SIST EN ISO 14389:2023
(Main)Textiles - Determination of the phthalate content - Tetrahydrofuran method (ISO 14389:2022)
Textiles - Determination of the phthalate content - Tetrahydrofuran method (ISO 14389:2022)
This document specifies a method of determining phthalates in textiles with gas chromatography–
mass spectrometry (GC-MS).
This document is applicable to textile products where there is a risk of the presence of some phthalates.
Textilien - Bestimmung des Phthalatanteils - Tetrahydrofuran-Verfahren (ISO 14389:2022)
Dieses Dokument legt ein Verfahren für die Bestimmung von Phthalaten in Textilien durch Gaschroma-tographie-Massenspektrometrie (GC-MS) fest.
Dieses Dokument ist für textile Erzeugnisse, bei denen die Gefahr des Vorhandenseins einiger Phthalate besteht, anzuwenden.
WARNUNG — Dieses Dokument verlangt die Verwendung von Substanzen und/oder die Anwendung von Verfahren, die gesundheitsschädlich sein können, wenn keine geeigneten Vorsichtsmaßnahmen ergriffen werden. Es bezieht sich nur auf die technische Eignung und spricht den Anwender zu keinem Zeitpunkt von gesetzlichen Verpflichtungen frei, die im Zusammenhang mit der Gesundheit und Sicherheit stehen. Bei der Erarbeitung dieses Dokuments wurde davon ausgegangen, dass entsprechend geschulte und erfahrene Mitarbeiter mit der Ausführung seiner Bestimmungen betraut werden.
Textiles - Détermination de la teneur en phtalates - Méthode au tétrahydrofurane (ISO 14389:2022)
Le présent document spécifie une méthode de dosage de phtalates dans les textiles par chromatographie en phase gazeuse et spectrométrie de masse (GC-MS).
Le présent document s’applique aux produits textiles susceptibles de contenir certains phtalates.
Tekstilije - Določevanje ftalatov - Tetrahidrofuranska metoda (ISO 14389:2022)
Ta dokument določa metodo za določevanje ftalatov v tekstilijah s plinsko kromatografijo
z masno spektrometrijo (GC-MS).
Ta dokument se uporablja za tekstilne izdelke, pri katerih obstaja tveganje za prisotnost nekaterih ftalatov.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 14389:2023
01-januar-2023
Nadomešča:
SIST EN ISO 14389:2014
Tekstilije - Določevanje ftalatov - Tetrahidrofuranska metoda (ISO 14389:2022)
Textiles - Determination of the phthalate content - Tetrahydrofuran method (ISO
14389:2022)
Textilien - Bestimmung des Phthalatanteils - Tetrahydrofuran-Verfahren (ISO
14389:2022)
Textiles - Détermination de la teneur en phtalates - Méthode au tétrahydrofurane (ISO
14389:2022)
Ta slovenski standard je istoveten z: EN ISO 14389:2022
ICS:
59.060.01 Tekstilna vlakna na splošno Textile fibres in general
SIST EN ISO 14389:2023 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 14389:2023
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SIST EN ISO 14389:2023
EN ISO 14389
EUROPEAN STANDARD
NORME EUROPÉENNE
October 2022
EUROPÄISCHE NORM
ICS 59.060.01 Supersedes EN ISO 14389:2014
English Version
Textiles - Determination of the phthalate content -
Tetrahydrofuran method (ISO 14389:2022)
Textiles - Détermination de la teneur en phtalates - Textilien - Bestimmung des Phthalatanteils -
Méthode au tétrahydrofurane (ISO 14389:2022) Tetrahydrofuran-Verfahren (ISO 14389:2022)
This European Standard was approved by CEN on 18 September 2022.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 14389:2022 E
worldwide for CEN national Members.
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SIST EN ISO 14389:2023
EN ISO 14389:2022 (E)
Contents Page
European foreword . 3
2
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SIST EN ISO 14389:2023
EN ISO 14389:2022 (E)
European foreword
This document (EN ISO 14389:2022) has been prepared by Technical Committee ISO/TC 38 "Textiles"
in collaboration with Technical Committee CEN/TC 248 “Textiles and textile products” the secretariat of
which is held by BSI.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by April 2023, and conflicting national standards shall be
withdrawn at the latest by April 2023.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN ISO 14389:2014.
Any feedback and questions on this document should be directed to the users’ national standards
body/national committee. A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the
United Kingdom.
Endorsement notice
The text of ISO 14389:2022 has been approved by CEN as EN ISO 14389:2022 without any modification.
