ISO/FDIS 7012-1
(Main)Paints and varnishes — Determination of preservatives in water-dilutable coating materials — Part 1: Determination of in-can free formaldehyde
Paints and varnishes — Determination of preservatives in water-dilutable coating materials — Part 1: Determination of in-can free formaldehyde
Peintures et vernis — Dosage des agents de préservation dans les produits de peinture diluables à l’eau — Partie 1: Dosage du formaldéhyde libre en pot
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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 1:
Voting terminates on:
2025-02-26
Determination of in-can free
formaldehyde
Peintures et vernis — Dosage des agents de préservation dans les
produits de peinture diluables à l’eau —
Partie 1: Dosage du formaldéhyde libre en pot
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 1:
Voting terminates on:
Determination of in-can free
formaldehyde
Peintures et vernis — Dosage des agents de préservation dans les
produits de peinture diluables à l’eau —
Partie 1: Dosage du formaldéhyde libre en pot
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
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be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
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Published in Switzerland Reference number
ii
Contents Page
Foreword .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 3
4.1 General .3
4.2 Equilibria of in-can free formaldehyde in the coating matrix .3
4.3 Equilibria of in-can free formaldehyde during extraction .3
4.4 Equilibria of in-can free formaldehyde during derivatization .3
4.5 Principle of Method A: Derivatization with acetylacetone (ACAC) combined with
photometric detection .3
4.5.1 Derivatization with ACAC.3
4.5.2 Detection and quantification with a spectral photometer .4
4.6 Principle of Method B: Derivatization with dinitrophenylhydrazine (DNPH) combined
with liquid chromatography (LC) separation and UV/VIS detection .4
4.6.1 Derivatization with DNPH .4
4.6.2 Separation, detection and quantification with LC-UV/VIS .4
4.7 Principle of Method C: Liquid chromatography (LC) separation followed by post-
column derivatization with ACAC and subsequent quantification with UV/VIS detection .4
4.7.1 Separation of free formaldehyde by liquid chromatography .4
4.7.2 Post-column derivatization with acetylacetone (ACAC) and quantification with
UV/VIS detection .4
5 Apparatus . 4
5.1 General .4
5.2 General apparatus .4
5.3 Apparatus for extraction .4
5.4 Apparatus for method A .5
5.5 Apparatus for method B .5
5.5.1 LC [HPLC or ultra-performance liquid chromatography (UHPLC)] system .5
5.5.2 Appropriate column .5
5.5.3 Vials .5
5.6 Apparatus for method C .6
5.6.1 LC [HPLC or ultra-performance liquid chromatography (UHPLC)] system with
post-column reactor .6
5.6.2 Appropriate column (e.g. RPC8, RPC18 column) .6
6 Reagents and materials . 6
6.1 General .6
6.2 General reagents .6
6.2.1 Demineralized water .6
6.2.2 Formaldehyde solution .6
6.2.3 Formaldehyde stock solution .6
6.2.4 Formaldehyde working solutions for calibration .6
6.2.5 Carrez solutions (optional) .7
6.3 Method A: Reagents for derivatization with ACAC .7
6.4 Method B: Reagents for derivatization with DNPH .7
6.5 Method C: Reagents for post-column derivatization with ACAC .7
6.6 Reagents for titration of formaldehyde standard .8
7 Procedure . 8
7.1 Sampling .8
7.2 Extraction .8
7.3 Analysis and detection of Method A .9
7.3.1 Procedure for derivatization with ACAC .9
7.3.2 Photometric analysis of calibration solutions .9
iii
7.3.3 Sample measurement for photometric analysis .10
7.3.4 Quantification of the in-can free formaldehyde content .10
7.4 Analysis and detection of Method B .10
7.4.1 Procedure for derivatization with DNPH .10
7.4.2 Operation conditions .11
7.4.3 Blank determination .11
7.4.4 Analysis of calibration solution .11
7.4.5 Sample measurement .11
7.4.6 Quality check . 12
7.4.7 Calculation of in-can free formaldehyde content . 12
7.5 Analysis and detection of Method C . 12
7.5.1 Operation conditions . 12
7.5.2 Blank determination . 12
7.5.3 Analysis of calibration solution . 12
7.5.4 Sample measurement .
...
