1、January 2010DEUTSCHE NORM English price group 17No part of this standard may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 13.040.30!$tY“1568154w
2、ww.din.deDDIN EN 13890Workplace exposure Procedures for measuring metals and metalloids in airborne particles Requirements and test methodsEnglish version of DIN EN 13890:2010-01Exposition am Arbeitsplatz Messung von Metallen und Metalloiden in luftgetragenen Partikeln Anforderungen und Prfverfahren
3、Englische Fassung DIN EN 13890:2010-01SupersedesDIN EN 13890:2003-02www.beuth.deDocument comprises pages43DIN EN 13890:2010-01 National foreword This document has been prepared by Technical Committee CEN/TC 137 “Assessment of workplace exposure to chemical and biological agents” (Secretariat: DIN, G
4、ermany). The responsible German body involved in its preparation was the Normenausschuss Sicherheitstechnische Grundstze (Safety Design Principles Standards Committee), Working Committee NA 095-03-01 AA Mess-strategien und Anforderungen an Messverfahren. EN ISO 3696 referred to in clause 2 “Normativ
5、e references” has been published as DIN ISO 3696:1991-06. Amendments This standard differs from DIN EN 13890:2003-02 as follows: a) The title of the standard has been changed. b) The criteria for assessing the performance of procedures for measuring metals and metalloids have been adapted to the gen
6、eral requirements for the performance of procedures for measuring chemical agents in workplace atmospheres as specified in EN 482. c) The calculation model for the uncertainty of measurement has been revised and brought in line with the Guide to the expression of uncertainty in measurement (GUM, pub
7、lished as DIN V ENV 13005:1999-06). d) The standard has been editorially revised. Previous editions DIN EN 13890: 2003-02 2 EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 13890September 2009ICS 13.040.30 Supersedes EN 13890:2002 English VersionWorkplace exposure - Procedures for measuring metals
8、andmetalloids 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 luftge
9、tragenen 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 altera
10、tion. 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 transla
11、tionunder 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, Gre
12、ece, 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 C
13、entre: 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: EEN 13890:2009 (E) 2 Contents Page Foreword 3Introduction .41 Scope 52 Normative references 53 Terms and definitions .54 Princi
14、ple 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 recovery . 108.
15、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 estimation of expande
16、d uncertainty 37Bibliography . 40DIN EN 13890:2010-01 EN 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 Standard s
17、hall 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 this docum
18、ent 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 the fr
19、amework 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 measur
20、ement 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, Germany,
21、 Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. DIN EN 13890:2010-01 EN 13890:2009 (E) 4 Introduction This European Standard provides a framework fo
22、r 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 metall
23、oids 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 othe
24、r chemical agents that are present as or in airborne particles, e.g. sulphuric acid mist. DIN EN 13890:2010-01 EN 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 parti
25、cles 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 E
26、N 482. 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
27、 Standard 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 triox
28、ide. 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 atm
29、ospheres 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 an
30、d test 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 a
31、irborne 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 Eur
32、opean 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. DIN EN 13890:2010-01 EN 13890:2009 (E) 6 4 Principle For measuring procedures that involve sample d
33、issolution, 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 again
34、st the performance 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 determ
35、ined by 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 b
36、y analysis 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 a
37、ir samples 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,
38、 a cause 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 u
39、ncertainty 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
40、. In accordance 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 an
41、d metalloids 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, to
42、gether with 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 inter
43、ferences. 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. DIN EN 13890:2010-01 EN 13890:2009 (E) 7 5.1.2 Method performa
44、nce For all metals 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 fo
45、r which the sample 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, i
46、ncluding suitable 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
47、measuring procedure 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 inhalab
48、le sampler, a 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 fl
49、uorescence spectrometry (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 Performance requirements 5.2.1 Quantification limit For each metal and metalloid included in the scope of the measuring proce