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1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS EN 1948-2 : 1997 The E
2、uropean Standard EN 1948-2 : 1996 has the status of a British Standard ICS 13.040.40 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Stationary source emissions Determination of the mass concentration of PCDDs/PCDFs Part 2. Extraction and clean-up Licensed Copy: sheffieldun sh
3、effieldun, na, Tue Nov 07 09:10:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN 1948-2 : 1997 This British Standard, having been prepared under the direction of the Health and Environment Sector Board, was published under the authority of the Standards Board and comes into effect on 15 October 1
4、997 BSI 1997 The following BSI references relate to the work on this standard: Committee reference EH/2 Draft for comment 95/521170 DC ISBN 0 580 27684 8 Amendments issued since publication Amd. No.DateText affected Committees responsible for this British Standard The preparation of this British Sta
5、ndard was entrusted to Technical Committee EH/2, Air quality, upon which the following bodies were represented: British Cement Association British Coal Corporation Chartered Institute of Environmental Health Combustion Engineering Association Department of Health Environment Agency GAMBICA (BEAMA Lt
6、d.) Health and Safety Executive Institute of Petroleum Laboratory of the Government Chemist Royal Society of Chemistry TES (Bretby Limited) Wood Panel Industries Federation The following bodies were also represented in the drafting of the standard, through subcommittees and panels: AEATechnology Agr
7、icultural Development and Advisory Service Asbestos Information Centre Ltd. British Ceramic Research Ltd. British Gas plc Castings Development Centre Council of Gas Detection and Environmental Monitoring Department of the Environment Electricity Association Environmental Services Association Institu
8、te of Wastes Management Isa England Section (Environmental Section) UK Steel Association Licensed Copy: sheffieldun sheffieldun, na, Tue Nov 07 09:10:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BSI 1997i BS EN 1948-2 : 1997 National foreword This Part of BS EN 1948 has been prepared by Technical C
9、ommittee EH/2, and is the English language version of EN 1948-2 : 1996 Stationary source emissions Determination of the mass concentration of PCDDs/PCDFs Part 2: Extraction and clean-up, published by the European Committee for Standardization (CEN). This British Standard is published under the direc
10、tion of the Health and Environment Sector Board whose Technical Committee EH/2 has the responsibility to: aid enquirers to understand the text; present to the responsible European committee any enquiries on interpretation, or proposals for change, and keep UK interests informed; monitor related inte
11、rnational and European developments and promulgate them in the UK. NOTE. International and European Standards, as well as overseas standards, are available from Customer Services, BSI, 389 Chiswick High Road, London W4 4AL. Cross-references The British Standards which implement international or Euro
12、pean publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled International Standards Correspondence index, or by using the Find facility of the BSI Standards Electronic Catalogue. Compliance with a British Standard does not of itself confer im
13、munity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the EN title page, pages 2 to 24, an inside back cover and a back cover. Licensed Copy: sheffieldun sheffieldun, na, Tue Nov 07 09:10:35 GMT+00:00 2006, Uncontrolled Copy, (c
14、) BSI iiblank Licensed Copy: sheffieldun sheffieldun, na, Tue Nov 07 09:10:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI CEN European Committee for Standardization Comite Europe en de Normalisation Europa isches Komitee fu r Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1996 Copyr
15、ight reserved to CEN members Ref. No. EN 1948-2 : 1996 E EUROPEAN STANDARDEN 1948-2 NORME EUROPE ENNE EUROPA ISCHE NORM December 1996 ICS 13.040.40 Descriptors: Air, quality, air pollution, gaseous effluents, emission, determination, concentration, PCDD, PCDF, samples, extraction, quality control, p
16、urity English version Stationary source emissions Determination of the mass concentration of PCDDs/PCDFs Part2: Extraction and clean-up Emissions de sources fixes De termination de la concentration massique en PCDDs/PCDFs Partie 2: Extraction et purification Emissionen aus stationa ren Quellen Besti
17、mmung der Massenkonzentrationen von PCDDs/PCDFs Teil 2: Extraktion und Reinigung This European Standard was approved by CEN on 1996-12-27. 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 nation
18、al standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards 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
19、other language made by translation under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Icelan
20、d, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. Licensed Copy: sheffieldun sheffieldun, na, Tue Nov 07 09:10:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 2 EN 1948-2 : 1996 BSI 1997 Foreword This European Standard has been prepared b
21、y 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 June 1997, and conflicting national standards shall be withd
22、rawn at the latest by June 1997. This European Standard 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). For relationship with EU Directive(s), see informative annex C, which is
23、an integral part of this standard. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Nethe
24、rlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. This European Standard was elaborated by AENOR (Spain) AFNOR (France) BSI (United Kingdom) DIN (Germany) DS (Denmark) NNI (Netherlands) NSF (Norway) ON (Austria) SFS (Finland) SIS (Sweden) SNV (Switzerland) UNI (Italy) The
25、precision and the performance characteristics were determined in four comparative and validation trials at waste incinerators sponsored by the Commission of the European Communities, the European Free Trade Association and the German Federal Environment Agency. This European Standard EN 1948 : 1996
26、consists of: Part 1.Sampling Part 2.Extraction and clean-up Part 3.Identification and quantification All three parts are necessary for the performance of the dioxin measurements. The European Standard was developed on the basis of the following national standards or guidelines: NFX 43-313 : 1991Air
