Leather - Chemical tests - Determination of formaldehyde content (ISO/TS 17226:2003)

The formaldehyde contents are understood to be the quantity of formaldehyde contained in a water extract from the leather. This International Standard includes two methods for the determination of free and released formaldehyde in leathers. One method is relatively simple with regard to the laboratory equipment (photometric method), while the other needs more sophisticated equipment (HPLC method). The second method is selective and not sensitive to coloured extracts.

Leder - Chemische Prüfungen - Bestimmung des Formaldehydgehaltes (ISO/TS 17226:2003)

Diese Technische Spezifikation enthält zwei Verfahren zur Bestimmung von freiem und freigesetztem Formaldehyd in Leder. Das eine Verfahren (Abschnitt 5) ist hinsichtlich der Laboratoriumsausrüstung relativ einfach (kolorimetrisches Verfahren), während das andere Verfahren (Abschnitt 4) eine hochentwickeltere Ausrüstung (HPLC-Verfahren) erfordert. Das zweite Verfahren ist selektiv und gegen gefärbte Extrakte unempfindlich.
Der Formaldehydgehalt ist als die Menge an Formaldehyd zu verstehen, die in einem wässrigen Extrakt des Leders enthalten ist.
Die beiden analytischen Verfahren sollten ähnliche Trends, jedoch nicht zwangsläufig dasselbe absolute Ergebnis aufweisen.

Cuir - Essais chimiques - Détermination de la formaldéhyde (ISO/TS 17226:2003)

La teneur en formaldéhyde correspond à la quantité de formaldéhyde contenue dans un extrait aqueux provenant du cuir. La présente norme internationale inclut deux méthodes pour le dosage du formaldéhyde libre et libéré dans les cuirs. La première méthode est plus simple en ce qui concerne l'équipement de laboratoire (méthode photométrique), la seconde nécessite un équipement plus complexe (méthode HPLC, chromatographie en phase liquide à haute performance). La deuxième méthode est sélective et n'est pas sensible aux extraits de couleur.

Usnje – Kemični preskusi – Določevanje formaldehida (ISO/TS 17226:2003)

General Information

Status
Withdrawn
Publication Date
14-Aug-2003
Withdrawal Date
15-Jul-2008
Current Stage
9960 - Withdrawal effective - Withdrawal
Start Date
16-Jul-2008
Completion Date
16-Jul-2008

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SLOVENSKI STANDARD
SIST-TS CEN ISO/TS 17226:2004
01-maj-2004
8VQMH±.HPLþQLSUHVNXVL±'RORþHYDQMHIRUPDOGHKLGD ,6276
Leather - Chemical tests - Determination of formaldehyde content (ISO/TS 17226:2003)
Leder - Chemische Prüfungen - Bestimmung des Formaldehydgehaltes (ISO/TS
17226:2003)
Cuir - Essais chimiques - Détermination de la formaldéhyde (ISO/TS 17226:2003)
Ta slovenski standard je istoveten z: CEN ISO/TS 17226:2003
ICS:
59.140.30 Usnje in krzno Leather and furs
SIST-TS CEN ISO/TS 17226:2004 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TS CEN ISO/TS 17226:2004

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SIST-TS CEN ISO/TS 17226:2004
TECHNICAL SPECIFICATION
CEN ISO/TS 17226
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
August 2003
ICS 59.140.30
English version
Leather - Chemical tests - Determination of formaldehyde
content (ISO/TS 17226:2003)
Cuir - Essais chimiques - Détermination de la Leder - Chemische Prüfungen - Bestimmung des
formaldéhyde (ISO/TS 17226:2003) Formaldehydgehaltes (ISO/TS 17226:2003)
This Technical Specification (CEN/TS) was approved by CEN on 1 April 2003 for provisional application.
The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the CEN/TS can be converted into a European Standard.
CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available. It
is permissible to keep conflicting national standards in force (in parallel to the CEN/TS) until the final decision about the possible
conversion of the CEN/TS into an EN is reached.
CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,
Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and United
Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2003 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN ISO/TS 17226:2003 E
worldwide for CEN national Members.