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2024-07-12
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ISO/FDIS 7012--1:2024(en)
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ISO TC 35/SC 16/WG 1
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Secretariat: DIN
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Date: 2024-12-18
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Paints and varnishes — Determination of preservatives in water-dilutable coating
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materials —
Part 1: Determination of in-can free formaldehyde Style Definition: List Number 1: Tab stops: Not at 0.7
cm + 1.4 cm + 2.1 cm + 2.8 cm + 3.5 cm + 4.2 cm +
4.9 cm + 5.6 cm + 6.3 cm + 7 cm
Peintures et vernis — Dosage des agents de préservation dans les produits de peinture diluables à
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l’eau — Partie 1: Dosage du formaldéhyde libre en pot
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Style Definition: ANNEX
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All rights reserved. Unless otherwise specified, or required in the context of its implementation, no Kingdom)
part of this publication may be reproduced or utilized otherwise in any form or by any means,
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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)
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Email: copyright@iso.orgcopyright@iso.org
Kingdom)
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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
Foreword . v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 3
5 Apparatus . 5
6 Reagents and materials . 7
7 Procedure . 10
8 Precision . 16
9 Test report . 17
Annex A (normative) Titration methods for the determination of formaldehyde content . 18
A.1 Determination of formaldehyde concentration: Iodometric method . 18
A.2 Determination of formaldehyde concentration: pH-value method . 18
Annex B (informative) Example of HPLC conditions for method B . 21
Annex C (informative) Example of HPLC conditions for method C . 22
Annex D (informative) Results of the interlaboratory test . 23
Bibliography . 25
Foreword . v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 3
5 Apparatus . 5
6 Reagents and materials . 7
7 Procedure . 10
8 Precision . 16
9 Test report . 17
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Annex A (normative) Titration methods for the determination of formaldehyde content . 18
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A.1 Determination of formaldehyde concentration: Iodometric method . 18
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A.2 Determination of formaldehyde concentration: pH-value method . 18
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iii
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Annex B (informative) Example of HPLC conditions for method B . 21
Annex C (informative) Example of HPLC conditions for method C . 22
Annex D (informative) Results of the interlaboratory test . 23
Bibliography . 25
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iv © ISO 2024 – All rights reserved
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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
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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
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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
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cooperation between ISO and CEN (Vienna Agreement).
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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
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www.iso.org/members.htmlwww.iso.org/members.html.
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v
FINAL DRAFT International Standard ISO/FDIS 7012-1:2024(en)
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header
Paints and varnishes — Determination of preservatives in water-
dilutable coating materials —
Part 1: Determination of in-can free formaldehyde
1 Scope
This document specifies the apparatus and the analytical methodmethods for determining the
concentration of in-can free formaldehyde in water-dilutable coating materials.
This document can also be applied forto polymer dispersions.
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cm + 2.1 cm + 2.8 cm + 3.5 cm + 4.2 cm + 4.9 cm +
The determination method A for in-can free formaldehyde described in this document can beis only of
5.6 cm + 6.3 cm + 7 cm
limited suitability for pigmented systems, as the inherent coloration of the material can have an influence
on the detection.
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
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approved method
text, Don't adjust space between Asian text and numbers
[SOURCE: ISO 11890-2:2020, 3.7]
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stops: 17.2 cm, Right
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3.2
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in-can free formaldehyde con
...
