DIN EN ISO 12010-2014 Water quality - Determination of short-chain polychlorinated alkanes (SCCPs) in water - Method using gas chromatography-mass spectrometry (GC-MS) and negative.pdf

1、July 2014Translation by DIN-Sprachendienst.English price group 15No 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、.060.50!%7H.“2203711www.din.deDDIN EN ISO 12010Water quality Determination of short-chain polychlorinated alkanes (SCCPs) in water Method using gas chromatography-mass spectrometry (GC-MS) andnegative-ion chemical ionization (NCI) (ISO 12010:2012);English version EN ISO 12010:2014,English translatio

3、n of DIN EN ISO 12010:2014-07Wasserbeschaffenheit Bestimmung von kurzkettigen Chloralkanen (SCCP) in Wasser Verfahren mittels Gaschromatographie-Massenspektrometrie (GC-MS) und negativerchemischer Ionisation (NCI) (ISO 12010:2012);Englische Fassung EN ISO 12010:2014,Englische bersetzung von DIN EN I

4、SO 12010:2014-07Qualit de leau Dtermination des alcanes polychlors chane courte (SCCP) dans leau Mthode par chromatographie gazeuse-spectromtrie de masse (CG-SM) avec ionisationchimique ngative (ICN) (ISO 12010:2012);Version anglaise EN ISO 12010:2014,Traduction anglaise de DIN EN ISO 12010:2014-07w

5、ww.beuth.deDocument comprises 36 pagesIn case of doubt, the German-language original shall be considered authoritative.07.14 DIN EN ISO 12010:2014-07 2 A comma is used as the decimal marker. National foreword The text of ISO 12010:2012 has been prepared by Technical Committee ISO/TC 147 “Water quali

6、ty” and has been taken over as EN ISO 12010:2014 by Technical Committee CEN/TC 230 “Water analysis” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Wasserwesen (Water Practice Standards Committee), Working Committee NA 119-01-03-02-11 AK C

7、hlorparaffine of NA 119-01-03 AA Wasseruntersuchung. Designation of the method: Determination of short-chain polychlorinated alkanes (SCCPs) in water Method using gas chromatography-mass spectrometry (GC-MS) and negative-ion chemical ionization (NCI) (H 47): Method DIN EN ISO 12010 H 47 This documen

8、t has been prepared under mandate M/424 “Development and enhancement of European standards to determine the chemical and ecological water quality in support of the Water Framework Directive (WFD)” (Directive 2000/60/EC of the European Parliament and of the Council of 23 October 2000 establishing a f

9、ramework for Community action in the field of water policy*) which was given to CEN by the European Commission. The method specified in this standard supports compliance with the requirements given in Annex I of the Directive 2008/105/EC of the European Parliament and of the Council of 16 December 2

10、008 on environmental quality standards in the field of water policy*). The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 5667-1 DIN EN ISO 5667-1 ISO 5667-3 DIN EN ISO 5667-3 ISO 8466-1 DIN 38402-51 *)Registered in the DITR database of DI

11、N Software GmbH, obtainable from: Beuth Verlag GmbH, 10772 Berlin. DIN EN ISO 12010:2014-07 3 National Annex NA (informative) Bibliography DIN 38402-51, German standard methods for the examination of water, waste water and sludge; general information (group A) Calibration of analytical methods, eval

12、uation of analytical results and linear calibration functions used to determine the performance characteristics of analytical methods (A 51) DIN EN ISO 5667-1, Water quality Sampling Part 1: Guidance on the design of sampling programmes and sampling techniques DIN EN ISO 5667-3, Water quality Sampli

13、ng Part 3: Preservation and handling of water samples Directive 2000/60/EC of the European Parliament and of the Council of 23 October 2000 establishing a framework for Community action in the field of water policy Directive 2008/105/EC of the European Parliament and of the Council of 16 December 20

14、08 on environmental quality standards in the field of water policy, amending and subsequently repealing Council Directives 82/176/EEC, 83/513/EEC, 84/156/EEC, 84/491/EEC, 86/280/EEC and amending Directive 2000/60/EC DIN EN ISO 12010:2014-07 4 This page is intentionally blank EUROPEAN STANDARD NORME

