EN ISO 23861:2022
(Main)Workplace air - Chemical agent present as a mixture of airborne particles and vapour - Requirements for evaluation of measuring procedures using samplers (ISO 23861:2022)
Workplace air - Chemical agent present as a mixture of airborne particles and vapour - Requirements for evaluation of measuring procedures using samplers (ISO 23861:2022)
This document specifies requirements for the evaluation of measuring procedures using samplers for the determination of a chemical agent present in the workplace atmosphere as a mixture of airborne particles and vapour.
The procedures given in this document provide results only for the sum of airborne particles and vapour. The concentration is calculated in terms of mass per unit volume.
NOTE The physical behaviour of a mixture of airborne particles and vapour is described in Annex A. Examples of substances which can be present in multiple phases are toluene diisocyanate, diethanolamine, ethyleneglycol and tributylphosphate.
This document can also be applied to complex mixtures, such as metal working fluids or bitumen fumes.
This document is applicable to samplers and measuring procedures using these samplers in which sampling and analysis are carried out in separate stages.
Luft am Arbeitsplatz - Als Mischung aus luftgetragenen Partikeln und Dampf vorliegender chemischer Arbeitsstoff - Anforderungen an die Bewertung von Messverfahren mit Sammlern (ISO 23861:2022)
Dieses Dokument legt Anforderungen an die Bewertung von Messverfahren mit Sammlern zur Bestimmung eines in der Umgebungsluft am Arbeitsplatz als Mischung aus luftgetragenen Partikeln und Dampf vorliegenden chemischen Arbeitsstoffs fest.
Die in diesem Dokument angegebenen Verfahren liefern nur Ergebnisse für die Summe aus luftgetragenen Partikeln und Dampf. Die Konzentration wird als Masse je Volumeneinheit berechnet.
ANMERKUNG Das physikalische Verhalten einer Mischung aus luftgetragenen Partikeln und Dampf wird in Anhang A beschrieben. Beispiele für Stoffe, die in mehreren Phasen vorhanden sein können, sind Toluol-Diisocyanat, Diethanolamin, Ethylenglykol und Tributylphosphat.
Dieses Dokument kann ebenfalls auf komplexe Mischungen wie Metallbearbeitungsflüssigkeiten (Kühlschmierstoffe) oder Bitumendämpfe angewendet werden.
Dieses Dokument ist anwendbar auf Sammler und Messverfahren, die diese Sammler, bei denen Probenahme und Analyse in getrennten Schritten vorgenommen werden, verwenden.
Air des lieux de travail - Agent chimique présent sous forme de mélange de particules en suspension dans l’air et de vapeur - Exigences d’évaluation des procédures de mesure utilisant des dispositifs de prélèvement (ISO 23861:2022)
Le présent document spécifie les exigences d’évaluation des procédures de mesure utilisant des dispositifs de prélèvement pour la détermination d’un agent chimique présent dans l’atmosphère des lieux de travail sous forme de mélange de particules en suspension dans l’air et de vapeur.
Les procédures spécifiées dans le présent document ne fournissent des résultats que pour la somme des particules en suspension dans l’air et de la vapeur. La concentration est calculée en termes de masse par unité de volume.
NOTE Le comportement physique d’un mélange de particules en suspension dans l’air et de vapeur est décrit dans l’Annexe A. Le toluène diisocyanate, la diéthanolamine, l’éthylène glycol et le tributhylphosphate sont des exemples de substances qui peuvent être présentes en plusieurs phases.
Le présent document peut également s’appliquer aux mélanges complexes tels que les fluides d’usinage ou les fumées de bitume.
Le présent document s’applique aux dispositifs de prélèvement et aux procédures de mesure utilisant ces dispositifs, au cours desquelles le prélèvement et l’analyse sont effectués à des étapes distinctes.
