ISO/FDIS 8124-6

Safety of toys — Part 6: Certain phthalate esters

Sécurité des jouets — Partie 6: Certains esters de phtalates

General Information

• Status: Not Published
• ICS: 97.200.50 - Toys
• Technical Committee: ISO/TC 181 - Safety of toys
• Drafting Committee: ISO/TC 181/WG 6 - Phthalate plasticizers in toys
• Current Stage: 5020 - FDIS ballot initiated: 2 months. Proof sent to secretariat
• Start Date: 13-Apr-2023
• Completion Date: 13-Apr-2023

Relations

• Revises: ISO 8124-6:2018 - Safety of toys — Part 6: Certain phthalate esters in toys and children's products
• Effective Date: 23-Apr-2020

Standards Content (Sample)

DRAFT INTERNATIONAL STANDARD
ISO/DIS 8124-6
ISO/TC 181 Secretariat: DS
Voting begins on: Voting terminates on:
2022-06-27 2022-09-19
Safety of toys —
Part 6:
Certain phthalate esters in toys and children's products
Sécurité des jouets —

Partie 6: Dosage de certains esters de phtalates dans les jouets et produits pour enfants

ICS: 97.200.50
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
This document is circulated as received from the committee secretariat.
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
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USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 8124-6:2022(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
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PROVIDE SUPPORTING DOCUMENTATION. © ISO 2022
---------------------- Page: 1 ----------------------
ISO/DIS 8124-6:2022(E)
DRAFT INTERNATIONAL STANDARD
ISO/DIS 8124-6
ISO/TC 181 Secretariat: DS
Voting begins on: Voting terminates on:
Safety of toys —
Part 6:
Certain phthalate esters in toys and children's products
Sécurité des jouets —

Partie 6: Dosage de certains esters de phtalates dans les jouets et produits pour enfants

ICS: 97.200.50
COPYRIGHT PROTECTED DOCUMENT
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENT AND APPROVAL. IT IS
© ISO 2022
THEREFORE SUBJECT TO CHANGE AND MAY
This document is circulated as received from the committee secretariat.

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

NOT BE REFERRED TO AS AN INTERNATIONAL

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on STANDARD UNTIL PUBLISHED AS SUCH.

the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below

IN ADDITION TO THEIR EVALUATION AS

or ISO’s member body in the country of the requester. BEING ACCEPTABLE FOR INDUSTRIAL,

TECHNOLOGICAL, COMMERCIAL AND
ISO copyright office
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STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
CH-1214 Vernier, Geneva
POTENTIAL TO BECOME STANDARDS TO
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Reference number
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NATIONAL REGULATIONS.
Website: www.iso.org ISO/DIS 8124-6:2022(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
Published in Switzerland
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
© ISO 2022 – All rights reserved
PROVIDE SUPPORTING DOCUMENTATION. © ISO 2022
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ISO/DIS 8124-6:2022(E)
Contents Page

Foreword ..........................................................................................................................................................................................................................................v

Introduction .............................................................................................................................................................................................................................. vi

1 Scope (mandatory) .............................................................................................................................................................................................. 1

2 Normative references (mandatory) .................................................................................................................................................. 1

3 Terms and definitions (mandatory) ........................................................................................................................................... ......1

4 Principle ........................................................................................................................................................................................................................ 2

5 Reagents ........................................................................................................................................................................................................................ 2

6 Apparatus .................................................................................................................................................................................................................... 3

7 Selection of test portion ............................................................................................................................................................................... 4

7.1 General principle .................................................................................................................................................................................. 4

7.2 Individual test ......................................................................................................................................................................................... 4

7.3 Composite test ........................................................................................................................................................................................ 5

8 Procedure ....................................................................................................................................................................................................................5

8.1 General ........................................................................................................................................................................................................... 5

8.2 Sample weighing ................................................................................................................................................................................... 5

8.2.1 Individual test ....................................................................................................................................................................... 5

8.2.2 Composite test ...................................................................................................................................................................... 5

8.3 Extraction ................................................................................................................................................................................................... 5

8.3.1 Options of extraction method ................................................................................................................................. 5

8.3.2 Method A ................................... ........................................................................................................ ......................................... 5

8.3.3 Method B .................................................................................................................................................................................... 6

8.3.4 Method C .................................................................................................................................................................................... 6

8.4 Sample solution for analysis ....................................................................................................................................................... 6

8.4.1 General ........................................................................................................................................................................................ 6

8.4.2 Quantification by external standard (ES) calibration ...................................................................... 7

8.4.3 Quantification by IS calibration ............................................................................................................................ 7

8.5 Determination ......................................................................................................................................................................................... 8

8.5.1 GC-MS conditions ............................................................................................................................................................... 8