3
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SIST EN ISO 14389:2023
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SIST EN ISO 14389:2023
INTERNATIONAL ISO
STANDARD 14389
Second edition
2022-10
Textiles — Determination of the
phthalate content — Tetrahydrofuran
method
Textiles — Détermination de la teneur en phtalates — Méthode au
tétrahydrofurane
Reference number
ISO 14389:2022(E)
© ISO 2022
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SIST EN ISO 14389:2023
ISO 14389:2022(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2022
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
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
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SIST EN ISO 14389:2023
ISO 14389:2022(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 2
6 Apparatus . 2
7 Procedure .3
7.1 Cross-contamination provisions . 3
7.2 Preparation of standard solutions . 3
7.2.1 Internal standard solution. 3
7.2.2 Preparation of stock standard solutions . 3
7.2.3 Preparation of the calibration solutions . 3
7.3 Ultrasonic extraction and determination of phthalates . 4
7.3.1 General . 4
7.3.2 Preparation of test specimen . 4
7.3.3 Extraction procedure . 4
7.3.4 Phthalates determination . 5
8 Calculation of the results .5
8.1 Calculation based on the corrected mass (by default) . 5
8.2 Calculation based on the total mass (when relevant) . 6
9 Test report . 6
Annex A (normative) Calculations .7
Annex B (informative) Example of test parameters by GC-MS .10
Annex C (informative) Determination of PVC mass fraction by chemical method .12
Annex D (informative) Statistical data .15
Bibliography .21
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SIST EN ISO 14389:2023
ISO 14389:2022(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.
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).
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. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
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 38, Textiles, in collaboration with the
European Committee for Standardization (CEN) Technical Committee CEN/TC 248,Textiles and textile
products, in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna
Agreement).
This second edition cancels and replaces the first edition (ISO 14389:2014), which has been technically
revised.
The main changes are as follows:
— addition of the Clause 2 “Normative references” and renumbering of subsequent clauses;
— replacement of the original internal standard (DCHP) with Benzyl 2-ethyl-hexyl phthalate;
— addition of five detected phthalates (including DCHP);
— replacement of the term “plasticized or soften material” with “plasticized material” in 3.1 (former
2.1);
— revision of the terms and definitions in 3.2 (former 2.2) and 3.3 (former 2.3);
— deletion of the frequency of thermostatic ultrasonic bath in 6.3 (former 5.3);
— deletion of “in duplicate” in 7.3.1 (former 6.2.1);
— revision of extract temperature from “(60 ± 5) °C” to “about 60 °C” in 7.3.3 (former 6.2.3);
— revision of Formula (1) and Formula (2) in Clause 8 (former Clause 7);
— addition of the example of determining the mass of the plastic component (coating) in Annex A.
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.
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SIST EN ISO 14389:2023
ISO 14389:2022(E)
Introduction
This document covers a test method for the determination of some phthalates in textile articles.
Phthalates are commonly used as plasticizers in polymers. Phthalates are an issue for textile
manufacturers and retailers due to their use within motifs, coated fabrics, plastisol prints, buttons, etc.
Phthalates are controversial because high doses of many phthalates have shown hormonal activity in
rodent studies. Studies on rodents involving large amounts of phthalates have shown damage to the
liver, the kidneys, the lungs, and the developing testes.
Due to their potential effect as endocrine disruptors, some of the listed phthalates are toxic in
reproduction. The listed phthalates are based on those which have been restricted in some regulations
(for example, in the European Union).
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SIST EN ISO 14389:2023
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SIST EN ISO 14389:2023
INTERNATIONAL STANDARD ISO 14389:2022(E)
Textiles — Determination of the phthalate content —
Tetrahydrofuran method
WARNING — This document calls for the use of substances and/or procedures that can be
injurious to health if adequate precautions are not taken. It refers only to technical suitability
and does not absolve the user from legal obligations relating to health and safety at any stage.
It has been assumed in the drafting of this document that the execution of its provisions is
entrusted to appropriately qualified and experienced operators.
1 Scope
This document specifies a method of determining phthalates in textiles with gas chromatography–
mass spectrometry (GC-MS).
This document is applicable to textile products where there is a risk of the presence of some phthalates.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological 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/
3.1
plasticized material
plastic material that is treated with chemicals to make it more flexible
Note 1 to entry: For this specific document, the chemicals are phthalates.
EXAMPLE Examples of plastic material: coating, pigment print binder, etc.
3.2
overall treated
with a continuous finish, coating or print
3.3
locally treated
with a discontinuous finish, coating or print
3.4
representative specimen
specimen obtained by mixing pieces of all the different treated parts and colours
4 Principle
The phthalates are extracted from textile specimen by ultrasonic bath with tetrahydrofuran. As
the plastic polymer is partially or completed dissolved, the phthalate extraction is followed by the
1
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SIST EN ISO 14389:2023
ISO 14389:2022(E)
precipitation of the dissolved polymer using the appropriate solvent (acetonitrile, n-hexane, etc.).
Centrifugate the extract and then take a suitable volume of the organic solution for analysis. Gas
chromatography–mass spectrometry (GC–MS) is used to identify individual phthalates in the specimen
and quantify them by using an internal standard (IS).
5 Reagents
Unless otherwise specified, use only reagents of recognized analytical grade.
1)
5.1 Tetrahydrofuran (THF), CAS Registry Number® (CAS RN®): 109-99-9.
5.2 Solvents used for the precipitation. Examples are:
a) Acetonitrile, CAS Registry Number® (CAS RN®): 75-05-8; or
b) n-Hexane, CAS Registry Number® (CAS RN®): 110-54-3.