Zrak na delovnem mestu - Kemični agensi, prisotni kot zmesi lebdečih delcev in par - Zahteve za vrednotenje merilnih postopkov z vzorčevalniki (ISO 23861:2022)
Ta dokument določa zahteve glede zmogljivosti in preskusne metode v predpisanih laboratorijskih pogojih za vrednotenje vzorčevalnikov s črpanjem, ki se uporabljajo v povezavi s črpalko za vzorčenje zraka, in postopkov za uporabo teh vzorčevalnikov pri določevanju polhlapnih kemičnih agensov v zraku na delovnem mestu. Postopki iz tega dokumenta zagotavljajo rezultate samo za vsoto lebdečih delcev in par. Koncentracija se izračuna kot masa na enoto prostornine. Ta dokument se uporablja za vzorčevalnike s črpanjem in merilne postopke za uporabo teh vzorčevalnikov, v katerih vzorčenje in analiza potekata v ločenih fazah.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-januar-2023
Nadomešča:
SIST EN 13936:2014
Zrak na delovnem mestu - Kemični agensi, prisotni kot zmesi lebdečih delcev in
par - Zahteve za vrednotenje merilnih postopkov z vzorčevalniki (ISO 23861:2022)
Workplace air - Chemical agent present as a mixture of airborne particles and vapour -
Requirements for evaluation of measuring procedures using samplers (ISO 23861:2022)
Luft am Arbeitsplatz - Als Mischung aus luftgetragenen Partikeln und Dampf vorliegender
chemischer Arbeitsstoff - Anforderungen an die Bewertung von Messverfahren mit
Sammlern (ISO 23861:2022)
Air des lieux de travail - Agent chimique présent sous forme de mélange de particules en
suspension dans l’air et de vapeur - Exigences d’évaluation des procédures de mesure
utilisant des dispositifs de prélèvement (ISO 23861:2022)
Ta slovenski standard je istoveten z: EN ISO 23861:2022
ICS:
13.040.30 Kakovost zraka na delovnem Workplace atmospheres
mestu
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN ISO 23861
EUROPEAN STANDARD
NORME EUROPÉENNE
October 2022
EUROPÄISCHE NORM
ICS 13.040.30 Supersedes EN 13936:2014
English Version
Workplace air - Chemical agent present as a mixture of
airborne particles and vapour - Requirements for
evaluation of measuring procedures using samplers (ISO
23861:2022)
Air des lieux de travail - Agent chimique présent sous Luft am Arbeitsplatz - Als Mischung aus luftgetragenen
forme de mélange de particules en suspension dans Partikeln und Dampf vorliegender chemischer
l'air et de vapeur - Exigences d'évaluation des Arbeitsstoff - Anforderungen an die Bewertung von
procédures de mesure utilisant des dispositifs de Messverfahren mit Sammlern (ISO 23861:2022)
prélèvement (ISO 23861:2022)
This European Standard was approved by CEN on 23 September 2022.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 23861:2022 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
European foreword
This document (EN ISO 23861:2022) has been prepared by Technical Committee ISO/TC 146 "Air
quality" in collaboration with Technical Committee CEN/TC 137 “Assessment of workplace exposure to
chemical and biological agents” the secretariat of which is held by DIN.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by April 2023, and conflicting national standards shall be
withdrawn at the latest by April 2023.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN 13936:2014.
Any feedback and questions on this document should be directed to the users’ national standards
body/national committee. A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the
United Kingdom.
Endorsement notice
The text of ISO 23861:2022 has been approved by CEN as EN ISO 23861:2022 without any modification.
