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1、DRAFT FOR DEVELOPMENT DD CEN/TS 1948-4:2007 Stationary source emissions Determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs Part 4: Sampling and analysis of dioxin-like PCBs ICS 13.040.40 ? Licensed Copy: London South Bank University, London South Bank University, Sat Sep 01
2、03:12:46 GMT+00:00 2007, Uncontrolled Copy, (c) BSI DD CEN/TS 1948-4:2007 This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 31 August 2007 BSI 2007 ISBN 978 0 580 58013 0 National foreword This Draft for Development is the UK implementatio
3、n of CEN/TS 1948-4:2007. This publication is not to be regarded as a British Standard. It is being issued in the Draft for Development series of publications and is of a provisional nature. It should be applied on this provisional basis, so that information and experience of its practical applicatio
4、n can be obtained. Comments arising from the use of this Draft for Development are requested so that UK experience can be reported to the European organization responsible for its conversion to a European standard. A review of this publication will be initiated not later than 3 years after its publi
5、cation by the European organization so that a decision can be taken on its status. Notification of the start of the review period will be made in an announcement in the appropriate issue of Update Standards. According to the replies received by the end of the review period, the responsible BSI Commi
6、ttee will decide whether to support the conversion into a European Standard, to extend the life of the Technical Specification or to withdraw it. Comments should be sent to the Secretary of the responsible BSI Technical Committee at British Standards House, 389 Chiswick High Road, London W4 4AL. The
7、 UK participation in its preparation was entrusted by Technical Committee EH/2, Air quality, to Subcommittee EH/2/1, Stationary source emission. A list of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport to include all the nec
8、essary provisions of a contract. Users are responsible for its correct application. Amendments issued since publication Amd. No. DateComments Licensed Copy: London South Bank University, London South Bank University, Sat Sep 01 03:12:46 GMT+00:00 2007, Uncontrolled Copy, (c) BSI TECHNICAL SPECIFICAT
9、ION SPCIFICATION TECHNIQUE TECHNISCHE SPEZIFIKATION CEN/TS 1948-4 July 2007 ICS 13.040.40 English Version Stationary source emissions - Determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs - Part 4: Sampling and analysis of dioxin-like PCBs Emissions de sources fixes - Dtermin
10、ation de la concentration massique en PCDD/PCDF et PCB de type dioxine - Partie 4 : Prlvement et analyse de 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 Tec
11、hnical Specification (CEN/TS) was approved by CEN on 16 June 2007 for provisional application. The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their comments, particularly on the question whether the CEN/TS can
12、 be converted into a European Standard. CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to
13、 the CEN/TS) until the final decision about the possible conversion of the CEN/TS into an EN is reached. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,
14、Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels
15、 2007 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. CEN/TS 1948-4:2007: E Licensed Copy: London South Bank University, London South Bank University, Sat Sep 01 03:12:46 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 2 Contents Page Intro
16、duction.4 1 Scope 4 2 Normative references5 3 Terms and definitions .5 4 Symbols and abbreviations7 5 Principle of the measurement procedure8 6 Device, materials and 13C12-labelled standards9 7 Safety measures 10 8 Measurement procedure.11 9 Method validation and quality control requirements.18 10 Q
17、uality control requirements for the measurement.20 11 Quality assurance criteria for extraction/clean-up/quantification procedure blanks.22 12 Performance characteristics (informative) .23 13 Interferences (informative) .24 Annex A (informative) Toxicity and toxic equivalency25 Annex B (informative)
18、 Example for clean-up of PCB and the separation from PCDD/PCDFs27 B.1 General27 B.2 Method29 Annex C (informative) Possible interferences in dioxin-like PCB analysis.35 Annex D (informative) Measurement of the marker PCB 28, 52, 101, 138, 153, and 180 in addition to the 12 non- and mono-ortho-PCB38
19、Bibliography41 CEN/TS 1948-4:2007 Licensed Copy: London South Bank University, London South Bank University, Sat Sep 01 03:12:46 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 3 Foreword This document (CEN/TS 1948-4:2007) has been prepared by Technical Committee CEN/TC 264 “Air quality”, the secretariat
20、 of which is held by DIN. The European Standard EN 1948:2006 consists of several parts dealing with the determination of the 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: Identificati
21、on and quantification of PCDDs/PCDFs Part 4: Sampling and analysis of dioxin-like PCBs (Technical Specification CEN/TS) The first three parts are necessary for the performance of the dioxin measurements. In addition this Technical Specification, CEN/TS 1948-4, describes the sampling, extraction and
22、analyses of dioxin-like PCBs and will be transferred to a European Standard after corresponding validation measurements. 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 identify
23、ing any or all such patent rights. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to announce this Technical Specification: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Gr
24、eece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. CEN/TS 1948-4:2007 Licensed Copy: London South Bank University, London South Bank University, Sat Sep 0
25、1 03:12:46 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 4 Introduction A group of chlorinated aromatic compounds similar to polychlorinated dibenzodioxins (PCDDs) and polychlori- nated dibenzofurans (PCDFs) is known as polychlorinated biphenyls (PCBs) which consists of 209 individual substances (see F
26、igure 1 for the basic structure). PCBs have been produced over approximately 50 years until the end of the 1990s with different uses in open and closed systems, e.g. as electrical insulators or dielectric fluids in capacitors and transformers, specialised hydraulic fluids, as a plasticiser in sealin
27、g material etc. World-wide, more than one million tons of PCBs were produced. PCDD/PCDF as well as PCBs are emitted during thermal processes. PCB can contribute considerably 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
