Plastics — Polymer dispersions — Determination of free formaldehyde

This document specifies two methods for the determination of free formaldehyde (HCHO) in polymer dispersions. This document is applicable to acrylic, acrylonitrile butadiene, carboxylated styrene-butadiene and vinyl acetate polymer dispersions. It is also applicable to polymer dispersions of other compositions. Method A (UV/Vis spectrometer method) is applicable to polymer dispersions with a free-formaldehyde content higher than 10 mg/kg. Method B (HPLC method) is applicable for determining lower formaldehyde contents or carrying out arbitration analyses.

Plastiques — Dispersions de polymères — Dosage du formaldéhyde libre

La présente Norme internationale décrit deux méthodes pour la détermination du formaldéhyde libre (HCHO) dans les dispersions de polymères. Le mode opératoire a été évalué à l'aide de dispersions de polymères acryliques, d'acrylonitrile-butadiène, de styrène-butadiène carboxylé et d'acétate de vinyle. Ces deux méthodes d'essai peuvent également s'appliquer aux dispersions de polymères de compositions différentes. La méthode A est la méthode recommandée pour les dispersions de polymères ayant une teneur en formaldéhyde libre supérieure à 10 mg/kg. La méthode B est recommandée lorsque des teneurs inférieures en formaldéhyde doivent être déterminées ou que des analyses d'arbitrage doivent être réalisées. Ces deux méthodes permettent de minimiser les variations de concentration en formaldéhyde pouvant conduire à des changements de propriétés physiques ou chimiques des dispersions de polymères. Il n'existe aucune restriction connue à ces méthodes lorsqu'elles sont utilisées comme indiqué dans la présente Norme internationale.

General Information

Status
Published
Publication Date
05-Dec-2024
Current Stage
6060 - International Standard published
Start Date
06-Dec-2024
Due Date
06-Dec-2024
Completion Date
06-Dec-2024
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International
Standard
ISO 15373
Second edition
Plastics — Polymer dispersions —
2024-12
Determination of free formaldehyde
Plastiques — Dispersions de polymères — Dosage du
formaldéhyde libre
Reference number
© ISO 2024
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
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Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Interference. 2
5.1 Method A .2
5.2 Method B .2
6 Reagents (method A and B) . 2
7 Apparatus . 4
8 Procedure . 7
8.1 Preparation of test solution .7
8.1.1 Dilution of test sample.7
8.1.2 Filtration .7
8.1.3 Centrifugation . .7
8.1.4 Coagulation .7
8.2 Blank solution .8
8.3 Check test (method B) .8
8.4 Calibration .8
8.4.1 Method A . . .8
8.4.2 Method B . .8
8.5 Determination of formaldehyde .10
8.5.1 Method A . . .10
8.5.2 Method B .10
9 Calculation .10
10 Precision for method B .11
10.1 Precision estimates .11
10.2 Repeatability .11
10.3 Reproducibility . . 12
10.4 Bias . 12
11 Test report .12
Bibliography .13

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 61, Plastics, Subcommittee SC 9, Thermoplastic
materials.
This second edition cancels and replaces the first edition (ISO 15373:2001), which has been technically
revised.
The main changes are as follows:
— text is revised according to the latest ISO Directive, Part 2.
— added Figure 1, as illustration of the principle of this method.
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
International Standard ISO 15373:2024(en)
Plastics — Polymer dispersions — Determination of free
formaldehyde
1 Scope
This document specifies two methods for the determination of free formaldehyde (HCHO) in polymer
dispersions.
This document is applicable to acrylic, acrylonitrile butadiene, carboxylated styrene-butadiene and vinyl
acetate polymer dispersions. It is also applicable to polymer dispersions of other compositions.
Method A (UV/Vis spectrometer method) is applicable to polymer dispersions with a free-formaldehyde
content higher than 10 mg/kg.
Method B (HPLC method) is applicable for determining lower formaldehyde contents or carrying out
arbitration analyses.
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 2227, Formaldehyde solutions for industrial use — Determination of formaldehyde content
ISO 3696, Water for analytical laboratory use — Specification and test methods
3 Terms and definitions
No terms and definitions are listed in this document.
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
— IEC Electropedia: available at https:// www .electropedia .org/
4 Principle
The polymers dispersed in a polymer dispersion are separated from the aqueous phase by filtration,
centrifuge or coagulation. The resulting aqueous sample solution containing formaldehyde reacts with
2,4-pentanedione to yield a lutidine derivative (see Figure 1), which can be analysed by UV detector at 410 nm.
Figure 1 — Reaction of formaldehyde with 2,4-pentanedione

In method A, 2,4-pentanedione is added directly to the resulting aqueous solution. Absorption at 410 nm is
measured with a UV/Vis spectrometer. The concentration of formaldehyde is determined using a calibration
plot obtained by plotting the absorption at 410 nm of formaldehyde standards against the corresponding
formaldehyde concentrations.
In method B, formaldehyde in the resulting aqueous solution is separated from other species by liquid
chromatography on an octadecyldimethylsilyl (C18) reversed-phase column using an aqueous mobile phase.
The detection system includes a post-column reactor which produces a lutidine derivative by reaction of
formaldehyde with 2,4-pentanedione and a UV/Vis detector operating at 410 nm. The concentration of free
formaldehyde in the resulting aqueous solution is determined using peak areas from the standard and
sample chromatograms (calibration by external standard).
5 Interference
5.1 Method A
The following species have been identified as possible interferants in the method:
— acetaldehyde;
— glyoxylic acid.
However, interference by acetaldehyde and glyoxylic acid is to be expected only when the species concerned
is present in excess amounts (100-fold and more) compared with the formaldehyde concentration.
5.2 Method B
This method is specific for formaldehyde because potential interferants such as acetaldehyde, acetone,
benzaldehyde, formamide, formic acid, glyoxylic acid and propionaldehyde are either chromatographically
separated from formaldehyde or do not react with the post-column reagent.
However, to adapt for various composition in different polymer dispersions, extended chromatography run
time is recommended to allow for late-eluting compounds in Method B. Compounds which remain on the
column after an analysis have potential interference with the formaldehyde peak in subsequent runs.
6 Reagents (method A and B)
Unless otherwise stated,
...

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