INTERNATIONAL ISO
STANDARD 23861
First edition
2022-09
Workplace air — Chemical agent
present as a mixture of airborne
particles and vapour — Requirements
for evaluation of measuring
procedures using samplers
Air des lieux de travail — Agent chimique présent sous forme de
mélange de particules en suspension dans l’air et de vapeur —
Exigences d’évaluation des procédures de mesure utilisant des
dispositifs de prélèvement
Reference number
ISO 23861:2022(E)
ISO 23861:2022(E)
© ISO 2022
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
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii
ISO 23861:2022(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Symbols and abbreviated terms.2
5 Sampler types . . 3
6 Requirements . 3
6.1 General . 3
6.2 Sampler requirements . 3
6.2.1 General . 3
6.2.2 Flow resistance and stability of the air flow . 3
6.2.3 Connecting parts . 3
6.2.4 Pumps . . 4
6.3 Measuring procedure requirements . 4
6.3.1 Sampling procedure requirements . 4
6.3.2 Analytical procedure requirements . 4
6.3.3 Expanded uncertainty . 6
6.3.4 Method description . 6
7 General test conditions .6
7.1 Reagents . 6
7.2 Apparatus . 6
8 Test methods . 6
8.1 Spiking method . 6
8.1.1 General . 6
8.1.2 Deposit of the analyte on the first collection substrate . 6
8.1.3 Deposit of the analyte on the other collection substrates of a type A sampler . 7
8.1.4 Transfer of the analyte . 7
8.2 Evaluation of measuring procedures . 8
8.2.1 General . 8
8.2.2 Storage after sampling . 8
8.3 Uncertainty of the measurement . 9
8.3.1 Calculation of the combined standard uncertainty . 9
8.3.2 Calculation of the expanded uncertainty . 9
9 Test report . 9
Annex A (informative) Physical behaviour of a mixture of airborne particles and vapour .10
Annex B (informative) Possible approaches to sample mixtures of airborne particles and
vapour .14
Annex C (informative) Estimation of uncertainty of measurement .17
Bibliography .20
iii
ISO 23861:2022(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, in collaboration with the European Committee for Standardization (CEN)
Technical Committee CEN/TC 137, Assessment of workplace exposure to chemical and biological agents,
in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna Agreement).
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 23861:2022(E)
Introduction
This document provides a framework for assessing the performance of procedures for measuring a
chemical agent present as a mixture of airborne particles and vapour against the general requirements
for the performance of procedures for measuring chemical agents in workplace atmospheres as
specified in ISO 20581.
This document enables manufacturers, users of samplers, developers and users of procedures for
measuring a chemical agent present as a mixture of airborne particles and vapour to adopt a consistent
approach to method validation.
This document is based on EN 13936.
v
INTERNATIONAL STANDARD ISO 23861:2022(E)
Workplace air — Chemical agent present as a mixture
of airborne particles and vapour — Requirements for
evaluation of measuring procedures using samplers
1 Scope
This document specifies requirements for the evaluation of measuring procedures using samplers for
the determination of a chemical agent present in the workplace atmosphere as a mixture of airborne
particles and vapour.
The procedures given in this document provide results only for the sum of airborne particles and
vapour. The concentration is calculated in terms of mass per unit volume.
NOTE The physical behaviour of a mixture of airborne particles and vapour is described in Annex A.
Examples of substances which can be present in multiple phases are toluene diisocyanate, diethanolamine,
ethyleneglycol and tributylphosphate.
This document can also be applied to complex mixtures, such as metal working fluids or bitumen fumes.
This document is applicable to samplers and measuring procedures using these samplers in which
sampling and analysis are carried out in separate stages.
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 7708, Air quality — Particle size fraction definitions for health-related sampling
ISO 13137, Workplace atmospheres — Pumps for personal sampling of chemical and biological agents —
Requirements and test methods
ISO 18158, Workplace air — Terminology
ISO 20581, Workplace air — General requirements for the performance of procedures for the measurement
of chemical agents
ISO 21832, Workplace air — Metals and metalloids in airborne particles — Requirements for evaluation of
measuring procedures
ISO 22065:2020, Workplace air — Gases and vapours — Requirements for evaluation of measuring
procedures using pumped samplers
EN 13205-1, Workplace exposure — Assessment of sampler performance for measurement of airborne
particle concentrations — Part 1: General requirements
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 terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
ISO 23861:2022(E)
— IEC Electropedia: available at https:// www .electropedia .org/
3.1
mixed-phase sampler
sampler or sampling train that is used to collect airborne particles and vapours onto one or more
collection substrates
[SOURCE: ISO 18158:2016, 2.2.2.1.7, modified — the given cross-references have been removed.]