5.3 The list of phthalates determined by this method is given in Table 1. Other phthalates can be
analysed by this method if the laboratory performs a validation.
Table 1 — List of phthalates
a
No. Substance Abbreviation CAS RN®
1 Di-cyclo-hexyl phthalate DCHP 84-61-7
2 Di-iso-nonyl phthalate DINP 28553-12-0 or 68515-48-0
3 Bis-(2-ethylhexyl) phthalate DEHP 117-81-7
4 Di-n-octyl phthalate DNOP 117-84-0
5 Di-iso-decyl phthalate DIDP 26761-40-0 or 68515-49-1
6 Butyl benzyl phthalate BBP 85-68-7
7 Di-butyl phthalate DBP 84-74-2
8 Di-iso-butyl phthalate DIBP 84-69-5
9 Di-n-pentyl phthalate DPP 131-18-0
1,2-benzenedicarboxylic acid;
10 DIHP 71888-89-6
Di-C -branched alkyl esters, C -rich
6-8 7
11 Bis-(2-methoxyethyl) phthalate DMEP 117-82-8
12 Di-iso-pentyl phthalate DIPP 605-50-5
13 Di-n-hexyl phthalate DNHP 84-75-3
14 N-pentyl-iso-pentyl phthalate PIPP 776297-69-9
15 Di-iso-hexyl phthalate DIHxP 71850-09-4
a
Not all commercially available phthalate standards are of analytical grade.
5.4 Benzyl 2-ethyl-hexyl phthalate, CAS Registry Number® (CAS RN®): 27215-22-1, internal
standard (IS). Other internal standards (for example, deuterated phthalates) can be used if the
laboratory performs a validation.
6 Apparatus
6.1 Gas chromatography, coupled with mass spectrometer (GC–MS).
1) CAS Registry Number® is a trademark of CAS corporation. This information is given for the convenience of
users of this document and does not constitute an endorsement by ISO of the product named. Equivalent products
may be used if they can be shown to lead to the same results.
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SIST EN ISO 14389:2023
ISO 14389:2022(E)
6.2 Vial, airtight glassware to be sealed with a PTFE septum. 40 ml vials have been found suitable.
6.3 Thermostatic ultrasonic bath, with controllable heating capable of maintaining a temperature
of about 60 °C in water bath.
6.4 Glass flasks with glass stoppers. 100 ml glass flasks have been found suitable.
6.5 Calibrated volumetric flasks, of capacities 50 ml and 100 ml.
6.6 Volumetric device, of capacities 10 ml and 20 ml.
6.7 Analytical balance, with a resolution of 0,1 mg.
6.8 Centrifuge.
7 Procedure
WARNING — The vapour of the organic solvents is highly flammable, especially at high
temperature. Allow glassware to cool down before use.
7.1 Cross-contamination provisions
Glassware and/or equipment used shall be free from phthalates in order to minimize cross-
contamination. For pre-used glassware, after washing, should be given an extra rinse with 0,1 mol/l
nitric acid, water and finally with acetone. Glassware should be completely dried before use. To avoid
contamination, do not use any plastic container (for example, for water).
7.2 Preparation of standard solutions
7.2.1 Internal standard solution
Prepare a 1 000 mg/l stock standard solution of the internal standard in the solvent used for the
precipitation (5.2) after the ultrasonic extraction (see 7.3).
7.2.2 Preparation of stock standard solutions
Separately prepare a series of 1 000 mg/l individual stock standard solutions of the individual phthalate
(5.3) in the solvent used for the precipitation.
For example, weigh 50,0 mg of a phthalate in a 50 ml volumetric flask and fill the volumetric flask up
to the mark with the solvent used for the precipitation and mix thoroughly to dissolve completely the
substance.
Most of the stock standards may be made in a mixed stock. This saves time and effort when preparing
calibration solutions. DINP, DIDP and DIHP have overlapping peaks. It is recommended to make up
these stock standard solutions separately, as their calibration solutions have to be made in higher (for
example, 5 times) concentrations than for the other phthalates because of their multi-peak nature.
7.2.3 Preparation of the calibration solutions
From the stock standard solutions, prepare at least five appropriate phthalate calibration solutions
(example of concentrations at 1 mg/l, 3 mg/l, 15 mg/l, 30 mg/l and 90 mg/l as described in the Table 2),
each containing an equal amount of the target phthalates (5.3) and an amount of internal standard (5.4)
in a mixture of tetrahydrofuran and the solvent used for the precipitation, mixed by volume at a ratio of
1:2 (1/3 of tetrahydrofuran to 2/3 of the other solvent), as shown in Table 2. Each calibration solution
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SIST EN ISO 14389:2023
ISO 14389:2022(E)
should have a final internal standard concentration of 5 mg/l. Prepare one calibration blank. Analyse
the calibration solutions and calibration blank by the GC-MS. Qualitatively analyse the result to ensure
proper retention times and the absence of contamination and built up the calibration curve.
