Workplace atmospheres - Procedures for measuring metals and metalloids in airborne paticles - Requirements and test methods

This European Standard specifies performance requirements and test methods for procedures for measuring metals and metalloids in airborne particles collected on a suitable substrate, e.g. a filter.

Arbeitsplatzatmosphäre - Verfahren zur quantitativen Bestimmung von Metallen und Metalloiden in Schwebstoffen - Anforderungen und Prüfverfahren

Diese Europäische Norm legt Leistungsanforderungen und Prüfverfahren für Verfahren zur quantitativen Bestimmung von Metallen und Metalloiden in Schwebstoffen fest, die auf einem geeigneten Substrat, z.B. einem Filter, gesammelt wurden.

Atmosphères des lieux de travail - Procédures de mesurage des métaux et métalloïdes dans les particules en suspension dans l'air - Exigences et méthodes d'essai

La présente Norme européenne précise les exigences de performance et les méthodes d'essai pour l'évaluation des procédures de mesurage des métaux et métalloïdes présents dans les particules en suspension dans l'air recueillies sur un substrat approprié, par exemple un filtre.
La présente Norme européenne ne s'applique pas aux procédures de mesurage des métaux ou métalloïdes présents dans des gaz ou des vapeurs inorganiques, par exemple le mercure, l'arsine, etc. (voir l'EN 838 [1] et l'EN 1076 [2]), ni aux procédures de mesurage des métaux et métalloïdes présents dans des composés pouvant exister sous forme de mélange de particules/vapeurs, par exemple le trioxyde d'arsenic (voir l'ENV 13936 [3]).
La présente Norme européenne s'applique aux procédures de mesurage qui dissocient l'étape d'échantillonnage de l'étape d'analyse, mais elle ne précise aucune exigence métrologique concernant la collecte, le transport et le stockage des échantillons, dans la mesure où ces exigences sont traitées dans l'EN 13205.
La présente Norme européenne prescrit une méthode permettant de déterminer l'erreur systématique (ou biais) et la fidélité de la méthode d'analyse ainsi que de combiner celle-ci au biais et à la fidélité de la méthode d'échantillonnage afin d'estimer l'incertitude globale de la procédure de mesurage dans son ensemble.
En l'absence de procédure de mesurage d'un métal ou métalloïde particulier satisfaisant aux exigences de la présente Norme européenne, il est recommandé d'utiliser une procédure de mesurage dont les performances sont les plus proches possibles des exigences spécifiées.

Zrak na delovnem mestu - Postopki za merjenje kovin in polkovin v lebdečih delcih - Zahteve in preskusne metode

General Information

Status
Withdrawn
Publication Date
22-Oct-2002
Withdrawal Date
15-Sep-2009
Current Stage
9960 - Withdrawal effective - Withdrawal
Due Date
16-Sep-2009
Completion Date
16-Sep-2009

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SLOVENSKI STANDARD
SIST EN 13890:2003
01-marec-2003

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=DKWHYHLQSUHVNXVQHPHWRGH

Workplace atmospheres - Procedures for measuring metals and metalloids in airborne

paticles - Requirements and test methods
Arbeitsplatzatmosphäre - Verfahren zur quantitativen Bestimmung von Metallen und
Metalloiden in Schwebstoffen - Anforderungen und Prüfverfahren

Atmospheres des lieux de travail - Procédures de mesurage des métaux et métalloides

dans les particules en suspension dans l'air - Exigences et méthodes d'essai
Ta slovenski standard je istoveten z: EN 13890:2002
ICS:
13.040.30 Kakovost zraka na delovnem Workplace atmospheres
mestu
SIST EN 13890:2003 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN 13890:2003
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SIST EN 13890:2003
EUROPEAN STANDARD
EN 13890
NORME EUROPÉENNE
EUROPÄISCHE NORM
October 2002
ICS 13.040.30
English version
Workplace atmospheres - Procedures for measuring metals and
metalloids in airborne paticles - Requirements and test methods

Atmosphères des lieux de travail - Procédures de Arbeitsplatzatmosphäre - Verfahren zur quantitativen

mesurage des métaux et métalloïdes dans les particules en Bestimmung von Metallen und Metalloiden in

suspension dans l'air - Exigences et méthodes d'essai Schwebstoffen - Anforderungen und Prüfverfahren

This European Standard was approved by CEN on 9 September 2002.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European

Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national

standards may be obtained on application to the 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

under the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the official

versions.

CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,

Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels

© 2002 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 13890:2002 E

worldwide for CEN national Members.
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SIST EN 13890:2003
EN 13890:2002 (E)
Contents
page

Foreword......................................................................................................................................................................4

Introduction .................................................................................................................................................................5

1 Scope ..............................................................................................................................................................5

2 Normative references ....................................................................................................................................5

3 Terms and definitions....................................................................................................................................6

3.1 EN 1540 definitions........................................................................................................................................6

3.2 Measurement terms .......................................................................................................................................6

3.3 Sampling terms ..............................................................................................................................................6

3.4 Statistical terms .............................................................................................................................................7

4 Principle..........................................................................................................................................................8

5 Requirements .................................................................................................................................................8

5.1 General requirements....................................................................................................................................8

5.1.1 Scope of the measuring procedure..............................................................................................................8

5.1.2 Method performance .....................................................................................................................................8

5.1.3 Safety information .........................................................................................................................................9

5.1.4 Samplers.........................................................................................................................................................9

5.1.5 Sampling pumps ............................................................................................................................................9

5.1.6 Quantification limit ........................................................................................................................................9

5.1.7 Other detailed requirements.........................................................................................................................9

5.2 Analytical recovery ........................................................................................................................................9

5.3 Overall uncertainty ........................................................................................................................................9

6 Reagents.........................................................................................................................................................9

7 Reference samples ......................................................................................................................................10

7.1 Standard solutions ......................................................................................................................................10

7.2 Reference materials.....................................................................................................................................10

7.3 Reference air samples.................................................................................................................................10

8 Apparatus .....................................................................................................................................................10

9 Test methods................................................................................................................................................11

9.1 Detection limits and quantification limits..................................................................................................11

9.1.1 Determination of detection limits and quantification limits ....................................................................11

9.1.2 Comparison of results with the acceptance criteria ................................................................................11

9.2 Selection of test methods for determination of analytical bias and precision......................................11

9.3 Analytical bias..............................................................................................................................................11

9.3.1 Consideration of the analytical bias of procedures for soluble metals and metalloids.......................11

9.3.2 Determination of the analytical bias of procedures that involve sample dissolution or

dispersion of the collected airborne particles in a liquid ........................................................................11

9.4 Analytical precision .....................................................................................................................................12

9.4.1 Determination of the analytical precision of procedures that involve sample transformation

prior to analysis ...........................................................................................................................................12

9.4.2 Estimation of the analytical precision of procedures that do not involve sample transformation.....13

9.5 Estimation of overall uncertainty ...............................................................................................................13

10 Test report ....................................................................................................................................................14

Annex A (informative) Guidance on selection of test methods...........................................................................15

Annex B (informative) Guidance on determination of analytical bias ................................................................16

B.1 Determination of the analytical bias of procedures that involve sample dissolution ..........................16

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SIST EN 13890:2003
EN 13890:2002 (E)

B.2 Determination or estimation of the analytical bias of procedures that do not involve a sample

transformation..............................................................................................................................................16

Annex C (informative) Example of estimation of overall uncertainty .................................................................17

Annex D (informative) Estimation of overall uncertainty .....................................................................................19

D.1 General performance requirements for measurement of chemical agents in air .................................19

D.2 Combination of sampler bias and analytical bias ....................................................................................20

D.3 Combination of sampling and analytical precision..................................................................................20

Consideration of sampler bias and analytical bias ...............................................................................................20

D.4.1 Sampler bias.................................................................................................................................................20

D.4.2 Sampling precision......................................................................................................................................21

D.5 Estimation of overall uncertainty...............................................................................................................21

D.5.1 General case.................................................................................................................................................21

D.5.2 Estimation of overall uncertainty of procedures for measuring metals and metalloids in

inhalable dust...............................................................................................................................................21

D.5.3 Estimation of overall uncertainty of procedures for measuring metals and metalloids in

respirable dust .............................................................................................................................................22

Bibliography ..............................................................................................................................................................23

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SIST EN 13890:2003
EN 13890:2002 (E)
Foreword

This document EN 13890:2002 has been prepared by Technical Committee CEN/TC 137 "Assessment of

workplace exposure", 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 endorsement, at the latest by April 2003, and conflicting national standards shall be withdrawn at the latest by

April 2003.
Annexes A, B, C and D are informative.