3.2
joint extraction mode
procedure that simultaneously extracts and analyses all collection substrates contained in the mixed-
phase sampler (3.1), resulting in a unique quantification of the analyte for each air sample
3.3
separate extraction mode
procedure that separately extracts and analyses the collection substrates contained in the mixed-phase
sampler (3.1), resulting in multiple quantifications for each air sample that are summed to give the final
result
4 Symbols and abbreviated terms
NOTE For symbols used for calculation of combined standard uncertainty see C.2.
U.S. EPA is the United States environmental protection agency
k is the coverage factor
K
is the coefficient of variation
v
LV is the limit value
m
is the minimum mass which shall be quantified
min
m
is the mass determined on the collection substrate for airborne particles, in milligrams;
p
m
is the mass determined on the collection substrate for vapour, in the same unit as for m .
v
p
N is the number of extractions realized to analyse all collection substrates, control sections excluded
Q is the recommended air flow rate of the mixed-phase sampler
R
is the analytical recovery
an
RH is the relative humidity
SVOC is a semi-volatile organic compound
t
is the minimum sampling time
min
u
is the combined standard uncertainty
c
U is the expanded uncertainty
γ
is the distribution coefficient for airborne particles, in percentage;
d,p
γ
is the distribution coefficient for vapour, in percentage;
d,v
ρ
is the limit value considered
LV
x is the fraction of LV
ISO 23861:2022(E)
5 Sampler types
Samplers are classified based on differences in the collection substrate because of differences in the
analytical procedures.
Where the vapour phase is collected on a sorbent bed, the mixed-phase sampler is classified as type A
sampler.
Where the vapour phase is collected on an impregnated filter, the mixed-phase sampler is classified as
type B sampler.
NOTE Other systems, for example denuder and filter or impinger and filter, can be used alternatively for
specific chemical agents. See Annex B.
6 Requirements
6.1 General
The measuring procedure used shall comply with the requirements of ISO 20581 and those clauses of
ISO 13137, ISO 21832, ISO 22065 and EN 13205-1 which apply.
When the use of a sampler for measurement of a particular mixture of airborne particles and vapour is
claimed, the sampler shall meet the requirements specified in 6.2. Measuring procedures shall meet the
requirements specified in 6.3.
Known or suspected interferences as well as the results of any tests performed to evaluate interferences,
including suitable and sufficient information to minimize their effects shall be presented in the method
description as required by 6.3.4.
6.2 Sampler requirements
6.2.1 General
The sampler shall comply with the general requirements given in EN 13205-1 and with the performance
requirements for pumped samplers prescribed in ISO 22065:2020, 6.2.2 to 6.2.6.
6.2.2 Flow resistance and stability of the air flow
The back pressure of the mixed-phase sampler shall not exceed the maximum values specified for the
pump performance test in ISO 13137, unless the combination of mixed-phase sampler and pump has
been tested and shown to be able to sample for the required sampling period.
The air flow through the sampling train associated with the pump shall be measured over the entire
sampling period and not deviate more than 5 % as specified in ISO 13137.
Pumps used with size-selective mixed-phase samplers shall also meet the requirements of the pump
pulsation test as specified in ISO 13137.
6.2.3 Connecting parts
The volume of any connecting parts between collection substrates within the mixed-phase sampler
shall be kept to a minimum and any connection shall be made of an inert material that
— does not retain the chemical agent of interest,
— does not react with the chemical agent of interest,
— does not emit chemical agents that can interfere with the one of interest, and
ISO 23861:2022(E)
— is resistant to solvents, if applicable.
6.2.4 Pumps
Pumps used in the measuring procedure shall conform with ISO 13137.
6.3 Measuring procedure requirements
6.3.1 Sampling procedure requirements
6.3.1.1 General
Measuring procedures shall specify the use of a mixed-phase sampler designed to collect the inhalable
fraction of airborne particles, as defined in ISO 7708, and vapour.
The requirements specified in ISO 22065:2020, 6.3.1, shall apply according to the types of collection
substrates that are used in the mixed-phase sampler.
NOTE Due to the particularity of mixed-phase samplers, some requirements are adapted from ISO 22065 as
given in 6.3.1.2 and 6.3.1.3.
