1、BRITISH STANDARDBS EN 15549:2008Air quality Standard method for the measurement of the concentration of benzoapyrene in ambient airICS 13.040.20g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g3
2、7g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN 15549:2008This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 April 2008 BSI 2008ISBN 978 0 580 56099 6National forewordThis British Standard is the UK implementation of EN 15549:2008. The UK p
3、articipation in its preparation was entrusted by Technical Committee EH/2, Air quality, to Subcommittee EH/2/3, Ambient atmospheres.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 necessary provisi
4、ons of a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunity from legal obligations.Amendments/corrigenda issued since publicationDate CommentsEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 15549March 2008ICS 13.040.20English Versi
5、onAir quality - Standard method for the measurement of theconcentration of benzoapyrene in ambient airQualit de lair - Mthode normalise pour le mesurage dela concentration de benzoapyrne dans lair ambiantLuftbeschaffenheit - Messverfahren zur Bestimmung derKonzentration von Benzoapyren in LuftThis E
6、uropean Standard was approved by CEN on 2 February 2008.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 references
7、concerning such nationalstandards may be obtained on application to the CEN Management Centre 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 into its
8、own language and notified to the CEN Management Centre has the same status as theofficial versions.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, Lithuan
9、ia, Luxembourg, 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 2008 CEN Al
10、l rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15549:2008: EEN 15549:2008 (E) 2 Contents Page Foreword3 Introduction.4 1 Scope 5 2 Normative references 5 3 Terms and definitions .5 4 Symbols and abbreviations7 5 Principle of the method.8
11、6 Requirements.9 7 Reagents and gases 11 8 Apparatus .12 9 Sampling.13 10 Sample preparation .14 11 Analysis 15 12 Quantification.17 13 Quality control .21 14 Determination of measurement uncertainty .23 15 Interferences 25 16 Reporting of results.26 Annex A (informative) Sampling systems 27 Annex B
12、 (informative) Extraction methods (examples of experimental conditions) .30 Annex C (informative) Example for clean-up procedure.32 Annex D (informative) Parameters for analysis (examples) .33 Annex E (informative) Assessment of performance indicators and uncertainty contributions .35 Annex F (infor
13、mative) Results of laboratory and field tests .44 Bibliography50 BS EN 15549:2008EN 15549:2008 (E) 3 Foreword This document (EN 15549:2008) 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
14、a national standard, either by publication of an identical text or by endorsement, at the latest by September 2008, and conflicting national standards shall be withdrawn at the latest by September 2008. Attention is drawn to the possibility that some of the elements of this document may be the subje
15、ct of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document 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)
16、. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy
17、, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. BS EN 15549:2008EN 15549:2008 (E) 4 Introduction The European Directive 2004/107/EC prescribes the reference methodology for the measurement
18、of benzoapyrene (BaP) in ambient air and states that the method shall be a method based on manual PM10 sampling systems described in EN 12341 or equivalent. Hence, this European Standard describes a method in which the sampling systems fulfil this requirement. However, in the course of drafting this
19、 European Standard it became clear that in certain circumstances, in the presence of oxidants such as ozone, BaP may be degraded. In specific situations this may result in losses of BaP of 50 %. It has been shown that the degradation due to ozone can be substantially reduced by including an ozone de
20、nuder in the sampling system. To date only a limited number of experiments has been performed in order to evaluate the particular conditions under which the denuder systems can be efficiently used. Consequently, the application of ozone denuders lacks sufficient validation to be a normative part of
21、this European Standard. In order to have a complete picture of the performance of ozone denuder systems further information is required on: efficiency under variable atmospheric conditions, regeneration time after exposure to high humidity, maximum capacity for ozone, maximum sample volume and maxim
22、um sampling period, stability of catalyst, maximum period of use, particle losses. Examples of sampling using an ozone denuder are given in Annex A. The experimental evidence collected so far is presented in Annex F. It is recommended that further work is undertaken to provide data of BaP comparison
23、s with and without ozone denuders. BS EN 15549:2008EN 15549:2008 (E) 5 1 Scope This document specifies a measurement method for the determination of particulate benzoapyrene (BaP) in ambient air, which can be used in the framework of the Council Directive 96/62/EC 1 and the Directive 2004/107/EC 2.
