Safety of toys — Part 5: Determination of total concentration of certain elements in toys

ISO 8124-5:2015 specifies methods of sampling and digestion prior to analysis of the total concentration of the elements antimony, arsenic, barium, cadmium, chromium, lead, mercury, and selenium from toy materials and from parts of toys. Digestion methods for the elements mentioned above are specified for the following types of toy materials: coatings of paints, varnishes, lacquers, printing inks, polymers, and similar coatings; polymeric and similar materials, including laminates, whether textile-reinforced or not, but excluding other textiles; paper, paperboard, and cardboard; natural or synthetic textiles; metallic materials whether coated or not; other materials, whether mass-coloured or not (e.g. wood, fibreboard, hardboard, bone, and leather); materials intended to leave a trace (e.g. the graphite materials in pencils and liquid ink in pens); pliable modelling materials, including modelling clays and gels; paints to be used as such in the toy, including finger paints, varnishes, lacquers, and similar materials in solid or liquid form; packaging materials that form part of the toy or have intended play value.

Sécurité des jouets — Partie 5: Détermination de la concentration totale de certains éléments dans les jouets

General Information

Status
Published
Publication Date
01-Jun-2015
Technical Committee
Drafting Committee
Current Stage
9093 - International Standard confirmed
Start Date
07-Sep-2020
Completion Date
07-Sep-2020
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INTERNATIONAL ISO
STANDARD 8124-5
First edition
2015-06-01
Safety of toys —
Part 5:
Determination of total concentration
of certain elements in toys
Sécurité des jouets —
Partie 5: Détermination de la concentration totale de certains
éléments dans les jouets
Reference number
ISO 8124-5:2015(E)
ISO 2015
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ISO 8124-5:2015(E)
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© ISO 2015, Published in Switzerland

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ii © ISO 2015 – All rights reserved
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ISO 8124-5:2015(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 2

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

5 Reagents and apparatus ............................................................................................................................................................................... 3

5.1 Reagents........................................................................................................................................................................................................ 3

5.2 Apparatus .................................................................................................................................................................................................... 3

5.2.1 Microwave digestion system ................................................................................................................................. 3

5.2.2 High pressure microwave digestion vessel ............................................................................................... 3

6 Selection and composition of test portions .............................................................................................................................. 4

6.1 Selection of test portions ............................................................................................................................................................... 4

6.2 Compositing of test portions ....................................................................................................................................................... 5

7 Preparation of test portions ..................................................................................................................................................................... 5

7.1 Coatings of paint, varnish, lacquer, printing ink, polymer and similar coatings ............................ 5

7.2 Polymeric and similar materials, including laminates, whether textile-reinforced

or not, but excluding other textiles ....................................................................................................................................... 5

7.3 Paper, paperboard and cardboard .......................................................................................................................................... 5

7.4 Natural or synthetic textiles ........................................................................................................................................................ 6

7.5 Other materials, whether mass-coloured or not ....................................................................................................... 6

7.6 Materials intended to leave a trace ........................................................................................................................................ 6

7.7 Pliable modelling materials, including modelling clays, and gels ............................................................... 6

7.8 Paints, including finger paints, varnishes, lacquers, and similar materials, in solid

or liquid form ........................................................................................................................................................................................... 6

7.8.1 Materials in solid form ................................................................................................................................................ 6

7.8.2 Materials in liquid form ............................................................................................................................................. 6

7.9 Metallic materials whether or not partly coated ....................................................................................................... 7

8 Digestion of test portions and instrumental analysis .................................................................................................... 7

8.1 Microwave digestion .......................................................................................................................................................................... 7

8.1.1 If the instrumental analysis technique is ICP-MS ................................................................................ 7

8.1.2 If the instrumental analysis technique is ICP-AES .............................................................................. 8

8.1.3 Microwave digestion conditions ........................................................................................................................ 8

8.1.4 Cooling and dilution ...................................................................................................................................................... 8

8.2 Hot plate and hot block digestion of test portion ..................................................................................................... 8

8.2.1 If the instrumental analysis technique is ICP-AES .............................................................................. 8

8.2.2 If the instrumental analysis technique is ICP-MS ................................................................................ 9

9 Detection limits of the instrumental method ......................................................................................................................... 9

10 Expression of results .....................................................................................................................................................................................10

11 Test report ................................................................................................................................................................................................................10

Annex A (informative) Background and rationale ..............................................................................................................................11

Bibliography .............................................................................................................................................................................................................................15

© ISO 2015 – All rights reserved iii
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ISO 8124-5:2015(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 on the meaning of ISO specific terms and expressions related to conformity

assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers

to Trade (TBT), see the following URL: Foreword — Supplementary information.
The committee responsible for this document is ISO/TC 181, Safety of toys.

ISO 8124 consists of the following parts, under the general title Safety of toys:

— Part 1: Safety aspects related to mechanical and physical properties
— Part 2: Flammability
— Part 3: Migration of certain elements

— Part 4: Swings, slides and similar activity toys for indoor and outdoor family domestic use

— Part 5: Determination of total concentration of certain elements in toys
— Part 6: Certain phthalate esters in toys and children’s products
— Part 7: Requirements and test methods for finger paints
— Part 8: Age determination guidelines
iv © ISO 2015 – All rights reserved
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ISO 8124-5:2015(E)
Introduction
See A.1 (use and applicability).