6.3.1.2 Air flow rate
For type A samplers, the air flow rate constrained by the particle-size selector of the sampler should not
exceed the maximal air flow rate of the sorbent tube. If not, the air flow should be split to achieve this
requirement.
For type B samplers, the maximum air flow rate to ensure complete sampling according to
ISO 22065:2020, 6.3.1.3.1, shall comply with the air flow rate required by the particle-size selector used.
6.3.1.3 Storage condition after sampling
When tested in accordance with the procedure prescribed in 8.2.2, the mean analytical recovery after
storage shall not differ by more than 10 % from the value before storage.
6.3.2 Analytical procedure requirements
6.3.2.1 General
The requirements given in ISO 22065:2020, 6.3.2, shall apply according to the types of collection
substrates that are used in the mixed-phase sampler.
NOTE Due to the particularity of mixed-phase samplers, some requirements are adapted from ISO 22065 as
stated in 6.3.2.2 to 6.3.2.5.
6.3.2.2 Extraction of the collection substrates
The extraction procedure shall ensure that all phases are extracted and presented for analysis of total
mass of the analyte(s) of interest.
When collection substrates are extracted and analysed separately, the masses determined on each
collection substrate shall not be interpreted as an accurate separation of a particle fraction or vapour
ISO 23861:2022(E)
fraction as these fractions were not stabilized during the sampling period and thus, transfer can occur
between collection substrates.
NOTE A preponderance of analyte on the portion of the sampler intended for either particulate or vapour
collection can give valuable guidance regarding the environment and the control measures, including respiratory
protection measures, which can be needed for implementation. Samplers which consist of a filter and adsorbent
are not able to give an accurate assessment of partition, but samplers have been and are being designed to
provide more accurate information.
6.3.2.3 Analytical limit of quantification
The analytical limit of quantification shall be lower than or equal to m . The minimum mass of
min
analyte m that would be collected for the minimum air sample volume specified in the measuring
min
procedure at the following concentrations is calculated by Formula (1):
x⋅ρ
()
LV
m = ⋅⋅Qt (1)
min min
N
where
m
is the minimum mass which shall be quantified;
min
x
is the fraction of LV considered as follows:
— x=01, for substances with long-term limit value, and
— x=05, for substances with short-term limit value;
ρ
is the limit value considered;
LV
N is the number of extractions realized to analyse all collection substrates, control sections
excluded;
Q is the recommended air flow rate of the mixed-phase sampler;
t
is the minimum sampling time.
min
6.3.2.4 Analytical recovery
For extraction when tested in accordance with ISO 22065:2020, 8.3.2.2.3, the analytical recovery R
an
shall be ≥75 % with K ≤ 10 % at each loading.
v
The values given for analytical recovery are targets; lower values may be used provided equivalent
precision is achieved.
6.3.2.5 Blank value
In order to obtain acceptable values for the limit of quantification of the method, the blank values of the
collection substrates should be as low as technically possible.
When tested in accordance with ISO 22065:2020, 8.3.2.3, the total of the blank values shall be less than
one-tenth of the mass calculated by Formula (1).
NOTE Higher blank values can be allowed provided the requirement of 6.3.2.3 is met.
Where it is known that a blank value is significant and varies between batches of samplers, it shall be
checked for each batch.
ISO 23861:2022(E)
6.3.3 Expanded uncertainty
When tested in accordance with ISO 22065:2020, 8.3, the expanded uncertainty of the measuring
procedure as a whole, including the measurement of airborne particles and vapour, shall comply with
the requirements of ISO 20581. For the uncertainty budget of the airborne particles, the numbers given
for inhalable samplers in ISO 21832:2018, C.3.4, can be used.
When fractions are analysed separately, the expanded uncertainty can be calculated according to
Clause C.3.
6.3.4 Method description
ISO 22065:2020, 6.3.4, shall apply.
7 General test conditions
7.1 Reagents
Use only reagents of recognized analytical grade.
7.2 Apparatus
Test equipment as stated in ISO 22065:2020, 7.2.2 to 7.2.7, shall be used except for 7.2.3.