8.5.2 Identification ......................................................................................................................................................................... 8

8.5.3 Calibration ................................... ........................................................................................................ ..................................... 9

9 Calculation ...............................................................................................................................................................................................................10

9.1 Individual test ...................................................................................................................................................................................... 10

9.1.1 External standard (ES) calculation ................................................................................................................ 10

9.1.2 Internal standard (IS) calculation ................................................................................................................... 10

9.2 Composite test ..................................................................................................................................................................................... 11

9.2.1 Concentration calculation ....................................................................................................................................... 11

9.2.2 Judgment for next action .......................................................................................................................................... 11

9.2.3 Examples ................................................................................................................................................................................12

10 Quality control ....................................................................................................................................................................................................13

10.1 LOQ of method (LOQ ) ........................................................................................................................................... ......................13

10.2 Method blank ........................................................................................................................................................................................ 13

10.3 Recovery ....................................................................................................................................................................................................13

10.4 Calibration check ............................................................................................................................................................................... 13

11 Precision ....................................................................................................................................................................................................................13

12 Test report ...............................................................................................................................................................................................................13

Annex A (normative) Phthalate esters ...........................................................................................................................................................14

Annex B (informative) Precision of the method ...................................................................................................................................15

Annex C (informative) Soxhlet extractor and solvent extractor .........................................................................................19

iii
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ISO/DIS 8124-6:2022(E)

Annex D (informative) Composite test ...........................................................................................................................................................22

Annex E (normative) Ultrasonic bath performance check ........................................................................................................28

Annex F (informative) Example of GC-MS conditions .....................................................................................................................31

Annex G (informative) Background and rationale ............................................................................................................................36

Bibliography .............................................................................................................................................................................................................................39

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ISO/DIS 8124-6:2022(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 181, Safety of toys.
A list of all parts in the ISO 8124 series can be found on the ISO website.

This third edition of ISO 8124-6 cancels and replaces the second edition (ISO 8124-6:2018), which has

been technically revised.
The main changes compared to ISO 8124-6:2018 are as follows:
— addition of a new definition for instrument detection limit in (3.9);
— replacement of “4 °C” with “0 °C to 8 °C” in (5.3, 5.4, 5.5.2, and 5.5.3);
— addition of a maximum test portion for the composite test in (8.1);
— addition of a clean-up step in (8.3.1);

— addition of the volume of the final solution may be adjusted from 1 ml to 50 ml in (8.3.2.1, 8.3.2.2.1

and 8.3.2.2.2);
— addition of the composite test model in Annex D status;
— addition of a list including other phthalate esters in G.2;

— Clause 7 has been modified significantly. The normative requirements have been moved from

Annex D to Clause 7 and Annex D has subsequently been changed into an informative annex.

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ISO/DIS 8124-6:2022(E)
Introduction

This document is largely based upon the existing Chinese national standard GB/T 22048-2015. Relevant

standards of some countries and regions are referred to as well.

This document does not set out limits for phthalate esters. It is intended to be used as a method

standard in conformity assessment. The user of this document is therefore advised to be aware of

relevant national requirements.

In some countries phthalate ester requirements for toys are also applicable to children’s products and

children’s product materials are generally similar to those of toys. This document, whose scope covers

various materials, is therefore applicable to both toys and children’s products.

Annex A and Annex E are normative, whereas Annex B, Annex C, Annex D, Annex F, and Annex G are for

information only. However, they are crucial and helpful for the correct interpretation of this document.

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DRAFT INTERNATIONAL STANDARD ISO/DIS 8124-6:2022(E)
Safety of toys —
Part 6:
Certain phthalate esters in toys and children's products

WARNING — Persons using this document should be familiar with normal laboratory practice.

This document does not purport to address all of the safety problems, if any, associated with its

use. It is the responsibility of the user to establish appropriate safety and health practices.

IMPORTANT — It is absolutely essential that tests conducted in accordance with this document

should be carried out by suitably trained staff.
1 Scope (mandatory)

This document specifies a method for the determination of di-iso-butyl phthalate (DIBP), di-n-butyl

phthalate (DBP), benzyl-butyl phthalate (BBP), bis-(2-ethylhexyl) phthalate (DEHP), di-n-octyl

phthalate (DNOP), di-iso-nonyl phthalate (DINP) and di-iso-decyl phthalate (DIDP) (as specified in

Annex A) in toys and children’s products.