Table 2 — Examples of calibration solutions
Operation items Blank L1 L2 L3 L4 L5
Concentration of phthalate (mg/l) 0 1 3 15 30 90
Volumetric flask (ml) 50 100 100 50 50 50
Volume of phthalate stock solution (ml) / 0,1 0,3 0,75 1,5 4,5
Volume of internal solution (ml) 0,25 0,5 0,5 0,25 0,25 0,25
with a mixture of 1/3 of tetrahydrofuran to 2/3 of the sol-
Fill up to the mark
vent used for the precipitation
If target ions other than 149 are used for quantification of DEHP, DNOP, DINP, DIDP and DIHP, all the
listed phthalates may be calibrated and quantified together.
Typical quantification ions for phthalates are shown in Annex B.
If DIDP and DINP overlap in the chromatogram; choose target ions indicated in Annex B.
In case the concentration of some phthalate in the extraction solution of a specimen lies outside the
limits of the calibration curve, dilute the solution with a mixture of 1/3 of tetrahydrofuran to 2/3 of the
solvent used for the precipitation containing 5 mg/l of the internal standard, so that the phthalates in
the sample can be properly quantified.
NOTE The stock standard solutions are stored at 0 °C to 4 °C for up to six months, and the working solutions
are stored at 0 °C to 4 °C for up to three months, or sooner if ongoing quality control indicates problems.
7.3 Ultrasonic extraction and determination of phthalates
7.3.1 General
Ultrasonic extraction is performed using tetrahydrofuran on test specimens prepared from each textile
sample, followed by precipitation of the (partially or completed) dissolved plastic component using an
appropriate solvent, centrifugation, and determination of phthalates. A blank is run in parallel to avoid
errors caused by contamination from the laboratory environment.
NOTE For example, polyvinylchloride (PVC) is completely dissolved in tetrahydrofuran.
7.3.2 Preparation of test specimen
A representative test specimen shall be prepared by mixing and cutting pieces from every coated area/
part of the textile sample (see Annex A for further information on coating types). Cut the representative
specimen into small pieces (less than 5 mm in the greatest dimension), homogenize it, and weigh
(0,30 ± 0,01) g of these pieces in the vial (6.2).
Using an appropriate volumetric device (6.6), add to vial 10 ml of tetrahydrofuran (5.1) containing
5 mg/l of internal standard (5.4) and seal it tightly.
7.3.3 Extraction procedure
Place the vial in the ultrasonic bath (6.3) at about 60 °C for 1 h ± 5 min to allow the extraction of
phthalates (by complete or partial dissolution of the polymer). Then, remove the vial from the bath and
let it stand still until the extraction solution cools down to room temperature.
Ensure that the vial remain airtight in the ultrasonic bath (6.3) throughout the entire extraction
process.
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SIST EN ISO 14389:2023
ISO 14389:2022(E)
Using an appropriate volumetric device (6.6), add dropwise to the vial 20 ml of the solvent used for the
precipitation (5.2) containing 5 mg/l of internal standard.
Shake the vial vigorously (preferably on a vortex type shaker) for at least 30 s and allow them to stand
still for (30 ± 2) min in order to allow the precipitation of polymer.
-1
Centrifugate the vial at least 700 g (for example, 2 500 min for 10 cm radius) by the centrifuge (6.8) for
at least 10 min to drive and settle any remaining suspended precipitates of polymer in organic phase to
the bottom to obtain a transparent organic solution. Then, withdraw and transfer a specimen aliquot of
the organic solution into a suitable GC sampling vial for GC-MS analysis.
CAUTION — Direct injection into GC-MS of suspended matter solution or cloudy solution might
contaminate the equipment.
If necessary, prepare further diluted solutions using an appropriate volume of a mixture of
tetrahydrofuran (5.1) and the solvent used for the precipitation (5.2) mixed by volume at a ratio of 1:2
(1/3 of tetrahydrofuran to 2/3 of the other solvent) containing 5 mg/l of the internal standard (5.4) and
then repeat the analysis.
7.3.4 Phthalates determination
Determinate the phthalates extracted in 7.3.3 by GC-MS (6.1).
An example of the parameters for GC-MS analysis of target phthalates is given in Annex B.
The statistical data of interlaboratory trials in the first edition is shown in Annex D.
In some cases when the phthalates level is very low, it may be necessary to increase the mass of the test
specimens.
8 Calculation of the results
8.1 Calculation based on the corrected mass (by default)
From the calibration graph, determine the response of each phthalate, corrected for the internal
standard peak area, and interpolate the concentration of the phthalate, in milligrams per litre (mg/l),
correcting for any dilutions. Subtract the blank concentration from the specimen concentration.
Calculate the result using Formula (1):
Vb×−()aF×
w = (1)
c
m ×10 000
c
where
w is the mass fraction of the individual phthalate, based on the corrected mass of the test specimen
c
(%);
V is 30 ml, that is the total volume of the phthalate solution before any dilution (10 ml of tetrahy-
drofuran used for the extraction +20 ml of the solvent used in the precipitation step);
m is the corrected mass of specimen (g);
c
a is the concentration of the individual phthalate of the blank solution (mg/l);
b is the concentration of the individual phthalate of the specimen solution (mg/l);
F is the dilution factor.