NOTE 1 A dynamic system for generating, pre-mixing and delivering a known concentration of a test
atmosphere that contains known concentrations of vapour and particles of a semi-volatile compound is
technically difficult to obtain compared to a test atmosphere containing only vapour as prescribed in ISO 22065.
The apparatus described in ISO 22065:2020, 7.2.3, can be used to generate the test atmospheres of pure air in the
climatic conditions required by the tests.
NOTE 2 Test atmospheres generated at high concentrations tend to bias towards the aerosol phase compared
to lower concentrations that can be observed in the workplace; therefore, it is important that the concentrations
in the test atmosphere are relevant to the sampling situations at workplaces.
8 Test methods
8.1 Spiking method
8.1.1 General
The spiking method allows the deposit of the analyte on the collection substrates under controlled
conditions. Only if no standard atmosphere chamber for mixtures of vapour and aerosols is available
the spiking method described in 8.1.2 shall be used.
Tests prescribed in 8.2 need the analyte to be spiked on the collection substrates. Due to the semi-
volatile characteristic of the analyte, this spiking shall be made as required by 8.1.2 to 8.1.4.
8.1.2 Deposit of the analyte on the first collection substrate
8.1.2.1 Type A samplers
The first collection substrate of a type A sampler is a filter. A deposit of the analyte in the form of a spot
with micropipette or syringe shall be avoided due to the dramatic reduction of the evaporation surface
in comparison with the one presented by the micrometric airborne particles collected on the surface of
the filter during the sampling period. If so, the transfer of the analyte from the filter to the sorbent bed
will not be realistic.
ISO 23861:2022(E)
The analyte shall be deposited on the filter by a syringe with a volume of solution that permits to wet
80 % to 90 % of the front surface of the filter. To do so, the analyte can be diluted in a non-interfering
solvent to deliver the appropriate mass of analyte on the collection substrate.
To prevent any loss of the analyte of interest, a volatile solvent should be used that evaporates at room
temperature within a short period. If this is not possible, the solvent used shall not interfere with the
sorbent bed or the analytical method.
8.1.2.2 Type B samplers
As far as possible, the analyte shall be homogeneously deposited on the impregnated filter to ensure
that the analyte can react with the reagent of impregnation.
The analyte can be diluted in a non-interfering solvent to deliver the appropriate mass of analyte on the
collection substrate.
8.1.3 Deposit of the analyte on the other collection substrates of a type A sampler
During tests regarding the analytical method (see ISO 22065:2020, 8.3.2.1), the analytical recovery
(see ISO 22065:2020, 8.3.2.2), the verification of sampler capacity (see ISO 22065:2020, 8.3.1.1) and the
subsequent collection substrates of a type A sampler, which are sorbent beds, require to be spiked.
The spiking of those collection substrates may preferentially be realized by adding a known mass of
analyte corresponding to the required loading of the corresponding test into a small vessel (e.g. empty
sampling tube, pipette reservoir), using a micropipette or syringe. The analyte can be pure or diluted
in a solvent (usually the desorption solvent). The vessel shall be heated enough to permit the rapid
volatilisation of the mass of analyte deposited inside, while air is sampled from the vessel by pumping
onto the collection substrate (recommended flow rate and sampling time shall be used). Check that all
the analyte has evaporated after sampling by rinsing the vessel and any connections with desorption
solvent and analysing the rinsate.
In the case where this technique is not suitable due to the physical properties of the analyte, the analyte
can be spiked directly in the sorbent bed by a micropipette or syringe and diluting in a non-interfering
solvent, if necessary.
8.1.4 Transfer of the analyte
In function of the extraction method and the type of the sampler, air shall be sampled through the
sampler during or after the spike to allow the analyte to be transferred through all the collection
substrate as it does during a sampling session.
Whatever the sampler type, the tests regarding the limit of quantification (see ISO 22065:2020,
8.3.2.1), the recovery (see ISO 22065:2020, 8.3.2.2), and the evaluation of the conditions of storage (see
ISO 22065:2020, 8.3.1.6.1), require to pump pure air through the samplers at (20 ± 2) °C and a relative
humidity of (50 ± 5) % during the recommended sampling time at the recommended flow rate.
