1、BS EN 13890:2009ICS 13.040.30NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDWorkplace exposure Procedures formeasuring metalsand metalloids inairborne particles Requirements and testmethodsThis British Standardwas published under theauthority of the StandardsPo
2、licy and StrategyCommittee on 31 October2009. BSI 2009ISBN 978 0 580 58636 1Amendments/corrigenda issued since publicationDate CommentsBS EN 13890:2009National forewordThis British Standard is the UK implementation of EN 13890:2009. Itsupersedes BS EN 13890:2002 which is withdrawn.The UK participati
3、on in its preparation was entrusted to TechnicalCommittee EH/2/2, Work place atmospheres.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for
4、its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.BS EN 13890:2009EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 13890September 2009ICS 13.040.30 Supersedes EN 13890:2002 English VersionWorkplace exposure - Procedures for measuring metals andm
5、etalloids in airborne particles - Requirements and test methodsExposition sur les lieux de travail - Procdures pour lemesurage des mtaux et mtallodes dans les particules ensuspension dans lair - Exigences et mthodes dessaiExposition am Arbeitsplatz - Messung von Metallen undMetalloiden in luftgetrag
6、enen Partikeln - Anforderungen undPrfverfahrenThis European Standard was approved by CEN on 8 August 2009.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
7、. Up-to-date lists and bibliographical references 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 translation
8、under the responsibility of a CEN member into its 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,
9、 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 EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centr
10、e: Avenue Marnix 17, B-1000 Brussels 2009 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 13890:2009: EBS EN 13890:2009EN 13890:2009 (E) 2 Contents Page Foreword 3Introduction .41 Scope 52 Normative references 53 Terms and definition
11、s .54 Principle 65 Requirements .65.1 Method description 65.2 Performance requirements .76 Reagents and materials 86.1 Reagents .86.2 Standard solutions 86.3 Test materials .96.4 Reference air samples .97 Apparatus .98 Test methods 98.1 Detection limits and quantification limits .98.2 Analytical rec
12、overy . 108.3 Measurement uncertainty 129 Test report . 13Annex A (informative) Guidance on determination of analytical recovery 14Annex B (informative) Estimation of uncertainty of measurement . 16Annex C (informative) Interpolation of standard deviation 35Annex D (informative) Example of estimatio
13、n of expanded uncertainty 37Bibliography . 40BS EN 13890:2009EN 13890:2009 (E) 3 Foreword This document (EN 13890:2009) has been prepared by Technical Committee CEN/TC 137 “Assessment of workplace exposure to chemical and biological agents”, the secretariat of which is held by DIN. This European Sta
14、ndard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by March 2010, and conflicting national standards shall be withdrawn at the latest by March 2010. Attention is drawn to the possibility that some of the elements of thi
15、s 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 document supersedes EN 13890:2002. The major technical changes between this European Standard and the previous edition are as follows: a) Adaptation of
16、 the framework for assessing the performance of procedures for measuring metals and metalloids against the general requirements for the performance of procedures for measuring chemical agents in workplace atmospheres as specified in EN 482; b) Revision of the calculation model for the uncertainty of
17、 measurement to comply with EN 482 and ENV 13005. 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, G
18、ermany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. BS EN 13890:2009EN 13890:2009 (E) 4 Introduction This European Standard provides a framework
19、for assessing the performance of procedures for measuring metals and metalloids against the general requirements for the performance of procedures for measuring chemical agents in workplace atmospheres as specified in EN 482. It enables producers and users of procedures for measuring metals and meta
20、lloids in airborne particles to adopt a consistent approach to method validation. Although this European Standard has been written for assessing the performance of procedures for measuring metals and metalloids, it can be used as the basis for assessing the performance of procedures for measuring ot
21、her chemical agents that are present as or in airborne particles, e.g. sulphuric acid mist. BS EN 13890:2009EN 13890:2009 (E) 5 1 Scope This European Standard specifies performance requirements and test methods for the evaluation of procedures for measuring metals and metalloids in airborne particle
22、s sampled onto a suitable collection substrate, e.g. a filter. This European Standard specifies a method for estimating the uncertainties associated with random and systematic errors and combining them to calculate the expanded uncertainty of the measuring procedure as a whole, as prescribed in EN 4
23、82. This European Standard is applicable to measuring procedures in which sampling and analysis is carried out in separate stages, but it does not specify performance requirements for collection, transport and storage of samples, since these are dealt with in EN 13205 and ISO 15767. This European St
24、andard is not applicable to procedures for measuring metals or metalloids present as inorganic gases or vapours, e.g. mercury, arsenic (see EN 838 and EN 1076), or to procedures for measuring metals and metalloids in compounds that could be present as a particle/vapour mixture, e.g. arsenic trioxide
25、. 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, the latest edition of the referenced document (including any amendments) applies. EN 481, Workplace atmosp
26、heres Size fraction definitions for measurement of airborne particles EN 482:2006, Workplace atmospheres General requirements for the performance of procedures for the measurement of chemical agents EN 1232:1997, Workplace atmospheres Pumps for personal sampling of chemical agents Requirements and t
27、est methods EN 1540:1998, Workplace atmospheres Terminology EN 12919, Workplace atmospheres Pumps for the sampling of chemical agents with a volume flow rate of over 5 l/min Requirements and test methods EN 132051)Workplace atmospheres Assessment of performance of instruments for measurement of airb
