1、 g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58Cd, As and Ni in the PM10 fraction of suspended particulate matterThe European Standard EN 14902:20
2、05 has the status of a British StandardICS 13.040.20Ambient air quality Standard method for the measurement of Pb, BRITISH STANDARDBS EN 14902:2005Incorporating corrigendum no. 1BS EN 14902:2005This British Standard was published under the authority of the Standards Policy and Strategy Committee on
3、27 September 2005 BSI 2007ISBN 0 580 46678 7Compliance with a British Standard cannot confer immunity from legal obligations.Amendments issued since publicationAmd. No. Date Comments17049 Corrigendum No. 130 April 2007 Equation 5 replacedNational forewordThis British Standard was published by BSI. I
4、t is the UK implementation of EN 14902:2005, incorporating corrigendum October 2006.The UK participation 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 subcommittee can be obtained on
5、request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 14902August 2005ICS 13.040.20 Incorporating corrigendum October 2006English versionAmb
6、ient air quality - Standard method for the measurement ofPb, Cd, As and Ni in the PM10 fraction of suspended particulatematterQualit de lair ambiant - Mthode normalise pour lamesure de Pb, Cd, As et Ni dans la fraction MP10 de lamatire particulaire en suspensionAuenluftbeschaffenheit - Standardisier
7、tes Verfahren zurBestimmung von Pb/Cd/As/Ni als Bestandteil der PM10Fraktion des SchwebstaubesThis European Standard was approved by CEN on 27 June 2005.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the statu
8、s 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 (English, French, German). A vers
9、ion 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, Czech Republic, Denmark, Estonia,
10、 Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR
11、 NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2005 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14902:2005: EEN 14902:2005 (E) 2 Contents Page Foreword .3 1 Scope 4 2 Normative references.5 3 Terms, definitions an
12、d abbreviations .5 4 Principle8 5 Requirements .9 6 Reagents and gases.10 7 Apparatus .11 8 Sampling.12 9 Analysis 14 10 Quality control22 11 Calculation of results.23 12 Estimation of the measurement uncertainty of the method26 13 Performance characteristics determined in field tests .27 14 Reporti
13、ng of results .32 Annex A (informative) Examples of closed vessel microwave digestion procedures 33 Annex B (informative) Typical laboratory filter blank values as determined in the field validation tests35 Annex C (informative) Analytical interferences36 Annex D (informative) Approach to uncertaint
14、y estimation used in the field validation tests .40 Annex E (normative) List of minimum QA / QC procedures46 Annex F (informative) Procedure for the determination of the uncertainty of the method for an individual laboratory 48 Annex ZA (informative) Relationship with EU Directives 53 Bibliography .
15、54 EN 14902:2005 (E) 3 Foreword This European Standard (EN 14902:2005) 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 a national standard, either by publication of an identical text or by
16、 endorsement, at the latest by February 2006, and conflicting national standards shall be withdrawn at the latest by February 2006. This European Standard has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association (see Annex ZA). According to th
17、e CEN/CENELEC Internal Regulations, 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, Luxemb
18、ourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EN 14902:2005 (E) 4 1 Scope This European Standard specifies a method for the determination of particulate lead (Pb), cadmium (Cd), arsenic (As) and nickel (Ni) in ambient air that
19、can be used in the framework of the European Council Directive on Ambient Air Quality Assessment and Management 1 and the 1st2 and 4th3 Daughter Directives. Performance requirements with which the method has to comply are specified in this European Standard. The performance characteristics of the me
20、thod were determined in comparative field validation tests carried out at four European locations (see 4). This European Standard specifies a method for sampling of Pb, Cd, As and Ni as part of the PM10 aerosol, microwave digestion of the samples and analysis by graphite furnace atomic absorption sp
21、ectrometry or by inductively coupled plasma (quadrupole) mass spectrometry. This European Standard is applicable for the measurement of Pb, Cd, As and Ni as part of the PM10 aerosol fraction in the concentration ranges listed in Table 1. Table 1 Working ranges of the method in ng/m From To Pb 1 4 00
22、0 Cd 0,1 50 As 0,5 350 Ni 2 100 The actual lower limits of the working ranges depend upon the variability of the laboratory filter blank (5.3.1). The lower limits of the working ranges given in Table 1 are expected values based upon performance achieved in the field validation tests. Similarly the u
23、pper limits of the working ranges have been set arbitrarily based upon the maximum daily values measured during the field validation tests. The method can be applied to higher concentrations provided the PM10 collection characteristics of the sampler are not compromised. EN 14902:2005 (E) 5 2 Normat
24、ive references The following referenced documents are indispensable for the application of this European Standard. 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 qualit
25、y Determination of the PM10 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 measurement13 Terms, definitions and abbreviations 3.1 Terms and defin
26、itions For the purpose of this European Standard, the following terms and definitions apply. 3.1.1 analysis all operations carried out after sample preparation to determine the amount or concentration of the metals or metalloid of interest present in the sample 3.1.2 blank solution solution prepared
27、 from a laboratory filter blank or a field filter blank by the process of sample dissolution NOTE A laboratory filter blank solution or a field filter blank solution might need to be subjected to further operations, e.g. dilution and/or addition of an internal standard(s), if such operations are app
28、lied to the sample solutions in order to produce test solutions that are ready for analysis. 3.1.3 calibration blank solution calibration solution prepared without addition of stock standard solution or working standard solution, for which the concentration of the analyte(s) of interest is considere