The sampler capacity verification test (see ISO 22065:2020, 8.3.1.2) requires pumping pure air
through the samplers at the recommended maximum flow rate at (20 ± 2) °C and a relative humidity of
(80 ± 5) %.
Table 1 summarizes the spiking and transfer conditions in function of the required tests and the
extraction mode used.
ISO 23861:2022(E)
Table 1 — Spiking and transfer conditions in function of the required tests and the extraction
mode
Joint extraction mode Separate extraction mode
Tests
First collection Subsequent collec- First collection Subsequent collec-
substrate tion substrates substrate tion substrates
ISO 22065:2020,
Spike and pump air at (20 ± 2) °C and Spike and pump air at (20 ± 2) °C and
8.3.1.2
(80 ± 5) %RH (80 ± 5) %RH
Sampler capacity
ISO 22065:2020,
Spike and pump air Spike and pump air
8.3.1.6.1
Spike at (20 ± 2) °C and Spike at (20 ± 2) °C and
(80 ± 5) %RH (80 ± 5) %RH
Storage conditions
ISO 22065:2020,
Spike and pump air
8.3.2.1 Spike and pump air at (20 ± 2) °C and
Spike at (20 ± 2) °C and
Limit of quantifica- (50 ± 5) %RH
(50 ± 5) %RH
tion
ISO 22065:2020,
Spike and pump air Spike and pump air
8.3.2.2
Spike at (20 ± 2) °C and Spike at (20 ± 2) °C and
(50 ± 5) %RH (50 ± 5) %RH
Analytical recovery
The temperature chosen should be a temperature considered normal for workplaces and this can vary
from the recommended temperature given in ISO 22065.
8.2 Evaluation of measuring procedures
8.2.1 General
Perform the tests given in ISO 22065:2020, Clause 8, using the procedure and conditioned air prescribed
in 8.1 rather than sampling a known concentration of vapour as required in ISO 22065, except for the
storage test (see 8.2.2).
8.2.2 Storage after sampling
Perform storage tests on samples according to ISO 22065:2020, 8.3.1.6.1, then stabilize the collection
substrate as prescribed in the sampling method and verify that the analytical recovery determined
from the combined results from the collection substrate for airborne particles and the collection
substrate for vapour meets the requirements of 6.3.1.3.
Multiple methods can be used and combined as needed to stabilize the analyte on the collection
substrates (see also B.6):
— close without leakage the sampler train, allowing vapour to be passively collected on sorbent bed or
impregnated collection substrate,
— close without leakage each collection substrates individually,
— cool the collection substrates below 4 °C,
— transfer the analyte collected on the first filter of a type A sampler to the sorbent bed by pumping
additional pure air through the sampler train, until complete transfer, and
— extract the analyte right after the sampling session.
— place in a black box in case of photo-sensitive analyte.
ISO 23861:2022(E)
8.3 Uncertainty of the measurement
8.3.1 Calculation of the combined standard uncertainty
Calculate the combined standard uncertainty u taking into account the relevant uncertainty
c
components associated with airborne particles and vapour, according to Annex C.
8.3.2 Calculation of the expanded uncertainty
Calculate the expanded uncertainty of the measuring procedure, U , using a coverage factor k = 2,
according to Formula (2):
Uu=×2 (2)
c
9 Test report
The test report shall contain at least the following information:
a) a reference to this document, i.e. ISO 23861:2022;
b) detailed description and identification of the sampling system components tested, including
all collection substrates and for commercial devices name of manufacturer(s) and product
identification(s);
c) complete identification of test atmospheres used plus details of independent measuring methods,
where used;
d) details of the pump(s) used for testing;
e) details of analytical methods used for testing;
f) determined values for recovery efficiency, blank value, sampler capacity and storage losses;
g) statistical analyses of the test results and calculations of expanded uncertainty;
h) statement of whether the acceptance criteria are met;
i) any unusual features noted during the determinations;
j) any operations not included in this document that can have influence on the results;
k) the technical justification for omitting or altering any of the tests, if done;
l) the date of test report and testing period.
