Workplace air — Determination of metals and metalloids in airborne particulate matter by inductively coupled plasma atomic emission spectrometry — Part 2: Sample preparation

This document specifies a number of suitable methods for preparing test solutions from samples of airborne particulate matter collected using the method specified in ISO 15202‑1, for subsequent determination of metals and metalloids by ICP‑AES using the method specified in ISO 15202‑3. It contains information about the applicability of the methods with respect to the measurement of metals and metalloids for which limit values have been set. The methods can also be used in the measurement of some metals and metalloids for which limit values have not been set but no information about its applicability is provided in this case. NOTE The sample preparation methods described in this document are generally suitable for use with analytical techniques other than ICP‑AES, e.g. atomic absorption spectrometry (AAS) by ISO 8518[5] and ISO 11174[10] and inductively coupled plasma mass spectrometry (ICP‑MS) by ISO 30011[11]. The method specified in Annex B is applicable when making measurements for comparison with limit values for soluble metal or metalloid compounds. One or more of the sample dissolution methods specified in Annexes C through H are applicable when making measurements for comparison with limit values for total metals and metalloids and their compounds. Information on the applicability of individual methods is given in the scope of the annex in which the method is specified. The following is a non-exclusive list of metals and metalloids for which limit values have been set (see References [14] and [15]) and for which one or more of the sample dissolution methods specified in this document are applicable. However, there is no information available on the effectiveness of any of the specified sample dissolution methods for those elements in italics. Aluminium Calcium Magnesium Selenium Tungsten Antimony Chromium Manganese Silver Uranium Arsenic Cobalt Mercury Sodium Vanadium Barium Copper Molybdenum Strontium Yttrium Beryllium Hafnium Nickel Tantalum Zinc Bismuth Indium Phosphorus Tellurium Zirconium Boron Iron Platinum Thallium Caesium Lead Potassium Tin Cadmium Lithium Rhodium Titanium ISO 15202 is not applicable to the determination of elemental mercury or arsenic trioxide, since mercury vapour and arsenic trioxide vapour are not collected using the sampling method specified in ISO 15202‑1.

Air des lieux de travail — Détermination des métaux et métalloïdes dans les particules en suspension dans l'air par spectrométrie d'émission atomique avec plasma à couplage inductif — Partie 2: Préparation des échantillons

Le présent document spécifie plusieurs méthodes appropriées de préparation de solutions d'essai à partir d'échantillons de matière particulaire en suspension dans l'air prélevés en utilisant la méthode spécifiée dans l'ISO 15202-1, en vue du dosage des métaux et métalloïdes par ICP-AES à l'aide de la méthode spécifiée dans l'ISO 15202-3. Il contient des informations relatives à l'applicabilité des méthodes par rapport au dosage de métaux et métalloïdes pour lesquels des valeurs limites ont été établies. Ces méthodes peuvent également être utilisées pour le dosage de certains métaux et métalloïdes pour lesquels les valeurs limites n'ont pas été établies mais, dans ce cas, aucune information sur leur applicabilité n'est disponible. NOTE Les méthodes de préparation d'échantillons décrites dans le présent document sont généralement appropriées pour une utilisation conjointe avec d'autres techniques d'analyse que l'ICP-AES, par exemple la spectrométrie d'absorption atomique (AAS) définie dans l'ISO 8518[5] et l'ISO 11174[10] et la spectrométrie de masse avec plasma à couplage inductif (ICP-MS) définie dans l'ISO 30011[11]. La méthode spécifiée à l'Annexe B est applicable pour effectuer des mesurages de comparaison avec des valeurs limites de composés solubles de métaux ou métalloïdes. Une ou plusieurs des méthodes de mise en solution d'échantillon spécifiées aux Annexes C à H sont applicables pour effectuer des mesurages de comparaison avec des valeurs limites de métaux et métalloïdes totaux et leurs composés. Des informations concernant les possibilités d'application des méthodes individuelles sont données dans le domaine d'application de l'annexe dans laquelle la méthode est spécifiée. L'ISO 15202 n'est pas applicable pour la détermination du mercure élémentaire ni de l'anhydride arsénieux, dans la mesure où les vapeurs de mercure et les vapeurs d'anhydride arsénieux ne sont pas recueillies en utilisant la méthode de prélèvement spécifiée dans l'ISO 15202-1.

Zrak na delovnem mestu - Določevanje kovin in polkovin v lebdečih delcih z atomsko emisijsko spektrometrijo z induktivno sklopljeno plazmo - 2. del: Priprava vzorcev

General Information

Status
Published
Publication Date
04-May-2020
Current Stage
6060 - International Standard published
Start Date
24-Mar-2020
Completion Date
05-May-2020

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SLOVENSKI STANDARD
SIST ISO 15202-2:2020
01-november-2020
Nadomešča:
SIST ISO 15202-2:2013
Zrak na delovnem mestu - Določevanje kovin in polkovin v lebdečih delcih z

atomsko emisijsko spektrometrijo z induktivno sklopljeno plazmo - 2. del: Priprava

vzorcev

Workplace air - Determination of metals and metalloids in airborne particulate matter by

inductively coupled plasma atomic emission spectrometry - Part 2: Sample preparation

Air des lieux de travail - Détermination des métaux et métalloïdes dans les particules en

suspension dans l'air par spectrométrie d'émission atomique avec plasma à couplage

inductif - Partie 2: Préparation des échantillons
Ta slovenski standard je istoveten z: ISO 15202-2:2020
ICS:
13.040.30 Kakovost zraka na delovnem Workplace atmospheres
mestu
SIST ISO 15202-2:2020 en,fr

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

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SIST ISO 15202-2:2020
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SIST ISO 15202-2:2020
INTERNATIONAL ISO
STANDARD 15202-2
Third edition
2020-05
Workplace air — Determination of
metals and metalloids in airborne
particulate matter by inductively
coupled plasma atomic emission
spectrometry —
Part 2:
Sample preparation
Air des lieux de travail — Détermination des métaux et métalloïdes
dans les particules en suspension dans l'air par spectrométrie
d'émission atomique avec plasma à couplage inductif —
Partie 2: Préparation des échantillons
Reference number
ISO 15202-2:2020(E)
ISO 2020
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SIST ISO 15202-2:2020
ISO 15202-2:2020(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2020

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting

on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address

below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved
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SIST ISO 15202-2:2020
ISO 15202-2:2020(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

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

3 Terms and definitions ..................................................................................................................................................................................... 2

4 Principle ........................................................................................................................................................................................................................ 3

5 Requirements .......................................................................................................................................................................................................... 3

6 Reactions ...................................................................................................................................................................................................................... 3

7 Reagents ........................................................................................................................................................................................................................ 3

8 Laboratory apparatus ..................................................................................................................................................................................... 4

9 Procedure..................................................................................................................................................................................................................... 4

9.1 Soluble metal and metalloid compounds ......................................................................................................................... 4

9.2 Total metals and metalloids and their compounds ................................................................................................. 5

9.3 Mixed exposure ....................................................................................................................................................................................... 5

10 Special cases .............................................................................................................................................................................................................. 5

10.1 Action to be taken if there is doubt about the effectiveness of the selected sample

dissolution method ............................................................................................................................................................................. 5

10.2 Action to be taken when particles have become dislodged from the filter during

transportation ......................................................................................................................................................................................... 6

10.3 Action to be taken regarding sampler wall deposits .............................................................................................. 6

11 Laboratory records ............................................................................................................................................................................................ 6

Annex A (informative) Safety precautions to be observed when using hydrofluoric and

perchloric acids ..................................................................................................................................................................................................... 7

Annex B (normative) Sample dissolution method for soluble metal and metalloid compounds .........8

Annex C (normative) Sample dissolution using nitric acid and hydrochloric acid on a hotplate ......14

Annex D (normative) Sample dissolution using hydrofluoric and nitric acids and ultrasonic

agitation ......... .............................................................................................................................................................................................................18

Annex E (normative) Sample dissolution using sulfuric acid and hydrogen peroxide on a

hotplate .......................................................................................................................................................................................................................21

Annex F (normative) Sample dissolution using nitric acid and perchloric acid on a hotplate .............25

Annex G (normative) Sample dissolution in a closed vessel microwave dissolution system .................29

Annex H (normative) Sample dissolution at 95 °C using a hot block ...............................................................................35

Annex I (normative) Action to be taken when there is visible, undissolved, particulate

material after sample dissolution ...................................................................................................................................................38

Annex J (informative) Sampler wall deposits ...........................................................................................................................................44

Bibliography .............................................................................................................................................................................................................................47

© ISO 2020 – All rights reserved iii
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SIST ISO 15202-2:2020
ISO 15202-2:2020(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www .iso .org/

iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 146, Air quality, Subcommittee SC 2,

Workplace atmospheres.

This third edition cancels and replaces the second edition (ISO 15202-2:2012), which has been

technically revised. The main changes compared to the previous edition are as follows:

— Definitions that appear in ISO 18158 have been removed from ISO 15202-2, with ISO 18158 being

added as a reference (replacing references to EN 1540).

— References to EN 482 have been replaced with ISO 20581, and references to EN 13890 have been

replaced with ISO 21832.

— Information regarding digestion of acid-soluble internal capsules has been added to Annexes C, D, E,

F, G and H.
— The text has been editorially updated.
A list of all parts in the ISO 15202 series can be found on the ISO website.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
iv © ISO 2020 – All rights reserved
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SIST ISO 15202-2:2020
ISO 15202-2:2020(E)
Introduction

The health of workers in many industries is at risk through exposure by inhalation of toxic metals

and metalloids. Industrial hygienists and other public health professionals need to determine the

effectiveness of measures taken to control workers' exposure, and this is generally achieved by making

workplace air measurements. This document has been published in order to make available a method

for making valid exposure measurements for a wide range of metals and metalloids in use in industry.

It will be of benefit to agencies concerned with health and safety at work, industrial hygienists and

other public health professionals, analytical laboratories, industrial users of metals and metalloids and

their workers.

ISO 15202, published in three parts, specifies a generic method for the determination of the mass

concentration of metals and metalloids in workplace air using inductively coupled plasma atomic

emission spectrometry (ICP-AES).

— ISO 15202-1 gives details of relevant International, European and National Standards which specify

characteristics, performance requirements and test methods relating to sampling equipment. It

also augments guidance provided elsewhere on assessment strategy and measurement strategy,

as well as specifying a method for collecting samples of airborne particulate matter for subsequent

chemical analysis.

— ISO 15202-2 describes a number of procedures for preparing sample solutions for analysis by

ICP-AES.

— ISO 15202-3 gives requirements and test methods for the analysis of sample solutions by ICP-AES.

The sample preparation methods described in this part of ISO 15202 are generally suitable for use with

analytical techniques other than ICP-AES; e.g. atomic absorption spectroscopy (AAS) and inductively

coupled plasma mass spectrometry (ICP-MS).

It has been assumed in the drafting of this document that the execution of its provisions and the

interpretation of the results obtained are entrusted to appropriately qualified and experienced people.