28、orne particle concentrations EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696:1987) 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 482:2006 and EN 1540:19982)apply. 1) All references to EN 13205 in this Europe
29、an Standard refer to the ongoing revision of EN 13205:2001. 2) EN 1540:1998 is currently subject to revision. Until the revised EN is published the definitions given in EN 482:2006 take precedence. BS EN 13890:2009EN 13890:2009 (E) 6 4 Principle For measuring procedures that involve sample dissoluti
30、on, instrumental detection limits are determined by repeat analysis of the calibration blank solution. For all measuring procedures, method detection limits and quantification limits are determined by analysis of laboratory blanks. The determined quantification limits are then assessed against the p
31、erformance requirements specified in 5.2.1. Analytical recovery is determined by one of a number of different methods, depending upon the nature of the measuring procedure under evaluation. For measuring procedures for soluble compounds of metals and metalloids, analytical recovery is determined by
32、analysis of spiked laboratory blanks (except for procedures that incorporate a design-based sample dissolution method (see A.1.1), for which it is taken to be 100 %). For measuring procedures for total metals and metalloids that involve sample dissolution, analytical recovery is determined by analys
33、is of pure compounds, reference materials or reference air samples. For measuring procedures for total metals and metalloids that involve analysis of the sample on the collection substrate, analytical recovery is determined by analysis of reference air samples, by the analysis of workplace air sampl
34、es that are characterised by subsequent analysis using a reference procedure or it is estimated from theory. The determined analytical recovery is then assessed against the performance requirements specified in 5.2.2. Measurement uncertainty is estimated using a structured approach. Firstly, a cause
35、 and effect diagram is constructed to identify individual random and non-random uncertainty components of a measuring procedure. After simplification to resolve any duplication, the resulting diagram is used to identify components for which uncertainty estimates are required. Each of these uncertain
36、ty components is then estimated or calculated from experimental data, combined to obtain an estimate of the uncertainty of the measurement method as a whole and multiplied by an appropriate coverage factor to calculate the expanded uncertainty of the method, following the guidance in Annex B. In acc
37、ordance with 5.2.3, the determined expanded uncertainty is then assessed against the general performance requirements specified in EN 482. 5 Requirements 5.1 Method description 5.1.1 Scope The scope of the measuring procedure shall give at least information about the following: the metals and metall
38、oids covered by the measuring procedure; the analytical technique(s) used in the measuring procedure; the range of concentrations of metals and metalloids in air for which the measuring procedure has been shown to meet the acceptance criteria for expanded uncertainty prescribed in EN 482, together w
39、ith the associated range of sampled air volumes (e.g. 0,01 mg m-3 to 0,5 mg m-3for sampled air volumes in the range 240 l to 960 l); any form of the metals and metalloids for which the sample preparation method described has been shown to be or is known to be ineffective; and any known interferences
40、. NOTE If there is no procedure for measuring a particular metal or metalloid that meets the requirements of this European Standard, a measuring procedure whose performance is nearest to the specified requirements should be used. BS EN 13890:2009EN 13890:2009 (E) 7 5.1.2 Method performance For all m
41、etals and metalloids included in the scope of the method, the measuring procedure shall give comprehensive information about method performance, including the following: the detection and quantification limits of the measuring procedure; the analytical recovery for all test materials for which the s
42、ample preparation method has been shown to be effective; all random and non-random uncertainty components of the measuring procedure, together with their estimated or experimentally determined values, and the resulting expanded uncertainty; and full details of any known interferences, including suit
43、able and sufficient information on how to minimise their effects, if applicable. 5.1.3 Safety information The measuring procedure shall provide suitable and sufficient information on the safety hazards associated with the reagents and equipment used in the procedure. 5.1.4 Samplers The measuring pro
44、cedure shall: require the user to select samplers that are designed to collect an appropriate fraction of airborne particles, as defined in EN 481, according to the particle size fraction(s) that is applicable to the limit value for the metals and metalloids of interest (e.g. an inhalable sampler, a
45、 thoracic sampler or a respirable sampler); specify that the samplers shall comply with the provisions of EN 13205; and require, if appropriate, for procedures that do not involve sample dissolution, calibration of the analytical instrument used to be sampler specific, e.g. for X-ray fluorescence sp
46、ectrometry (XRF). 5.1.5 Sampling pumps The measuring procedure shall require the user to use sampling pumps that comply with the provisions of EN 1232 or EN 12919. 5.1.6 Other requirements Where necessary, the measuring procedure shall give other requirements, e.g. for the collection substrate. 5.2
47、Performance requirements 5.2.1 Quantification limit For each metal and metalloid included in the scope of the measuring procedure, determine the lower limit of the working range of the method that will be satisfactory for the intended measurement task. For example, if the measurement task is testing
48、 compliance with long-term limit values, use Equation (1) to calculate the least amount of the metal or metalloid that needs to be quantified when it is to be determined at a concentration of 0,1 times its limit value: (1) BS EN 13890:2009EN 13890:2009 (E) 8 where is the lower limit of the required
49、analytical range of the metal or metalloid, in micrograms; is the limit value for the metal or metalloid, in milligrams per cubic metre; is the design flow rate of the sampler to be used, in litres per minute; and is the minimum sampling time that will be used, in minutes. For procedures that involve sample dissolution, calculate the lower limit of the required working range for each metal and metalloid, in micrograms per millilitre, by divi