28、experts of the World Health Organisation (WHO) defined toxicity equivalent factors (TEFs) for PCDDs/PCDFs and twelve PCBs, known as dioxin-like PCBs 9;10 (see Annex A). These twelve dioxin- like PCBs consist of four non-ortho PCBs and eight mono-ortho PCBs (no or only one chlorine atoms in 2-, 2-, 6
29、- and 6-position), having a planar or mostly planar structure, see Figure 1. This document deals with the determination of these dioxin-like PCBs in emissions from stationary sources. Only skilled operators who are trained in handling highly toxic compounds should apply this document. Figure 1 Struc
30、ture of PCB 1 Scope This document specifies sampling from stationary sources, extraction, clean-up, identification and quantification procedures of the dioxin-like PCBs. The procedure described lays down requirements to measure the PCB congeners given in Annex A (see Table A.1). It is applicable to
31、the twelve non- and mono- ortho PCB designated by the WHO. It is optimised to measure PCB concentrations in the range of 0,01 ng WHO-TEQPCB/m3. In addition to the 12 non- and mono-ortho-PCB the present document is also applicable to measure further PCB-congeners like the so-called “marker PCB” 28, 5
32、2, 101, 138, 153, 180 (see Annex D). This document specifies a framework of quality control requirements which have to be fulfilled by any PCB sampling, extraction, clean-up, identification and quantification methods to be applied. It is assumed that due to their similar chemical behaviour PCBs may
33、be sampled from stationary sources together with the PCDDs/PCDFs by the same methods. The complete sampling procedure is described in the EN 1948-1. Each of the three sampling methods of EN 1948-1 can be combined with the methods described CEN/TS 1948-4:2007 Licensed Copy: London South Bank Universi
34、ty, London South Bank University, Sat Sep 01 03:12:46 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 5 in this document to complete the measurement procedure. EN 1948-1 is an integral part of the complete measurement procedure and is necessary for the determination of PCBs. In addition it is possible to
35、 measure PCBs together with PCDDs/PCDFs by applying EN 1948 Part 1, Part 2, Part 3 and CEN/TS 1948 Part 4. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, t
36、he latest edition of the referenced document (including any amendments) applies. EN 1948-1:2006, Stationary source emissions - Determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs - Part 1: Sampling of PCDDs/PCDFs EN 1948-2:2006, Stationary source emissions - Determination of
37、the mass concentration of PCDDs/PCDFs and dioxin-like PCBs - Part 2: Extraction and clean-up of PCDDs/PCDFs 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/PCDFs EN 13284-1,
38、 Stationary source emissions Determination of low range mass concentration of dust Part 1: Manual gravimetric method 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 1948-1:2006, EN 1948-2:2006, EN 1948-3:2006 and the following apply. 3.1 analytical bl
39、ank value value determined by a blank sample covering the complete analytical procedure including extraction, clean-up, identification and quantification including all the relevant reagents and materials 3.2 congener one of the 209 individual PCBs 3.3 dioxin-like PCBs non- and mono-ortho PCB with an
40、 affinity to the Ah-receptor, showing similar toxical effects as the 2,3,7,8- substituted PCDDs/PCDFs according to WHO Error! Bookmark not defined. 3.4 extraction standard 13C 12-labelled PCBs, added before extraction and used for calculating results 3.5 field blank value value determined by a blank
41、 sample covering a specific procedure to ensure that no significant contamination has occurred during all steps of measurement and to check that the operator can achieve a quantification level adapted to the task 3.6 I-TEF international toxic equivalent factor defined by NATO/CCMS in 1988 11 (for de
42、tailed description, see EN 1948-1:2006, Annex A) CEN/TS 1948-4:2007 Licensed Copy: London South Bank University, London South Bank University, Sat Sep 01 03:12:46 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 6 3.7 I-TEQ international toxic equivalent obtained by weighting the mass determined with the
43、corresponding I-TEF (for a detailed description, see EN 1948-1:2006, Annex A) 3.8 isokinetic sampling sampling at a flow rate such that the velocity and direction of the gas entering the sampling nozzle are the same as the velocity and direction of the gas in the duct at the sampling point EN 13284-
44、1:2001, definition 3.5 3.9 keeper solvent of high boiling point added to the sampling standard solution 3.10 Limit of detection (LOD) minimum value of the measurand for which the measuring system is not in the basic state, with a stated probability NOTE 1 The detection limit, also referred to as cap
45、ability of detection, is defined by reference to the applicable basic state. But it may be different from “zero“, for instance for oxygen measurement as well as when gas chromatographs are used. EN ISO 9169:2006, definition 2.2.10 12 NOTE 2 The measurement value can be distinguished from the analyti
46、cal blank value with a confidence of 99 %. The limit of detection is expressed as the mean analytical blank value (bave) plus three times the standard deviation of the analytical blank (sb). bave sbLOD3+= (1) where LOD is the detection limit; bave is the mean analytical blank value; sb is standard d
47、eviation of the analytical blank. NOTE 3 In this document the limit of detection should preferably be calculated from the analytical blank bave. If this is not possible, the limit of detection can be calculated from the signal to noise ratio according to 8.1 of EN 1948-3:2006 (resp. 10.3 of this doc
48、ument). 3.11 limit of quantification (LOQ) limit above which a quantification of the measurand is possible, expressed as the mean analytical blank value plus, either, five to ten times the standard deviation of the analytical blank. The factor F depends to the accepted measurement uncertainty bave s
49、FbLOQ+= (2) where LOQ is the quantification limit; bave is the mean analytical blank value; sb is standard deviation of the analytical blank CEN/TS 1948-4:2007 Licensed Copy: London South Bank University, London South Bank University, Sat Sep 01 03:12:46 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 7 NOTE In this document the limit of quantification should preferably be calculated from the analytical blank bave. If this is not possible, the limit of quantificatio