© ISO 2020 – All rights reserved v
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SIST ISO 15202-2:2020
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SIST ISO 15202-2:2020
INTERNATIONAL STANDARD ISO 15202-2:2020(E)
Workplace air — Determination of metals and metalloids
in airborne particulate matter by inductively coupled
plasma atomic emission spectrometry —
Part 2:
Sample preparation

WARNING — The use of this document may involve hazardous materials, operations and

equipment. This document does not purport to address any safety problems associated with

its use. It is the responsibility of the user of this document to establish appropriate safety and

health practices and determine the applicability of regulatory limitations prior to use.

1 Scope

This document specifies a number of suitable methods for preparing test solutions from samples of

airborne particulate matter collected using the method specified in ISO 15202-1, for subsequent

determination of metals and metalloids by ICP-AES using the method specified in ISO 15202-3. It

contains information about the applicability of the methods with respect to the measurement of metals

and metalloids for which limit values have been set. The methods can also be used in the measurement

of some metals and metalloids for which limit values have not been set but no information about its

applicability is provided in this case.

NOTE The sample preparation methods described in this document are generally suitable for use with

[5]

analytical techniques other than ICP-AES, e.g. atomic absorption spectrometry (AAS) by ISO 8518 and

[10] [11]

ISO 11174 and inductively coupled plasma mass spectrometry (ICP-MS) by ISO 30011 .

The method specified in Annex B is applicable when making measurements for comparison with limit

values for soluble metal or metalloid compounds.

One or more of the sample dissolution methods specified in Annexes C through H are applicable when

making measurements for comparison with limit values for total metals and metalloids and their

compounds. Information on the applicability of individual methods is given in the scope of the annex in

which the method is specified.

The following is a non-exclusive list of metals and metalloids for which limit values have been set (see

References [14] and [15]) and for which one or more of the sample dissolution methods specified in this

document are applicable. However, there is no information available on the effectiveness of any of the

specified sample dissolution methods for those elements in italics.
Aluminium Calcium Magnesium Selenium Tungsten
Antimony Chromium Manganese Silver Uranium
Arsenic Cobalt Mercury Sodium Vanadium
Barium Copper Molybdenum Strontium Yttrium
Beryllium Hafnium Nickel Tantalum Zinc
Bismuth Indium Phosphorus Tellurium Zirconium
© ISO 2020 – All rights reserved 1
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SIST ISO 15202-2:2020
ISO 15202-2:2020(E)
Boron Iron Platinum Thallium
Caesium Lead Potassium Tin
Cadmium Lithium Rhodium Titanium

ISO 15202 is not applicable to the determination of elemental mercury or arsenic trioxide, since

mercury vapour and arsenic trioxide vapour are not collected using the sampling method specified in

ISO 15202-1.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements 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.

ISO 15202-1, Workplace air — Determination of metals and metalloids in airborne particulate matter by

inductively coupled plasma atomic emission spectrometry — Part 1: Sampling

ISO 15202-3, Workplace air — Determination of metals and metalloids in airborne particulate matter by

inductively coupled plasma atomic emission spectrometry — Part 3: Analysis
ISO 18158, Workplace air — Terminology

ISO 21832, Workplace air — Metals and metalloids in airborne particles — Requirements for evaluation of

measuring procedures
3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 18158 and the following apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org
3.1
sample dissolution

process of obtaining a solution containing all analytes of interest from a sample, which might or might

not involve complete dissolution of the sample
3.2
sample solution
solution prepared from a sample by the process of sample dissolution (3.1)

Note 1 to entry: A sample solution might need to be subjected to further operations, e.g. dilution, or addition, or

both, of an internal standard(s), in order to produce a test solution (3.3).
SOURCE: Adapted from EN 14902:2005, 3.1.22.
3.3
test solution

blank solution or sample solution (3.2) that has been subjected to all operations required to bring it into

a state in which it is ready for analysis

Note 1 to entry: “Ready for analysis” includes any required dilution or addition, or both, of an internal standard.

If a blank solution or sample solution (3.2) is not subject to any further operations before analysis, it is a test

solution.
SOURCE: EN 14902:2005, 3.1.30.
2 © ISO 2020 – All rights reserved
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SIST ISO 15202-2:2020
ISO 15202-2:2020(E)
4 Principle

4.1 Airborne particles containing metals and metalloids are collected by drawing a measured volume

of air through a collection substrate, typically a filter mounted in a sampler designed to collect an

appropriate size fraction of airborne particles, using the method specified in ISO 15202-1.

4.2 An appropriate and suitable sample dissolution method is selected from those specified in

Annexes B through H, taking into consideration the metals and metalloids which are to be determined,

the limit values that have been set for those metals and metalloids, the applicability of the methods for

dissolution of the metals and metalloids of interest from materials which could be present in the test

atmosphere and the availability of the required laboratory apparatus.

4.3 The sample and collection substrate are then treated to dissolve the metals and metalloids of

interest using the selected sample dissolution method.

4.4 The resultant test solution is subsequently analysed for the metals and metalloids of interest by

inductively coupled plasma-atomic emission spectrometry using the method specified in ISO 15202-3.

NOTE Sample preparation methods described in Annexes B through H are generally suitable for use with

[5] [10] [11]

analytical techniques other than ICP-AES, e.g. AAS by ISO 8518 and ISO 11174 and ICP-MS by ISO 30011 .

For ICP-MS, changes could be required in the concentrations of acids or the dilution factors used to prepare

test solutions. Furthermore, some acids, such as hydrochloric acid, are not recommended for test solutions for

analysis by ICP-MS.
5 Requirements

The measuring procedure as a whole (covered by ISO 15202-1, ISO 15202-2 and ISO 15202-3) shall

conform to any relevant performance requirements for measuring chemical agents in workplace air

[12]
(for example ISO 20581 and ISO 21832).
6 Reactions

In general, the majority of particulate metals and metalloids and particulate metal and metalloid

compounds which are commonly of interest in samples of workplace air are converted to water-soluble

ions by one or more of the sample dissolution methods specified in this document. However, if there

is any doubt about whether a method will exhibit the required analytical recovery for a particular

application, it is necessary to investigate this before proceeding with the method (see 10.1).

7 Reagents

During the analysis, use only reagents of analytical grade and only water as specified in 7.1.

NOTE 1 Safety precautions to be observed when using hydrofluoric and perchloric acids are given in Annex A.

NOTE 2 Details of reagents that are required for use in Annexes B through I are given in the annex concerned.

NOTE 3 It could be necessary to use acids of higher purity in order to obtain an adequate detection limit for

some metals and metalloids.
[3]

7.1 Water, conforming with the requirements for ISO 3696 grade 2 water (electrical conductivity

less than 0,1 mS/m and resistivity greater than 0,01 MΩ⋅m at 25 °C).

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 MΩ⋅m (usually expressed by manufacturers of

water purification systems as 18 MΩ⋅cm).
© ISO 2020 – All rights reserved 3
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SIST ISO 15202-2:2020
ISO 15202-2:2020(E)
7.2 Nitric acid (HNO ), concentrated,ρ ≈ 1,42 g ml , w ≈ 70 % mass fraction.
HNO HNO
3 3

The concentration of the metals and metalloids of interest shall be less than 0,1 µg ml .

WARNING — Concentrated nitric acid is corrosive and oxidizing, and nitric acid fumes are

irritant. Avoid exposure by contact with the skin or eyes, or by inhalation of fumes. Use suitable

personal protective equipment (including suitable gloves, face shield or safety spectacles, etc.)

when working with the concentrated or dilute nitric acid and carry out sample dissolution with

concentrated nitric acid in open vessels in a fume hood.
7.3 Nitric acid, diluted 1 + 9.

Carefully and slowly begin adding 50 ml of concentrated nitric acid (7.2) to 450 ml of water (7.1) in a 1 l

polypropylene bottle (8.5). Add the acid in small aliquots. Between additions, swirl to mix and run cold

tap water over the side of the bottle to cool the contents. Do not allow the tap water to contaminate the

contents of the bottle. When the addition of the concentrated nitric acid is complete, swirl the bottle

to mix the contents, allow to cool to room temperature, close the bottle with its screw cap and mix

thoroughly.
8 Laboratory apparatus
Usual laboratory apparatus and, in particular, the following.

8.1 Disposable gloves, impermeable and powder free, to avoid the possibility of contamination from

the hands and to protect them from contact with toxic and corrosive substances. PVC gloves are suitable.

8.2 Glassware, beakers and one-mark volumetric flasks conforming to the requirements of

[1] [2]

ISO 1042 , made of borosilicate glass conforming with the requirements of ISO 3585 , cleaned before

use by soaking in 1 + 9 nitric acid (7.3) for at least 24 h and then rinsing thoroughly with water (7.1).

Alternatively, the glassware may be cleaned with a suitable laboratory detergent using a laboratory

washing machine.

8.3 Flat-tipped forceps, non-metallic (e.g. plastic or plastic-coated), for unloading filters from

samplers or from filter transport cassettes.
[6]

8.4 Piston-operated volumetric instruments, conforming with the requirements of ISO 8655-1

[9]

and tested in accordance with ISO 8655-6 , including pipettors conforming with the requirements of

[7] [8]

ISO 8655-2 and dispensers conforming with the requirements of ISO 8655-5 , for dispensing leach

solution, acids, etc.
8.5 Polypropylene bottle, 1 l capacity, with leakproof screw cap.

A bottle made of an alternative plastic may be used provided that it is suitable for the intended use

(see 7.3).

NOTE Details of laboratory apparatus that are required for use in Annexes B through I are given in the annex

concerned.
9 Procedure
9.1 Soluble metal and metalloid compounds

9.1.1 If results are required for comparison with limit values for soluble metal or metalloid compounds,

or both, use the sample dissolution method specified in Annex B to prepare test solutions for analysis by

the method specified in ISO 15202-3.
4 © ISO 2020 – All rights reserved
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SIST ISO 15202-2:2020
ISO 15202-2:2020(E)

9.1.2 Alternatively, if it is known that no insoluble compounds of the metals or metalloids, or both,

of interest are used in the workplace and that none are produced in the processes carried out, prepare

test solutions for analysis by the method specified in ISO 15202-3, using one of the sample dissolution

methods for total metals and metalloids and their compounds prescribed in Annexes C through H, and

compare the results with the limit value for the soluble metals or metalloids, or both, concerned.

The methods prescribed in Annexes C through H are not specific for soluble metal or metalloid

compounds, or both. However, in the circumstances described above, they may be used as an alternative

to the method described in Annex B, if this is more convenient.
9.2 Total metals and metalloids and their compounds

9.2.1 If results are required for comparison with limit values for total metals or metalloids, or both,

and their compounds, select a suitable sample dissolution method from those specified in Annexes C

through H. Take into consideration the applicability of each method for dissolution of the metals and

metalloids of interest from materials that could be present in the test atmosphere (refer to the clause on

the effectiveness of the sample dissolution method in the annex in which the method is specified) and the

availability of the required laboratory apparatus.