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SIST EN ISO 14389:2023
ISO 14389:2022(E)
The determination of the corrected mass of test specimen shall be in accordance with Annex A.
Examples of the calculation are also given. Overall treated materials are illustrated in Figure A.1 and
locally treated materials in Figure A.2.
If the corrected mass of the test specimen, m , cannot be obtained, give a remark in the test report and
c
calculate the result according to 8.2.
8.2 Calculation based on the total mass (when relevant)
If the corrected mass of the test specimen, m , in accordance with Annex A, cannot be obtained and
c
used for the calculation of the results, then calculate the result using Formula (2).
Vb×−()aF×
w = (2)
T
m ×10 000
T
w
...
SLOVENSKI STANDARD
oSIST prEN ISO 14389:2022
01-januar-2022
Tekstilije - Določevanje ftalatov - Tetrahidrofuranska metoda (ISO/DIS 14389:2021)
Textiles - Determination of the phthalate content - Tetrahydrofuran method (ISO/DIS
14389:2021)
Textilien - Bestimmung des Phthalatanteils - Tetrahydrofuran-Verfahren (ISO/DIS
14389:2021)
Textiles - Détermination de la teneur en phtalates - Méthode au tétrahydrofurane
(ISO/DIS 14389:2021)
Ta slovenski standard je istoveten z: prEN ISO 14389
ICS:
59.060.01 Tekstilna vlakna na splošno Textile fibres in general
oSIST prEN ISO 14389:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN ISO 14389:2022
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oSIST prEN ISO 14389:2022
DRAFT INTERNATIONAL STANDARD
ISO/DIS 14389
ISO/TC 38 Secretariat: JISC
Voting begins on: Voting terminates on:
2021-10-28 2022-01-20
Textiles — Determination of the phthalate content —
Tetrahydrofuran method
Textiles — Détermination de la teneur en phtalates — Méthode au tétrahydrofurane
ICS: 59.060.01
THIS DOCUMENT IS A DRAFT CIRCULATED
This document is circulated as received from the committee secretariat.
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
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oSIST prEN ISO 14389:2022
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Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 2
6 Apparatus . 2
7 Procedure. 3
7.1 Preparation of standard solutions . 3
7.1.1 Internal standard solution . 3
7.1.2 Preparation of stock standard solutions . 3
7.1.3 Preparation of the calibration solutions . 3
7.2 Ultrasonic extraction and determination of phthalates . 4
7.2.1 General. 4
7.2.2 Preparation of test specimen . 4
7.2.3 Extraction procedure . 5
7.2.4 Phthalates determination . 5
8 Calculation of the results . 5
8.1 Calculation based on the corrected mass (by default). 5
8.2 Calculation based on the total mass (when relevant) . 6
9 Test report . 6
Annex A (normative) Calculations . 7
Annex B (informative) Example of test parameters by GC-MS .10
Annex C (informative) Determination of PVC mass fraction by chemical method .12
Annex D (informative) Statistical data.15
Bibliography .23
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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 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).
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. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/ patents).
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 38, Textiles.
This second edition cancels and replaces the first edition (ISO 14389:2014), which has been technically
revised.
The main changes compared to the previous edition are as follows:
— in clause 5, four detected substances have been added, the original internal standard (DCHP)
has been replaced with Benzyl 2-ethyl-hexyl phthalate and DCHP has been regarded as detected
substance;
— in 6.3, the frequency of thermostatic ultrasonic bath has been deleted;
— in 7.2.1, “in duplicate” has been deleted;
— in 7.2.3, extract temperature has been changed from (60 ± 5) °C to about 60 °C;
— in Annex A, the example of determining the mass of the plastic component (coating) has been added.
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.
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Introduction
This document covers a test method for the determination of some phthalates in textile articles.
Phthalates are commonly used as plasticizers in polymers. Phthalates are an issue for textile
manufacturers and retailers due to their use within motifs, coated fabrics, plastisol prints, buttons, etc.
Phthalates are controversial because high doses of many phthalates have shown hormonal activity in
rodent studies. Studies on rodents involving large amounts of phthalates have shown damage to the
liver, the kidneys, the lungs, and the developing testes.
Due to their potential effect as endocrine disruptors, some of the listed phthalates are toxic in
reproduction. The listed phthalates are based on those which have been restricted in some regulations
(e.g. in the European Union).
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oSIST prEN ISO 14389:2022
DRAFT INTERNATIONAL STANDARD ISO/DIS 14389:2021(E)
Textiles — Determination of the phthalate content —
Tetrahydrofuran method
WARNING — This document calls for the use of substances and/or procedures that might be
injurious to health if adequate precautions are not taken. It refers only to technical suitability
and does not absolve the user from legal obligations relating to health and safety at any stage.
It has been assumed in the drafting of this document that the execution of its provisions is
entrusted to appropriately qualified and experienced operators.
1 Scope
This document specifies a method of determining phthalates in textiles with gas chromatography–
mass spectrometry (GC-MS) with mass selective detector.
This document is applicable to textile products where there is a risk of the presence of some phthalates.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological 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/
3.1
plasticized or softened material
plastic material that is treated with chemicals to make it more flexible
Note 1 to entry: For this specific document, the chemicals are phthalates.