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 1:
Dosage du formaldéhyde libre en
pot
Paints and varnishes — Determination of preservatives in water-
dilutable coating materials —
Part 1: Determination of in-can free formaldehyde
LES DESTINATAIRES DU PRÉSENT PROJET SONT
INVITÉS À PRÉSENTER, AVEC LEURS OBSERVATIONS,
NOTIFICATION DES DROITS DE PROPRIÉTÉ DONT ILS
AURAIENT ÉVENTUELLEMENT CONNAISSANCE ET À
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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 1:
Dosage du formaldéhyde libre en pot
Paints and varnishes — Determination of preservatives in water-
dilutable coating materials —
Part 1: Determination of in-can free formaldehyde
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
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INTERNATIONALES DOIVENT PARFOIS ÊTRE CONSIDÉRÉS
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DU POINT DE VUE DE LEUR POSSI BILITÉ DE DEVENIR DES
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NORMES POUVANT
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SERVIR DE RÉFÉRENCE DANS LA RÉGLEMENTATION
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Publié en Suisse Numéro de référence
ii
Sommaire Page
Avant-propos .v
1 Domaine d’application . 1
2 Références normatives . 1
3 Termes et définitions . 1
4 Principe. 3
4.1 Généralités .3
4.2 Équilibres de formaldéhyde libre dans la matrice de produit de peinture .3
4.3 Équilibres de formaldéhyde libre en pot pendant l’extraction .3
4.4 Équilibres de formaldéhyde libre en pot pendant la dérivation .4
4.5 Principe de la méthode A: dérivation à l’acétylacétone (ACAC) associée à une détection
photométrique .4
4.5.1 Dérivation à l’ACAC .4
4.5.2 Détection et quantification avec un photomètre spectral .4
4.6 Principe de la méthode B: dérivation à la dinitrophénylhydrazine (DNPH) associée
à une séparation par chromatographie en phase liquide (CL) et à une détection UV/VIS .4
4.6.1 Dérivation à la DNPH .4
4.6.2 Séparation, détection et quantification par CL-UV/VIS .4
4.7 Principe de la méthode C: séparation par chromatographie en phase liquide (CL) suivie
d’une dérivation post-colonne à l’ACAC puis d’une quantification avec détection UV/VIS .4
4.7.1 Séparation du formaldéhyde libre par chromatographie en phase liquide .4
4.7.2 Dérivation post-colonne à l’acétylacétone (ACAC) et quantification avec
détection UV/VIS .4
5 Appareillage . 5
5.1 Généralités .5
5.2 Appareillage général .5
5.3 Appareillage d’extraction .5
5.4 Appareillage pour la méthode A .5
5.5 Appareillage pour la méthode B.5
5.5.1 Système de CL [CLHP ou chromatographie en phase liquide ultra-performance
(UHPLC)].5
5.5.2 Colonne appropriée .6
5.5.3 Flacons .6
5.6 Appareillage pour la méthode C .6
5.6.1 Système de CL [CLHP ou chromatographie en phase liquide ultra-performance
(UHPLC)] avec réacteur post-colonne .6
5.6.2 Colonne appropriée (par exemple, colonne à phase inverse RPC8 ou RPC18) .6
6 Réactifs et matériaux . 6
6.1 Généralités .6
6.2 Réactifs généraux .6
6.2.1 Eau déminéralisée .6
6.2.2 Solution de formaldéhyde.6
6.2.3 Solution-mère de formaldéhyde .7
6.2.4 Solutions de travail de formaldéhyde pour l’étalonnage .7
6.2.5 Solutions de Carrez (facultatives) .7
6.3 Méthode A: réactifs pour la dérivation à l’ACAC .7
6.4 Méthode B: réactifs pour la dérivation à la DNPH .7
6.5 Méthode C: réactifs pour la dérivation post-colonne à l’ACAC .8
6.6 Réactifs pour le titrage de l’étalon de formaldéhyde .8
7 Mode opératoire . 9
7.1 Échantillonnage .9
7.2 Extraction .9
7.3 Analyse et détection de la méthode A .9
7.3.1 Mode opératoire de dérivation à l’ACAC .9
iii
7.3.2 Analyse photométrique des solutions d’étalonnage .9
7.3.3 Mesurage de l’échantillon pour analyse photométrique .10
7.3.4 Quantification de la teneur en formaldéhyde libre en pot .10
7.4 Analyse et détection de la méthode B .11
7.4.1 Mode opératoire de dérivation à la DNPH .11
7.4.2 Conditions opératoires .11
7.4.3 Détermination à blanc .11
7.4.4 Analyse des solutions d’étalonnage .11
7.4.5 Mesurage de l’échantillon . 12
7.4.6 Contrôle qualité . 12
7.4.7 Calcul de la teneur de formaldéhyde libre en pot . 12
7.5 Analyse et détection de la méthode C . 13
7.5.1 Conditions opératoires . 13
7.5.2 Détermination à blanc . 13
7.5.3 Analyse des solutions d’étalonnage .
...
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