9.2.2 Use the selected sample dissolution method to prepare test solutions for analysis of total metals

and metalloids and their compounds by the method specified in ISO 15202-3.
9.3 Mixed exposure
9.3.1 If results are required

— for comparison with limit values for soluble metal and/or metalloid compounds and with limit

values for metals and/or metalloids and their insoluble compounds, or

— for comparison with limit values for soluble metal and/or metalloid compounds and with limit

values for total metals and/or metalloids and their compounds,
follow the instructions given in 9.3.2 and 9.3.3.

9.3.2 Use the sample dissolution method specified in Annex B to prepare test solutions for the

determination of soluble metal and metalloid compounds by the method specified in ISO 15202-3.

9.3.3 Select a suitable sample dissolution method for total metals and metalloids and compounds

(see 9.2). Use this to treat undissolved material from the method for soluble metal and metalloid

compounds (see B.6.7.1) and prepare test solutions for determination of metals and metalloids and their

insoluble compounds by the method specified in ISO 15202-3.
10 Special cases

10.1 Action to be taken if there is doubt about the effectiveness of the selected sample

dissolution method

10.1.1 If there is any doubt about whether the selected sample dissolution method will exhibit the

required analytical recovery when used for dissolution of the metals and metalloids of interest from

materials which could be present in the test atmosphere, determine its effectiveness for that particular

application. For total metals and metalloids, this may be achieved by analysing a bulk sample of known

composition which is similar in nature to the materials being used or produced in the workplace, e.g. a

certified reference material. For soluble metals and metalloids, analytical recovery is best determined by

analysing filters spiked with solution containing a known mass of the soluble compound of interest.

© ISO 2020 – All rights reserved 5
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SIST ISO 15202-2:2020
ISO 15202-2:2020(E)

NOTE In designing an experiment to determine the effectiveness of a sample dissolution method, the particle

size of a bulk sample can have a significant influence on the efficiency of its dissolution. Furthermore, microgram

amounts of relatively insoluble material are normally much more easily
...

SLOVENSKI STANDARD
oSIST ISO 15202-2:2020
01-julij-2020
Zrak na delovnem mestu - Določevanje kovin in polkovin v lebdečih delcih z

atomsko emisijsko spektrometrijo z induktivno sklopljeno plazmo - 2. del: Priprava

vzorcev

Workplace air - Determination of metals and metalloids in airborne particulate matter by

inductively coupled plasma atomic emission spectrometry - Part 2: Sample preparation

Air des lieux de travail - Détermination des métaux et métalloïdes dans les particules en

suspension dans l'air par spectrométrie d'émission atomique avec plasma à couplage

inductif - Partie 2: Préparation des échantillons
Ta slovenski standard je istoveten z: ISO 15202-2:2020
ICS:
13.040.30 Kakovost zraka na delovnem Workplace atmospheres
mestu
oSIST ISO 15202-2:2020 en,fr,de

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

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oSIST ISO 15202-2:2020
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oSIST ISO 15202-2:2020
INTERNATIONAL ISO
STANDARD 15202-2
Third edition
2020-05
Workplace air — Determination of
metals and metalloids in airborne
particulate matter by inductively
coupled plasma atomic emission
spectrometry —
Part 2:
Sample preparation
Air des lieux de travail — Détermination des métaux et métalloïdes
dans les particules en suspension dans l'air par spectrométrie
d'émission atomique avec plasma à couplage inductif —
Partie 2: Préparation des échantillons
Reference number
ISO 15202-2:2020(E)
ISO 2020
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oSIST ISO 15202-2:2020
ISO 15202-2:2020(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2020

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting

on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address

below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved
---------------------- Page: 4 ----------------------
oSIST ISO 15202-2:2020
ISO 15202-2:2020(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

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

3 Terms and definitions ..................................................................................................................................................................................... 2

4 Principle ........................................................................................................................................................................................................................ 3

5 Requirements .......................................................................................................................................................................................................... 3

6 Reactions ...................................................................................................................................................................................................................... 3

7 Reagents ........................................................................................................................................................................................................................ 3

8 Laboratory apparatus ..................................................................................................................................................................................... 4

9 Procedure..................................................................................................................................................................................................................... 4

9.1 Soluble metal and metalloid compounds ......................................................................................................................... 4

9.2 Total metals and metalloids and their compounds ................................................................................................. 5

9.3 Mixed exposure ....................................................................................................................................................................................... 5

10 Special cases .............................................................................................................................................................................................................. 5

10.1 Action to be taken if there is doubt about the effectiveness of the selected sample

dissolution method ............................................................................................................................................................................. 5

10.2 Action to be taken when particles have become dislodged from the filter during

transportation ......................................................................................................................................................................................... 6

10.3 Action to be taken regarding sampler wall deposits .............................................................................................. 6

11 Laboratory records ............................................................................................................................................................................................ 6

Annex A (informative) Safety precautions to be observed when using hydrofluoric and

perchloric acids ..................................................................................................................................................................................................... 7

Annex B (normative) Sample dissolution method for soluble metal and metalloid compounds .........8

Annex C (normative) Sample dissolution using nitric acid and hydrochloric acid on a hotplate ......14

Annex D (normative) Sample dissolution using hydrofluoric and nitric acids and ultrasonic

agitation ......... .............................................................................................................................................................................................................18

Annex E (normative) Sample dissolution using sulfuric acid and hydrogen peroxide on a

hotplate .......................................................................................................................................................................................................................21

Annex F (normative) Sample dissolution using nitric acid and perchloric acid on a hotplate .............25

Annex G (normative) Sample dissolution in a closed vessel microwave dissolution system .................29

Annex H (normative) Sample dissolution at 95 °C using a hot block ...............................................................................35

Annex I (normative) Action to be taken when there is visible, undissolved, particulate

material after sample dissolution ...................................................................................................................................................38

Annex J (informative) Sampler wall deposits ...........................................................................................................................................44

Bibliography .............................................................................................................................................................................................................................47

© ISO 2020 – All rights reserved iii
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oSIST ISO 15202-2:2020
ISO 15202-2:2020(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www .iso .org/

iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 146, Air quality, Subcommittee SC 2,

Workplace atmospheres.

This third edition cancels and replaces the second edition (ISO 15202-2:2012), which has been

technically revised. The main changes compared to the previous edition are as follows:

— Definitions that appear in ISO 18158 have been removed from ISO 15202-2, with ISO 18158 being

added as a reference (replacing references to EN 1540).

— References to EN 482 have been replaced with ISO 20581, and references to EN 13890 have been

replaced with ISO 21832.

— Information regarding digestion of acid-soluble internal capsules has been added to Annexes C, D, E,

F, G and H.
— The text has been editorially updated.
A list of all parts in the ISO 15202 series can be found on the ISO website.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
iv © ISO 2020 – All rights reserved
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oSIST ISO 15202-2:2020
ISO 15202-2:2020(E)
Introduction

The health of workers in many industries is at risk through exposure by inhalation of toxic metals

and metalloids. Industrial hygienists and other public health professionals need to determine the

effectiveness of measures taken to control workers' exposure, and this is generally achieved by making

workplace air measurements. This document has been published in order to make available a method

for making valid exposure measurements for a wide range of metals and metalloids in use in industry.

It will be of benefit to agencies concerned with health and safety at work, industrial hygienists and

other public health professionals, analytical laboratories, industrial users of metals and metalloids and

their workers.

ISO 15202, published in three parts, specifies a generic method for the determination of the mass

concentration of metals and metalloids in workplace air using inductively coupled plasma atomic

emission spectrometry (ICP-AES).

— ISO 15202-1 gives details of relevant International, European and National Standards which specify

characteristics, performance requirements and test methods relating to sampling equipment. It

also augments guidance provided elsewhere on assessment strategy and measurement strategy,

as well as specifying a method for collecting samples of airborne particulate matter for subsequent

chemical analysis.

— ISO 15202-2 describes a number of procedures for preparing sample solutions for analysis by

ICP-AES.

— ISO 15202-3 gives requirements and test methods for the analysis of sample solutions by ICP-AES.

The sample preparation methods described in this part of ISO 15202 are generally suitable for use with

analytical techniques other than ICP-AES; e.g. atomic absorption spectroscopy (AAS) and inductively

coupled plasma mass spectrometry (ICP-MS).

It has been assumed in the drafting of this document that the execution of its provisions and the

interpretation of the results obtained are entrusted to appropriately qualified and experienced people.

© ISO 2020 – All rights reserved v
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oSIST ISO 15202-2:2020
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oSIST ISO 15202-2:2020
INTERNATIONAL STANDARD ISO 15202-2:2020(E)
Workplace air — Determination of metals and metalloids
in airborne particulate matter by inductively coupled
plasma atomic emission spectrometry —
Part 2:
Sample preparation

WARNING — The use of this document may involve hazardous materials, operations and

equipment. This document does not purport to address any safety problems associated with

its use. It is the responsibility of the user of this document to establish appropriate safety and

health practices and determine the applicability of regulatory limitations prior to use.

1 Scope

This document specifies a number of suitable methods for preparing test solutions from samples of

airborne particulate matter collected using the method specified in ISO 15202-1, for subsequent

determination of metals and metalloids by ICP-AES using the method specified in ISO 15202-3. It

contains information about the applicability of the methods with respect to the measurement of metals

and metalloids for which limit values have been set. The methods can also be used in the measurement

of some metals and metalloids for which limit values have not been set but no information about its

applicability is provided in this case.

NOTE The sample preparation methods described in this document are generally suitable for use with

[5]

analytical techniques other than ICP-AES, e.g. atomic absorption spectrometry (AAS) by ISO 8518 and

[10] [11]

ISO 11174 and inductively coupled plasma mass spectrometry (ICP-MS) by ISO 30011 .

The method specified in Annex B is applicable when making measurements for comparison with limit

values for soluble metal or metalloid compounds.

One or more of the sample dissolution methods specified in Annexes C through H are applicable when

making measurements for comparison with limit values for total metals and metalloids and their

compounds. Information on the applicability of individual methods is given in the scope of the annex in

which the method is specified.

The following is a non-exclusive list of metals and metalloids for which limit values have been set (see

References [14] and [15]) and for which one or more of the sample dissolution methods specified in this

document are applicable. However, there is no information available on the effectiveness of any of the

specified sample dissolution methods for those elements in italics.
Aluminium Calcium Magnesium Selenium Tungsten
Antimony Chromium Manganese Silver Uranium
Arsenic Cobalt Mercury Sodium Vanadium
Barium Copper Molybdenum Strontium Yttrium
Beryllium Hafnium Nickel Tantalum Zinc
Bismuth Indium Phosphorus Tellurium Zirconium
© ISO 2020 – All rights reserved 1
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oSIST ISO 15202-2:2020
ISO 15202-2:2020(E)
Boron Iron Platinum Thallium
Caesium Lead Potassium Tin
Cadmium Lithium Rhodium Titanium

ISO 15202 is not applicable to the determination of elemental mercury or arsenic trioxide, since

mercury vapour and arsenic trioxide vapour are not collected using the sampling method specified in

ISO 15202-1.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements 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.