According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following

countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland,

France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain,

Sweden, Switzerland and the United Kingdom.
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SIST EN 13890:2003
EN 13890:2002 (E)
Introduction

EN 482 prescribes general requirements for the performance of procedures for measuring chemical agents in

workplace atmospheres. These requirements include maximum values of overall uncertainty (a combination of

precision and bias) achievable under prescribed laboratory conditions.

This European Standard provides a framework for assessing the performance of procedures for measuring metals

and metalloids against the criteria specified in EN 482. It enables producers and users of procedures for measuring

metals and metalloids in airborne particles to adopt a consistent approach to method validation.

1 Scope

This European Standard specifies performance requirements and test methods for the evaluation of procedures for

measuring metals and metalloids in airborne particles collected on a suitable substrate, e.g. a filter.

This European Standard is not applicable to procedures for measuring metals or metalloids present in inorganic

gases or vapours, e.g. mercury, arsine, etc (see EN 838 [1] and EN 1076 [2]), or to procedures for measuring

metals and metalloids in compounds that could be present as a particle/vapour mixture, e.g. arsenic trioxide (see

ENV 13936 [3]).

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.

This European Standard specifies a method for determining the bias and precision of the analytical method and

combining this with the bias and precision of the sampling method to estimate the overall uncertainty of the

measuring procedure as a whole.

If there is no procedure for measuring a particular metal or metalloid which meets the requirements of this

European Standard, it is recommended to use a measuring procedure whose performance is nearest to the

specified requirements.
2 Normative references

This European Standard incorporates by dated or undated reference, provisions from other publications. These

normative references are cited at the appropriate places in the text, and the publications are listed hereafter. For

dated references, subsequent amendments to or revisions of any of these publications apply to this European

Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the

publication referred to applies (including amendments).

EN 481, Workplace atmospheres — Size fraction definitions for measurement of airborne particles.

EN 482:1994, Workplace atmospheres — General requirements for the performance of procedures for the

measurement of chemical agents.

EN 1232, Workplace atmospheres — Pumps for personal sampling of chemical agents — Requirements and test

methods.
EN 1540, 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.
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SIST EN 13890:2003
EN 13890:2002 (E)

EN 13205:2001, Workplace atmospheres — Assessment of performance of instruments for measurement of

airborne 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 European Standard, the following terms and definitions apply.

3.1 EN 1540 definitions

Averaging time, bias, chemical agent, limit value, measuring procedure, overall uncertainty, precision, specified

measuring range, true value, validation:
Definitions for these terms are as in EN 1540.
3.2 Measurement terms
3.2.1
analysis

all operations carried out after sample preparation to determine the amount or concentration of the metals or

metalloids of interest present in the sample
3.2.2
analytical method

all steps of the measuring procedure that describe the overall process of sample preparation and analysis

3.2.3
sampling method

all steps of the measuring procedure that describe the process of collecting an air sample

3.2.4
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
3.2.5
sample dissolution

process of obtaining a solution containing the analytes of interest from a sample.

NOTE This can or cannot involve complete dissolution of the sample.
3.2.6
reference sample

sample having a known or measured content or loading of the metals and metalloids of interest, which is analysed

to determine the analytical bias or the analytical precision of a measuring procedure

3.2.7
test solution

solution prepared by the process of sample dissolution and subjected to any further operations required to bring it

into a state in which it is ready for analysis
3.3 Sampling terms
3.3.1
collection substrate

medium on which airborne particles are collected, e.g. a filter or a polyurethane foam

