ISO/FDIS 7012-3
(Main)Paints and varnishes — Determination of preservatives in water-dilutable coating materials — Part 3: Determination of in-can isothiazolinones with LC-UV and LC-MS
Paints and varnishes — Determination of preservatives in water-dilutable coating materials — Part 3: Determination of in-can isothiazolinones with LC-UV and LC-MS
Peintures et vernis — Dosage des agents de préservation dans les produits de peinture diluables à l’eau — Partie 3: Dosage des isothiazolinones en pot par CL-UV et CL-SM
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FINAL DRAFT
International
Standard
ISO/TC 35/SC 16
Paints and varnishes —
Secretariat: DIN
Determination of preservatives in
Voting begins on:
water-dilutable coating materials —
2025-01-01
Part 3:
Voting terminates on:
2025-02-26
Determination of in-can
isothiazolinones with LC-UV and LC-
MS
Peintures et vernis — Dosage des agents de préservation dans les
produits de peinture diluables à l’eau —
Partie 3: Dosage des isothiazolinones en pot par CL-UV et CL-SM
RECIPIENTS OF THIS DRAFT ARE INVITED TO SUBMIT,
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Reference number
FINAL DRAFT
International
Standard
ISO/TC 35/SC 16
Paints and varnishes —
Secretariat: DIN
Determination of preservatives in
Voting begins on:
water-dilutable coating materials —
Part 3:
Voting terminates on:
Determination of in-can
isothiazolinones with LC-UV and LC-
MS
Peintures et vernis — Dosage des agents de préservation dans les
produits de peinture diluables à l’eau —
Partie 3: Dosage des isothiazolinones en pot par CL-UV et CL-SM
RECIPIENTS OF THIS DRAFT ARE INVITED TO SUBMIT,
WITH THEIR COMMENTS, NOTIFICATION OF ANY
RELEVANT PATENT RIGHTS OF WHICH THEY ARE AWARE
AND TO PROVIDE SUPPOR TING DOCUMENTATION.
© ISO 2025
IN ADDITION TO THEIR EVALUATION AS
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO-
ISO/CEN PARALLEL PROCESSING
LOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
INTERNATIONAL STANDARDS MAY ON OCCASION HAVE
the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below
TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL
or ISO’s member body in the country of the requester.
TO BECOME STAN DARDS TO WHICH REFERENCE MAY BE
MADE IN NATIONAL REGULATIONS.
ISO copyright office
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Published in Switzerland Reference number
ii
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Apparatus . 2
5.1 General .2
5.2 Equipment for extraction and sample preparation .2
5.3 LC-UV/VIS system . .3
5.4 LC-MS/MS or LC-MS system .3
6 Reagents and materials . 3
7 Sampling . 5
8 Procedure . 5
8.1 General .5
8.2 LC-UV/VIS method .5
8.2.1 Extraction of LC-UV/VIS .5
8.2.2 Operation conditions of LC-UV/VIS .6
8.2.3 Blank .6
8.2.4 Interferences of LC-UV/VIS .6
8.2.5 Calibration of LC-UV/VIS . .6
8.2.6 Determination by LC-UV/VIS .7
8.3 LC-MS method .7
8.3.1 Extraction of LC-MS .7
8.3.2 Further dilution . .7
8.3.3 Filtration .8
8.3.4 Operation conditions of LC-MS .8
8.3.5 Blank .8
8.3.6 Interferences of LC-MS .8
8.3.7 Calibration of LC-MS .8
8.3.8 Determination by LC-MS .9
9 Calculation . 9
10 Precision . 10
10.1 General .10
10.2 Repeatability limit, r . .10
10.3 Reproducibility limit, R .10
11 Test report . 10
Annex A (informative) Example of LC conditions .12
Annex B (informative) Example of multiple reaction monitoring LC-MS/MS conditions .15
Annex C (normative) Calculation of preservative content with standard addition for LC-MS
method .18
Annex D (informative) Mechanical method for homogenization and extraction.20
Annex E (informative) Results of the interlaboratory test .21
Bibliography .23
iii
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 document 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).
ISO draws attention to the possibility that the implementation of this document may involve the use of (a)
patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed patent
rights in respect thereof. As of the date of publication of this document, ISO had not received notice of (a)
patent(s) which may be required to implement this document. However, implementers are cautioned that
this may not represent the latest information, which may be obtained from the patent database available at
www.iso.org/patents. ISO shall not be held responsible for identifying any or all such patent rights.