ISO 15202-1, Workplace air — Determination of metals and metalloids in airborne particulate matter by

inductively coupled plasma atomic emission spectrometry — Part 1: Sampling

ISO 15202-3, Workplace air — Determination of metals and metalloids in airborne particulate matter by

inductively coupled plasma atomic emission spectrometry — Part 3: Analysis
ISO 18158, Workplace air — Terminology

ISO 21832, Workplace air — Metals and metalloids in airborne particles — Requirements for evaluation of

measuring procedures
3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 18158 and the following apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org
3.1
sample dissolution

process of obtaining a solution containing all analytes of interest from a sample, which might or might

not involve complete dissolution of the sample
3.2
sample solution
solution prepared from a sample by the process of sample dissolution (3.1)

Note 1 to entry: A sample solution might need to be subjected to further operations, e.g. dilution, or addition, or

both, of an internal standard(s), in order to produce a test solution (3.3).
SOURCE: Adapted from EN 14902:2005, 3.1.22.
3.3
test solution

blank solution or sample solution (3.2) that has been subjected to all operations required to bring it into

a state in which it is ready for analysis

Note 1 to entry: “Ready for analysis” includes any required dilution or addition, or both, of an internal standard.

If a blank solution or sample solution (3.2) is not subject to any further operations before analysis, it is a test

solution.
SOURCE: EN 14902:2005, 3.1.30.
2 © ISO 2020 – All rights reserved
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oSIST ISO 15202-2:2020
ISO 15202-2:2020(E)
4 Principle

4.1 Airborne particles containing metals and metalloids are collected by drawing a measured volume

of air through a collection substrate, typically a filter mounted in a sampler designed to collect an

appropriate size fraction of airborne particles, using the method specified in ISO 15202-1.

4.2 An appropriate and suitable sample dissolution method is selected from those specified in

Annexes B through H, taking into consideration the metals and metalloids which are to be determined,

the limit values that have been set for those metals and metalloids, the applicability of the methods for

dissolution of the metals and metalloids of interest from materials which could be present in the test

atmosphere and the availability of the required laboratory apparatus.

4.3 The sample and collection substrate are then treated to dissolve the metals and metalloids of

interest using the selected sample dissolution method.

4.4 The resultant test solution is subsequently analysed for the metals and metalloids of interest by

inductively coupled plasma-atomic emission spectrometry using the method specified in ISO 15202-3.

NOTE Sample preparation methods described in Annexes B through H are generally suitable for use with

[5] [10] [11]

analytical techniques other than ICP-AES, e.g. AAS by ISO 8518 and ISO 11174 and ICP-MS by ISO 30011 .

For ICP-MS, changes could be required in the concentrations of acids or the dilution factors used to prepare

test solutions. Furthermore, some acids, such as hydrochloric acid, are not recommended for test solutions for

analysis by ICP-MS.
5 Requirements

The measuring procedure as a whole (covered by ISO 15202-1, ISO 15202-2 and ISO 15202-3) shall

conform to any relevant performance requirements for measuring chemical agents in workplace air

[12]
(for example ISO 20581 and ISO 21832).
6 Reactions

In general, the majority of particulate metals and metalloids and particulate metal and metalloid

compounds which are commonly of interest in samples of workplace air are converted to water-soluble

ions by one or more of the sample dissolution methods specified in this document. However, if there

is any doubt about whether a method will exhibit the required analytical recovery for a particular

application, it is necessary to investigate this before proceeding with the method (see 10.1).

7 Reagents

During the analysis, use only reagents of analytical grade and only water as specified in 7.1.

NOTE 1 Safety precautions to be observed when using hydrofluoric and perchloric acids are given in Annex A.

NOTE 2 Details of reagents that are required for use in Annexes B through I are given in the annex concerned.

NOTE 3 It could be necessary to use acids of higher purity in order to obtain an adequate detection limit for

some metals and metalloids.
[3]

7.1 Water, conforming with the requirements for ISO 3696 grade 2 water (electrical conductivity

less than 0,1 mS/m and resistivity greater than 0,01 MΩ⋅m at 25 °C).

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 MΩ⋅m (usually expressed by manufacturers of

water purification systems as 18 MΩ⋅cm).
© ISO 2020 – All rights reserved 3
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oSIST ISO 15202-2:2020
ISO 15202-2:2020(E)
7.2 Nitric acid (HNO ), concentrated,ρ ≈ 1,42 g ml , w ≈ 70 % mass fraction.
HNO HNO
3 3

The concentration of the metals and metalloids of interest shall be less than 0,1 µg ml .

WARNING — Concentrated nitric acid is corrosive and oxidizing, and nitric acid fumes are

irritant. Avoid exposure by contact with the skin or eyes, or by inhalation of fumes. Use suitable

personal protective equipment (including suitable gloves, face shield or safety spectacles, etc.)

when working with the concentrated or dilute nitric acid and carry out sample dissolution with

concentrated nitric acid in open vessels in a fume hood.
7.3 Nitric acid, diluted 1 + 9.

Carefully and slowly begin adding 50 ml of concentrated nitric acid (7.2) to 450 ml of water (7.1) in a 1 l

polypropylene bottle (8.5). Add the acid in small aliquots. Between additions, swirl to mix and run cold

tap water over the side of the bottle to cool the contents. Do not allow the tap water to contaminate the

contents of the bottle. When the addition of the concentrated nitric acid is complete, swirl the bottle

to mix the contents, allow to cool to room temperature, close the bottle with its screw cap and mix

thoroughly.
8 Laboratory apparatus
Usual laboratory apparatus and, in particular, the following.

8.1 Disposable gloves, impermeable and powder free, to avoid the possibility of contamination from

the hands and to protect them from contact with toxic and corrosive substances. PVC gloves are suitable.

8.2 Glassware, beakers and one-mark volumetric flasks conforming to the requirements of

[1] [2]

ISO 1042 , made of borosilicate glass conforming with the requirements of ISO 3585 , cleaned before

use by soaking in 1 + 9 nitric acid (7.3) for at least 24 h and then rinsing thoroughly with water (7.1).

Alternatively, the glassware may be cleaned with a suitable laboratory detergent using a laboratory

washing machine.

8.3 Flat-tipped forceps, non-metallic (e.g. plastic or plastic-coated), for unloading filters from

samplers or from filter transport cassettes.
[6]

8.4 Piston-operated volumetric instruments, conforming with the requirements of ISO 8655-1

[9]

and tested in accordance with ISO 8655-6 , including pipettors conforming with the requirements of

[7] [8]

ISO 8655-2 and dispensers conforming with the requirements of ISO 8655-5 , for dispensing leach

solution, acids, etc.
8.5 Polypropylene bottle, 1 l capacity, with leakproof screw cap.

A bottle made of an alternative plastic may be used provided that it is suitable for the intended use

(see 7.3).

NOTE Details of laboratory apparatus that are required for use in Annexes B through I are given in the annex

concerned.
9 Procedure
9.1 Soluble metal and metalloid compounds

9.1.1 If results are required for comparison with limit values for soluble metal or metalloid compounds,

or both, use the sample dissolution method specified in Annex B to prepare test solutions for analysis by

the method specified in ISO 15202-3.
4 © ISO 2020 – All rights reserved
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oSIST ISO 15202-2:2020
ISO 15202-2:2020(E)

9.1.2 Alternatively, if it is known that no insoluble compounds of the metals or metalloids, or both,

of interest are used in the workplace and that none are produced in the processes carried out, prepare

test solutions for analysis by the method specified in ISO 15202-3, using one of the sample dissolution

methods for total metals and metalloids and their compounds prescribed in Annexes C through H, and

compare the results with the limit value for the soluble metals or metalloids, or both, concerned.

The methods prescribed in Annexes C through H are not specific for soluble metal or metalloid

compounds, or both. However, in the circumstances described above, they may be used as an alternative

to the method described in Annex B, if this is more convenient.
9.2 Total metals and metalloids and their compounds

9.2.1 If results are required for comparison with limit values for total metals or metalloids, or both,

and their compounds, select a suitable sample dissolution method from those specified in Annexes C

through H. Take into consideration the applicability of each method for dissolution of the metals and

metalloids of interest from materials that could be present in the test atmosphere (refer to the clause on

the effectiveness of the sample dissolution method in the annex in which the method is specified) and the

availability of the required laboratory apparatus.

9.2.2 Use the selected sample dissolution method to prepare test solutions for analysis of total metals

and metalloids and their compounds by the method specified in ISO 15202-3.
9.3 Mixed exposure
9.3.1 If results are required

— for comparison with limit values for soluble metal and/or metalloid compounds and with limit

values for metals and/or metalloids and their insoluble compounds, or

— for comparison with limit values for soluble metal and/or metalloid compounds and with limit

values for total metals and/or metalloids and their compounds,
follow the instructions given in 9.3.2 and 9.3.3.

9.3.2 Use the sample dissolution method specified in Annex B to prepare test solutions for the

determination of soluble metal and metalloid compounds by the method specified in ISO 15202-3.

9.3.3 Select a suitable sample dissolution method for total metals and metalloids and compounds

(see 9.2). Use this to treat undissolved material from the method for soluble metal and metalloid

compounds (see B.6.7.1) and prepare test solutions for determination of metals and metalloids and their

insoluble compounds by the method specified in ISO 15202-3.
10 Special cases

10.1 Action to be taken if there is doubt about the effectiveness of the selected sample

dissolution method

10.1.1 If there is any doubt about whether the selected sample dissolution method will exhibit the

required analytical recovery when used for dissolution of the metals and metalloids of interest from

materials which could be present in the test atmosphere, determine its effectiveness for that particular

application. For total metals and metalloids, this may be achieved by analysing a bulk sample of known

composition which is similar in nature to the materials being used or produced in the workplace, e.g. a

certified reference material. For soluble metals and metalloids, analytical recovery is best determined by

analysing filters spiked with solution containing a known mass of the soluble compound of interest.

© ISO 2020 – All rights reserved 5
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oSIST ISO 15202-2:2020
ISO 15202-2:2020(E)

NOTE In designing an experiment to determine the effectiveness of a sample dissolution method, the particle

size of a bulk sample can have a significant influence on the efficiency of its dissolution. Furthermore, microgram

amounts of relatively insoluble material are normally much more easily dissolved than mi

...