This document is applicable to toys and children’s products which are made of plastics, textiles, coatings

and liquids. This document has been validated for polyvinylchloride (PVC) plastics, polyurethane

(PU) plastics and some representative paint coatings (see Annex B). It might also be applicable to

other phthalate esters (see G.2) and other product materials provided that adequate validation is

demonstrated.
2 Normative references (mandatory)

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 2758, Paper — Determination of bursting strength

ISO 8124-1:2018, Safety of toys — Part 1: Safety aspects related to mechanical and physical properties

3 Terms and definitions (mandatory)
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
laboratory sample

toy or children’s product in the form in which it is marketed or intended to be marketed

Note 1 to entry: Text of the note.
3.2
base material
material upon which coatings may be formed or deposited
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ISO/DIS 8124-6:2022(E)
3.3
coating

layers of material formed or deposited on the base material of toys or children’s products, including

paints, varnishes, lacquers, inks, polymers or other substances of a similar nature, whether they

contain metallic particles or not, no matter how they have been applied to the toy or children’s product

and which can be removed by scraping with a sharp blade
3.4
scraping
mechanical process for removal of coatings (3.3) down to the base material (3.2)
3.5
test portion

portion of homogeneous material taken from a corresponding part of the laboratory sample for analysis

3.6
composite test portion

mixed test portion formed by physically mixing several test portions of similar materials

Note 1 to entry: This term excludes the compositing of dissimilar materials; for example, compositing textiles

and paint coatings are not permitted.
3.7
composite test
test performed on the composite test portion (3.6)
3.8
limit of quantification
LOQ

lowest amount of the analyte in the sample that can be quantitatively determined with defined precision

and accuracy under the stated experimental conditions
3.9
method blank

aliquot of solvents that is treated exactly as a sample, including exposure to glassware, apparatus and

conditions used for a particular test, but with no added sample

Note 1 to entry: Method blank data are used to assess contamination from the laboratory environment.

4 Principle

The test portion of a toy or children’s product is extracted through a Soxhlet extractor, solvent extractor

(see Annex C) or ultrasonic bath with dichloromethane. Phthalate esters in the extract are determined

qualitatively and quantitatively by gas chromatography-mass spectrometry (GC-MS).

5 Reagents

5.1 Dichloromethane, CAS No. 75-09-2, analytical grade or higher, free of phthalate esters.

5.2 Phthalate esters reference substances, DIBP, DBP, BBP, DEHP, DNOP, DINP and DIDP (as

specified in Annex A), minimum of 95 % purity.

5.3 Stock solution, 100 mg/l of DIBP, DBP, BBP, DEHP, DNOP each, and 500 mg/l of DINP, DIDP each in

dichloromethane (5.1).
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ISO/DIS 8124-6:2022(E)
5.4 External standard (ES) calibration solutions

A series of calibration standard solutions (of at least five equidistant calibrations in the range of 0,2 mg/l

to 10 mg/l for DIBP, DBP, BBP, DEHP and DNOP, 1 mg/l to 50 mg/l for DINP and DIDP) is prepared by

transferring 0,1 ml to 5 ml of the stock solution (5.3) to a 50 ml volumetric flask and making up to the

mark with dichloromethane.

Calibration standard solutions should be properly stored at 0 °C to 8 °C to prevent change of

concentration. It is recommended that the solution be prepared at least monthly.
5.5 Internal standard (IS) calibration solutions
5.5.1 Internal reference substances

Benzyl benzoate (BB, CAS No. 120-51-4) or di-n-amyl phthalate (DAP, CAS No. 131-18-0) (also known as

di-n-pentyl phthalate (DPP)), minimum of 95 % purity.

The internal reference substances should not be present in the test portion matrix. Other compounds,

such as isotopically labelled phthalate esters, can be used as alternative internal reference substances.

5.5.2 Internal stock solution
250 mg/l of BB, DAP or others, in dichloromethane.

IS solutions should be properly stored at 0 °C to 8 °C to prevent change of concentration. It is

recommended that these solutions be prepared at least every three months.
5.5.3 Internal standard calibration solutions

A series of calibration standard solutions (of at least five equidistant calibrations in the range of

0,2 mg/l to 10 mg/l for DIBP, DBP, BBP, DEHP and DNOP, 1 mg/l to 50 mg/l for DINP and DIDP) is

prepared by transferring 0,1 ml to 5 ml of the stock solution (5.3) to a 50 ml volumetric flask and

adding 2 ml of the IS stock solution (5.5.2) before making up to the mark with dichloromethane. Each

of the calibration standards contains 10 mg/l IS.

IS calibration solutions should be properly stored at 0 °C to 8 °C to prevent change of concentration. It

is recommended that these solutions be prepared at least monthly.
6 Apparatus
6.1 General

Phthalate esters are common contaminants which can affect the test result even at a low level of

concentration. In order to prevent interference and cross-contamination, any type of plastic apparatus

that could affect the analysis should be avoided, and glassware and equipment should be scrupulously

cleaned before use.
6.2 Normal laboratory glassware

6.3 Gas chromatography-mass spectrometer (GC-MS), with a capillary column coupled to a mass

spectrometric detector (electron ionization, EI) used for the analysis. See 8.4.1.