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SIST-TS CEN ISO/TS 17226:2004
CEN ISO/TS 17226:2003 (E)
Foreword
This document (CEN ISO/TS 17226:2003) has been prepared by Technical Committee CEN/TC
289 "Leather", the secretariat of which is held by UNI, in collaboration with the International
Union of Leather Technologists and Chemists Societies (IULTCS).
It is based on Method IUC 19 of the International Union of Leather Technologists and Chemists
Societies.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of
the following countries are bound to announce this CEN Technical Specification: Austria,
Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden,
Switzerland and the United Kingdom.
Endorsement notice
The text of ISO/TS 17226:2003 has been approved by CEN as CEN ISO/TS 17226:2003 without
any modifications.
NOTE Normative references to International Standards are listed in Annex ZA (normative).
2

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SIST-TS CEN ISO/TS 17226:2004
CEN ISO/TS 17226:2003 (E)
Annex ZA
(normative)
Normative references to international publications
with their relevant European publications
This European Standard incorporates by dated or undated reference, provisions from other
publications. These normative references are cited at the appropriate places in the text and the
publications are listed hereafter. For dated references, subsequent amendments to or revisions of
any of these publications apply to this European Standard only when incorporated in it by
amendment or revision. For undated references the latest edition of the publication referred to
applies (including amendments).
NOTE Where an International Publication has been modified by common modifications, indicated
by (mod.), the relevant EN/HD applies.
Publication Year Title EN Year
ISO 4044 1977 Leather - Preparation of EN ISO 4044 1998
chemical test samples
ISO 3696 1987 Water for analytical laboratory EN ISO 3696 1995
use - Specification and test
methods
ISO 2418 2002 Leather - Chemical, physical and EN ISO 2418 2002
mechanical and fastness tests -
Sampling location
ISO 2419 2002 Leather - Physical and EN ISO 2419 2002
mechanical tests - Sample
preparation and conditioning
3

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SIST-TS CEN ISO/TS 17226:2004

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SIST-TS CEN ISO/TS 17226:2004

TECHNICAL ISO/TS
SPECIFICATION 17226
IULTCS/
IUC 19
First edition
2003-08-15

Leather — Chemical tests —
Determination of formaldehyde content
Cuir — Essais chimiques — Détermination de la formaldéhyde




Reference number
ISO/TS 17226:2003(E)
IULTCS/IUC 19
©
ISO 2003

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SIST-TS CEN ISO/TS 17226:2004
ISO/TS 17226:2003(E)
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ii © ISO 2003 — All rights reserved

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SIST-TS CEN ISO/TS 17226:2004
ISO/TS 17226:2003(E)
Contents Page
Fore word. iv
1 Scope. 1
2 Normative references . 1
3 Preparation and standardisation of formaldehyde stock solution . 1
4 Chromatographic HPLC method . 2
5 Colourimetric method. 5
6 Expression of results . 8
7 Test report . 8
Annex A (informative) Precision . 9
© ISO 2003 — All rights reserved iii

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SIST-TS CEN ISO/TS 17226:2004
ISO/TS 17226:2003(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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards adopted
by the technical committees are circulated to the member bodies for voting. Publication as an International
Standard requires approval by at least 75 % of the member bodies casting a vote.
In other circumstances, particularly when there is an urgent market requirement for such documents, a technical
committee may decide to publish other types of normative document:
 an ISO Publicly Available Specification (ISO/PAS) represents an agreement between technical experts in an
ISO working group and is accepted for publication if it is approved by more than 50 % of the members of the
parent committee casting a vote;
 an ISO Technical Specification (ISO/TS) represents an agreement between the members of a technical
committee and is accepted for publication if it is approved by 2/3 of the members of the committee casting a
vote.
An ISO/PAS or ISO/TS is reviewed after three years in order to decide whether it will be confirmed for a further
three years, revised to become an International Standard, or withdrawn. If the ISO/PAS or ISO/TS is confirmed, it is
reviewed again after a further three years, at which time it must either be transformed into an International
Standard or be withdrawn.
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.
ISO/TS 17226 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, the secretariat of which is held by UNI, in
accordance with the Agreement on technical cooperation between ISO and CEN (Vienna Agreement). This method
is technically similar to the method in IUC 19 which was declared an official method at the IULTCS Delegates
meeting on 31st May 2003 in Cancun, Mexico. This edition differs slightly in the text compared with IUC 19.