INTERNATIONAL ISO
STANDARD 15202-2
Third edition
2020-05
Workplace air — Determination of
metals and metalloids in airborne
particulate matter by inductively
coupled plasma atomic emission
spectrometry —
Part 2:
Sample preparation
Air des lieux de travail — Détermination des métaux et métalloïdes
dans les particules en suspension dans l'air par spectrométrie
d'émission atomique avec plasma à couplage inductif —
Partie 2: Préparation des échantillons
Reference number
ISO 15202-2:2020(E)
ISO 2020
---------------------- Page: 1 ----------------------
ISO 15202-2:2020(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2020

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting

on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address

below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 15202-2:2020(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

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

3 Terms and definitions ..................................................................................................................................................................................... 2

4 Principle ........................................................................................................................................................................................................................ 3

5 Requirements .......................................................................................................................................................................................................... 3

6 Reactions ...................................................................................................................................................................................................................... 3

7 Reagents ........................................................................................................................................................................................................................ 3

8 Laboratory apparatus ..................................................................................................................................................................................... 4

9 Procedure..................................................................................................................................................................................................................... 4

9.1 Soluble metal and metalloid compounds ......................................................................................................................... 4

9.2 Total metals and metalloids and their compounds ................................................................................................. 5

9.3 Mixed exposure ....................................................................................................................................................................................... 5

10 Special cases .............................................................................................................................................................................................................. 5

10.1 Action to be taken if there is doubt about the effectiveness of the selected sample

dissolution method ............................................................................................................................................................................. 5

10.2 Action to be taken when particles have become dislodged from the filter during

transportation ......................................................................................................................................................................................... 6

10.3 Action to be taken regarding sampler wall deposits .............................................................................................. 6

11 Laboratory records ............................................................................................................................................................................................ 6

Annex A (informative) Safety precautions to be observed when using hydrofluoric and

perchloric acids ..................................................................................................................................................................................................... 7

Annex B (normative) Sample dissolution method for soluble metal and metalloid compounds .........8

Annex C (normative) Sample dissolution using nitric acid and hydrochloric acid on a hotplate ......14

Annex D (normative) Sample dissolution using hydrofluoric and nitric acids and ultrasonic

agitation ......... .............................................................................................................................................................................................................18

Annex E (normative) Sample dissolution using sulfuric acid and hydrogen peroxide on a

hotplate .......................................................................................................................................................................................................................21

Annex F (normative) Sample dissolution using nitric acid and perchloric acid on a hotplate .............25

Annex G (normative) Sample dissolution in a closed vessel microwave dissolution system .................29

Annex H (normative) Sample dissolution at 95 °C using a hot block ...............................................................................35

Annex I (normative) Action to be taken when there is visible, undissolved, particulate

material after sample dissolution ...................................................................................................................................................38

Annex J (informative) Sampler wall deposits ...........................................................................................................................................44

Bibliography .............................................................................................................................................................................................................................47

© ISO 2020 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 15202-2:2020(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www .iso .org/

iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 146, Air quality, Subcommittee SC 2,

Workplace atmospheres.

This third edition cancels and replaces the second edition (ISO 15202-2:2012), which has been

technically revised. The main changes compared to the previous edition are as follows:

— Definitions that appear in ISO 18158 have been removed from ISO 15202-2, with ISO 18158 being

added as a reference (replacing references to EN 1540).

— References to EN 482 have been replaced with ISO 20581, and references to EN 13890 have been

replaced with ISO 21832.

— Information regarding digestion of acid-soluble internal capsules has been added to Annexes C, D, E,

F, G and H.
— The text has been editorially updated.
A list of all parts in the ISO 15202 series can be found on the ISO website.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
iv © ISO 2020 – All rights reserved
---------------------- Page: 4 ----------------------
ISO 15202-2:2020(E)
Introduction

The health of workers in many industries is at risk through exposure by inhalation of toxic metals

and metalloids. Industrial hygienists and other public health professionals need to determine the

effectiveness of measures taken to control workers' exposure, and this is generally achieved by making

workplace air measurements. This document has been published in order to make available a method

for making valid exposure measurements for a wide range of metals and metalloids in use in industry.

It will be of benefit to agencies concerned with health and safety at work, industrial hygienists and

other public health professionals, analytical laboratories, industrial users of metals and metalloids and

their workers.

ISO 15202, published in three parts, specifies a generic method for the determination of the mass

concentration of metals and metalloids in workplace air using inductively coupled plasma atomic

emission spectrometry (ICP-AES).

— ISO 15202-1 gives details of relevant International, European and National Standards which specify

characteristics, performance requirements and test methods relating to sampling equipment. It

also augments guidance provided elsewhere on assessment strategy and measurement strategy,

as well as specifying a method for collecting samples of airborne particulate matter for subsequent

chemical analysis.

— ISO 15202-2 describes a number of procedures for preparing sample solutions for analysis by

ICP-AES.

— ISO 15202-3 gives requirements and test methods for the analysis of sample solutions by ICP-AES.

The sample preparation methods described in this part of ISO 15202 are generally suitable for use with

analytical techniques other than ICP-AES; e.g. atomic absorption spectroscopy (AAS) and inductively

coupled plasma mass spectrometry (ICP-MS).

It has been assumed in the drafting of this document that the execution of its provisions and the

interpretation of the results obtained are entrusted to appropriately qualified and experienced people.

© ISO 2020 – All rights reserved v
---------------------- Page: 5 ----------------------
INTERNATIONAL STANDARD ISO 15202-2:2020(E)
Workplace air — Determination of metals and metalloids
in airborne particulate matter by inductively coupled
plasma atomic emission spectrometry —
Part 2:
Sample preparation

WARNING — The use of this document may involve hazardous materials, operations and

equipment. This document does not purport to address any safety problems associated with

its use. It is the responsibility of the user of this document to establish appropriate safety and

health practices and determine the applicability of regulatory limitations prior to use.

1 Scope

This document specifies a number of suitable methods for preparing test solutions from samples of

airborne particulate matter collected using the method specified in ISO 15202-1, for subsequent

determination of metals and metalloids by ICP-AES using the method specified in ISO 15202-3. It

contains information about the applicability of the methods with respect to the measurement of metals

and metalloids for which limit values have been set. The methods can also be used in the measurement

of some metals and metalloids for which limit values have not been set but no information about its

applicability is provided in this case.

NOTE The sample preparation methods described in this document are generally suitable for use with

[5]

analytical techniques other than ICP-AES, e.g. atomic absorption spectrometry (AAS) by ISO 8518 and

[10] [11]

ISO 11174 and inductively coupled plasma mass spectrometry (ICP-MS) by ISO 30011 .

The method specified in Annex B is applicable when making measurements for comparison with limit

values for soluble metal or metalloid compounds.

One or more of the sample dissolution methods specified in Annexes C through H are applicable when

making measurements for comparison with limit values for total metals and metalloids and their

compounds. Information on the applicability of individual methods is given in the scope of the annex in

which the method is specified.

The following is a non-exclusive list of metals and metalloids for which limit values have been set (see

References [14] and [15]) and for which one or more of the sample dissolution methods specified in this

document are applicable. However, there is no information available on the effectiveness of any of the

specified sample dissolution methods for those elements in italics.
Aluminium Calcium Magnesium Selenium Tungsten
Antimony Chromium Manganese Silver Uranium
Arsenic Cobalt Mercury Sodium Vanadium
Barium Copper Molybdenum Strontium Yttrium
Beryllium Hafnium Nickel Tantalum Zinc
Bismuth Indium Phosphorus Tellurium Zirconium
© ISO 2020 – All rights reserved 1
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ISO 15202-2:2020(E)
Boron Iron Platinum Thallium
Caesium Lead Potassium Tin
Cadmium Lithium Rhodium Titanium

ISO 15202 is not applicable to the determination of elemental mercury or arsenic trioxide, since

mercury vapour and arsenic trioxide vapour are not collected using the sampling method specified in

ISO 15202-1.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements 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.

ISO 15202-1, Workplace air — Determination of metals and metalloids in airborne particulate matter by

inductively coupled plasma atomic emission spectrometry — Part 1: Sampling

ISO 15202-3, Workplace air — Determination of metals and metalloids in airborne particulate matter by

inductively coupled plasma atomic emission spectrometry — Part 3: Analysis
ISO 18158, Workplace air — Terminology

ISO 21832, Workplace air — Metals and metalloids in airborne particles — Requirements for evaluation of

measuring procedures
3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 18158 and the following apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org
3.1
sample dissolution

process of obtaining a solution containing all analytes of interest from a sample, which might or might

not involve complete dissolution of the sample
3.2
sample solution
solution prepared from a sample by the process of sample dissolution (3.1)

Note 1 to entry: A sample solution might need to be subjected to further operations, e.g. dilution, or addition, or

both, of an internal standard(s), in order to produce a test solution (3.3).
SOURCE: Adapted from EN 14902:2005, 3.1.22.
3.3
test solution

blank solution or sample solution (3.2) that has been subjected to all operations required to bring it into

a state in which it is ready for analysis

Note 1 to entry: “Ready for analysis” includes any required dilution or addition, or both, of an internal standard.

If a blank solution or sample solution (3.2) is not subject to any further operations before analysis, it is a test

solution.
SOURCE: EN 14902:2005, 3.1.30.
2 © ISO 2020 – All rights reserved
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ISO 15202-2:2020(E)
4 Principle

4.1 Airborne particles containing metals and metalloids are collected by drawing a measured volume

of air through a collection substrate, typically a filter mounted in a sampler designed to collect an

appropriate size fraction of airborne particles, using the method specified in ISO 15202-1.

4.2 An appropriate and suitable sample dissolution method is selected from those specified in

Annexes B through H, taking into consideration the metals and metalloids which are to be determined,

the limit values that have been set for those metals and metalloids, the applicability of the methods for

dissolution of the metals and metalloids of interest from materials which could be present in the test

atmosphere and the availability of the required laboratory apparatus.

4.3 The sample and collection substrate are then treated to dissolve the metals and metalloids of

interest using the selected sample dissolution method.

4.4 The resultant test solution is subsequently analysed for the metals and metalloids of interest by

inductively coupled plasma-atomic emission spectrometry using the method specified in ISO 15202-3.

NOTE Sample preparation methods described in Annexes B through H are generally suitable for use with

[5] [10] [11]

analytical techniques other than ICP-AES, e.g. AAS by ISO 8518 and ISO 11174 and ICP-MS by ISO 30011 .

For ICP-MS, changes could be required in the concentrations of acids or the dilution factors used to prepare

test solutions. Furthermore, some acids, such as hydrochloric acid, are not recommended for test solutions for

analysis by ICP-MS.
5 Requirements

The measuring procedure as a whole (covered by ISO 15202-1, ISO 15202-2 and ISO 15202-3) shall

conform to any relevant performance requirements for measuring chemical agents in workplace air

[12]
(for example ISO 20581 and ISO 21832).
6 Reactions

In general, the majority of particulate metals and metalloids and particulate metal and metalloid

compounds which are commonly of interest in samples of workplace air are converted to water-soluble

ions by one or more of the sample dissolution methods specified in this document. However, if there

is any doubt about whether a method will exhibit the required analytical recovery for a particular

application, it is necessary to investigate this before proceeding with the method (see 10.1).

7 Reagents

During the analysis, use only reagents of analytical grade and only water as specified in 7.1.

NOTE 1 Safety precautions to be observed when using hydrofluoric and perchloric acids are given in Annex A.

NOTE 2 Details of reagents that are required for use in Annexes B through I are given in the annex concerned.

NOTE 3 It could be necessary to use acids of higher purity in order to obtain an adequate detection limit for

some metals and metalloids.
[3]

7.1 Water, conforming with the requirements for ISO 3696 grade 2 water (electrical conductivity

less than 0,1 mS/m and resistivity greater than 0,01 MΩ⋅m at 25 °C).

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 MΩ⋅m (usually expressed by manufacturers of

water purification systems as 18 MΩ⋅cm).
© ISO 2020 – All rights reserved 3
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ISO 15202-2:2020(E)
7.2 Nitric acid (HNO ), concentrated,ρ ≈ 1,42 g ml , w ≈ 70 % mass fraction.
HNO HNO
3 3

The concentration of the metals and metalloids of interest shall be less than 0,1 µg ml .