15、EUROPENNE EUROPISCHE NORM EN ISO 12010 April 2014 ICS 13.060.50 English Version Water quality - Determination of short-chain polychlorinated alkanes (SCCPs) in water - Method using gas chromatography-mass spectrometry (GC-MS) and negative-ion chemical ionization (NCI) (ISO 12010:2012) Qualit de leau

16、 - Dtermination des alcanes polychlors chane courte (SCCP) dans leau - Mthode par chromatographie gazeuse-spectromtrie de masse (CG-SM) avec ionisation chimique ngative (ICN)Wasserbeschaffenheit - Bestimmung von kurzkettigen Chloralkanen (SCCP) in Wasser - Verfahren mittels Gaschromatographie-Massen

17、spektrometrie (GC-MS) und negativer chemischer Ionisation (NCI) (ISO 12010:2012) This European Standard was approved by CEN on 11 April 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 nat

18、ional 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 in three official versions (English, French, German). A ve

19、rsion 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 standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus,

20、 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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdo

21、m. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 12010

22、:2014 E(ISO 12010:2012) Contents Page DIN EN ISO 12010:2014-07 EN ISO 12010:2014 (E) 2 Foreword 3 Introduction .4 1 Scope 5 2 Normative references 5 3 Principle 5 4 Interferences 6 5 Reagents and standards .6 6 Apparatus .10 7 Sampling and sample pretreatment .11 8 Procedure .11 8.1 Extraction with

23、liquid-liquid extraction method .11 8.2 Extraction of samples with higher content of suspended matter 11 8.3 Extract clean-up .12 8.4 Measurement and integration of the chromatogram .13 8.5 Calibration 13 9 Expression of results 16 10 Test report 16 Annex A (informative) Additional quality control c

24、heck solutions 17 Annex B (informative) Explanation of the calibration of the sum of SCCPs with multiple linear regression .18 Annex C (informative) Typical GC-MS conditions .23 Annex D (informative) Typical chromatograms of standard solutions 1 g/ml 26 Annex E (informative) Presentation of goodness

25、 of fit .27 Annex F (informative) Example for recoveries of quality assurance solutions 28 Annex G (informative) Chromatogram of a real water sample with a sum of SCCPs concentration of 2,59 g/l 29 Annex H (informative) Precision data 31 Bibliography 32 Foreword The text of ISO 12010:2012 has been p

26、repared by Technical Committee ISO/TC 147 “Water quality” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 12010:2014 by Technical Committee CEN/TC 230 “Water analysis” the secretariat of which is held by DIN. This European Standard shall be given the sta

27、tus of a national standard, either by publication of an identical text or by endorsement, at the latest by October 2014, and conflicting national standards shall be withdrawn at the latest by October 2014. Attention is drawn to the possibility that some of the elements of this document may be the su

28、bject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. According to the CEN-CENELEC Internal Regulations,

29、the national standards organizations 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, Lat

30、via, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 12010:2012 has been approved by CEN as EN ISO 12010:2014 without any modification. DIN EN ISO 12010:201

31、4-07 EN ISO 12010:2014 (E) 3 IntroductionThe user should be aware that particular problems might require the specifications of additional marginal conditions.DIN EN ISO 12010:2014-07 EN ISO 12010:2014 (E) 4 WARNING Persons using this International Standard should be familiar with normal laboratory p

32、ractice. This International Standard does not purport 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.IMPORTANT It is abs

33、olutely essential that tests conducted in accordance to this International Standard be carried out by suitably qualified staff.1 ScopeThis International Standard specifies a method for the quantitative determination of the sum of short-chain polychlorinated n-alkanes, also known as short-chain polyc

34、hlorinated paraffins (SCCPs), in the carbon bond range n-C10to n-C13inclusive, in mixtures with chlorine mass fractions (“contents”) between 49 % and 67 %, including approximately 6 300 of approximately 8 000 congeners.This method is applicable to the determination of the sum of SCCPs in unfiltered

35、surface water, ground water, drinking water and waste water using gas chromatography-mass spectrometry with electron capture negative ionization (GC-ECNI-MS).The method can be applied to samples containing 0,1 g/l to 10 g/l. Depending on the waste water matrix, the lowest detectable concentration is

36、 estimated to be 0,1 g/l.2 Normative referencesThe 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 amendments) applies.ISO

37、 5667-1, Water quality Sampling Part 1: Guidance on the design of sampling programmes and sampling techniquesISO 5667-3, Water quality Sampling Part 3: Preservation and handling of water samplesISO 8466-1, Water quality Calibration and evaluation of analytical methods and estimation of performance c

38、haracteristics Part 1: Statistical evaluation of the linear calibration functionISO/TS 13530, Water quality Guidance on analytical quality control for chemical and physicochemical water analysis3 PrincipleDetermination of the sum of SCCPs in the carbon bond range n-C10to n-C13inclusive, in technical

39、 and environmental transposed mixtures with chlorine mass fractions (“contents”) between 49 % and 67 % (e.g. approximately 3 to 10 chlorine atoms per molecule) and independent of the C-number distribution pattern of the congeners. No recognition of the chlorine content is necessary.SCCPs in whole wa

40、ter samples are fortified with an internal standard and extracted using liquid-liquid extraction with an organic solvent. The sample enrichment procedure is followed by a clean-up procedure to eliminate interfering compounds. Gas chromatography (GC) is undertaken using a short capillary column withi

41、n a short DIN EN ISO 12010:2014-07 EN ISO 12010:2014 (E) 5 retention time range. The detection of selected mass fragments is carried out using mass spectrometry (MS) in selected ion-monitoring mode using electron capture negative ionization mode (ECNI). The selection of the mass fragments is specifi

42、c for the variety of technical mixtures as well as for their chlorine content and C-number distribution patterns. Alternative mass fragment combinations for qualification are also given in this International Standard.The selected ion chromatogram is integrated over the full retention time range of t

43、he SCCPs. The quantification of the sum of SCCPs is carried out after establishing a calibration by multiple linear regression, measuring solutions of different technical mixtures fortified with an internal standard.The calibration requires a minimum of three different composed standard mixtures, ea

44、ch of which resembles the C-number distribution pattern and chlorine content of different technical mixtures. This is to reflect the variety of chlorine contents and C-number distribution patterns of technical SCCP mixtures and SCCP levels found in environmental samples, which cannot be described by

45、 a single defined standard substance.The method allows a quantification of the sum of SCCPs expected to be within an expanded measurement uncertainty of less than 50 %.4 InterferencesNon-specific matrix interferences, as well as interferences from other environmental situations, are dealt with using

46、 the given clean-up procedure. Following the entire procedure, including the concentration factor of approximately 5 000, the following pollutants have been tested and found not to cause interferences below the following concentrations.Potential interfering compounds Highest concentration level at w

47、hich no interferences higher than the limit of detection are detectedAroclor 1262a0,5 g/lAroclor 1242a0,5 g/lAroclor 1221a1 g/lCampheclor 0,2 g/lHalowax 1014a1 g/lHalowax 1051a1 g/lTechnical chlordane 0,5 g/lMCCP (medium-chain chlorinated n-alkanes) 42 % 0,2 g/lMCCP (medium-chain chlorinated n-alkan

48、es) 52 % 0,2 g/lMCCP (medium-chain chlorinated n-alkanes) 57 % 0,2 g/laProduct available commercially. This information is given for the convenience of users of this document and does not constitute an endorsement by ISO of this product.If the clean-up procedure is repeated, interferences can be fur

49、ther reduced.5 Reagents and standardsUse solvents and reagents of sufficient purity, i.e. with negligibly low concentrations of SCCPs (e.g. lower than the limit of detection of the method).NOTE Check blanks regularly over the entire procedure to ensure they are suitable and establish proper analytical control.DIN EN ISO 12010:2014-07 EN ISO 12010:2014 (E) 6 5.1 Solvents for extraction and preparation of stock solutions. T