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SIST EN 13890:2003
EN 13890:2002 (E)
3.3.2
inhalable sampler
sampler which collects the inhalable fraction of airborne particles
3.3.3
particle/vapour mixture
aerosol consisting of airborne particles and vapour
[ENV 13936 [3]]
3.3.4
respirable sampler
sampler which collects the respirable fraction of airborne particles
3.3.5
sample

collection substrate and the airborne particles collected on it, including, if appropriate, airborne particles collected

on the internal surfaces of the sampler
3.3.6
sampler
device for collecting airborne particles
3.4 Statistical terms
3.4.1
analytical bias
bias of the analytical method
3.4.2
analytical precision
imprecision arising from analytical variability
3.4.3
analytical recovery

ratio of the mass of analyte measured in a sample to the known mass of analyte in that sample, expressed as a

percentage
3.4.4
detection limit

lowest concentration of an analyte that the analytical process can reliably detect

3.4.5
quantification limit

lowest concentration of an analyte that the analytical process can report with a specified degree of certainty

3.4.6
sampler bias
bias of the sampling method
3.4.7
sampling precision

combination of the imprecision of the aerosol sampling process and the imprecision arising from the flow rate

variability
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SIST EN 13890:2003
EN 13890:2002 (E)
4 Principle

Sampler bias and sampling precision are estimated by examining sampler performance data reported in the

scientific literature.

For measuring procedures that specify a method for the determination of soluble metals and metalloids, the

analytical bias is, by definition, taken to be zero.

For measuring procedures that specify a method for the determination of total metals and metalloids that involves

sample dissolution, the analytical bias is determined by assessing the effectiveness of the sample dissolution

method described in the procedure. This is achieved by analysing reference samples, which can be pure

compounds, bulk reference materials and/or samples of dust on collection substrates, and determining the

analytical recovery of the metals and metalloids of interest. The analytical recovery is then carefully scrutinised to

determine a typical upper limit for the analytical bias.

For measuring procedures that do not involve sample dissolution, e.g. X-ray fluorescence spectrometry, the

analytical bias is determined by comparison with a reference method or by analysis of a reference material.

Alternatively, in some instances, it can be estimated theoretically.

For measuring procedures that involve sample dissolution, the analytical precision is determined by analysing

reference samples prepared by spiking collection substrates with standard solutions of the metals and metalloids of

interest. The repeatability of measurements made on collection substrates spiked with various sample loadings

(corresponding to different concentrations of metal or metalloid in air and air sample volumes) gives a measure of

the precision of the analytical method for different averaging times across the measuring ranges specified in

EN 482.

For measuring procedures that do not involve sample dissolution, the analytical precision is determined in a similar

manner, by analysing reference samples prepared by loading collection substrates with known amounts of dust.

Alternatively, in some instances, it can be estimated theoretically.

The determined analytical bias and analytical precision are combined with the estimated sampler bias and

sampling precision to estimate the overall uncertainty of the measuring procedure as a whole. This is then

assessed against the general performance requirements prescribed in EN 482.
5 Requirements
5.1 General requirements
5.1.1 Scope of the measuring procedure

The scope of the measuring procedure shall give information about the following:

 the metals and metalloids that are covered by the measuring procedure, and the analytical techniques used;

 the working range;

 metal and metalloid compounds and/or dusts that could be found in workplace air, for which the sample

preparation method described is known to be inadequate;
 any known interferences.
5.1.2 Method performance

The measuring procedure shall give information about method performance, including the following:

 metal and metalloid compounds and/or dusts for which the sample preparation method described has been

shown to be effective;
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SIST EN 13890:2003
EN 13890:2002 (E)

 the range of concentrations of metals and metalloids in air and sample volumes over which the measurement

method has been shown to meet the acceptance criteria for overall uncertainty prescribed in EN 482;

 the detection limits and quantification limits of the analytical method for the metals and metalloids of interest;

 full details of any known interferences, including suitable and sufficient information on how to minimise their

effects.
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 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 exposure limits for the

metals and metalloids of interest (for example, an inhalable sampler or a respirable sampler can be used);

 specify that the samplers shall comply with the provisions of EN 13205.
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 Quantification limit

When tested in accordance with 9.1, the quantification limit shall be lower than the mass of metal or metalloid that

would be sampled at 0,1 times the limit value for the minimum air sample volume specified in the measuring

procedure.
5.1.7 Other detailed requirements

Where necessary, the measuring procedure shall give other detailed requirements, e.g. for the collection substrate.