WARNING — Concentrated nitric acid is corrosive and oxidizing, and nitric acid fumes are

irritant. Avoid exposure by contact with the skin or eyes, or by inhalation of fumes. Use suitable

personal protective equipment (including suitable gloves, face shield or safety spectacles, etc.)

when working with the concentrated or dilute nitric acid and carry out sample dissolution with

concentrated nitric acid in open vessels in a fume hood.
7.3 Nitric acid, diluted 1 + 9.

Carefully and slowly begin adding 50 ml of concentrated nitric acid (7.2) to 450 ml of water (7.1) in a 1 l

polypropylene bottle (8.5). Add the acid in small aliquots. Between additions, swirl to mix and run cold

tap water over the side of the bottle to cool the contents. Do not allow the tap water to contaminate the

contents of the bottle. When the addition of the concentrated nitric acid is complete, swirl the bottle

to mix the contents, allow to cool to room temperature, close the bottle with its screw cap and mix

thoroughly.
8 Laboratory apparatus
Usual laboratory apparatus and, in particular, the following.

8.1 Disposable gloves, impermeable and powder free, to avoid the possibility of contamination from

the hands and to protect them from contact with toxic and corrosive substances. PVC gloves are suitable.

8.2 Glassware, beakers and one-mark volumetric flasks conforming to the requirements of

[1] [2]

ISO 1042 , made of borosilicate glass conforming with the requirements of ISO 3585 , cleaned before

use by soaking in 1 + 9 nitric acid (7.3) for at least 24 h and then rinsing thoroughly with water (7.1).

Alternatively, the glassware may be cleaned with a suitable laboratory detergent using a laboratory

washing machine.

8.3 Flat-tipped forceps, non-metallic (e.g. plastic or plastic-coated), for unloading filters from

samplers or from filter transport cassettes.
[6]

8.4 Piston-operated volumetric instruments, conforming with the requirements of ISO 8655-1

[9]

and tested in accordance with ISO 8655-6 , including pipettors conforming with the requirements of

[7] [8]

ISO 8655-2 and dispensers conforming with the requirements of ISO 8655-5 , for dispensing leach

solution, acids, etc.
8.5 Polypropylene bottle, 1 l capacity, with leakproof screw cap.

A bottle made of an alternative plastic may be used provided that it is suitable for the intended use

(see 7.3).

NOTE Details of laboratory apparatus that are required for use in Annexes B through I are given in the annex

concerned.
9 Procedure
9.1 Soluble metal and metalloid compounds

9.1.1 If results are required for comparison with limit values for soluble metal or metalloid compounds,

or both, use the sample dissolution method specified in Annex B to prepare test solutions for analysis by

the method specified in ISO 15202-3.
4 © ISO 2020 – All rights reserved
---------------------- Page: 9 ----------------------
ISO 15202-2:2020(E)

9.1.2 Alternatively, if it is known that no insoluble compounds of the metals or metalloids, or both,

of interest are used in the workplace and that none are produced in the processes carried out, prepare

test solutions for analysis by the method specified in ISO 15202-3, using one of the sample dissolution

methods for total metals and metalloids and their compounds prescribed in Annexes C through H, and

compare the results with the limit value for the soluble metals or metalloids, or both, concerned.

The methods prescribed in Annexes C through H are not specific for soluble metal or metalloid

compounds, or both. However, in the circumstances described above, they may be used as an alternative

to the method described in Annex B, if this is more convenient.
9.2 Total metals and metalloids and their compounds

9.2.1 If results are required for comparison with limit values for total metals or metalloids, or both,

and their compounds, select a suitable sample dissolution method from those specified in Annexes C

through H. Take into consideration the applicability of each method for dissolution of the metals and

metalloids of interest from materials that could be present in the test atmosphere (refer to the clause on

the effectiveness of the sample dissolution method in the annex in which the method is specified) and the

availability of the required laboratory apparatus.

9.2.2 Use the selected sample dissolution method to prepare test solutions for analysis of total metals

and metalloids and their compounds by the method specified in ISO 15202-3.
9.3 Mixed exposure
9.3.1 If results are required

— for comparison with limit values for soluble metal and/or metalloid compounds and with limit

values for metals and/or metalloids and their insoluble compounds, or

— for comparison with limit values for soluble metal and/or metalloid compounds and with limit

values for total metals and/or metalloids and their compounds,
follow the instructions given in 9.3.2 and 9.3.3.

9.3.2 Use the sample dissolution method specified in Annex B to prepare test solutions for the

determination of soluble metal and metalloid compounds by the method specified in ISO 15202-3.

9.3.3 Select a suitable sample dissolution method for total metals and metalloids and compounds

(see 9.2). Use this to treat undissolved material from the method for soluble metal and metalloid

compounds (see B.6.7.1) and prepare test solutions for determination of metals and metalloids and their

insoluble compounds by the method specified in ISO 15202-3.
10 Special cases

10.1 Action to be taken if there is doubt about the effectiveness of the selected sample

dissolution method

10.1.1 If there is any doubt about whether the selected sample dissolution method will exhibit the

required analytical recovery when used for dissolution of the metals and metalloids of interest from

materials which could be present in the test atmosphere, determine its effectiveness for that particular

application. For total metals and metalloids, this may be achieved by analysing a bulk sample of known

composition which is similar in nature to the materials being used or produced in the workplace, e.g. a

certified reference material. For soluble metals and metalloids, analytical recovery is best determined by

analysing filters spiked with solution containing a known mass of the soluble compound of interest.

© ISO 2020 – All rights reserved 5
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ISO 15202-2:2020(E)

NOTE In designing an experiment to determine the effectiveness of a sample dissolution method, the particle

size of a bulk sample can have a significant influence on the efficiency of its dissolution. Furthermore, microgram

amounts of relatively insoluble material are normally much more easily dissolved than milligram amounts.

10.1.2 If the analytical recovery is less than the minimum acceptable value prescribed in ISO 21832

(analytical recovery at least 90 % with a coefficient of variation less than 5 %), investigate the use of an

alternative sample dissolution method. This may be a method not specified in this document if it can be

demonstrated that its analytical recovery meets the requirements of ISO 21832.

10.1.3 Do not use a correction factor to compensate for an apparently ineffective sample dissolution

method, since this might equally lead to erroneous results.

10.2 Action to be taken when particles have become dislodged from the filter during

transportation

When the filter transport cassettes or samplers are opened, it is advisable to look for evidence that

particles have become dislodged from the filter during transportation. If this appears to have occurred,

wash the internal surfaces of the filter transport cassette or sampler in the sample dissolution vessel

in order to recover the material concerned. Before analysis is carried out, inform the originator of the

sample of the condition in which it was received so that the originator can make a judgement as to

whether it is to be analysed.
10.3 Action to be taken regarding sampler wall deposits

Particles are frequently found to have deposited on the interior walls of samplers, an

...

NORME ISO
INTERNATIONALE 15202-2
Troisième édition
2020-05
Air des lieux de travail —
Détermination des métaux et
métalloïdes dans les particules
en suspension dans l'air par
spectrométrie d'émission atomique
avec plasma à couplage inductif —
Partie 2:
Préparation des échantillons
Workplace air — Determination of metals and metalloids in airborne
particulate matter by inductively coupled plasma atomic emission
spectrometry —
Part 2: Sample preparation
Numéro de référence
ISO 15202-2:2020(F)
ISO 2020
---------------------- Page: 1 ----------------------
ISO 15202-2:2020(F)
DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2020

Tous droits réservés. Sauf prescription différente ou nécessité dans le contexte de sa mise en œuvre, aucune partie de cette

publication ne peut être reproduite ni utilisée sous quelque forme que ce soit et par aucun procédé, électronique ou mécanique,

y compris la photocopie, ou la diffusion sur l’internet ou sur un intranet, sans autorisation écrite préalable. Une autorisation peut

être demandée à l’ISO à l’adresse ci-après ou au comité membre de l’ISO dans le pays du demandeur.

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Publié en Suisse
ii © ISO 2020 – Tous droits réservés
---------------------- Page: 2 ----------------------
ISO 15202-2:2020(F)
Sommaire Page

Avant-propos ..............................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Domaine d’application ................................................................................................................................................................................... 1

2 Références normatives ................................................................................................................................................................................... 2

3 Termes et définitions ....................................................................................................................................................................................... 2

4 Principe .......................................................................................................................................................................................................................... 3

5 Exigences ...................................................................................................................................................................................................................... 3

6 Réactions ...................................................................................................................................................................................................................... 4

7 Réactifs ........................................................................................................................................................................................................................... 4

8 Appareillage de laboratoire ...................................................................................................................................................................... 4

9 Mode opératoire.................................................................................................................................................................................................... 5

9.1 Composés solubles de métaux et métalloïdes ............................................................................................................. 5

9.2 Métaux et métalloïdes totaux et leurs composés ...................................................................................................... 5

9.3 Exposition mixte .................................................................................................................................................................................... 6

10 Cas particuliers ...................................................................................................................................................................................................... 6

10.1 Action à mener s’il existe un doute concernant l’efficacité de la méthode de mise

en solution d’échantillon choisie ............................................................................................................................................. 6

10.2 Action à mener lorsque les particules se sont détachées du filtre pendant le transport ....... 7

10.3 Action à mener en présence de dépôts sur les parois du dispositif de prélèvement ................. 7

11 Enregistrements de laboratoire ........................................................................................................................................................... 7

Annexe A (informative) Précautions de sécurité à respecter lors de l’utilisation d’acide

fluorhydrique et perchlorique ............................................................................................................................................................... 8

Annexe B (normative) Méthode de mise en solution d’échantillon pour les composés

solubles de métaux et métalloïdes .................................................................................................................................................... 9

Annexe C (normative) Mise en solution d’échantillon à l’aide d’acide nitrique et d’acide

chlorhydrique sur plaque chauffante ..........................................................................................................................................15

Annexe D (normative) Mise en solution d’échantillon à l’aide d’acide fluorhydrique et

d’acide nitrique par agitation par ultrason ...........................................................................................................................19

Annexe E (normative) Mise en solution en utilisant de l’acide sulfurique et du peroxyde

d’hydrogène sur plaque chauffante ...............................................................................................................................................23

Annexe F (normative) Mise en solution en utilisant de l’acide nitrique et de l’acide

perchlorique sur plaque chauffante .............................................................................................................................................28

Annexe G (normative) Mise en solution d’échantillon dans un système de digestion par

micro-ondes en récipient fermé ........................................................................................................................................................33

Annexe H (normative) Mise en solution d’échantillon à 95 °C sur bloc chauffant .............................................39

Annexe I (normative) Action à mener en présence de particules visibles, non dissoutes,

après mise en solution d’échantillon ...........................................................................................................................................43

Annexe J (informative) Dépôts sur les parois des dispositifs de prélèvement ......................................................49

Bibliographie ...........................................................................................................................................................................................................................52

© ISO 2020 – Tous droits réservés iii
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ISO 15202-2:2020(F)
Avant-propos

L'ISO (Organisation internationale de normalisation) est une fédération mondiale d'organismes

nationaux de normalisation (comités membres de l'ISO). L'élaboration des Normes internationales est

en général confiée aux comités techniques de l'ISO. Chaque comité membre intéressé par une étude

a le droit de faire partie du comité technique créé à cet effet. Les organisations internationales,

gouvernementales et non gouvernementales, en liaison avec l'ISO participent également aux travaux.

