DIN EN 1948-3-2006 Stationary source emissions - Determination of the mass concentration of PCDDs PCDFs and dioxin-like PCBs - Part 3 Identification and quantification of PCDDs PCD.pdf

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1、 DEUTSCHE NORMJune 2006DIN EN 1948-3 ICS 13.040.40 Supersedes DIN EN 1948-3:1997-05 Stationary source emissions Determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs Part 3: Identification and quantification of PCDDs/PCDFs English version of DIN EN 1948-3:2006-06 Emissionen aus

2、 stationren Quellen Bestimmung der Massenkonzentration von PCDD/PCDF und dioxin-hnlichen PCB Teil 3: Identifizierung und Quantifizierung von PCDD/PCDF Englische Fassung DIN EN 1948-3:2006-06 Document comprises 51 pages No part of this standard may be reproduced without prior permission of DIN Deutsc

3、hes Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany, has the exclusive right of sale for German Standards (DIN-Normen). English price group 18 www.din.de www.beuth.de !,o/6“10.06 9761219DIN EN 1948-3:2006-06 2 National foreword This standard has been prepared by CEN/TC 26

4、4 Air quality (Secretariat: Germany), Working Group WG 1 Dioxins Emissions (Secretariat and Convenorship: Germany). The responsible German body involved in its preparation was the Kommission Reinhaltung der Luft (KRdL) im VDI und DIN (VDI/DIN Air Quality Commission). This European Standard has been

5、prepared under a mandate given to CEN by the European Commission and the European Free Trade Association to support Essential Requirements of EU Directive 94/67/EC of 16 December 1994 on the incineration of hazardous waste. This directive is now replaced by EU Directive 2000/76/EC of 4 December 2000

6、 on the incineration of waste, and this European Standard also supports the Essential Requirements of the new EU Directive 2000/76/EC. In Annex III of EU-Directive 2000/76/EC it is specified that Sampling and analysis of all pollutants including dioxins and furans as well as reference measurement me

7、thods to calibrate automated measurement systems shall be carried out as given by CEN Standards. The revision of this EN between 2001 and 2004 only refers to the normative part. The information given in the informative annexes as examples of operation are kept unchanged, as they represent the state

8、of the art at the time of validation measurements of EN 1948:1996 between 1992 and 1995. The precision and the performance characteristics were determined between 1992 and 1995 in four comparative and validation trials at waste incinerators sponsored by the European Commission, the European Free Tra

9、de Association and the German Federal Environment Agency. Amendments This standard differs from DIN EN 1948-3:1997-05 as follows: a) Extension of the scope: DIN EN 1948 can now also be applied for wide concentration ranges and various emission sources and the described measurement methods are also s

10、uitable for the determination of other low-volatile substances, e.g. of dioxine-like PCBs. b) Inclusion of new terms and definitions, and corrections: The following terms are concerned: field blank, analytical blank, sampling standard, recovery standard, dioxin-like PCBs, isokinetic sampling, limit

11、of detection, limit of quantification, WHO-TEF/WHO-TEQ. c) Addition and correction of requirements for: identification; quantification; quantification of HRGC/HRMS results; calculation of measurement results. d) Inclusion of a new informative Annex B for estimation of the measurement uncertainty. A

12、detailed list of all amendments is given in the foreword to EN 1948-3:2006. Previous editions DIN EN 1948-3: 1997-05 DIN EN 1948-3:2006-06 3 National Annex NA (informative) Bibliography VDI 2464-1, Ambient air measurement Indoor air measurement Measurement of polychlorinated biphynyls (PCBs) GC/MS m

13、ethod for PCB 28, 52, 101,138, 153, 180 VDI 2464-2, Ambient air measurement Indoor air measurement Measurement of polychlorinated biphynyls (PCBs) HR-GC/HR-MS method for coplanar PCBs VDI 3498-1, Ambient air measurement Indoor air measurement Measurement of polychlorinated dibenzo-p-dioxins and dibe

14、nzofurans Method using large filters VDI 3498-2, Ambient air measurement Indoor air measurement Measurement of polychlorinated dibenzo-p-dioxins and dibenzofurans Method using small filters VDI 3499-1, Emission measurement Determination of polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans

15、(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 3499-2, Emission measurement Determination of polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs) Filter/condenser method Example

16、of application of DIN EN 1948 for the concentration range 0,1 ng I-TEQ/m3VDI 3499-3, Emission measurement Determination of polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs) Cooled probe method Example of application of DIN EN 1948 for the concentration range 0,1 ng I-TEQ/m3EUROPEAN

17、 STANDARDNORME EUROPENNEEUROPISCHE NORMEN 1948-3March 2006ICS 13.040.40 Supersedes EN 1948-3:1996 English VersionStationary source emissions - Determination of the massconcentration of PCDDs/PCDFs and dioxin-like PCBs - Part 3:Identification and quantification of PCDDs/PCDFsEmissions de sources fixe

18、s - Dtermination de laconcentration massique en PCDD/PCDF et PCB de typedioxine - Partie 3: Identification et quantification dePCDD/PCDFEmissionen aus stationren Quellen - Bestimmung derMassenkonzentration von PCDD/PCDF und dioxin-hnlichen PCB - Teil 3: Identifizierung und Quantifizierungvon PCDD/PC

19、DFThis European Standard was approved by CEN on 23 January 2006.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 ref

20、erences concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member int

21、o its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Lu

22、xembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2006 CEN All righ

23、ts of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 1948-3:2006: EEN 1948-3:2006 (E) 2 Contents Page Foreword3 Introduction .6 1 Scope 7 2 Normative references 7 3 Terms and definitions .7 4 Symbols and abbreviations10 5 Principles of identification

24、 and quantification11 6 Reagents, materials and equipment 11 7 Safety measures 11 8 Quality control requirements for identification and quantification11 9 Quality assurance criteria for extraction/clean-up/quantification procedure blanks.13 10 Calibration of the HRGC/HRMS14 11 Quantification of HRGC

25、/HRMS results 15 12 Calculation of the measurement results .18 13 Analytical report.18 14 Performance characteristics 19 15 Interferences 21 Annex A (informative) Examples of operation of gas chromatography / mass spectrometry analysis of PCDDs/PCDFs in emission samples22 Annex B (informative) Estim

26、ation of the measuring uncertainty and precision of the determination of polychlorinated dibenzo-p-dioxins and dibenzofurans31 Annex C (informative) Mass of ions monitored for PCDDs and PCDFs .35 Annex D (informative) Relative abundance of chlorine isotope ions and their ratio for PCDD/PCDF congener

27、s containing 4 to 8 chlorine substituents .36 Annex E (informative) Further general recommendations for separation, detection and quantification of PCDDs/PCDFs.37 Annex F (informative) Variability determination based on the results of the validation tests .39 Annex G (informative) Relation to EU Dir

28、ectives 47 Bibliography 48 EN 1948-3:2006 (E) 3 Foreword This European Standard (EN 1948-3:2006) has been prepared by Technical Committee CEN/TC 264 “Air quality”, the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication

29、of an identical text or by endorsement, at the latest by September 2006, and conflicting national standards shall be withdrawn at the latest by September 2006. 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 sha

30、ll not be held responsible for identifying any or all such patent rights. This European Standard supersedes EN 1948-3:1996. This European Standard has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association to support Essential Requirements of EU

31、 Directive 94/67/EC of 16 December 1994 i on the incineration of hazardous waste. This directive is now replaced by EU Directive 2000/76/EC of 4 December 2000 on the incineration of waste ii and this European Standard also supports the Essential Requirements of the new EU Directive 2000/76/EC (see a

32、lso Annex G). The precision and the performance characteristics were determined between 1992 and 1995 in four comparative and validation trials at waste incinerators sponsored by the European Commission, the European Free Trade Association and the German Federal Environment Agency. The revision of t

33、his EN between 2001 and 2004 only refers to the normative part. The information given in the informative annexes as examples of operation are kept unchanged, as they represent the state of the art at the time of the validation measurements of EN 1948:1996 between 1992 and 1995. This European Standar