ISO 23861:2022(E)
Annex A
(informative)
Physical behaviour of a mixture of airborne particles and vapour
A.1 Generation of a mixture of airborne particles and vapour
The behaviour of a mixture of airborne particles and vapour at workplace air has been studied (see
Reference [1] to [3]). Theoretical models which can calculate the behaviour of such a mixture can
be found in the literature, but they are limited to the conditions underlying the mixture which are
unknown in most cases of workplace atmospheres.
Semi-volatile compounds are present as a mixture of airborne particles and vapour in workplace air.
It is essential that the physical characteristics of the chemical agent of interest are investigated to
characterize the state of the chemical agent at the workplace. Even if semi-volatile compounds have
low vapour pressure at room temperature, volatility increases with increasing process temperature, so
that the process can result in forming aerosol-vapour mixtures. The sampling of a mixture of airborne
particles and vapour is strongly influenced by the sampling conditions (e.g. sampling time, flow rate)
and environmental conditions (temperature and pressure).
At room temperature, most semi-volatile compounds are liquids but there are also solids with a
significant vapour pressure (e.g. arsenic trioxide). At room temperature, semi-volatile compounds
normally have quite a low vapour pressure; nevertheless, the way in which a compound is used in the
workplace can result in forming droplet-vapour-mixtures. There are two principal mechanisms by
which a mixture of airborne particles and vapour is formed:
— A: partial evaporation of chemical agents used as a liquid or solid;
EXAMPLE 1 Processes in which liquids are nebulised during the machining of metals, ceramics etc., processes
in which mists are generated by gas-bubbles breaking on the surface of liquids (e.g. electroplating) and liquid
spraying processes (e.g. paint spraying).
— B: condensation of a chemical agent in thermal processes in which a semi-volatile compound
evaporates and, subsequently cools down to ambient temperature.
EXAMPLE 2 Hot bitumen application, laser cutting and metalworking processes.
A.2 Theoretical identification of the semi-volatile behaviour of a chemical agent
There is no generally accepted definition of semi-volatile compounds. The U.S. EPA defined a semi-
volatile organic compound (SVOC) as a compound having a boiling point ranging from 240 °C to 400 °C.
The advantage of this definition is that boiling point is available for almost all compounds present in
the workplace atmospheres. EN 13936 defined a SVOC with the vapour pressure of the compounds,
ranging from 0,001 Pa to 100 Pa. The advantage of this definition is that saturated vapour pressure
is the real parameter that governs the evaporation of a chemical agent rather than the boiling point.
Disadvantage is that the vapour pressure is not available for many substances. EN 13936 also indicates
that this corresponds to a range for the boiling point from about 180 °C to about 350 °C.
Figure A.1 presents the saturated vapour pressure of 254 compounds registered in the Metropol
database (see Reference [8]), according to their boiling point. Volatile compounds show a good
correlation between those parameters. As the volatility decreases, this correlation becomes less clear,
likely resulting from the difficulty of making measurements of low vapour pressure.
Experience in recent years has shown that the limits for vapour pressure originally set in EN 13936
were well chosen for semi-volatile materials, but that the limits for the boiling point range are too
ISO 23861:2022(E)
broad. From the literature, it can be derived that significant amounts of droplet-vapour-mixtures only
occur from a boiling temperature of about 200 °C and that substances with boiling points above 320 °C
at room temperature only have a low vapour content.
Key
X boiling point at atmospheric pressure, in °C
Y saturated vapour pressure at 20 °C to 25 °C, in Pa
temperature range for semi-volatile compounds according to the U.S. EPA
saturated vapour pressure range for semi-volatile compounds according to EN 13936
compound (data point)
Figure A.1 — Saturated vapour pressure in function of the boiling point of 254 compounds
registered in the Metropol database (see Reference [8])
A.3 Experimental determination of the semi-volatile behaviour of a chemical
agent
A.3.1 General
When saturated vapour pressure is not available in the literature, the theoretical considerations above
cannot be applied. Thus, an experimental protocol is proposed to determine if a chemical agent should
be sampled and collected as a mixture of parti
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