L'ISO collabore étroitement avec la Commission électrotechnique internationale (IEC) en ce qui

concerne la normalisation électrotechnique.

Les procédures utilisées pour élaborer le présent document et celles destinées à sa mise à jour sont

décrites dans les Directives ISO/IEC, Partie 1. Il convient, en particulier, de prendre note des différents

critères d'approbation requis pour les différents types de documents ISO. Le présent document a été

rédigé conformément aux règles de rédaction données dans les Directives ISO/IEC, Partie 2 (voir www

.iso .org/ directives).

L'attention est attirée sur le fait que certains des éléments du présent document peuvent faire l'objet de

droits de propriété intellectuelle ou de droits analogues. L'ISO ne saurait être tenue pour responsable

de ne pas avoir identifié de tels droits de propriété et averti de leur existence. Les détails concernant

les références aux droits de propriété intellectuelle ou autres droits analogues identifiés lors de

l'élaboration du document sont indiqués dans l'Introduction et/ou dans la liste des déclarations de

brevets reçues par l'ISO (voir www .iso .org/ brevets).

Les appellations commerciales éventuellement mentionnées dans le présent document sont données

pour information, par souci de commodité, à l’intention des utilisateurs et ne sauraient constituer un

engagement.

Pour une explication de la nature volontaire des normes, la signification des termes et expressions

spécifiques de l'ISO liés à l'évaluation de la conformité, ou pour toute information au sujet de l'adhésion

de l'ISO aux principes de l’Organisation mondiale du commerce (OMC) concernant les obstacles

techniques au commerce (OTC), voir www .iso .org/ avant -propos.

Le présent document a été élaboré par le comité technique ISO/TC 146, Qualité de l’air, sous-comité SC 2,

Atmosphères des lieux de travail.

Cette troisième édition annule et remplace la deuxième édition (ISO 15202-2:2012), qui a fait l’objet

d’une révision technique. Les principales modifications par rapport à l’édition précédente sont les

suivantes:

— les définitions figurant dans l’ISO 18158 ont été supprimées de l’ISO 15202-2, et la référence à

l’ISO 18158 a été ajoutée en remplacement des références à l’EN 1540;

— les références à l’EN 482 ont été remplacées par l’ISO 20581, et les références à l’EN 13890 ont été

remplacées par l’ISO 21832;

— des informations relatives à la digestion des capsules internes solubles dans l’acide ont été ajoutées

dans les Annexes C, D, E, F, G et H;
— le texte a fait l’objet d’une mise à jour rédactionnelle.

Une liste de toutes les parties de la série ISO 15202 se trouve sur le site Web de l’ISO.

Il convient que l’utilisateur adresse tout retour d’information ou toute question concernant le présent

document à l’organisme national de normalisation de son pays. Une liste exhaustive desdits organismes

se trouve à l’adresse www .iso .org/ fr/ members .html.
iv © ISO 2020 – Tous droits réservés
---------------------- Page: 4 ----------------------
ISO 15202-2:2020(F)
Introduction

La santé des travailleurs dans de nombreuses industries est en danger du fait de l’exposition par

inhalation aux métaux et aux métalloïdes toxiques. Les hygiénistes industriels et autres professionnels

de santé publique ont besoin de déterminer l’efficacité des mesures prises pour contrôler l’exposition

des travailleurs et cela s’effectue en général en réalisant des mesurages de l’air du lieu de travail. Le

présent document a été publié dans le but de mettre à disposition une méthode permettant d’effectuer

des mesurages d’exposition valides pour un large éventail de métaux et de métalloïdes utilisés dans

l’industrie. Il sera utile aux organismes concernés par la santé et la sécurité sur le lieu de travail, aux

hygiénistes industriels et autres professionnels de santé publique, aux laboratoires d’analyses, aux

industriels utilisateurs de métaux et métalloïdes et à leurs employés.

L’ISO 15202, publiée en trois parties, spécifie une méthode générique pour la détermination de la

concentration en masse des métaux et métalloïdes sur le lieu de travail en utilisant la spectrométrie

d’émission atomique avec plasma à couplage inductif (ICP-AES):

— L’ISO 15202-1 donne les détails des Normes internationales, européennes et nationales appropriées

qui spécifient les caractéristiques, les exigences de performance et les méthodes d’essai se rapportant

à l’équipement de prélèvement. Elle complète les conseils donnés par ailleurs sur la stratégie

d’évaluation et la stratégie de mesurage et spécifie une méthode de prélèvement d’échantillons de

matière particulaire en suspension dans l’air en vue d’une analyse chimique ultérieure.

— L’ISO 15202-2 décrit plusieurs méthodes de préparation des solutions d’échantillons pour analyse

par ICP-AES.

— L’ISO 15202-3 définit les exigences et les méthodes d’essai pour l’analyse de solutions d’échantillons

par ICP-AES.

Les méthodes de préparation d’échantillons décrites dans la présente partie de l’ISO 15202 sont

généralement appropriées pour une utilisation avec d’autres techniques d’analyse que l’ICP-AES, par

exemple la spectrométrie d’absorption atomique (AAS) et la spectrométrie de masse avec plasma à

couplage inductif (ICP-MS).

Lors de l’élaboration du présent document, il a été présumé que les personnes chargées de l’exécution

de ses dispositions et de l’interprétation des résultats obtenus ont les qualifications et l’expérience

appropriées.
© ISO 2020 – Tous droits réservés v
---------------------- Page: 5 ----------------------
NORME INTERNATIONALE ISO 15202-2:2020(F)
Air des lieux de travail — Détermination des métaux et
métalloïdes dans les particules en suspension dans l'air
par spectrométrie d'émission atomique avec plasma à
couplage inductif —
Partie 2:
Préparation des échantillons

AVERTISSEMENT — L’utilisation du présent document peut impliquer l’emploi de produits et

la mise en œuvre de modes opératoires et d’appareillages à caractère dangereux. Le présent

document n’a pas pour but d’aborder tous les problèmes de sécurité liés à son utilisation. Il

incombe à l’utilisateur du présent document d’établir, avant de l’utiliser, des pratiques d’hygiène

et de sécurité appropriées et de déterminer l’applicabilité des restrictions réglementaires.

1 Domaine d’application

Le présent document spécifie plusieurs méthodes appropriées de préparation de solutions d’essai à

partir d’échantillons de matière particulaire en suspension dans l’air prélevés en utilisant la méthode

spécifiée dans l’ISO 15202-1, en vue du dosage des métaux et métalloïdes par ICP-AES à l’aide de la

méthode spécifiée dans l’ISO 15202-3. Il contient des informations relatives à l’applicabilité des

méthodes par rapport au dosage de métaux et métalloïdes pour lesquels des valeurs limites ont

été établies. Ces méthodes peuvent également être utilisées pour le dosage de certains métaux et

métalloïdes pour lesquels les valeurs limites n’ont pas été établies mais, dans ce cas, aucune information

sur leur applicabilité n’est disponible.

NOTE Les méthodes de préparation d’échantillons décrites dans le présent document sont généralement

appropriées pour une utilisation conjointe avec d’autres techniques d’analyse que l’ICP-AES, par exemple la

[5] [10]

spectrométrie d’absorption atomique (AAS) définie dans l’ISO 8518 et l’ISO 11174 et la spectrométrie de

[11]
masse avec plasma à couplage inductif (ICP-MS) définie dans l’ISO 30011 .

La méthode spécifiée à l’Annexe B est applicable pour effectuer des mesurages de comparaison avec des

valeurs limites de composés solubles de métaux ou métalloïdes.

Une ou plusieurs des méthodes de mise en solution d’échantillon spécifiées aux Annexes C à H sont

applicables pour effectuer des mesurages de comparaison avec des valeurs limites de métaux et

métalloïdes totaux et leurs composés. Des informations concernant les possibilités d’application des

méthodes individuelles sont données dans le domaine d’application de l’annexe dans laquelle la méthode

est spécifiée.

La liste suivante est une liste non exhaustive des métaux et métalloïdes pour lesquels des valeurs

limites ont été déterminées (voir Références [14] et [15]) et pour lesquels au moins une des méthodes de

mise en solution d’échantillon spécifiées dans le présent document est applicable. Il n’existe cependant

pas d’informations disponibles sur l’efficacité de l’ensemble de ces méthodes de mise en solution

d’échantillon spécifiées pour les éléments indiqués en italique.
© ISO 2020 – Tous droits réservés 1
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ISO 15202-2:2020(F)
Aluminium Calcium Lithium Potassium Tungstène
Antimoine Césium Magnésium Rhodium Uranium
Argent Chrome Manganèse Sélénium Vanadium
Arsenic Cobalt Mercure Sodium Yttrium
Baryum Cuivre Molybdène Strontium Zinc
Béryllium Étain Nickel Tantale Zirconium
Bismuth Fer Phosphore Tellure
Bore Hafnium Platine Thallium
Cadmium Indium Plomb Titane

L’ISO 15202 n’est pas applicable pour la détermination du mercure élémentaire ni de l’anhydride

arsénieux, dans la mesure où les vapeurs de mercure et les vapeurs d’anhydride arsénieux ne sont pas

recueillies en utilisant la méthode de prélèvement spécifiée dans l’ISO 15202-1.
2 Références normatives

Les documents suivants sont cités dans le texte de sorte qu’ils constituent, pour tout ou partie de leur

contenu, des exigences du présent document. Pour les références datées, seule l’édition citée s’applique.

Pour les références non datées, la dernière édition du document de référence s’applique (y compris les

éventuels amendements)

ISO 15202-1, Air des lieux de travail — Détermination des métaux et métalloïdes dans les particules en

suspension dans l’air par spectrométrie d’émission atomique avec plasma à couplage inductif — Partie 1:

Prélèvement d’échantillons

ISO 15202-3, Air des lieux de travail — Détermination des métaux et métalloïdes dans les particules en

suspension dans l'air par spectrométrie d'émission atomique avec plasma à couplage inductif — Partie

3: Analyse
ISO 18158, Qualité de l'air — Terminologie

ISO 21832, Air des lieux de travail — Métaux et métalloïdes dans les particules en suspension dans l'air —

Exigences relatives à l'évaluation des procédures de mesure
3 Termes et définitions

Pour les besoins du présent document, les termes et définitions de l’ISO 18158 ainsi que les suivants,

s’appliquent.

