BS EN 1948-3-2006 Stationary source emissions - Determination of the mass concentration of PCDDs PCDFs and dioxin-like PCBs - Identification and quantification of PCDDs PCDFs《固定源排放.pdf

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1、BRITISH STANDARDBS EN 1948-3:2006Stationary source emissions Determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs Part 3: Identification and quantification of PCDDs/PCDFsThe European Standard EN 1948-3:2006 has the status of a British StandardICS 13.040.40g49g50g3g38g50g51g60g

2、44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN 1948-3:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee o

3、n 31 March 2006 BSI ISBN 0 580 48045 3National forewordThis British Standard is the official English language version of EN 1948-3:2006. It supersedes BS EN 1948-3:1997 which is withdrawn.The UK participation in its preparation was entrusted by Technical Committee EH/2, Air quality, to Subcommittee

4、EH/2/1, Stationary source emissions, which has the responsibility to: A list of organizations represented on this subcommittee can be obtained on request to its secretary.Cross-referencesThe British Standards which implement international or European publications referred to in this document may be

5、found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online.This publication does not purport to include all the necessary provisions of a contract. Users are re

6、sponsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and kee

7、p UK interests informed; monitor related international and European developments and promulgate them in the UK.Summary of pagesThis document comprises a front cover, an inside front cover, the EN title page, pages 2 to 48, an inside back cover and a back cover.The BSI copyright notice displayed in t

8、his document indicates when the document was last issued.Amendments issued since publicationAmd. No. Date CommentsEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 1948-3March 2006ICS 13.040.40 Supersedes EN 1948-3:1996 English VersionStationary source emissions - Determination of the massconcentrat

9、ion of PCDDs/PCDFs and dioxin-like PCBs - Part 3:Identification and quantification of PCDDs/PCDFsEmissions de sources fixes - Dtermination de laconcentration massique en PCDD/PCDF et PCB de typedioxine - Partie 3: Identification et quantification dePCDD/PCDFEmissionen aus stationren Quellen - Bestim

10、mung derMassenkonzentration von PCDD/PCDF und dioxin-hnlichen PCB - Teil 3: Identifizierung und Quantifizierungvon PCDD/PCDFThis 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 givin

11、g 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 member.This European Standard exists in three official versions

12、(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 the national standards bodies of Austria, Belgium, Cyprus,

13、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 United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EURO

14、PEN 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 1948-3:2006: EEN 1948-3:2006 (E) 2 Contents Page Foreword 3 Introduction6 1

15、 Scope .7 2 Normative references .7 3 Terms and definitions.7 4 Symbols and abbreviations10 5 Principles of identification and quantification11 6 Reagents, materials and equipment11 7 Safety measures .11 8 Quality control requirements for identification and quantification.11 9 Quality assurance crit

16、eria for extraction/clean-up/quantification procedure blanks 13 10 Calibration of the HRGC/HRMS14 11 Quantification of HRGC/HRMS results 15 12 Calculation of the measurement results .18 13 Analytical report18 14 Performance characteristics19 15 Interferences .21 Annex A (informative) Examples of ope

17、ration of gas chromatography / mass spectrometry analysis of PCDDs/PCDFs in emission samples 22 Annex B (informative) Estimation of the measuring uncertainty and precision of the determination of polychlorinated dibenzo-p-dioxins and dibenzofurans.31 Annex C (informative) Mass of ions monitored for

18、PCDDs and PCDFs 35 Annex D (informative) Relative abundance of chlorine isotope ions and their ratio for PCDD/PCDF congeners containing 4 to 8 chlorine substituents 36 Annex E (informative) Further general recommendations for separation, detection and quantification of PCDDs/PCDFs 37 Annex F (inform

19、ative) Variability determination based on the results of the validation tests.39 Annex G (informative) Relation to EU Directives 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

20、 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 shall be withdrawn at the latest by September 2006. Attention is drawn

21、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 EN 1948-3:1996. This European Standard has been prepared under a mandat

22、e 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 replaced by EU Directive 2000/76/EC of 4 December 2000 on the incineration

23、of waste ii and this European Standard also supports the Essential Requirements of the new EU Directive 2000/76/EC (see also 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