29、d to be zero 3.1.4 calibration solution solution used for calibration of the analytical instrument, containing the analyte(s) of interest at (a) suitable concentration(s), prepared by dilution of the stock standard solution(s) or the working standard solution(s) NOTE The technique of matrix-matching
30、 is normally used when preparing calibration solutions. 3.1.5 certified reference material reference material, in which one or more of 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 bo
31、dy 5 3.1.6 field filter blank filter that is taken through the same procedure as a sample, except that no air is drawn through it. It is transported to the sampling site, mounted in the sampling unit, dismounted, returned to the laboratory and worked up in the same way as a sample 1Equal to ISO Guid
32、e 30 (GUM) Geneva 1993. EN 14902:2005 (E) 6 3.1.7 internal standard solution solution added to sample, blank and calibration solutions to correct for instrumental fluctuations during analysis, containing (a) suitable element(s) at (a) suitable concentration(s) 3.1.8 instrumental detection limit lowe
33、st amount of an analyte that is detectable using an instrument, as determined by repeated measurements of a reagent blank 3.1.9 laboratory filter blank unused filter that does not leave the laboratory and is taken through the same analytical procedure as a sample. This filter is taken from the same
34、batch as used for sampling 3.1.10 limit value level fixed on the basis of scientific knowledge, with the aim of avoiding, preventing or reducing harmful effects on human health and/or the environment as a whole, to be attained within a given period and not to be exceeded once attained 3.1.11 matrix
35、interference non-spectral interference matrix effect interference of a non-spectral nature caused by a difference between the matrix of the calibration and test solutions 3.1.12 matrix-matching technique, used to minimise the effect of matrix interferences on analytical results, that involves prepar
36、ation of calibration solutions in which the concentrations of acids and other major solutes are matched with those in the test solutions 3.1.13 method detection limit lowest amount of an analyte that is detectable using the method, as determined by analysis of laboratory filter blanks 3.1.14 PM10 ta
37、rget specification for sampling the thoracic particles EN 12341:1998 3.1.15 PM10 reference sampler by convention, a sampling instrument that possesses the required performance characteristics, in order to assess the PM 10 mass concentration EN 12341:1998 3.1.16 PM10 sampler sampling instrument whose
38、 performance has been demonstrated to be equivalent to a PM 10 reference sampler 3.1.17 quality control solution solution that is analysed together with the sample solutions to provide information on the repeatability of the analytical method, results for which are plotted on a quality control chart
39、 to verify that a method is performing satisfactorily EN 14902:2005 (E) 7 3.1.18 quantification limit lowest amount of an analyte that is quantifiable with a given confidence level using the method, as determined by analysis of laboratory filter blanks 3.1.19 reagent blank solution solution that con
40、tains all the reagents used during the analysis of the sample, but without the sample and filter matrix 3.1.20 repeatability (of results of measurements) closeness of the agreement between the results of successive measurements of the same measurand carried out under the same conditions of measureme
41、nt 6 3.1.21 reproducibility (of results of measurements) closeness of the agreement between the results of measurements of the same measurand carried out under changed conditions of measurement 6 3.1.22 sample solution solution prepared from a sample by the process of sample dissolution NOTE A sampl
42、e solution might need to be subjected to further operations, e.g. dilution and/or addition of an internal standard(s), in order to produce a test solution that is ready for analysis. 3.1.23 sampling method all steps of the measuring procedure that describe the process of collecting an air sample 3.1
43、.24 sample preparation all operations carried out on a sample, after transportation and storage, to prepare it for analysis, including transformation of the sample into a measurable state, where necessary 3.1.25 sample digestion sample dissolution process of obtaining a solution containing the analy
44、tes of interest from a sample. This can involve complete dissolution of the sample 3.1.26 stock standard solution solution used for preparation of calibration solutions, containing one or more of the analyte(s) of interest at (a) concentration(s) traceable to national or International Standards 3.1.
45、27 sub-sample (of a filter) part of a large filter, cut out for analytical reasons, that is representative of the whole 3.1.28 suspended particulate matter notion of all particles surrounded by air in a given, undisturbed volume of air EN 12341:1998 3.1.29 target value concentration in the ambient a
46、ir fixed with the aim of avoiding, preventing or reducing harmful effects on human health and the environment as a whole, to be attained where possible over a given period 3 EN 14902:2005 (E) 8 3.1.30 test solution blank solution or sample solution that has been subjected to all operations required
47、to bring it into a state in which it is ready for analysis, e.g. dilution and/or addition of an Internal Standard(s) NOTE If subject to no further operations before analysis, then the blank test solution is identical to the blank solution. The same is true for the sample test solution and sample sol
48、utions. 3.1.31 uncertainty (of a measurement) parameter associated with the result of a measurement that characterises the dispersion of the values that could reasonably be attributed to the measurand ENV 13005:1999 3.1.32 working standard solution solution prepared by dilution of the stock standard
49、 solution(s), that contains the analyte(s) of interest at (a) concentration(s) better suited to preparation of calibration solutions 3.2 Abbreviations AAS atomic absorption spectrometry; amu atomic mass unit; CRM certified reference material; GFAAS graphite furnace atomic absorption spectrometry; HDPE high density polyethylene; HVS high volume sampler, as described in EN 12341:1998, Annex B.2; ICP-MS inductively coupled plasma mass spectrometry; LDPE low density polyethylene; LVS low volume sampler, a
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