EXAMPLE Examples of plastic material: coating, pigment print binder, etc.
3.2
overall treated textiles
textiles with a continuous finish, coating or print
3.3
locally treated textiles
textiles with a discontinuous finish, coating or print
3.4
representative specimen
specimen obtained by mixing pieces of all the different treated parts and colours
4 Principle
The phthalates are extracted from textile specimen by ultrasonic generator with tetrahydrofuran.
As the plastic polymer is partially or completed dissolved, the phthalate extraction is followed by the
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precipitation of the dissolved polymer using the appropriate solvent (acetonitrile, n-hexane, etc.). After
centrifugation and dilution of the extract to volume, gas chromatography–mass spectrometry (GC-
MS) is used to identify individual phthalates in the specimen and quantify them by using an internal
standard (IS).
5 Reagents
Unless otherwise specified, use only reagents of recognized analytical grade.
5.1 Tetrahydrofuran (THF), CAS number: 109-99-9.
5.2 Solvents used for the precipitation. Examples are:
5.2.1 Acetonitrile, CAS number: 75-05-8.
5.2.2 n-Hexane, CAS number: 110-54-3.
5.3 List of phthalates determined by this document in Table 1
Table 1 — List of phthalates
a
No. Substance Abbreviation CAS RN®
5.3.1 Di-cyclo-hexyl phthalate DCHP 84-61-7
5.3.2 Di-iso-nonyl phthalate DINP 28553-12-0 or 68515-48-0
5.3.3 Bis-(2-ethylhexyl) phthalate DEHP 117-81-7
5.3.4 Di-n-octyl phthalate DNOP 117-84-0
5.3.5 Di-iso-decyl phthalate DIDP 26761-40-0 or 68515-49-1
5.3.6 Butyl benzyl phthalate BBP 85-68-7
5.3.7 Di-butyl phthalate DBP 84-74-2
5.3.8 Di-iso-butyl phthalate DIBP 84-69-5
5.3.9 Di-n-pentyl phthalate DPP 131-18-0
1,2-benzenedicarboxylic acid;
5.3.10 DIHP 71888-89-6
Di-C -branched alkyl esters, C -rich
6-8 7
5.3.11 Bis-(2methoxyethyl) phthalate DMEP 117-82-8
5.3.12 Di-iso-pentyl phthalate DIPP 605-50-5
5.3.13 Di-n-hexyl phthalate DNHP 84-75-3
5.3.14 N-pentyl-iso-pentyl phthalate PIPP 776297-69-9
5.3.15 Di-iso-hexyl phthalate DIHxP 71850-09-4
a
Not all commercially available phthalate standards are of analytical grade.
5.4 Benzyl 2-ethyl-hexyl phthalate, CAS number: 27215-22-1, internal standard (IS).
6 Apparatus
6.1 Gas chromatograph-mass spectrometry (GC-MS).
6.2 Vial, airtight glassware to be sealed with a PTFE septum. 40 ml vials have been found suitable.
6.3 Thermostatic ultrasonic bath, with controllable heating capable of maintaining a temperature of
about 60 °C.
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6.4 Glass flasks with glass stoppers. 100 ml glass flasks have been found suitable.
6.5 Calibrated volumetric flasks, of capacities 50 ml and 100 ml.
6.6 Volumetric device, of capacities 10 ml and 20 ml.
6.7 Balance, with a resolution of 0,1 mg.
6.8 Water bath.
6.9 Rotary evaporator.
7 Procedure
WARNING — The vapour of the organic solvents is highly flammable, especially at high
temperature. Allow glassware to cool down before use.
Avoid direct contact between the samples and glassware and/or equipment used in order to minimize
cross-contamination. Glassware, after washing, should be given an extra rinse with 0,1 N nitric
acid, water and finally with acetone. Glassware should be completely dried before use. To avoid
contamination, do not use any plastic container (e.g. for water).
7.1 Preparation of standard solutions
7.1.1 Internal standard solution
Prepare a 1 000 mg/l stock standard solution of the internal standard in the solvent used for the
precipitation (5.2) after the ultrasonic extraction (see 7.2).
7.1.2 Preparation of stock standard solutions
Separately prepare a series of 1 000 mg/l individual stock standard solutions of the individual phthalate
(5.3) in the solvent used for the precipitation.
For example, weigh 50,0 mg of a phthalate in a 50 ml volumetric flask and fill the volumetric flask up
to the mark with the solvent used for the precipitation and mix thoroughly to dissolve completely the
substance.
Most of the stock standards may be made in a mixed stock. This saves time and effort when preparing
calibration solutions. DINP, DIDP and DIHP have overlapping peaks. It is recommended to make up
these stock standard solutions separately, as their calibration solutions have to be made in higher (5x)
concentrations than for the other phthalates because of their multi-peak nature.