24、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 annexes as examples of operation are kept unchanged, as they represent the

25、 state of the art at the 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 PCDFs in stationary source emissions: Part 1: Sampling of PCDDs/PCDFs;

26、 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 analyses of dioxin-like PCBs the Technical Specification CEN/TS 1948-4

27、1is 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 1948-3: 1. Title: Broadening of the title with regard to the future EN 1948-4 for the determina

28、tion of dioxin-like PCBs 2. Foreword: 1) To be published. EN 1948-3:2006 (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 elaboration of EN 1948 Update of the hint regarding mandate of the standar

29、disation 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 “Examples of operation” is kept unchanged and represents the state of the

30、 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 can be applied for wide concentration ranges and various emission

31、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 1948-2:2006 5. Clause 3 Terms and definitions: Distinction between Clau

32、se 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 clarification Corrected definition of “sampling standard“: only fu

33、rans “Syringe standard“ renamed to read “recovery standard“ Corrected definition of “recovery standard“: only dioxins Additional 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

34、 detection Additional definition and calculation of limit of quantification Additional definition of WHO-TEF/WHO-TEQ 6. Clause 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 abs

35、ence of interferences is documented. Deletion of the permission that other techniques which show that they meet the requirements 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 t

36、o the 13C-labelled congeners. Clarification of the requirement, that the signal-to-noise ratio of the raw data as documented 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

37、quantification: Correction of the requirements for quantification in 8.3.a, c, e, f, g, h, i h) Calculation of the quantification 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

38、 of the quantification scheme (Table 1): Quantification of dioxins with 13C-labelled dioxins, quantification of furans with 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 fu

39、ran extraction standards 9. Clause 12 Calculation of measurement results: Combination of formerly two formulas to one formula 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

40、 and the accuracy of polychlorinated PCDD/PCDF determination 11. Annex G: Update of the hint regarding mandate of the standardisation 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 Regulat

41、ions, 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, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norw

42、ay, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EN 1948-3:2006 (E) 6 Introduction Two groups of related chlorinated aromatic ethers are known as polychlorinated dibenzodioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs); they consist of a total

43、 of 210 individual substances (congeners): 75 PCDDs and 135 PCDFs. PCDDs and PCDFs can form in the combustion of organic materials; they also occur as undesirable by-products in the manufacture or further processing of chlorinated organic chemicals. PCDDs/PCDFs enter the environment via these emissi

44、on paths and through the use of contaminated materials. In fact, they are universally present at very small concentrations. The 2,3,7,8-substituted congeners are toxicologically significant. Toxicologically much less significant than the tetrachlorinated to octachlorinated dibenzodioxins/dibenzofura

45、ns are the 74 monochlorinated to trichlorinated dibenzodioxins/dibenzofurans (for toxicity equivalent factors, see Annex A of EN 1948-1:2006). Only skilled operators who are trained in handling highly toxic compounds should apply the method described in this European Standard. EN 1948-3:2006 (E) 7 1

46、 Scope This European Standard specifies the identification and quantification procedures of the sampled PCDDs/PCDFs. It is an integral part of the complete measurement procedure. The use of the other two parts of this standard, EN 1948-1:2006 and EN 1948-2:2006, describing sampling and extraction an

47、d clean-up, respectively, is necessary for the determination of the PCDDs/PCDFs. This European Standard has been designed to measure PCDD/PCDF concentrations at about 0,1 ng I-TEQ/m3in stationary source emissions. This European Standard specifies both method validation and a framework of quality con

48、trol requirements which shall be fulfilled by any PCDD/PCDF identification and quantification methods to be applied. Some methods are described in detail in Annex A as examples of proven procedures. Each of the three sampling methods (Part 1) can be combined with the extraction and clean-up (Part 2)

49、 and the identification and quantification (Part 3) to complete the measurement procedure. During comparison measurements of the three sampling methods on municipal waste incinerators at the level of about 0,1 ng I-TEQ/m3these methods have been deemed comparable within the expected range of uncertainty. Validation trials were performed on the flue gas of municipal waste incinerators at the level of about 0,1 ng I-TEQ/m3and a dust loading of from 1 mg/m3to 15 mg/m3. Although this European Standard is primar