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 35, Paints and varnishes, Subcommittee SC 16,
Chemical analysis, in collaboration with the European Committee for Standardization (CEN) Technical
Committee CEN/TC 139, Paints and varnishes, in accordance with the Agreement on technical cooperation
between ISO and CEN (Vienna Agreement).
A list of all parts in the ISO 7012 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
FINAL DRAFT International Standard ISO/FDIS 7012-3:2024(en)
Paints and varnishes — Determination of preservatives in
water-dilutable coating materials —
Part 3:
Determination of in-can isothiazolinones with LC-UV and LC-MS
1 Scope
This document specifies the apparatus and the anal
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ISO TC 35/SC 16/WG 1
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Secretariat: DIN
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Paints and varnishes — Determination of preservatives in water-dilutable coating
materials —
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Part 3: Determination of in-can isothiazolinones with LC-UV and LC-MS
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All rights reserved. Unless otherwise specified, or required in the context of its implementation, no
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part of this publication may be reproduced or utilized otherwise in any form or by any means,
Kingdom)
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
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Kingdom)
CP 401 • CH-1214 Vernier, Geneva
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Phone: + 41 22 749 01 11
Kingdom)
Email: copyright@iso.orgcopyright@iso.org
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Kingdom)
Website: www.iso.orgwww.iso.org
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Published in Switzerland.
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ii © ISO 2024 – All rights reserved
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Contents
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Foreword . iviv
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1 Scope . 11
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2 Normative references . 11
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3 Terms and definitions . 11
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4 Principle . 22
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5 Apparatus . 22
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6 Reagents and materials . 44
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7 Sampling . 55
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8 Procedure . 55
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9 Calculation . 99
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10 Precision . 10 .
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11 Test report . 11
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Annex A (informative) Example of LC conditions . 1212
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A.1 Instrument parameters . 1212
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A.2 Detection limits of instrument for LC-UV/VIS method . 1313
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A.3 Examples of typical chromatograms by LC . 1313
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Annex B (informative) Example of multiple reaction monitoring LC-MS/MS conditions . 1717
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B.1 Instrument parameters . 1717
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B.2 Typical MRM conditions and detection limits of instrument . 1818
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method . 22
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Annex D (informative) Mechanical method for homogenization and extraction . 24
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D.1 Apparatus . 24
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D.2.1 Homogenization and extraction with the aid of a stirrer and an ultrasonic water bath . 24
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D.2.2 Homogenization and extraction with the aid of a stirrer . 24
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Annex E (informative) Results of the interlaboratory test . 25
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Bibliography . 2727
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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 document should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directiveswww.iso.org/directives).
ISO draws attention to the possibility that the implementation of this document may involve the use of
(a) patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed
patent rights in respect thereof. As of the date of publication of this document, ISO had not received notice
of (a) patent(s) which may be required to implement this document. However, implementers are
cautioned that this may not represent the latest information, which may be obtained from the patent
database available at www.iso.org/patents.www.iso.org/patents. ISO shall not be held responsible for
identifying any or all such patent rights.
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.htmlwww.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 35, Paints and varnishes, Subcommittee
SC 16, Chemical analysis, in collaboration with the European Committee for Standardization (CEN)
Technical Committee CEN/TC 139, Paints and varnishes, in accordance with the Agreement on technical
cooperation between ISO and CEN (Vienna Agreement).
A list of all parts in the ISO 7012 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.htmlwww.iso.org/members.html.
Formatted: Line spacing: Exactly 11 pt
Formatted: Font: 11 pt
iv © ISO 2024 – All rights reserved
FINAL DRAFT International Standard ISO/FDIS 7012-3:2024(en)
Formatted: Centered
Formatted: Section start: New page, Different first page
header
Paints and varnishes — Determination of preservatives in water-
Formatted: Space After: 38 pt
dilutable coating materials —
Part 3: Determination of in-can isothiazolinones with LC-UV and
LC-MS
1 Scope
This document specifies the apparatus and the analytical methodmethods for determining the content of
in-can isothiazolinone preservatives in water-dilutable coating materials or related products.
This document is also applicable forto polymer dispersions. This document is generally applicable for n-
Formatted: Body Text, Tab stops: Not at 0.7 cm + 1.4
octyl-4-isothiazolin-3-one (OIT) and 4,5-dichloro-n-octyl-4-isothiazolin-3-one (DCOIT). However, the
cm + 2.1 cm + 2.8 cm + 3.5 cm + 4.2 cm + 4.9 cm +
standard was not validated for these compounds in the interlaboratory test. There are national standards 5.6 cm + 6.3 cm + 7 cm
covering these compounds.