5.2 Analytical recovery

When tested in accordance with 9.3.2 the upper limit of the 95 % confidence interval of the mean analytical

recovery shall be at least 90 % for all test materials.
5.3 Overall uncertainty

The overall uncertainty shall conform with the requirements specified in Table 1 of EN 482:1994.

6 Reagents

During the analysis, use only reagents of analytical grade, and only water complying with the requirements for

EN ISO 3696 grade 2 water (electrical conductivity less than 0,1 mS/m and resistivity greater than 0,01 MW

25 °C).

NOTE It is recommended that the water used be obtained from a water purification system that delivers ultrapure water

having a resistivity greater than 0,18 MW
  
  

  MW
water).
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SIST EN 13890:2003
EN 13890:2002 (E)
7 Reference samples
7.1 Standard solutions

Standard solutions with concentrations of the metals and metalloids of interest that are traceable to National and/or

International Standards. If commercial standard solutions are used observe the manufacturer's expiry date or

recommended shelf life.
7.2 Reference materials

For each metal or metalloid, a range of reference materials that is representative of the substances of interest that

could be present in the workplace atmosphere. The reference materials can be pure compounds of known

composition, certified reference materials or other well characterised materials (e.g. materials characterised in an

interlaboratory comparison). Follow the supplier's instructions when using certified reference materials.

NOTE 1 If there is a limit value for a specific compound, that compound should be included in the range of reference

materials.

NOTE 2 For a method that is intended to have general applicability, the range of reference materials should include

compounds and materials in industrial use and compounds and materials which could be generated by the work activity.

NOTE 3 It is important that the particle size of the reference materials be as close as possible to that of the particles

analysed, since inhalable particles are small and often much more easily soluble than coarse bulk materials.

7.3 Reference air samples

Samples of dust on collection substrates (e.g. airborne particles collected on filters using a multiple simultaneous

sample collection system), having a known or measured loading of the metals and metalloids of interest.

8 Apparatus
Usual laboratory apparatus and resources and:

 a system for applying a known volume of standard solution to the collection substrate with a precision of better

than 1 %;

 an instrument or instruments for analysing the metals and metalloids of interest.

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SIST EN 13890:2003
EN 13890:2002 (E)
9 Test methods
9.1 Detection limits and quantification limits
9.1.1 Determination of detection limits and quantification limits

9.1.1.1 Prepare and analyse 10 unused collection substrates, as described in the measuring procedure.

Calculate the mean and standard deviation of the measured concentrations for each analyte. Multiply the standard

deviations by three to obtain the detection limits and by ten to obtain the quantification limits.

9.1.1.2 If there is no measurable response from the analytical instrument when the blanks are analysed, spike

10 unused collection substrates with an appropriate mass of analyte, such that the test solutions/suspensions

produced from them will have a concentration near the anticipated detection limit, and repeat the test described

in 9.1.1.1.
9.1.2 Comparison of results with the acceptance criteria

Compare the quantification limits obtained in 9.1.1 with the requirements of 5.1.6.

9.2 Selection of test methods for determination of analytical bias and precision

Different test methods are applicable for determination of analytical bias and precision, depending on the sample

preparation method used. Refer to annex A for guidance on which of the test methods described in this standard

are applicable for the measuring procedure to be evaluated.
9.3 Analytical bias

9.3.1 Consideration of the analytical bias of procedures for soluble metals and metalloids

Soluble compounds of metals and metalloids are defined by the specific leach solution and leach conditions used

in the measuring procedure prescribed for their determination when the limit value is set. This is because, except

for compounds that are very soluble or very insoluble in water, solubility can be dependent upon the nature of the

leach solution and parameters such as particle size, solute/solvent ratio, temperature etc. Consequently, the

sample dissolution method, by definition, gives appropriate results, and there is no analytical bias.

NOTE 1 Although the sample dissolution methods for soluble compounds are generally design-based, there are

circumstances in which they can give incorrect results. In particular, this can occur if a soluble compound reacts with the filter

material, or a contaminant on a filter, to produce an insoluble compound. For example, a low recovery will be obtained for

soluble silver compounds if the filter used is contaminated with chloride. It is therefore important that proper consideration is

given to chemical compatibility when selecting a filter for collecting samples of soluble compounds (see annex A of

...

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