DIN EN 1948-2-2006 Stationary source emissions - Determination of the mass concentration of PCDDs PCDFs and dioxin-like PCBs - Part 2 Extraction and clean-up of PCDDs PCDFs English.pdf

1、 DEUTSCHE NORMJune 2006DIN EN 1948-2 ICS 13.040.40 Supersedes DIN EN 1948-2:1997-05 Stationary source emissions Determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs Part 2: Extraction and clean-up of PCDDs/PCDFs English version of DIN EN 1948-2:2006-06 Emissionen aus stationre

2、n Quellen Bestimmung der Massenkonzentration von PCDD/PCDF und dioxin-hnlichen PCB Teil 2: Extraktion und Reinigung von PCDD/PCDF Englische Fassung DIN EN 1948-2:2006-06 Document comprises 39 pages No part of this standard may be reproduced without prior permission of DIN Deutsches Institut fr Normu

3、ng e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany, has the exclusive right of sale for German Standards (DIN-Normen). English price group 16 www.din.de www.beuth.de !,o/5“10.06 9761218DIN EN 1948-2:2006-06 2 National foreword This standard has been prepared by CEN/TC 264 Air quality (Secret

4、ariat: 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 prepared under a mand

5、ate 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 on the incineration

6、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 methods to calibrate au

7、tomated 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 of the art at the tim

8、e 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 Trade Association and th

9、e German Federal Environment Agency. Amendments This standard differs from DIN EN 1948-2:1997-05 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 suitable for the deter

10、mination 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 of detection, limit o

11、f quantification, WHO-TEF/WHO-TEQ. c) Addition and correction of requirements for: minimum information prior to analyses; sample pretreatment; addition of extraction standards; sample storage; extraction. A detailed list of all amendments is given in the foreword to EN 1948-2:2006. Previous editions

12、 DIN EN 1948-2: 1997-05 DIN EN 1948-2:2006-06 3 National Annex NA (informative) Bibliography VDI 2464-1, Ambient air measurement Indoor air measurement Measurement of polychlorinated biphynyls (PCBs) GC/MS method for PCB 28, 52, 101,138, 153, 180 VDI 2464-2, Ambient air measurement Indoor air measur

13、ement 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 dibenzofurans Method using large filters VDI 3498-2, Ambient air measurement Indoor air measureme

14、nt 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 (PCDFs) Dilution method Example of application of DIN EN 1948 for the concentration range 0,1

15、 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 of application of DIN EN 1948 for the concentration range 0,1 ng I-TEQ/m3VDI 3499-3, Emission

16、 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 STANDARDNORME EUROPENNEEUROPISCHE NORMEN 1948-2March 2006ICS 13.040.40 Supersedes EN 1948-2:

17、1996 English VersionStationary source emissions - Determination of the massconcentration of PCDDs/PCDFs and dioxin-like PCBs - Part 2:Extraction and clean-up of PCDDs/PCDFsEmissions de sources fixes - Dtermination de laconcentration massique en PCDD/PCDF et PCB de typedioxine - Partie 2: Extraction

18、et purification de PCDD/PCDFEmissionen aus stationren Quellen - Bestimmung derMassenkonzentration von PCDD/PCDF und dioxin-hnlichen PCB - Teil 2: Extraktion und Reinigung vonPCDD/PCDFThis European Standard was approved by CEN on 23 January 2006.CEN members are bound to comply with the CEN/CENELEC In

19、ternal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN membe

20、r.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 into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are

21、the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,Slovakia, Slovenia, Spain, Sweden, Switzerland and Unit

22、ed Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2006 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 1948-2:2006: EEN

23、 1948-2:2006 (E) 2 Contents Page Foreword3 Introduction .6 1 Scope 7 2 Normative references 7 3 Terms and definitions .7 4 Symbols and abbreviations10 5 Principle of the extraction and clean-up procedure.11 6 Device, materials and 13C12-labelled standards 12 7 Method validation and quality control r

24、equirements.13 8 Sample pre-treatment and extraction 14 9 Report .16 Annex A (informative) Examples of operation of extraction and clean-up methods 17 Annex B (informative) Relations to EU Directives 35 Bibliography 36 EN 1948-2:2006 (E) 3 Foreword This European Standard (EN 1948-2:2006) has been pr

25、epared 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 of an identical text or by endorsement, at the latest by September 2006, and conflicting national standards

26、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 shall not be held responsible for identifying any or all such patent rights. This European Standard supersedes

27、EN 1948-2:1996. 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 Directive 94/67/EC of 16 December 1994 i on the incineration of hazardous waste. This directive is now repl