6.4 Soxhlet extractor, see Figure C.1.
6.5 Solvent extractor, see Figure C.2.
6.6 Extraction thimble, made of cellulose.
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ISO/DIS 8124-6:2022(E)
6.7 Cotton wool, for extraction thimble.
6.8 Analytical balance, capable of measuring to an accuracy of 0,001 g.
6.9 Concentration apparatus, for example, a rotary evaporator.

6.10 Solid phase extraction (SPE) cartridge, 1 000 mg silica gel/6 ml tubes, or equivalent.

6.11 Volumetric flasks, of 5 ml, 10 ml, 25 ml, 50 ml and 100 ml nominal capacity.

6.12 Pipettes, of 0,1 ml, 0,5 ml, 1 ml, 2 ml, 5 ml and 10 ml nominal capacity.
6.13 Polytetrafluoroethylene (PTFE) membrane filter, of pore size 0,45 μm.

6.14 Ultrasonic bath, thermostatically controlled internally or externally, with the effective ultrasonic

2 2

power intensity ranging from 0,25 W/cm to 2,0 W/cm . The performance check of the ultrasonic bath

is performed as specified in Annex E.

EXAMPLE An ultrasonic bath with a total power consumption of 1 200 W, including 200 W of effective

ultrasonic power and 1 000 W of heating power, with an internal bath base area of 400 cm , will provide an

2 2
effective ultrasonic power intensity of 0,50 W/cm (=200 W/400 cm ).

6.15 Ultrasonic basket, usually supplied together with the ultrasonic bath. When hung on the

ultrasonic bath, its lowest level is approximately 3 cm to 5 cm above the bottom of the bath.

6.16 Airtight glass reaction vessel, pressure-resistant to at least 0,2 MPa and with a gross volume of

2 to 10 times the volume of dichloromethane. The reaction vessel should be tightly closed to prevent the

evaporation of dichloromethane during ultrasonic extraction.
6.17 Centrifuge, capable of centrifuging at (5 000 ± 500) g.
7 Selection of test portion
7.1 General principle
Individual test and composite test are used in this document.
7.2 Individual test

For materials in solid form, use a scalpel or other appropriate cutting instrument to cut a

representative portion from the laboratory sample into small pieces. For coatings, remove each different

coating from the laboratory sample by scraping. Extra care shall be taken to minimize the inclusion of

the base material. Each piece shall, in the uncompressed condition, have no dimension greater than

5 mm and be mixed uniformly.

For materials in liquid form, use appropriate apparatus, such as a pipette or syringe, to transfer

a representative portion from the laboratory sample. Extra care shall be taken to minimize cross

contamination.

A test portion of less than 10 mg from a single laboratory sample shall not be tested.

The requirement does not preclude the taking of reference portions from toy or children’s product

materials in a different form, provided that they are representative of the relevant material specified

above and the substrate upon which they are deposited.
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ISO/DIS 8124-6:2022(E)
7.3 Composite test

When used properly, the composite test serves the purpose of reducing test costs and improving

efficiency, without affecting the accuracy of the test. A composite test used for quantitative screening

shall meet all of the following conditions:

a) Only similar materials can be combined to form a composite test portion. The compositing of

dissimilar materials is not appropriate (e.g. compositing plastics and coatings);

b) Similar mass shall be weighed for each constituent test portion, the mass between any two

constituent test portions should not differ by over 10 %;
c) The LOQ of target phthalate esters is lower than 50 mg/kg;

When a composite test is used, the number of the constituent test portions shall be less than or equal to

3 (i.e. K ≤ 3). When the number greater than 3 (i.e. K>3) is used in forming the composite test portion in

accordance with Annex D.

Composite test is only allowed in cases when it is enough for judging conformance with requirements.

And if the conclusion of composite test is failed, further individual tests are needed to find failed

samples among composite test portions.

NOTE The composite testing cannot be used to solve the lack of mass of a test portion. If a constituent test

portion’s mass is not enough to perform an individual test, it is not possible to get a representative result through

composite testing either.
8 Procedure
8.1 General

Except for clause 8.2, following procedure are applicable to both individual test and composite test.

8.2 Sample weighing
8.2.1 Individual test

In general, weigh, to the nearest 1 mg, approximately 1 g of a single test portion into an extraction

thimble (6.6) or reaction vessel (6.16). If 1 g test portion cannot be obtained from a single laboratory

sample, sample as much as possible from more than one laboratory sample, but 0,05 g is recommended

as a minimum test port
...