DIN EN 1948-4-2014 Stationary source emissions - Determination of the mass concentration of PCDDs PCDFs and dioxin-like PCBs - Part 4 Sampling and analysis of dioxin-like PCBs Germ.pdf

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1、March 2014 Translation by DIN-Sprachendienst.English price group 24No 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、13.040.40!%,B“2099531www.din.deDDIN EN 1948-4Stationary source emissions Determination of the mass concentration of PCDDs/PCDFs anddioxin-like PCBs Part 4: Sampling and analysis of dioxin-like PCBs;English version EN 1948-4:2010+A1:2013,English translation of DIN EN 1948-4:2014-03Emissionen aus stat

3、ionren Quellen Bestimmung der Massenkonzentration von PCDD/PCDF und dioxin-hnlichen PCB Teil 4: Probenahme und Analyse dioxin-hnlicher PCB;Englische Fassung EN 1948-4:2010+A1:2013,Englische bersetzung von DIN EN 1948-4:2014-03missions de sources fixes Dtermination de la concentration massique en PCD

4、D/PCDF et PCB de type dioxine Partie 4: Prlvement et analyse des PCB de type dioxine;Version anglaise EN 1948-4:2010+A1:2013,Traduction anglaise de DIN EN 1948-4:2014-03SupersedesDIN EN 1948-4:2010-12www.beuth.deDocument comprises 7 pagesIn case of doubt, the German-language original shall be consid

5、ered authoritative.This standard has been included in the VDI/DIN Handbook on air quality, Volume 5. 603.14DIN EN 1948-4:2014-03 2 A comma is used as the decimal marker. National foreword This document (EN 1948-4:2010+A1:2013) has been prepared by Technical Committee CEN/TC 264 “Air quality”, Workin

6、g Group WG 1 “Dioxins Emissions” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Kommission Reinhaltung der Luft (KRdL) im VDI und DIN Normenausschuss (Commission on Air Pollution Prevention of VDI and DIN Standards Committee), Working Group NA 134-04-01-

7、13 UA Messen von PCB (Emission) of Section IV Umweltmesstechnik. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association, and supports essential requirements of EU Directive(s) (see informative Annex ZA). The precision and the p

8、erformance characteristics of the measurement of PCBs were determined between 2006 and 2008 with the active participation of German sampling and analytical laboratories in a comparison and validation trial at both a waste incinerator and a shredder plant, sponsored by the European Commission and the

9、 European Free Trade Association. This European Standard DIN EN 1948-4, Sampling and analysis of dioxin-like PCBs supplements EN 1948-1, Sampling of PCDDs/PCDFs, EN 1948-2, Extraction and clean-up of PCDDs/PCDFs, EN 1948-3, Identification and quantification of PCDDs/PCDFs and CEN/TS 1 948-5, L ong-t

10、erm s ampling o f P CDDs/PCDFs a nd P CBs, and serves as a basis for the determination of PCBs as the reference procedure. This document additionally includes important guidance for sampling and analysis over a broad concentration range gained during the validation measurements. Amendments This stan

11、dard differs from DIN EN 1948-4:2010-12 as follows: a) in Subclause 6.2, reference to EN 1948-1 has been added: The sampling standards (see Table 1) shall be added to the different sampling media before sampling and the extraction standards shall be added to the samples before extraction “(see EN 19

12、48-1).”; b) Table 1, footnote b), a second sentence has been added: Sampling Standards: Attention should be paid to possible co-elution problems of PCB 127 and PCB 105 on certain commercially available columns. “If the co-elution problems cannot be avoided, the sampling standard PCB 127 may be omitt

13、ed.” Previous editions DIN CEN/TS 1948-4: 2007-10 DIN EN 1948-4: 2010-12 DIN EN 1948-4:2014-03 3 National Annex NA (informative) Bibliography VDI 2464 Part 1, Ambient air measurement Indoor air measurement Measurement of polychlorinated biphenyls (PCBs) GC/MS method for PCB 28, 52, 101,138, 153, 180

14、 VDI 2464 Part 2, Ambient air measurement Indoor air measurement Measurement of polychlorinated biphenyls (PCBs) HR-GC/HR-MS method for coplanar PCBs VDI 2464 Part 3, Ambient air measurement Indoor air measurement Measurement of polybrominated diphenylether, hexabromocyclododecane and hexabromobenze