34、d EN 1948:2006 consists of three parts dealing with the determination of the mass concentration of PCDDs and PCDFs 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. All three part

35、s are necessary for the performance of the dioxin measurements. In addition for the sampling, extraction and analyses of dioxin-like PCBs the Technical Specification CEN/TS 1948-41is developed and will be transferred to a European Standard after corresponding validation measurements or after an appr

36、oval time of three years respectively. Important changes made in the revision of EN 1948-3: 1. Title: Broadening of the title with regard to the future EN 1948-4 for the determination of dioxin-like PCBs 2. Foreword: 1) To be published. EN 1948-3:2006 (E) 4 Deletion of all precursor documents which

37、were basis for elaboration of EN 1948 as well as the names of the standardisation bodies involved in the elaboration of EN 1948 Update of the hint regarding mandate of the standardisation project and regarding fulfilment of the Essential Requirements of EU Directives 94/67/EC and 2000/76/EC Addition

38、 of a hint, that the revision only refers to the normative parts of the standard. The Informative Annex A “Examples of operation” is kept unchanged and represents the state of the art at time of the validation measurements of EN 1948:1996 between 1992 and 1995 Addition of hint with regard to the fut

39、ure document EN 1948-4 dealing with the analyses of dioxin-like PCBs. 3. Scope: Addition of a hint, that EN 1948 can be applied for wide concentration ranges and various emission sources Addition of a hint, that the described measurement methods are suitable for determination of other low-volatile s

40、ubstances, e.g. of dioxin-like PCBs 4. Normative references: Update of the references to EN 1948-1:2006, EN 1948-2:2006 5. Clause 3 Terms and definitions: Distinction between Clause 3 “Terms and definitions“ and Clause 4 “Symbols and abbreviations“ resulting in a different numbering of the following

41、 chapters Corrected definition of “field blank“ for clarification Corrected definition of “analytical blank“ for clarification Corrected definition of “sampling standard“: only furans “Syringe standard“ renamed to read “recovery standard“ Corrected definition of “recovery standard“: only dioxins Add

42、itional definition of “dioxin-like PCBs“ Corrected definition and requirement of isokinetic sampling according to EN 13284-1:2001 Additional definition and calculation of limit of detection Additional definition and calculation of limit of quantification Additional definition of WHO-TEF/WHO-TEQ 6. C

43、lause 8.1 Minimum requirements for identification of PCDF/PCDD congeners: Deletion of the permission that resolution in the range of 6 000 to 10 000 might be acceptable if the absence of interferences is documented. Deletion of the permission that other techniques which show that they meet the requi

44、rements described in this Standard may be used for identification. EN 1948-3:2006 (E) 5 Uniform specification of retention times for all native congeners of +3 s to 0 s relative to the 13C-labelled congeners. Clarification of the requirement, that the signal-to-noise ratio of the raw data as documen

45、ted in Figure 1 shall be at least 3 : 1 for the native signal used for identification. Correction of the measurement of the base line noise 7. Clause 8.3 Minimum requirements for quantification: Correction of the requirements for quantification in 8.3.a, c, e, f, g, h, i h) Calculation of the quanti

46、fication limit according to new definition i) Additional requirement to carry out quantification based on two isotopes 8. Clause 11 Quantification of HRGC/HRMS results: Correction of the quantification scheme (Table 1): Quantification of dioxins with 13C-labelled dioxins, quantification of furans wi

47、th 13C-labelled furans Correction of calculation scheme for recovery rate of the sampling standards (Table 3): 13C-labelled furan sampling standards are related to 13C-labelled furan extraction standards 9. Clause 12 Calculation of measurement results: Combination of formerly two formulas to one for

48、mula for calculating the concentration of the emitted PCDD/PCDF and adaptation of the formula caption 10. Annex B: Additional Annex B for estimation of the measurement uncertainty and the accuracy of polychlorinated PCDD/PCDF determination 11. Annex G: Update of the hint regarding mandate of the sta

49、ndardisation project and regarding fulfilment of basic requirements of EU Directives 94/67/EC and 2000/76/EC 12. Bibliography: Update According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvi