DIN EN 15768-2015 Influence of materials on water intended for human consumption - GC-MS identification of water leachable organic substances German version EN 15768 2015《材料对人类生活用水.pdf

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1、May 2015 Translation by DIN-Sprachendienst.English price group 16No 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 13

2、.060.20; 67.250; 71.040.50!%B“2315891www.din.deDDIN EN 15768Influence of materials on water intended for human consumption GC-MS identification of water leachable organic substances;English version EN 15768:2015,English translation of DIN EN 15768:2015-05Einfluss von Materialien auf Wasser fr den me

3、nschlichen Gebrauch Identifizierung mittels GC-MS von durch Wasser auslaugbaren organischen Substanzen;Englische Fassung EN 15768:2015,Englische bersetzung von DIN EN 15768:2015-05Influence sur leau des matriaux en contact avec leau destine la consommationhumaine Identification par CG-SM de substanc

4、es organiques lixiviables leau;Version anglaise EN 15768:2015,Traduction anglaise de DIN EN 15768:2015-05www.beuth.deDocument comprises 36 pagesIn case of doubt, the German-language original shall be considered authoritative.04.15DIN EN 15768:2015-05 2 A comma is used as the decimal marker. National

5、 foreword This document (EN 15768:2015) has been prepared by Technical Committee CEN/TC 164 “Water supply” (Secretariat: AFNOR, France). The responsible German body involved in its preparation was the DIN-Normenausschuss Wasserwesen (DIN Standards Committee Water Practice), Working Committee NA 119-

6、07-09-01 UA Europische Prfverfahren zur trinkwasserhygienischen Eignung von Werkstoffen (Supporting standards, Mandat M/136). EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15768 January 2015 ICS 13.060.20; 67.250; 71.040.50 English Version Influence of materials on water intended for human co

7、nsumption - GC-MS identification of water leachable organic substances Influence sur leau des matriaux en contact avec leau destine la consommation humaine - Identification par CG-SM de substances organiques lixiviables leau Identifizierung mittels GC-MS von durch Wasser auslaugbaren organischen Sub

8、stanzen This European Standard was approved by CEN on 29 November 2014. 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 bibliograp

9、hical 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 made by translation under the responsibili

10、ty 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, Estonia, Finland, Former Yugoslav Republic o

11、f Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATI

12、ON EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15768:2015 EEinfluss von Materialien auf Wasser fr den menschlichen Gebrauch -E

13、N 15768:2015 (E) 2 Contents Page Foreword 4 Introduction .5 1 Scope 6 2 Normative references 6 3 Terms and definitions .6 4 Principle 9 5 Reagents .9 5.1 General 9 5.2 Required reagents .9 6 Apparatus 13 7 Storage of migration waters, procedural blanks and laboratory blanks 14 8 Method of analysis 1

14、4 8.1 Extraction procedure 14 8.2 GC-MS analysis . 15 8.2.1 Safety precautions 15 8.2.2 Mass spectrometer operating parameters . 15 8.2.3 Setting up the mass spectrometer and data system 15 8.2.4 Initial tuning and mass calibration of the mass spectrometer 15 8.3 Setting up the GC-MS system . 15 8.4

15、 GC-MS operating conditions for analysis of solvent extracts . 16 8.5 Production of required outputs from the GC-MS data system 17 9 Quality assurance (QA) and quality control (QC) procedures . 17 9.1 The mass calibration of the mass spectrometer . 17 9.2 The performance of the GC-MS system . 17 9.3

16、 The performance of the method 17 9.4 Performance of the analyst 18 9.5 Uncertainty of the method . 18 10 Expression of results . 18 10.1 Semi-quantitative estimation of concentrations of substances detected 18 10.2 Identification of substances detected 19 10.3 Reporting of results 19 11 Test report

17、 . 20 11.1 General . 20 11.2 Test results 21 Annex A (normative) Additional procedural details . 23 A.1 Checking suitability of apparatus used for concentrating solvent extracts 23 A.2 Procedure for calculation of recoveries of internal standards 23 A.3 Standard solutions for checking GC column perf

18、ormance . 24 Annex B (informative) Outline of general approach for identification of substances detected. 25 B.1 General approach - Introduction . 25 B.2 GC-MS Test Solution 25 DIN EN 15768:2015-05 EN 15768:2015 (E) 3 B.3 Typical Leachate 26 B.4 Identifying substances 26 B.5 Overloading 27 Annex C (

19、informative) Guidance on the interpretation of results 28 C.1 Introduction 28 C.2 Initial assessment of test report 28 C.3 Assessment of results of analysis 28 Annex D (informative) Guidance on the identification of substances . 30 D.1 A suggested strategy to assist in identifying substances in extr

20、acted leachates . 30 D.2 Resolution of co-eluting peaks 30 D.3 Proceeding when background subtraction does not help 31 D.4 Tentatively identifying a substance using boiling points and retention indices 31 D.5 Library search results and identifying “unknown” substances . 32 D.6 Interpretation of the

21、mass spectrum . 32 D.7 Reporting confidence in a substance identification 33 D.8 How to report alternative identifications and when this is appropriate 33 D.9 What to do if library search fails to assign a reasonable identification 34 DIN EN 15768:2015-05 EN 15768:2015 (E) 4 Foreword This document (

22、EN 15768:2015) has been prepared by Technical Committee CEN/TC 164 “Water supply”, the secretariat of which is held by AFNOR. 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 July 2015 and conflict

23、ing national standards shall be withdrawn at the latest by July 2015. 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 any or all such patent rights. This document ha

24、s been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. This document has been prepared on the basis of co-normative research project EVK1-CT 2000-00052 and work funded by DG Enterprise and Industry (Grant Agreement S12.403892). This document

25、describes methods of identification only, and should not be used or quoted as a specification. References to this document should indicate that the methods of identification used are in accordance with EN 15678:2015. According to the CEN-CENELEC Internal Regulations, the national standards organizat

26、ions 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malt

27、a, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 15768:2015-05 EN 15768:2015 (E) 5 Introduction Organic substances that migrate from products containing such substances have, when used in contact with water inten

28、ded for human consumption, the potential to cause health concerns for consumers. The potential health effects of these chemicals are assessed in three stages as follows: a) preparation of migration waters by exposing a portion of the material to water under controlled conditions; b) analysis of the

29、migration waters; c) assessment of the identities and concentrations of the substance detected. The analysis of organic substances present in migration waters can involve two different types of analytical methods as follows: d) a screening method, which allows a variety of substances to be detected

30、and a semi-quantitative assessment to be made of their concentrations; e) accurate quantitative methods for the determination of specific target substances known to be present in the chemical formulations of the materials. This standard describes the analytical procedures based upon gas chromatograp

31、hy and mass spectrometry (GC-MS) used to screen migration waters for organic substances derived from finished products such as pipes, protective coatings, membranes, etc. This method is suitable for migration waters from all products that can potentially release organic chemicals into water when the

32、y are used in contact with water intended for human consumption, and which are the subject of an application for approval by the national regulatory body. It may be one of several methods that form part of the overall approval process. The method may also be used as part of an approval audit process

33、. The method does not provide accurate quantitative results and other analytical methods are recommended for accurate quantitative determination of specific target substances. DIN EN 15768:2015-05 EN 15768:2015 (E) 6 1 Scope This European Standard describes a method for detecting and identifying org

34、anic chemicals that are amenable to GC-MS analysis using the procedures described and which can migrate from a product into water intended for human consumption. This European Standard does not provide all the necessary tools to completely identify all the substances that are detected. A method of s

35、emi-quantitatively estimating the concentrations of the organic substances detected is also provided, however, concentrations should only be seen as indicative. NOTE The method to be used for the preparation of migration waters is specified by separate ENs, as noted below. 2 Normative references EN