15、ne VDI 3498 Part 1, Ambient air measurement Indoor air measurement Measurement of polychlorinated dibenzo-p-dioxins and dibenzofurans: Method using large filters VDI 3498 Part 2, Ambient air measurement Indoor air measurement Measurement of polychlorinated dibenzo-p-dioxins and dibenzofurans: Method

16、 using small filters VDI 3499 Part 1, Emission measurement Determination of polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs) Dilution method; Example of application of DIN EN 1948 for the concentration range 0,1 ng I-TEQ/m3; Determination in filter dust, ash and slag VDI 3499 Part

17、 2, Emission measurement Determination of polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs) Filter/condenser method; Example of application of DIN EN 1948 for the concentration range 0,1 ng I-TEQ/m3VDI 3499 Part 3, Emission measurement Determination of polychlorinated dibenzo-p-dio

18、xins (PCDDs) and dibenzofurans (PCDFs) Cooled probe method; Example of application of DIN EN 1948 for the concentration range 0,1 ng I-TEQ/m3DIN EN 1948-4:2014-03 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 1948-4:2010+A1 December 2013 ICS 13.040.40 Supers

19、edes EN 1948-4:2010English Version Stationary source emissions - Determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs - Part4:Sampling and analysis of dioxin-like PCBs missions de sources fixes - Dtermination de la concentration massique en PCDD/PCDF et PCB de type dioxine - P

20、artie 4: Prlvement et analyse des PCB de type dioxine Emissionen aus stationren Quellen - Bestimmung der Massenkonzentration von PCDD/PCDF und dioxin-hnlichen PCB - Teil 4: Probenahme und Analyse dioxin-hnlicher PCB This European Standard was approved by CEN on 28 August 2010 and includes Amendment

21、1 approved by CEN on 23 October 2013. 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 n

22、ational 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 responsibility of a CEN member into its own la

23、nguage 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 of Macedonia, France, Germany, Gree

24、ce, 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 NORMALISATION EUROPISCHES KOMITEE FR NORMUNG

25、CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 1948-4:2010+A1:2013 EEN 1948-4:2010+A1:2013 (E) 2 Contents Page Foreword 4 Introduction .5 1 Scope 6 2 Normative

26、references 7 3 Terms and definitions .7 4 Symbols and abbreviations . 10 4.1 General . 10 4.2 Polychlorinated biphenyls . 11 5 Principle of the measurement procedure . 11 6 Device, materials and 13C12-labelled standards . 12 6.1 Device and materials 12 6.2 13C12-labelled standards . 12 7 Safety meas

27、ures . 13 8 Measurement procedure 13 8.1 Sampling 13 8.2 Extraction 13 8.3 Clean-up . 14 8.4 Final concentration of the sample extracts . 15 8.5 Addition of recovery standards . 15 8.6 Principle of identification and quantification . 15 8.7 Calibration of the HRGC/HRMS . 16 8.8 Quantification of HRG

28、C/HRMS results . 18 8.8.1 Quantification of the sample . 18 8.8.2 Calculation of the recovery rates of the extraction standards 18 8.8.3 Calculation of the recovery rates of the sampling standards 19 8.9 Calculation of the measurement results 20 8.10 Analytical report 20 9 Method validation . 21 9.1

29、 General . 21 9.2 Validation of sampling . 22 9.3 Validation of Analytical Extraction and Clean-up 22 9.3.1 Extraction 22 9.3.2 Clean-up . 22 10 Quality control requirements for the measurement 22 10.1 Use of a validated method . 22 10.2 Use of 13C12-labelled standards . 23 10.3 Minimum requirements

30、 for sampling 23 10.4 Minimum requirements for extraction and clean-up . 24 10.5 Minimum requirements for identification of PCB congeners 24 10.6 Minimum requirements for quantification 25 11 Quality assurance criteria for extraction/clean-up/quantification procedure blanks 26 11.1 Analytical blank.

31、 26 11.2 HRGC/HRMS blank . 26 DIN EN 1948-4:2014-03 EN 1948-4:2010+A1:2013 (E) 3 12 Performance characteristics 27 12.1 General . 27 12.2 Results of the validation campaign . 27 13 Interferences (informative) . 28 Annex A (informative) Toxicity and toxic equivalency 30 Annex B (informative) Examples

32、 of extraction and clean-up procedures 32 B.1 Example for clean-up of PCB and the separation from PCDD/PCDFs . 32 B.1.1 General . 32 B.1.2 Chromatography column I 34 B.1.3 Chromatography column II . 34 B.1.4 Additional clean-up I . 34 B.1.5 Additional clean-up II 35 B.1.5.1 General . 35 B.1.5.2 Carb

33、on Column 35 B.1.5.3 Preparation . 35 B.1.6 Addition of the recovery standard . 35 B.1.7 HRGC/HRMS-analysis . 35 B.2 Description of extraction and clean-up procedures used in the validation campaign 41 Annex C (informative) Evaluation of the performance characteristics . 43 C.1 General . 43 C.2 Inte

34、rlaboratory comparison study of the analytical method . 43 C.3 Accuracy. 44 C.4 Limits of detection (LOD) and limits of quantification (LOQ) . 46 C.5 Recovery. 48 C.6 Breakthrough . 49 Annex D (informative) Recommendations for measuring high concentrations of dioxin-like PCBs 51 Annex E (informative

35、) Possible interferences in dioxin-like PCB analysis 52 Annex F (informative) Measurement of the marker PCBs 28, 52, 101, 138, 153, and 180 in addition to the 12 dioxin-like PCBs 56 Annex G (informative) Measurement of hexachlorobenzene (HCB) 59 Annex H (informative) Significant technical changes .

36、60 Annex ZA (informative) Relationship between this European Standard and the essential requirements of EU Directives . 61 Bibliography 62 DIN EN 1948-4:2014-03 EN 1948-4:2010+A1:2013 (E) 4 Foreword This document (EN 1948-4:2010+A1:2013) has been prepared by Technical Committee CEN/TC 264 “Air quali

37、ty”, the secretariat of which is held by DIN. 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 June 2014, and conflicting national standards shall be withdrawn at the latest by June 2014. Attention

38、 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 includes Amendment 1 approved by CEN on 21 October 2013. This document supersedes

39、 EN 1948-4:2010. Annex H provides details of significant technical changes between this European Standard and the previous document CEN/TS 1948-4:2007. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association, and supports essent

40、ial requirements of EU Directive. For relationship with EU Directive(s), see informative Annex ZA, which is an integral part of this document. The start and finish of text introduced or altered by amendment is indicated by tags . EN 1948 consists of several parts dealing with the determination of th

41、e mass concentration of PCDDs, PCDFs and PCBs in stationary source emissions: Part 1: Sampling of PCDDs/PCDFs Part 2: Extraction and clean-up of PCDDs/PCDFs Part 3: Identification and quantification of PCDDs/PCDFs Part 4: Sampling and analysis of dioxin-like PCBs The first three parts are necessary

42、for the performance of the PCDD/PCDF measurements. In addition this document EN 1948-4 describes the sampling, extraction and analyses of dioxin-like PCBs and requires references to EN 1948-1, 2, 3. The precision and the performance characteristics of the measurement of PCBs were determined between

43、2006 and 2008 in a comparison and validation trial at both a waste incinerator and a shredder plant sponsored by the European Commission and the European Free Trade Association. The basic requirements of the determination of PCBs were first published as CEN/TS 1948-4, which served as a basis for the

44、se mandated validation measurements. This document EN 1948-4 additionally includes important guidance for sampling and analysis over a broad concentration range gained during the mandated validation measurements. According to the CEN/CENELEC Internal Regulations, the national standards organizations

45、 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, Malta, N

46、etherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 1948-4:2014-03 EN 1948-4:2010+A1:2013 (E) 5 Introduction Polychlorinated biphenyls (PCBs) are a group of chlorinated aromatic compounds similar in structure to polychl

47、orinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) which consist of 209 individual substances (see Figure 1 for the basic structure). PCBs have been produced intentionally over approximately 50 years until the end of the 1990s with different uses in open and closed systems,

48、 e.g. as electrical insulators or dielectric fluids in capacitors and transformers, specialised hydraulic fluids, as a plasticiser in sealing material, etc. Worldwide, more than one million tons of PCBs were produced. PCBs as well as PCDD/PCDF are emitted from thermal and other processes. PCB can co

49、ntribute to the Total WHO-TEQ as reported for Germany 1; 2, Great Britain 3, Poland 4, Spain 5, Japan 6; 7, Korea 8. In 1997 a group of experts of the World Health Organisation (WHO) defined toxicity equivalent factors (TEFs) for PCDDs/PCDFs and 12 PCBs, known as dioxin-like PCBs 9, 10 (see Annex A). These 12 dioxin-like PCBs consist of four non-ortho PCBs and eight mono-ortho PCBs (no or only one chlorine atoms in 2-, 2-, 6- and 6-position), having a planar or mostly planar s