28、aced 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 also Annex B). The precision and the performance characteristics were determined between 1992 and 1995 in fou

29、r 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 this EN between 2001 and 2004 only refers to the normative part. The information given in the informative ann

30、exes as examples of operation are kept unchanged, as they represent the state of the art at time of the validation measurements of EN 1948:1996 between 1992 and 1995. This European Standard EN 1948:2006 consists of three parts dealing with the determination of the mass concentration of PCDDs and PCD

31、Fs 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 parts are necessary for the performance of the dioxin measurements. In addition for the sampling, extraction and ana

32、lyses 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 approval time of three years respectively. Important changes made in the revision of EN 1948-2: 1. Title: Broadening

33、 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 1948-2:2006 (E) 4 Deletion of all precursor documents which were basis for elaboration of EN 1948 as well as the names of the standardisation bodies involved in the elabora

34、tion 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 of a hint, that the revision only refers to the normative parts of the standard. The Informative Annex A “Examp

35、les 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 future document EN 1948-4 dealing with the analyses of dioxin-like PCBs 3. Scope: Addition of a hint, that EN 1948

36、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 substances, e.g. of dioxin-like PCBs 4. Normative references: Update of the references to EN 1948-1:2006, EN 1948-

37、3:2006 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 chapters Corrected definition of “field blank“ for clarification Corrected definition of “analytical blank“ for

38、clarification Corrected definition of “sampling standard“: only furans “Syringe standard“ renamed to read “recovery standard“ Corrected definition of “recovery standard“: only dioxins Additional definition of “dioxin-like PCBs“ “Sampling volume“ renamed to read “volume of the sampling extract“ Corre

39、cted 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. Clause 5 Principle of the extraction and clean-

40、up procedure: Additional subclause 5.2 “Minimum information prior to analyses“ 7. Clause 7.2 Sample pre-treatment: Correction of the requirements regarding sample pre-treatment for better comprehensibility EN 1948-2:2006 (E) 5 8. Clause 8.1 Addition of extraction standards: Correction for better com

41、prehensibility 9. Clause 8.2 Sample storage: Requirement to store the samples 320 C) vapour phase transfer mechanisms and aerosol formation during solvent evaporation might lead to substantial losses when concentrating volumes below 10 ml). Depending on the method to be used for solvent volume reduc

42、tion the following precautions shall be taken into consideration: a) Rotary evaporators Losses might be substantial when reducing solvent volumes below 10 ml. Counter measures are the use of controlled vacuum conditions according to the vapour pressure and boiling point of the solvent, addition of a

43、 high-boiling solvent as a keeper as well as the use of specially shaped vessels (e.g. V-shaped). EN 1948-2:2006 (E) 16 b) Counter gas flow evaporators Volumes should not be reduced to less than 1 ml. c) Nitrogen flow An excessive flow of nitrogen which disturbs the solvent surface should be avoided

44、. The vial shape has also some influence on possible losses. V-shaped vials or vial inserts shall be used for volume reductions below around 200 l. 8.6 Addition of recovery standards The very last step before quantification is the addition of the recovery standards to measure the recovery rates of t

45、he extraction standards. The recovery standards according to Table 1 shall be added under following conditions: a) Recovery standards shall be added just prior to the quantification procedure. Samples with the recovery standard added which could not be analysed due to operational reasons (instrument

46、 failure), should be stored as briefly as possible and any further uncontrolled solvent evaporation shall be avoided. b) Recovery standards shall be added after the final volume reduction. Any further direct volume reduction shall be avoided. A slow evaporation at room temperature from the open samp

47、le vial to a volume of about 25 l is acceptable. 9 Report The contents of the report for sampling are described in EN 1948-1:2006 and for analysis in EN 1948-3:2006. EN 1948-2:2006 (E) 17 Annex A (informative) Examples of operation of extraction and clean-up methods A.1 General The revision of this

48、EN between 2001 and 2004 only refers to the normative part. The information given in this informative annex as examples of operation are kept unchanged, as they represent the state of the art at time of the validation measurements of EN 1948:1996 between 1992 and 1995. Polychlorinated dibenzo-p-diox

49、ins (PCDDs) and dibenzofurans (PCDFs) are extracted from the sampling media by soxhlet extraction, liquid/liquid extraction or rinsed with solvents (sampling train surfaces). Selected 13C12-isotope labelled 2,3,7,8-chlorine substituted PCDD/PCDF congeners are added to the different sampling media before extraction. Clean-up of the sample extract is performed by liquid chromatography. 13C12-isotope labelled congeners are added as recovery sta