24、This document specifies performance characteristics and performance criteria for the measurement method when it is used as a reference method. The performance characteristics of the measurement method are based on a sampling period of 24 h. This document describes a measurement method which comprise
25、s sampling of BaP as part of the PM10 particles, sample extraction and analysis by high performance liquid chromatography (HPLC) with fluorescence detector (FLD) or by gas chromatography with mass spectrometric detection (GC/MS). The method is applicable for the measurement of BaP in the concentrati
26、on range from approx. 0,04 ng/m3to approximately 20 ng/m3. The lower limit of the applicable range depends on the noise level of the detector and the variability of the laboratory filter blank. NOTE If the BaP concentration exceeds the calibration range the extract can be diluted. 2 Normative refere
27、nces The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 12341:1998, Air quality Determination of
28、the PM 10 fraction of suspended particulate matter Reference method and field test procedure to demonstrate reference equivalence of measurement methods ENV 13005:1999, Guide to the expression of uncertainty in measurement ISO 8258, Shewhart control charts (including ISO 8258:1993 Technical Corrigen
29、dum 1) 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 calibration solution solution used for calibration of the analytical instrument, containing the analyte of interest at a suitable concentration, prepared by dilution of the stock standard
30、 solution 3.2 certified reference material (CRM) reference material one or more of whose property values are certified by a technically valid procedure, accompanied by or traceable to a certificate or other documentation that is issued by a certifying body 3.3 external standard solution solution of
31、the analyte of known concentration 3.4 field blank filter filter that is taken through the same procedure as a sample, except that no air is drawn through it 3.5 internal standard solution solution of a known substance of known concentration, added to the sample before chromatographic analysis BS EN
32、 15549:2008EN 15549:2008 (E) 6 3.6 laboratory blank filter unused filter that does not leave the laboratory and is taken through the same analytical procedure as the sample 3.7 PM10 target specification for sampling the thoracic particles EN 12341:1998 3.8 reagent blank solution solution that contai
33、ns all the reagents used during analysis of the sample, but without the sample and filter matrix EN 14902:2005 27 3.9 stock standard solution solution used for preparing calibration solutions, containing the analyte of interest at a concentration traceable to national or international standards 3.10
34、 surrogate standard solution solution of a known substance and of known concentration, used to spike filters before extraction in order to check the recovery efficiency 3.11 target value concentration in the ambient air fixed with the aim of avoiding, preventing or reducing harmful effects on human
35、health and the environment, as a whole, to be attained where possible over a given period NOTE This definition originates from 2. The current value for BaP is 1 ng/m3for the total content in the PM10 fraction averaged over a calendar year. 3.12 uncertainty (of measurement) parameter associated with
36、the result of a measurement, that characterises the dispersion of the values that could reasonably be attributed to the measurand ENV 13005:1999 BS EN 15549:2008EN 15549:2008 (E) 7 4 Symbols and abbreviations 4.1 Symbols a is the slope of linear calibration function; ACis the peak area or peak heigh
37、t of BaP or of its characteristic ion in the chromatogram of the calibration solution; AEis the peak area or peak height of BaP or of its characteristic ion in the chromatogram of the sample extract; AIS is the peak area or peak height of the internal standard or of its characteristic ion in the chr
38、omatogram of the calibration solution; AISEis the peak area or peak height of the internal standard or of its characteristic ion in the chromatogram of the sample extract; b is the intercept of the linear calibration function; C is the concentration of BaP in ambient air in ng/m; DCis the detection
39、limit, expressed in ng/m; DMis the absolute detection limit in the sample in ng; f is the response factor of BaP; m is the mean of laboratory filter blanks in ng; mCis the mass of BaP in the calibration solution in ng; mCRMis the certified mass in the CRM in ng; mEis the mass of BaP in the sample ex
40、tract in ng; mFis the mass of BaP on the filter sample in ng; miis the individual filter blank in ng; mISis the mass of the internal standard in the calibration solution in ng; mISEis the mass of the internal standard in the sample extract in ng; mreg is themass of BaP calculated from the regression
41、 equation at the level of the calibration standard in ng; mSSEis the mass of the surrogate standard in the sample extract in ng; mSSFis the mass of the surrogate standard added to the filter in ng; m/z is the mass-to-charge ratio; BS EN 15549:2008EN 15549:2008 (E) 8 n is the number of analysed filte
42、rs; R is the recovery efficiency of BaP in %; Rsis the peak resolution; Slfbis the standard deviation of laboratory filter blanks in ng; s(mE) is the standard deviation of the replicate measurement results of the mass determined in ng; t is the sampling time in h; tn-1;0,95is the Student factor for
43、n measurements and a 95 % confidence interval; tR1is the retention time for peak 1 in min; tR2is the retention time for peak 2 in min; EV is the volume of the extract in ml; V is the volume of air sampled in m3; Vnis the nominal daily sampling volume in m; w1is the peak width of peak 1 in min; w2is
44、the peak width of peak 2 in min; Xais the measured mass fraction of BaP in mg/kg; Xcais the certified mass fraction of BaP in mg/kg. 4.2 Abbreviations BaP Benzoapyrene CRM Certified reference material DAD Diode array detector FLD Fluorescence detectorGC Gas chromatography HPLC High performance liqui
45、d chromatography MS Mass spectrometry 5 Principle of the method The method is divided into two main parts: first the sampling in the field and second the analysis in the laboratory. During sampling, particles are collected on a filter by sampling a measured volume of air by means of a sampler equiva
46、lent to one of those described in EN 12341. The sampling time is 24 h. The filter is transported to the laboratory. BaP is extracted using an organic solvent. If necessary, the extract is cleaned up. The resulting solution is analysed by HPLC/FLD or GC/MS. BS EN 15549:2008EN 15549:2008 (E) 9 6 Requi
47、rements 6.1 Siting requirements Specific siting requirements depend on the objectives of the measurements. For measuring in compliance with Directive 2004/107/EC then the instructions for siting samplers given in 2 shall be followed. 6.2 Sampling requirements The sampling system shall be equivalent
48、to EN 12341 (see 2). NOTE 1 Equivalence can be demonstrated by performing a side-by-side comparison of the system with a PM10 reference sampler. Guidance for the performance of such comparisons is given in 3. NOTE 2 In the presence of ozone BaP may degrade. In specific situations this may lead to lo
49、sses of BaP of 50 %. Whenever these effects are expected to be significant, the PM10 sampler may be equipped with an ozone denuder (see Annex A). The experimental evidence collected so far is presented in Annex F. However, the application of ozone denuders lacks sufficient validation to be a normative part of this European Standard. NOTE 3 Examples of sampling systems with and without denuder are presented in Annex A. 6.3 Analysis 6.3.1 Recovery efficiency Using the external or internal standard method for quantification
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