Fr

43、ance, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 12868:2017-04 EN 12868:2017 (E) 6 Introduction It has been show

44、n that feeding teats and soothers made of elastomer or rubber may release N-nitrosamines and substances capable of being converted into N-nitrosamines (N-nitrosatable substances). The Scientific Committee for Food of the European Union has given the opinion that N-nitrosamines and N-nitrosatable sub

45、stances may endanger human health owing to their toxicity 5. Hence in 1993, the European Commission issued Directive 93/11/EEC 1 controlling rubber and elastomeric teats and soothers releasing these substances. The Directive also provided basic rules for determining the release of these substances a

46、nd criteria for the method of analysis to be adopted. The purpose of this European Standard is to provide a detailed analytical method for the identification and determination of N-nitrosamines and N-nitrosatable substances released from teats and soothers in order that compliance with the requireme

47、nts of Directive 93/11/EEC may be tested. This method has been validated. The testing laboratories should take special care to observe occupational health and safety standards. Persons using this European Standard should be familiar with normal laboratory practice. This European Standard does not pu

48、rport 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 ensure compliance with any national regulatory conditions. DIN EN 12868:2017-04 EN 12868:2017 (E) 7 1 Scope This European Sta

49、ndard specifies the method for determining N-nitrosamines and N-nitrosatable substances released from elastomer or rubber teats in contact with artificial saliva salt solution for testing compliance with Directive 93/11/EEC. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edi