iv © ISO 2003 — All rights reserved

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SIST-TS CEN ISO/TS 17226:2004
TECHNICAL SPECIFICATION ISO/TS 17226:2003(E)

Leather — Chemical tests — Determination of formaldehyde
content
1 Scope
This Technical Specification includes two methods for the determination of free and released formaldehyde in
leathers. One method (Section 5) is relatively simple with regard to the laboratory equipment (colourimetric
method), while the other (Section 4) needs more sophisticated equipment (HPLC method). The second method is
selective and not sensitive to coloured extracts.
The formaldehyde content is taken to be the quantity of formaldehyde contained in a water extract from the
leather.
The two analytical methods should give similar trends but not necessarily the same absolute result.
2 Normative references

The following referenced documents are indispensable for the application 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 2418:2002, Leather - Chemical, physical and mechanical and fastness tests - Sampling location
ISO 2419:2002, Leather - Physical and mechanical tests - Sample preparation and conditioning
ISO 3696:1987, Water for analytical laboratory use - Specification and test methods
ISO 4044:1977, Leather - Preparation of chemical test samples
3 Preparation and standardisation of formaldehyde stock solution
3.1 Reagents
Unless otherwise stated only analytical grade chemicals are to be used. The water must be demineralised, grade 3
in accordance with ISO 3696. All solutions are aqueous solutions.
3.1.1 Formaldehyde solution, approx. 37 %;
3.1.2 0,05 M iodine solution, (i.e. 12,68 g iodine per l);
3.1.3 2M sodium hydroxide;
3.1.4 1,5 M sulphuric acid;
3.1.5 0,1 M sodium thiosulphate solution;
3.1.6 1 % starch solution, (i.e. 1 g in 100 ml water).
3.2 Procedure for the determination of formaldehyde in the stock solution
5 ml of the formaldehyde solution (3.1.1) is pipetted into a 1 000 ml volumetric flask which contains approximately
100 ml demineralised water and is subsequently filled with demineralised water up to the mark. This solution is the
formaldehyde stock solution.
© ISO 2003 — All rights reserved 1

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SIST-TS CEN ISO/TS 17226:2004
ISO/TS 17226:2003(E)
From this solution, 10 ml is pipetted into a 250 ml Erlenmeyer flask and mixed with 50 ml iodine solution (3.1.2) and
sodium hydroxide (3.1.3) is added until it turns yellow. It is allowed to settle for 15 min ± 1 min at 18 °C to 26 °C
and then 50 ml of sulphuric acid (3.1.4) is added while swirling.
After addition of 2 ml of starch solution (3.1.6), the excess iodine is titrated with sodium thiosulphate (3.1.5) until the
colour changes. Three individual determinations shall be made. A blank solution is titrated in the same manner.
( - )x x
V 0 V1 c1 M FA
=
CFA
2
C = concentration of the formaldehyde stock-solution, in mg / 10 ml;
FA
V = titre of the thiosulphate solution for the blank solution, in ml;
0
V = titre of the thiosulphate solution for the sample solution, in ml;
1
M = molecular weight of formaldehyde, 30,08 g/mol;
FA
c = concentration of the thiosulphate solution, M.
1
4 Chromatographic HPLC method
4.1 Principle
The process is selective. Formaldehyde is separated and quantified as a derivative from other aldehydes and
ketones by liquid chromatography. Detected is the free-formaldehyde and formaldehyde which is hydrolysed during
extraction to yield free-formaldehyde.
The sample is eluted with water at 40 °C. The eluate is mixed with 2,4 dinitrophenylhydrazine, whereby aldehydes
and ketones react to give the respective hydrazines. These are separated by means of a reversed-phase HPLC
method, detected at 350 nm and quantified.
4.2 Chemicals
Unless otherwise stated only analytical grade chemicals are to be used. The water must be demineralised, grade 3
in accordance with ISO 3696. All solutions are aqueous solutions.
2 © ISO 2003 — All rights reserved

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SIST-TS CEN ISO/TS 17226:2004
ISO/TS 17226:2003(E)
4.2.1 0,1% sodium dodecylsulphonate (detergent), 1 g in 1 000 ml water;
4.2.2 0,3 % DNPH (2,4 Dinitrophenylhydrazine) in conc. o-Phosphoric acid (85 %). (D
...

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