Chemicals for the leather tanning industry - Determination of cyclosiloxanes (ISO/DIS 23649:2024)

This document specifies a method for determining the total content of the following cyclosiloxanes in chemicals for the leather tanning industry:
—   octamethylcyclotetrasiloxane (D4);
—   decamethylcyclopentasiloxane (D5);
—   dodecamethylcyclohexasiloxane (D6);
This method requires the use of Gas chromatography (GC) equipped with a single quadrupole mass spectrometer (MS) to identify and quantify the cyclosiloxanes

Chemikalien für die Ledergerbereiindustrie - Bestimmung von Cyclosiloxanen in Imprägnierfettungsmitteln (ISO/DIS 23649:2024)

Kemikalije za industrijo strojenja usnja - Določanje ciklosiloksanov v hidroizolacijskih maščobnih sredstvih (ISO/DIS 23649:2024)

General Information

Status
Not Published
Publication Date
22-Apr-2025
Current Stage
4599 - Dispatch of FV draft to CMC - Finalization for Vote
Start Date
18-Oct-2024
Due Date
11-Mar-2025
Completion Date
18-Oct-2024

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SLOVENSKI STANDARD
01-maj-2024
Kemikalije za industrijo strojenja usnja - Določanje ciklosiloksanov v
hidroizolacijskih maščobnih sredstvih (ISO/DIS 23649:2024)
Chemicals for the leather tanning industry - Determination of cyclosiloxanes in
waterproofing fatliquors (ISO/DIS 23649:2024)
Chemikalien für die Ledergerbereiindustrie - Bestimmung von Cyclosiloxanen in
Imprägnierfettungsmitteln (ISO/DIS 23649:2024)
Ta slovenski standard je istoveten z: prEN ISO 23649
ICS:
59.140.30 Usnje in krzno Leather and furs
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

DRAFT
International
Standard
ISO/DIS 23649
IULTCS
IUC 400
IULTCS
Chemicals for the leather tanning
Secretariat: ISO
industry - Determination of
cyclosiloxanes in waterproofing
Voting begins on:
2024-03-12
fatliquors
Voting terminates on:
ICS: 59.140.30
2024-06-04
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENTS AND APPROVAL. IT
IS THEREFORE SUBJECT TO CHANGE
AND MAY NOT BE REFERRED TO AS AN
INTERNATIONAL STANDARD UNTIL
PUBLISHED AS SUCH.
This document is circulated as received from the committee secretariat.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL,
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STANDARDS MAY ON OCCASION HAVE TO
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POTENTIAL TO BECOME STANDARDS TO
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NATIONAL REGULATIONS.
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 SUPPORTING DOCUMENTATION.
Reference numbers
ISO/DIS 23649:2024(en)
IULTCS/IUC 400:2024(en)
DRAFT
ISO/DIS 23649:2024(en)
International
Standard
ISO/DIS 23649
IULTCS
IUC 400
IULTCS
Chemicals for the leather tanning
Secretariat: ISO
industry - Determination of
cyclosiloxanes in waterproofing
Voting begins on:
fatliquors
Voting terminates on:
ICS: 59.140.30
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENTS AND APPROVAL. IT
IS THEREFORE SUBJECT TO CHANGE
AND MAY NOT BE REFERRED TO AS AN
INTERNATIONAL STANDARD UNTIL
PUBLISHED AS SUCH.
This document is circulated as received from the committee secretariat.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL,
© ISO 2024
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
STANDARDS MAY ON OCCASION HAVE TO
ISO/CEN PARALLEL PROCESSING
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
BE CONSIDERED IN THE LIGHT OF THEIR
the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
or ISO’s member body in the country of the requester.
NATIONAL REGULATIONS.
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CP 401 • Ch. de Blandonnet 8
TO SUBMIT, WITH THEIR COMMENTS,
CH-1214 Vernier, Geneva
NOTIFICATION OF ANY RELEVANT PATENT
Phone: +41 22 749 01 11
RIGHTS OF WHICH THEY ARE AWARE AND TO
PROVIDE SUPPORTING DOCUMENTATION.
Email: copyright@iso.org
Website: www.iso.org
Reference numbers
Published in Switzerland ISO/DIS 23649:2024(en)
IULTCS/IUC 400:2024(en)
ii
ISO/DIS 23649:2024(en)
IULTCS/IUC 400:2024(en)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Apparatus . 1
6 Reagents . 2
7 Sampling and sample preparation . 3
8 Procedure . 3
8.1 Sample solution preparation .3
8.2 Liquid-liquid extraction.3
8.3 Instrumental analysis .4
9 Expression of results . 4
9.1 Calculation .4
10 Precision . 4
11 Test report . 4
Annex A (informative) Chromatographic analysis operating parameters for GC-MS . 6
Annex B (informative) Precision: reliability of the method . 7
Annex C (normative) Sample preparation for non-water-soluble chemicals . 8
Bibliography . 9

iii
ISO/DIS 23649:2024(en)
IULTCS/IUC 400:2024(en)
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).
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.
IULTCS, originally formed in 1897, is a world-wide organization of professional leather societies to further
the advancement of leather science and technology. IULTCS has three Commissions, which are responsible
for establishing international methods for the sampling and testing of leather. ISO recognizes IULTCS as an
international standardizing body for the preparation of test methods for leather.
This document was prepared by the Chemical Test Commission of the International Union of Leather
Technologists and Chemists Societies (IUC Commission, IULTCS), in collaboration with the European
Committee for Standardization (CEN) Technical Committee CEN/TC 289, Leather, 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/DIS 23649:2024(en)
IULTCS/IUC 400:2024(en)
Introduction
This document includes a procedure for analysing certain cyclosiloxanes using gas chromatography (GC)
with mass spectrometer (MS) equipment. With this analytical method octamethylcyclotetrasiloxane (D4),
decamethylcyclopentasiloxane (D5) and dodecamethylcyclohexasiloxane (D6) can be determined.
In the leather industry cyclosiloxanes (D4), (D5) and (D6) are used in the manufacture of silicone based
waterproofing fatliquors and can also be used in the production of silicone-based finishing chemicals
especially as handle modifiers.
At present, the official classification recognised in the EU is the following:
— Octamethylcyclotetrasiloxane(D4) as persistent, bioaccumulative and toxic (1)
— Decamethylcyclopentasiloxane (D5) as persistent, bioaccumulative and toxic (2)
— Dodecamethylcyclohexasiloxane (D6) as persistent, bioaccumulative and toxic (3).

v
ISO/DIS 23649:2024(en)
DRAFT International Standard
IULTCS/IUC 400:2024(en)
Chemicals for the leather tanning industry - Determination of
cyclosiloxanes in waterproofing fatliquors
1 Scope
This document specifies a method for determining the total content of the following cyclosiloxanes in
waterproofing fatliquors and other silicone-based chemicals for the leather tanning industry:
— octamethylcyclotetrasiloxane (D4);
— decamethylcyclopentasiloxane (D5);
— dodecamethylcyclohexasiloxane (D6);
This method requires the use of liquid chromatography (GC) equipped with a single quadrupole mass
spectrometer (MS) to identify and quantify the cyclosiloxanes.
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 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
After solubilizing the chemical sample in water, a liquid-liquid extraction with a hexane-ethyl acetate mixture
is performed and then the cyclosiloxanes are analysed by gas-chromatography with single quadrupole mass
spectrometry (GC-MS). Using an external calibration, quantification is performed taking into account the
recovery rate of the internal standard.
5 Apparatus
The usual laboratory apparatus and, in particular, the following shall be used:
5.1 Ultrasonic bath, capable of operating at room temperature.
...

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