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 1513, Paints and varnishes — Examination and preparation of test samples
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 15528, Paints, varnishes and raw materials for paints and varnishes — Sampling
3 Terms and definitions
For the purposes of this document, the following terms and definitions 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/obphttps://www.iso.org/obp
— IEC Electropedia: available at https://www.electropedia.org/https://www.electropedia.org/
3.1
ready for use
state of a product when it is mixed in accordance with the manufacturer’s instructions in the correct
proportions and thinned if required using the correct thinners so that it is ready for application by the
approved method
Formatted: std_section
[SOURCE: ISO 11890-2:2020, 3.7]
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3.2
stops: 17.2 cm, Right
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water-dilutable coating material
water-reducible coating material
Formatted: Font: Bold
water-based coating material
Formatted: Font: Bold
water-borne coating material
Formatted: Font: Bold
water-thinnable coating material
DEPRECATED: water paint
Formatted: Font: Bold
coating material whose viscosity is reduced by the addition of water
[SOURCE: ISO 4618:2023, 3.272]
Formatted: std_section
3.3
detection limit of instrument
three times the standard deviation of the result obtained in the blank test using a specific instrument
[SOURCE: ISO 8124-5: 2015, 3.5]
Formatted: std_section
3.4
in-can preservative
biocide used to prevent growth of microorganisms during storage of a stock solution of a coating material
or water-based coating material (3.2)
Formatted: Font: Not Italic
Formatted: cite_sec
[SOURCE: ISO 4618:2023, 3.141]
Formatted: std_section
4 Principle
The sample is extracted with suitable dilution solvent using an appropriate homogenization
...
PROJET FINAL
Norme
internationale
ISO/TC 35/SC 16
Peintures et vernis — Dosage des
Secrétariat: DIN
agents de préservation dans les
Début de vote:
produits de peinture diluables à
2025-01-01
l’eau —
Vote clos le:
2025-02-26
Partie 3:
Dosage des isothiazolinones en pot
par CL-UV et CL-SM
Paints and varnishes — Determination of preservatives in water-
dilutable coating materials —
Part 3: Determination of in-can isothiazolinones with LC-UV and
LC-MS
LES DESTINATAIRES DU PRÉSENT PROJET SONT
INVITÉS À PRÉSENTER, AVEC LEURS OBSERVATIONS,
NOTIFICATION DES DROITS DE PROPRIÉTÉ DONT ILS
AURAIENT ÉVENTUELLEMENT CONNAISSANCE ET À
FOURNIR UNE DOCUMENTATION EXPLICATIVE.
OUTRE LE FAIT D’ÊTRE EXAMINÉS POUR
ÉTABLIR S’ILS SONT ACCEPTABLES À DES FINS
INDUSTRIELLES, TECHNOLOGIQUES ET COM-MERCIALES,
AINSI QUE DU POINT DE VUE DES UTILISATEURS, LES
PROJETS DE NORMES
TRAITEMENT PARALLÈLE ISO/CEN
INTERNATIONALES DOIVENT PARFOIS ÊTRE CONSIDÉRÉS
DU POINT DE VUE DE LEUR POSSI BILITÉ DE DEVENIR DES
NORMES POUVANT
SERVIR DE RÉFÉRENCE DANS LA RÉGLEMENTATION
NATIONALE.
Numéro de référence
PROJET FINAL
Norme
internationale
ISO/TC 35/SC 16
Peintures et vernis — Dosage
Secrétariat: DIN
des agents de préservation
Début de vote:
dans les produits de peinture
2025-01-01
diluables à l’eau —
Vote clos le:
2025-02-26
Partie 3:
Dosage des isothiazolinones en pot
par CL-UV et CL-SM
Paints and varnishes — Determination of preservatives in water-
dilutable coating materials —
Part 3: Determination of in-can isothiazolinones with LC-UV
and LC-MS
LES DESTINATAIRES DU PRÉSENT PROJET SONT
INVITÉS À PRÉSENTER, AVEC LEURS OBSERVATIONS,
NOTIFICATION DES DROITS DE PROPRIÉTÉ DONT ILS
AURAIENT ÉVENTUELLEMENT CONNAISSANCE ET À
FOURNIR UNE DOCUMENTATION EXPLICATIVE.