36、12873-1, Influence of materials on water intended for human consumption - Influence due to migration - Part 1: Test method for factory-made products made from or incorporating organic or glassy (porcelain/vitreous enamel) materials EN 12873-2, Influence of materials on water intended for human consu

37、mption - Influence due to migration - Part 2: Test method for non-metallic and non-cementitious site-applied materials EN 12873-3, Influence of materials on water intended for human consumption - Influence due to migration - Part 3: Test method for ion exchange and adsorbent resins EN 12873-4, Influ

38、ence of materials on water intended for human consumption - Influence due to migration - Part 4: Test method for water treatment membranes EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696) 3 Terms and definitions For the purposes of this document, the follo

39、wing terms and definitions apply. 3.1 u atomic mass unit, defined as 1/12 of the mass of a single atom of carbon-12 in the gas phase (i.e. unbound), at rest and in its ground state 3.2 asymmetry factor Asmeasure of the absorption of a compound during gas chromatographic analysis Note 1 to entry: The

40、 asymmetry factor (As) can be derived from Formula (1). +=(a b)Abs2(1) where a is the distance from the leading edge of the peak at the point on the baseline where the perpendicular dropped from the peak maximum crosses it; b is the corresponding distance from the trailing edge of the peak. Locate t

41、he apex of the peaks that require their asymmetry values calculated. For each peak, drop a perpendicular line down at a right-angle to the baseline. DIN EN 15768:2015-05 EN 15768:2015 (E) 7 Note 2 to entry: Some manufacturers GC-MS software packages allow the calculation of peak asymmetries to be pr

42、oduced automatically. Check the criteria used for the measurement, as some packages perform the calculation at 5 % of the peak height. 3.3 electron impact ionization ionization by a beam of electrons 3.4 GC-MS analytical instrument comprising a gas chromatograph (GC) linked to a mass spectrometer (M

43、S) 3.5 GC-MS general survey analysis acquisition of a series of mass spectra (up to several thousand) during the course of a gas chromatographic run, by operating the mass spectrometer in a continuous cyclic scanning mode over a wide m/z range 3.6 injection standard organic substance added to the fi

44、nal solvent extract prior to analysis Note 1 to entry: An injection standard is added to allow the recoveries of the internal standards to be calculated, by providing a means of normalizing the GC-MS responses for solvent extracts and GC-MS standards. 3.7 internal standard organic substance added to

45、 the migration water at a known concentration prior to the commencement of the analysis Note 1 to entry: Internal standards are added for the following reasons (a) to demonstrate that the analysis has been undertaken successfully, and (b) to provide a reference to allow other substances detected to

46、be quantified. Ideally, the internal standards should not be present in the migration waters being analysed; for this reason, isotopically labelled standards are used. 3.8 test water water used to prepare the migration water, as specified in EN 12873-1, EN 12873-2, EN 12873-3 or EN 12873-4 depending

47、 on the material being tested 3.9 laboratory blank water, as specified in EN ISO 3696, known to contain negligible levels of contamination, to which internal standards (3.7) have been added and which is then analysed in the same way as the migration water Note 1 to entry: Laboratory blanks are used

48、to check for potential contamination of either migration waters or solvent extracts which may occur within the laboratory during the course of the analysis. 3.10 migration water aqueous solution that results from leaving test water in contact with the test material under the specified test condition

49、s 3.11 procedural blank aqueous solution that results from leaving test water in contact with tanks or containers identical to those used to prepare the migration water in the absence of the test material DIN EN 15768:2015-05 EN 15768:2015 (E) 8 Note 1 to entry: Procedural blanks are used to check for potential contamination of migration waters that can arise during the migration procedure. For example, substances can migrate from the tanks or containers used into the test water, or aerial contamination can occur if volatile substances are present in t