L’ISO et l’IEC tiennent à jour des bases de données terminologiques destinées à être utilisées en

normalisation, consultables aux adresses suivantes:

— ISO Online browsing platform: disponible à l’adresse https:// www .iso .org/ obp;

— IEC Electropedia: disponible à l’adresse http:// www .electropedia .org.
3.1
mise en solution de l’échantillon

processus permettant d’obtenir une solution contenant les analytes étudiés à partir d’un échantillon,

lequel processus peut, ou non, impliquer la mise en solution complète de l’échantillon

2 © ISO 2020 – Tous droits réservés
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ISO 15202-2:2020(F)
3.2
solution d’échantillon

solution préparée à partir d’un échantillon au moyen du processus de mise en solution de l’échantillon (3.1)

Note 1 à l'article: Il peut se révéler nécessaire de soumettre une solution d’échantillon à d’autres opérations, par

exemple à une dilution ou à un ajout d’étalon(s) interne(s), ou les deux, en vue de produire une solution d’essai (3.3).

SOURCE: Adaptée de l’EN 14902:2005, 3.1.22
3.3
solution d’essai

solution de blanc ou solution d’échantillon (3.2) qui a été soumise à toutes les opérations nécessaires

pour l’amener à un état dans lequel elle est prête pour l’analyse

Note 1 à l'article: L’expression «prête pour l’analyse» comprend toute dilution nécessaire ou tout ajout nécessaire

d’étalon(s) interne(s), ou les deux. Si une solution de blanc ou une solution d’échantillon (3.2) n’est pas soumise à

d’autres opérations avant l’analyse, il s’agit d’une solution d’essai.
SOURCE: EN 14902:2005, 3.1.30
4 Principe

4.1 Les particules en suspension dans l’air contenant des métaux et métalloïdes sont recueillies par

passage d’un volume d’air mesuré à travers un substrat de collecte, généralement un filtre monté dans

un dispositif de prélèvement étudié pour retenir une fraction de taille appropriée des particules dans

l’air, en utilisant la méthode spécifiée dans l’ISO 15202-1.

4.2 Une méthode de mise en solution d’échantillon appropriée et adéquate est choisie parmi celles

spécifiées aux Annexes B à H, en tenant compte des métaux et métalloïdes à déterminer, des valeurs

limites ayant été déterminées pour ces métaux et métalloïdes, des possibilités d’application de ces

méthodes de mise en solution des métaux et métalloïdes étudiés en fonction de la nature des matériaux

qui pourraient être présents dans l’atmosphère d’essai, ainsi que de la disponibilité de l’appareillage de

laboratoire nécessaire.

4.3 L’échantillon et le substrat de collecte sont alors traités pour mettre en solution les métaux et

métalloïdes étudiés en utilisant la méthode de mise en solution d’échantillon choisie.

4.4 La solution d’essai obtenue est ensuite analysée pour déterminer les métaux et métalloïdes

étudiés par spectrométrie d’émission atomique avec plasma à couplage inductif au moyen de la méthode

spécifiée dans l’ISO 15202-3.

NOTE Les méthodes de préparation d’échantillons décrites aux Annexes B à H sont généralement appropriées

pour une utilisation conjointe avec d’autres techniques d’analyse que l’ICP-AES, par exemple la spectrométrie

[5] [10]

d’absorption atomique (AAS) définie dans l’ISO 8518 et l’ISO 11174 et la spectrométrie de masse avec

[11]

plasma à couplage inductif (ICP-MS) définie dans l’ISO 30011 . Pour l’ICP-MS, il pourrait se révéler nécessaire

de modifier les concentrations d’acides ou les facteurs de dilution utilisés pour préparer les solutions d’essai.

En outre, certains acides, tels que l’acide chlorhydrique, ne sont pas recommandés pour les solutions d’essai

destinées à une analyse par ICP-MS.
5 Exigences

Le mode opératoire de mesurage dans son ensemble (couvert par l’ISO 15202-1, l’ISO 15202-2 et

l’ISO 15202-3) doit être conforme à toute exigence de performance concernant le mesurage des agents

[12]

chimiques présents dans l’air des lieux de travail (par exemple l’ISO 20581 et l’ISO 21832).

© ISO 2020 – Tous droits réservés 3
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ISO 15202-2:2020(F)
6 Réactions

En général, la majorité des particules de métaux et métalloïdes et des particules de composés de

métaux et métalloïdes qui sont communément étudiés dans les échantillons d’air des lieux de travail

est convertie en ions solubles dans l’eau par au moins l’une des méthodes de mise en solution spécifiées

dans le présent document. Cependant, s’il existe le moindre doute concernant la capacité de la méthode

à obtenir le taux de récupération analytique nécessaire pour une application particulière, il est alors

nécessaire d’étudier ce problème avant de poursuivre avec la méthode (voir 10.1).

7 Réactifs

Au cours de l’analyse, utiliser uniquement des réactifs de qualité analytique et uniquement de l’eau telle

que spécifiée en 7.1.

NOTE 1 Les précautions de sécurité à respecter lors de l’utilisation d’acide fluorhydrique et perchlorique sont

données dans l’Annexe A.

NOTE 2 Des détails concernant les réactifs nécessaires pour une utilisation aux Annexes B à I sont donnés

dans l’annexe concernée.

NOTE 3 Il pourrait se révéler nécessaire d’utiliser des acides de pureté supérieure de manière à obtenir une

limite de détection adéquate pour certains métaux et métalloïdes.
[3]

7.1 Eau, conforme aux exigences de l’ISO 3696 , qualité 2 (conductivité électrique inférieure à

0,1 mS/m et résistivité supérieure à 0,01 MΩ⋅m à 25 °C).

Il est recommandé d’utiliser une eau ayant été traitée dans un système de purification fournissant

une eau ultrapure, de résistivité supérieure à 0,18 MΩ⋅m (les fabricants expriment généralement cette

valeur sous la forme 18 MΩ⋅cm).

7.2 Acide nitrique (HNO ), concentré,ρ ≈ 1,42 g ml , fraction massique w ≈ 70 %.

3 HNO HNO
3 3
La teneur en métaux et métalloïdes étudiés doit être inférieure à 0,1 µg ml .

AVERTISSEMENT — L’acide nitrique concentré est corrosif et comburant et les fumées d’acide

nitrique sont irritantes. Éviter toute exposition par le contact avec la peau ou les yeux, ou

par inhalation de fumées. Utiliser un équipement de protection individuelle (y compris gants

appropriés, écran facial ou lunettes de protection, etc.) pour tout travail avec de l’acide nitrique

concentré ou dilué, et effectuer la mise en solution d’échantillon avec de l’acide nitrique

concentré dans des récipients ouverts sous une hotte.
7.3 Acide nitrique, dilué 1 + 9.

Commencer par ajouter soigneusement et lentement 50 ml d’acide nitrique concentré (7.2) à 450 ml

d’eau (7.1) dans une bouteille en polypropylène de 1 l (8.5). Verser l’acide par petites aliquotes. Entre

les ajouts, faire tourner pour mélanger et faire couler de l’eau courante froide sur la paroi de la bouteille

pour refroidir le contenu. Empêcher l’eau courante de contaminer le contenu de la bouteille. Après

ajout complet de l’acide nitrique concentré, faire tourner la bouteille pour mélanger le contenu, laisser

refroidir à température ambiante, fermer la bouteille avec son bouchon à vis et mélanger parfaitement.

8 Appareillage de laboratoire
Matériel courant de laboratoire et, en particulier, ce qui suit.

8.1 Gants à usage unique, imperméables et non poudrés, pour empêcher toute possibilité de

contamination par les mains et pour les protéger contre le contact avec des substances toxiques et

corrosives. Des gants en PVC sont adéquats.
4 © ISO 2020 – Tous droits réservés
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ISO 15202-2:2020(F)
[1]

8.2 Verrerie, béchers et fioles jaugées à un trait, conformes aux exigences de l’ISO 1042 , en verre

[2]

borosilicaté conforme aux exigences de l’ISO 3585 , nettoyés avant utilisation par trempage dans de

l’acide nitrique 1 + 9 (7.3) pendant au moins 24 h puis rinçage abondant avec de l’eau (7.1).

En variante, la verrerie peut être nettoyée avec un détergent de laboratoire approprié en utilisant une

machine à laver de laboratoire.

8.3 Pinces à bout plat, non métallique (par exemple en plastique ou recouvertes de plastique) pour

retirer les filtres des dispositifs de prélèvement ou des cassettes de transport de filtre.

[6]

8.4 Instruments volumétriques à piston, conformes aux exigences de l’ISO 8655-1 et soumis à essai

[9] [7]

conformément à l’ISO 8655-6 , comprenant des pipettes conformes aux exigences de l’ISO 8655-2 et

[8]

des dispenseurs conformes aux exigences de l’ISO 8655-5 , pour délivrer la solution de lixiviation, les

acides, etc.

8.5 Bouteille en polypropylène, d’une capacité de 1 l, munie d’un bouchon à vis étanche.

Une bouteille fabriquée dans un plastique différent peut être utilisée sous réserve qu’elle soit adéquate

pour l’utilisation prévue (voir 7.3).

NOTE Des détails concernant l’appareillage de laboratoire nécessaire pour une utilisation aux Annexes B à I

sont donnés dans l’annexe concernée.
9 Mode opératoire
9.1 Composés solubles de métaux et métalloïdes

9.1.1 S’il est nécessaire de comparer des résultats avec des valeurs limites pour les composés solubles

de métaux ou de métalloïdes, ou les deux, utiliser la méthode de mise en solution spécifiée à l’Annexe B

pour préparer les solutions d’essai destinées à l’analyse par la méthode spécifiée dans l’ISO 15202-3.

9.1.2 Lorsqu’il est certain qu’aucun composé insoluble des métaux ou des métalloïdes étudiés, ou les

deux, n’est utilisé sur le lieu de travail ni produit dans les processus mis en œuvre, une autre méthode

consiste à préparer des solutions d’essai pour analyse à l’aide de la méthode spécifiée dans l’ISO 15202-3,

en utilisant une des méthodes de mise en solution d’échantillon pour les métaux et métalloïdes totaux

et leurs composés spécifiées aux Annexes C à H, et à comparer les résultats avec les valeurs limites des

métaux ou métalloïdes solubles, ou les deux, concernés.

Les méthodes spécifiées aux Annexes C à H ne sont pas spécifiques aux composés solubles de métaux

ou de métalloïdes, ou les deux. Toutefois, dans les circonstances décrites ci-dessus, elles peuvent être

utilisées comme méthode alternative à la méthode décrite à l’Annexe B, si cela s’avère plus pratique.

9.2 Métaux et métalloïdes totaux et leurs composés

9.2.1 S’il est nécessaire de comparer des résultats avec des valeurs limites pour les métaux ou

métalloïdes totaux, ou les deux, et leurs composés, choisir une méthode de mise en solution d’échantillon

adéquate parmi celles spécifiées aux Annexes C à H. Tenir compte des possibilités d’application de chaque

méthode pour la mise en solution des métaux et métalloïdes en fonction de la nature des matériaux qui

pourraient être présents dans l’atmosphère d’essai (se rapporter à l’article sur l’efficacité de la méthode

de mise en solution d’échantillon à l’annexe spécifiant la méthode concernée), ainsi que de la disponibilité

des instruments de laboratoire nécessaires.

9.2.2 Utiliser la méthode de mise en solution d’échantillon pour préparer des solutions d’essai

destinées à l’analyse des métaux et métalloïdes
...

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