7.1.3 Preparation of the calibration solutions
From the stock standard solutions, prepare at least five appropriate phthalate calibration solutions
(example of concentrations at 1 mg/l, 3 mg/l, 15 mg/l, 30 mg/l and 90 mg/l as described in the Table 2),
each containing an equal amount of the target phthalates (5.3) and an amount of internal standard (5.4)
in a mixture of tetrahydrofuran and the solvent used for the precipitation, mixed by volume at a ratio
of 1:2 (33 parts tetrahydrofuran to 66 parts of the other solvent), as shown in Table 2. Each calibration
solution should have a final internal standard concentration of 5 mg/l. Prepare one calibration blank.
Analyse the calibration solutions and calibration blank with the GC-MS. Qualitatively analyse the result
to ensure proper retention times and the absence of contamination and built up the calibration curve.
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Table 2 — Examples of calibration solutions
Concentration Instructions
Blank In a 50 ml volumetric flask, add 0,25 ml of internal standard (5.4) stock solution; then,
fill up to the mark with a mixture of tetrahydrofuran and the solvent used for the pre-
cipitation, mixed by volume at a ratio of 1:2 (33 parts tetrahydrofuran to 66 parts of the
other solvent)
1 mg/l Add 0,1 ml of each stock standard solution in 100 ml volumetric flask plus 0,5 ml of the
internal standard (5.4) stock solution; then, fill up to the mark with a mixture of 33 parts
of tetrahydrofuran to 66 parts of the solvent used for the precipitation.
3 mg/l Add 0,3 ml of each stock standard solution in 100 ml volumetric flask plus 0,5 ml of the
internal standard (5.4) stock solution; then, fill up to the mark with a mixture of 33 parts
of tetrahydrofuran to 66 parts of the solvent used for the precipitation.
15 mg/l Add 0,75 ml of each stock standard solution in 50 ml volumetric flask plus 0,25 ml of the
internal standard (5.4) stock solution; then, fill up to the mark with a mixture of 33 parts
of tetrahydrofuran to 66 parts of the solvent used for the precipitation.
30 mg/l Add 1,5 ml of each stock standard solution in 50 ml volumetric flask plus 0,25 ml of the
internal standard (5.4) stock solution; then, fill up to the mark with a mixture of 33 parts
of tetrahydrofuran to 66 parts of the solvent used for the precipitation.
90 mg/l Add 4,5 ml of each stock standard solution in 50 ml volumetric flask plus 0,25 ml of the
internal standard (5.4) stock solution; then, fill up to the mark with a mixture of 33 parts
of tetrahydrofuran to 66 parts of the solvent used for the precipitation.
If target ions other than 149 are used for quantification of DEHP, DNOP, DINP, DIDP and DIHP, all the
listed phthalates may be calibrated and quantified together.
Typical quantification ions for phthalates are shown in Annex B.
If DIDP and DINP overlap in the chromatogram; choose target ions indicated in Annex B.
In case the concentration of some phthalate in the extraction solution of a specimen lies outside the
limits of the calibration curve, dilute the solution with a mixture of 33 parts of tetrahydrofuran to 66
parts of the solvent used for the precipitation containing 5 mg/l of the internal standard, so that the
sample can be properly quantified.
NOTE The stock standard solutions are stored at 0 °C to 4 °C for up to six months, and the working solutions
are stored at 0 °C to 4 °C for up to three months, or sooner if ongoing quality control indicates problems.
7.2 Ultrasonic extraction and determination of phthalates
7.2.1 General
Ultrasonic extraction is performed using tetrahydrofuran on test specimens prepared from each textile
sample, followed by precipitation of the (partially or completed) dissolved plastic component using an
appropriate solvent, centrifugation, and determination of phthalates. A blank is run in parallel to avoid
errors caused by contamination from the laboratory environment.
NOTE For example, polyvinylchloride (PVC) is completely dissolved in tetrahydrofuran.
7.2.2 Preparation of test specimen
A representative test specimen shall be prepared by mixing and cutting pieces from every coated area/
part of the textile sample (see Annex A for further information on coating types). Cut the representative
specimen into small pieces (less than 5 mm in the greatest dimension), homogenize it, and weigh
(0,30 ± 0,01) g of these pieces in the vial (6.2).
Using an appropriate volumetric graduated pipette (6.6), add to vial 10 ml of tetrahydrofuran (5.1)
containing 5 mg/l of internal standard (5.4) and seal it tightly.
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7.2.3 Extraction procedure
Place the vial in the ultrasonic bath (6.3) at about 60 °C for 1 h ± 5 min to allow the extraction of
phthalates (by complete or partial dissolution of the polymer).Then, remove the vial from the bath and
let them stand still until the extraction solution cools down to room temperature.
Ensure that the vial remain airtight in the ultrasonic bath (6.3) throughout the entire extraction
process.
Using an appropriate volumetric device, add dropwise to the vial 20 ml of the solvent used for the
precipitation (5.2) containing 5 mg/l of internal standard.
Shake the vial vigorously (preferably on a vortex type shaker) for at least 30 s and allow them to stand
still for (30 ± 2) min in order to allow the precipitation of polymer.