27、Quality Stationary Source Emissions Determination of PCDD/PCDF Nordic : 1987Recommended method for dioxin measurements in flue gases from waste incineration, Swedish Environmental Protection Agency Unichim Method No825 : 1989 Stationary source emission measurements Conveyed gas flows Sampling and de
28、termination of organic micropollutants Sampling PAH determination PCDD and PCDF determination PCB determination VDI 3499 Part 1 : 1990 (Draft) Emission measurement Measurement of residual materials Determination of polychlorinated dibenzodioxins and dibenzofurans in flue and stack gas of incineratio
29、n and firing plants Dilution method Determination in filter dust, potash and slag VDI 3499 Part 2 : 1993 (Draft) Emission measurement Determination of polychlorinated dibenzo-p-dioxins (PCDD) and dibenzofurans (PCDF) Filter/condenser method VDI 3499 Part 3 : 1996 (Draft) Emission measurement Determi
30、nation of polychlorinated dibenzo-p-dioxins (PCDD) and dibenzofurans (PCDF) Cooled probe method Licensed Copy: sheffieldun sheffieldun, na, Tue Nov 07 09:10:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 3 EN 1948-2 : 1996 BSI 1997 Contents Page Foreword2 Introduction4 1Scope4 2Normative referen
31、ces4 3Definitions and abbreviations5 3.1Definitions5 3.2Abbreviations5 4Principle of the extraction and clean-up procedure6 5Device, materials and 13C12-labelled standards6 5.1Device and materials6 5.2 13C12-labelled standards 6 6Method validation and quality control requirements8 6.1Use of 13C12-la
32、belled standards 8 6.2Sample pretreatment8 6.3Clean-up8 7Sample pretreatment and extraction8 7.1Addition of extraction standards8 7.2Sample storage9 7.3Extraction9 7.4Clean-up9 7.5Final concentration of the sample extract10 7.6Addition of syringe standards10 8Report10 Annexes A(informative) Examples
33、 of operation of extraction and clean-up methods11 B(informative) Bibliography23 C(informative) Clauses of this European Standard addressing essential requirements or other provisions of EU Directives24 Licensed Copy: sheffieldun sheffieldun, na, Tue Nov 07 09:10:35 GMT+00:00 2006, Uncontrolled Copy
34、, (c) BSI Page 4 EN 1948-2 : 1996 BSI 1997 Introduction Two groups of related chlorinated aromatic dibenzo ethers are known as polychlorinated dibenzodioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs); they consist of a total of 210 individual substances (congeners): 75 PCDDs and 135 PCDFs. P
35、CDDs and PCDFs can form in the combustion of organic materials; they also may occur as undesirable by-products in the manufacture or further processing of chlorinated organic chemicals. PCDDs/PCDFs enter the environment via these emission paths and through the use of contaminated materials. In fact,
36、 they are universally present in very small concentrations. The 2,3,7,8-chlorine substituted congeners are toxicologically significant. Toxicologically much less significant than the tetrachlorinated to octachlorinated dibenzodioxins/dibenzofurans are the 74 monochlorinated to trichlorinated dibenzo
37、dioxins/dibenzofurans (for toxicity equivalent factors, see annex A of EN 1948-1 : 1996). Only skilled operators who are trained in handling highly toxic compounds should apply this standard. 1 Scope The present Part of this standard specifies the extraction and clean-up procedures of the sampled PC
38、DDs/PCDFs. It is an integral part of the complete measurement procedure. The use of the other two Parts EN 1948-1 : 1996 and EN 1948-3 : 1996 describing sampling or identification and quantification, respectively, is necessary for the determination of the PCDDs/PCDFs. This standard has been designed
39、 to measure PCDD/PCDF concentrations at about 0,1 ng I-TEQ/m3 in stationary source emissions. This standard specifies both method validation and a framework of quality control requirements which have to be fulfilled by any PCDD/PCDF extraction and clean-up methods to be applied. Some methods are des
40、cribed 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) and the identification and quantification (Part 3) to complete the measurement procedure. During comparison measurements on a municipal
41、waste incinerator at the level of about 0,1 ng I-TEQ/m3 these three 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/m3 and a dust loading of from 1 mg/m3t
42、o 15 mg/m3. In principle it is not possible to evaluate the accuracy (trueness and precision) of emission measurements. Following the validation trials the internal and external variabilities were calculated for the process considered and are given in clause 13 of EN 1948-3 : 1996. These variabiliti
43、es give an indication of the variabilities which have been observed when using this standard and should be taken into account when expressing results. The procedure described in the three Parts of standard EN 1948 : 1996 lays down requirements in order to measure the 17 congeners required to calcula
44、te the total I-TEQ (see table A.1 of EN 1948-1 : 1996). 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text and the publications are listed hereafter.
45、For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies. EN 1948-1 : 1996Stationary source emission
46、s Determination of the mass concentration of PCDDs/PCDFs Part 1. Sampling EN 1948-3 : 1996Stationary source emissions Determination of the mass concentration of PCDDs/PCDFs Part 3: Identification and quantification A bibliography is shown in annex B (informative). Licensed Copy: sheffieldun sheffiel
47、dun, na, Tue Nov 07 09:10:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 5 EN 1948-2 : 1996 BSI 1997 3 Definitions and abbreviations 3.1 Definitions For the purposes of this standard, the following definitions apply: 3.1.1 spiking Addition of 13C12-labelled PCDD/PCDF standards. 3.1.2 isokinetic
48、sampling Sampling at a rate such that the velocity including the direction of the gas entering the sampling nozzle is the same as that of the gas in the duct at the sampling point. ISO 9096 : 1992 3.1.3 operational performance characteristics Measures which deal with the influence of the physical an
49、d chemical environment and maintenance problems, for example; mains voltage, temperature, supply of certain substances, set-up time, period of unattended operation. 3.1.4 statistical performance characteristics Measures which quantify, for measured values, the possible deviations resulting from the random part of the measuring process; these are, for example, repeatability or instability. 3.1.5 control blank A sample taken at the plant site in an identical manner to the normal samples including the spiking, bu