DOCUMENT PROTÉGÉ PAR COPYRIGHT
OUTRE LE FAIT D’ÊTRE EXAMINÉS POUR
ÉTABLIR S’ILS SONT ACCEPTABLES À DES FINS
© ISO 2025 INDUSTRIELLES, TECHNOLOGIQUES ET COM-MERCIALES,
AINSI QUE DU POINT DE VUE DES UTILISATEURS, LES
Tous droits réservés. Sauf prescription différente ou nécessité dans le contexte de sa mise en œuvre, aucune partie de cette
PROJETS DE NORMES
TRAITEMENT PARALLÈLE ISO/CEN
INTERNATIONALES DOIVENT PARFOIS ÊTRE CONSIDÉRÉS
publication ne peut être reproduite ni utilisée sous quelque forme que ce soit et par aucun procédé, électronique ou mécanique,
DU POINT DE VUE DE LEUR POSSI BILITÉ DE DEVENIR DES
y compris la photocopie, ou la diffusion sur l’internet ou sur un intranet, sans autorisation écrite préalable. Une autorisation peut
NORMES POUVANT
être demandée à l’ISO à l’adresse ci-après ou au comité membre de l’ISO dans le pays du demandeur.
SERVIR DE RÉFÉRENCE DANS LA RÉGLEMENTATION
NATIONALE.
ISO copyright office
Case postale 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Genève
Tél.: +41 22 749 01 11
E-mail: copyright@iso.org
Web: www.iso.org
Publié en Suisse Numéro de référence
ii
Sommaire Page
Avant-propos .iv
1 Domaine d’application . 1
2 Références normatives . 1
3 Termes et définitions . 1
4 Principe. 2
5 Appareillage . 2
5.1 Généralités .2
5.2 Équipement d’extraction et de préparation des échantillons.3
5.3 Système de CL-UV/VIS .3
5.4 Système de CL-SM/SM ou de CL-SM .3
6 Réactifs et matériaux . 4
7 Échantillonnage . 5
8 Mode opératoire . 5
8.1 Généralités .5
8.2 Méthode CL-UV/VIS .5
8.2.1 Extraction pour la CL-UV/VIS.5
8.2.2 Conditions opératoires de la CL-UV/VIS .6
8.2.3 Blanc .6
8.2.4 Interférences de CL-UV/VIS .6
8.2.5 Étalonnage de la CL-UV/VIS .6
8.2.6 Détermination par CL-UV/VIS .7
8.3 Méthode CL-SM .7
8.3.1 Extraction pour la CL-SM . .7
8.3.2 Dilution supplémentaire .8
8.3.3 Filtration .8
8.3.4 Conditions opératoires de la CL-SM .8
8.3.5 Blanc .8
8.3.6 Interférences de CL-SM . . .8
8.3.7 Étalonnage de la CL-SM .9
8.3.8 Dosage par LC-MS .10
9 Calcul .10
10 Fidélité . 10
10.1 Généralités .10
10.2 Limite de répétabilité, r .10
10.3 Limite de reproductibilité, R .11
11 Rapport d’essai .11
Annexe A (informative) Exemple de conditions de CL .12
Annexe B (informative) Exemple de conditions de CL-SM/SM en mode MRM .15
Annexe C (normative) Calcul de la teneur en agent de préservation avec ajout dosépour la
méthode CL-SM .18
Annexe D (informative) Méthode mécanique d’homogénéisation et d’extraction .20
Annexe E (informative) Résultats de l’essai interlaboratoires .21
Bibliographie .23
iii
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
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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’ISO attire l’attention sur le fait que la mise en application du présent document peut entraîner l’utilisation
d’un ou de plusieurs brevets. L’ISO ne prend pas position quant à la preuve, à la validité et à l’applicabilité de
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il y a lieu d’avertir les responsables de la mise en application du présent document que des informations
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Les appellations commerciales éventuellement mentionnées dans le présent document sont données pour
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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 ISO/TC 35, Peintures et vernis, sous-comité SC 16, Analyse
chimique, en collaboration avec le comité technique CEN/TC 139, Peintures et vernis, du Comité européen de
normalisation (CEN), conformément à l’Accord de coopération technique entre l’ISO et le CEN (Accord de
Vienne).
Une liste de toutes les parties de la série ISO 7012 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 normalisati
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