Centrifuge the vial at least 700 g (e.g. 2 500 r/min for 10 cm radius) for at least 10 min to drive and
settle any remaining suspended precipitates of polymer in organic phase to the bottom to obtain a
transparent organic solution. Then, withdraw and transfer a specimen aliquot of the organic solution
into two suitable GC sampling vial for GC-MS analysis.
CAUTION — Direct injection into GC-MS of suspended matter solution or cloudy solution might
contaminate the equipment.
If necessary, prepare further diluted solutions using an appropriate volume of a mixture of
tetrahydrofuran (5.1) and the solvent used for the precipitation (5.2) mixed by volume at a ratio of 1:2
(33 parts tetrahydrofuran to 66 parts of the other solvent) containing 5 mg/l of the internal standard
(5.4) and then repeat the analysis.
7.2.4 Phthalates determination
Determinate the phthalates extracted in 7.2.3 by GC-MS (6.1). An example of the parameters for GC-MS
analysis of target phthalates is given in Annex B.
In some cases when the phthalates level is very low, it may be necessary to increase the mass of the test
specimens.
8 Calculation of the results
8.1 Calculation based on the corrected mass (by default)
From the calibration graph, determine the response of each phthalate, taking into account the internal
standard peak area, and interpolate the concentration of the phthalate, in milligrams per litre (mg/l),
correcting for any dilutions. Subtract the blank concentration from the specimen concentration.
Calculate the result using Formula (1):
Vb××() Fa−
w = (1)
c
m ×10 000
c
where
w is the mass fraction of the individual phthalate, based on the corrected mass of the test specimen (%);
c
V is 30 ml, that is the total volume of the phthalate solution before any dilution (10 ml of tetrahydro-
furan used for the extraction +20 ml of the solvent used in the precipitation step);
m is the corrected mass of specimen (g);
c
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a is the concentration of the individual phthalate of the blank solution (mg/l);
b is the concentration of the individual phthalate of the specimen solution (mg/l);
F is the dilution factor.
The determination of the corrected mass of test specimen is given in Annex A, as well as an example
of the calculation. Overall treated material is illustrated in Figure A.1 and locally treated material in
Figure A.2.
If the corrected mass of the test specimen, m , cannot be obtained, give a remark in the test report and
c
calculate the result according to 8.2.
8.2 Calculation based on the total mass (when relevant)
If the corrected mass of the test specimen, m , as described in Annex A, cannot be obtained and used for
c
the calculation of the results, then calculate the result using Formula (2).
Vb××()Fa−
w = (2)
T
m ×10 000
T
where
w is the mass fraction of the individual phthalate, based on the total mass of the test specimen (%);
T
V is 30 ml, that is the total volume of the phthalate solution before any dilution (10 ml of tetrahy-
drofuran used for the extraction + 20 ml of the solvent used in the precipitation step);
m is the total mass of specimen (g);
T
a is the concentration of the individual phthalate of the blank solution (mg/l);
b is the concentration of the individual phthalate of the specimen solution (mg/l);
F is the dilution factor.
9 Test report
The test report shall include the following information:
a) a reference to this International Standard, i.e. ISO 14389;
b) all details necessary for complete identification of the sample tested;
c) details on the preparation of the specimens;
d) the value of the corrected mass, m , in grams (see 8.1); where relevant, the value of the total mass,
c
m , in grams (see 8.2);
T
e) the test results of each listed phthalate in the plasticized material or textile product, w (or, where
c
relevant, w ), expressed in percentage (%) or milligram per kilogram (mg/kg);
T
f) any deviation by agreement or otherwise from the procedure specified;
g) the date of the test.
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Annex A
(normative)
Calculations
A.1 Overall treated specimens
In the case of overall treated specimens, see Figure A.1:
Key
1 plastic component (coating)
2 fabric
Figure A.1 — Overall treated materials
The part of the coating is defined using Formula (A.1):
mm=− m (A.1)
12
where
m is the total mass of overall treated specimen (g);
1
m is the mass of textile component (g);
2
m is the mass of coating (g).
NOTE The mass of coating is the corrected mass of the specimen as described in Formula (1).
From a test specimen, where the total mass of overall treated specimen, m , is measured (g), the plastic
1
component (coating) is removed by a mechanical, thermal or chemical procedure (or a combination of
these). The plastic component, m, shall be determined by comparison with the textile component m .
2
NOTE An example of chemical procedure is given in Annex C.
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A.2 Locally treated specimens
A.2.1 In the case of locally treated specimens, see Figure A.2.
Key
1 plastic component (coating)
2 fabric
Figure A.2 — Locally treated specimen
The mass of the plastic component, m, expressed in grams (g), is calculated using Formula (A.2):
mm=−()mS× (A.2)
12
where
2
m is the surface density (mass divided by area) of treated area of specimen (g/m );
1
2
m is the surface density (mass divided by area) of textile material (g/m );
2
m is the mass of the plastic component (coating) (g);
NOTE The mass of the plastic component is the corrected mass of the specimen as described in
Formula (1).
2
S is the surface area of the treated area of the specimen (m );
Firstly, determine the surface density (mass divided by area) from an untreated part (only textile
material is involved) m .
2
From a test specimen:
—
...
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