This part of ISO 8124 defines a method for the determination of the total concentration of certain elements

in toy materials and can be used to decide whether there is a need to undertake migration testing in

accordance with the method specified in ISO 8124-3, Migration of certain elements or other equivalent

standards, e.g. EN 71-3:1994/AC:2002 or ASTM F963-11. A material can be considered to conform to

the requirements of ISO 8124-3:2010 if the total concentration results are below the soluble limits as

prescribed in ISO 8124-3:2010, Table 1. If the soluble limits in ISO 8124-3:2010, Table 1 are exceeded,

migration testing in accordance with ISO 8124-3:2010 will be required to determine compliance with

ISO 8124-3:2010.

In addition, decisions can be also taken, within the scope of this part of ISO 8124, on the compliance of

the material with any regulatory requirements that impose restrictions on the total concentration of

certain elements.

Where legal conformity requires migration testing, this part of ISO 8124 can only be used to non-

quantitatively confirm compliance with regulatory limits.

Users of this part of ISO 8124 are reminded that it has been developed only for the eight elements listed

in Table 1. The use of this method for other elements must be validated by the user.

© ISO 2015 – All rights reserved v
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INTERNATIONAL STANDARD ISO 8124-5:2015(E)
Safety of toys —
Part 5:
Determination of total concentration of certain elements in
toys
1 Scope

1.1 This part of ISO 8124 specifies methods of sampling and digestion prior to analysis of the total

concentration of the elements antimony, arsenic, barium, cadmium, chromium, lead, mercury, and

selenium from toy materials and from parts of toys.

NOTE Other elements can be determined by this method provided adequate analytical performance is

demonstrated. Manufacturers are encouraged to apply the test methods of this part of ISO 8124 and the limits

from ISO 8124-3 to raw materials used in the manufacture of toys to give increased certainty of conformity to the

requirements of ISO 8124-3.

1.2 Digestion methods for the elements mentioned in 1.1 are specified for the following types of toy

materials:

— coatings of paints, varnishes, lacquers, printing inks, polymers, and similar coatings;

— polymeric and similar materials, including laminates, whether textile-reinforced or not, but

excluding other textiles;
— paper, paperboard, and cardboard;
— natural or synthetic textiles;
— metallic materials whether coated or not;

— other materials, whether mass-coloured or not (e.g. wood, fibreboard, hardboard, bone, and leather);

— materials intended to leave a trace (e.g. the graphite materials in pencils and liquid ink in pens);

— pliable modelling materials, including modelling clays and gels;

— paints to be used as such in the toy, including finger paints, varnishes, lacquers, and similar materials

in solid or liquid form;

— packaging materials that form part of the toy or have intended play value (see A.2.1, packaging).

NOTE Digestion methods for glass, ceramic, and other siliceous materials or fluorinated polymers or

fluorinated polymer coatings are not described, and these types of materials are outside the scope of this part of

ISO 8124 (see A.1, use and applicability).
2 Normative references

The following documents, in whole or in part, are normatively referenced in this document and are

indispensable for its application. For dated references, only the edition cited applies. For undated

references, the latest edition of the referenced document (including any amendments) applies.

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

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ISO 8124-5:2015(E)
ISO 8124-3, Safety of toys — Part 3: Migration of certain elements
ISO 3696, Water for analytical laboratory use — Specification and test methods
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
base material
material upon which coatings (3.2) can be formed or deposited
3.2
coating

all layers of material formed or deposited on the base material (3.1)of a toy, 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

Note 1 to entry: This definition includes metallic coatings deposited on a metal surface such as an electroplated

coating. However, electroplating will only require testing if it can be removed by scraping (3.8); otherwise, it may

be tested with the base material.
3.3
complete digestion
complete breakdown of the original material leaving only insoluble residues
3.4
composite test portion

test portion (3.9) that is composed of more than one similar material type or colour of material

3.5
detection limit of instrument

three times the standard deviation of the result obtained in the blank test using a specific instrument

3.6
laboratory sample

toy either in the form in which it is marketed, or in the form in which it is intended to be marketed

3.7
sample blank

solution that has undergone the same digestion processes used for the digestion of test portions (3.9)

and consists of all reagents excluding the test portion
3.8
scraping

mechanical process for removal of coatings (3.2) down to the base material (3.1) using a sharp blade

such as a scalpel
3.9
test portion
single material taken from an accessible part of a laboratory sample (3.6)

Note 1 to entry: This definition precludes the compositing of dissimilar materials, e.g. compositing textiles and

paint coatings is not permitted.
4 Principle

The prepared test portion is digested in highly acidic conditions at high temperature using a hot plate

digestion, a hot block digestion technique, or a microwave digestion system. Hot acid digestion destroys

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ISO 8124-5:2015(E)

the material matrix allowing the elements of interest to be solubilised and quantified by a suitable

analytical instrument (see Clause 9, detection limits of the instrumental method).

5 Reagents and apparatus
5.1 Reagents

Only reagents of recognized analytical grade or equivalent shall be used. The concentration of the

analyte or interfering substances in the reagents and water shall be negligible compared to the lowest

concentration to be determined.

“Trace metal” grade or equivalent reagents shall be used for the calibration standards used for the final

instrumentation quantification stage.
5.1.1 Nitric acid, concentrated, 1,40 g/ml, 65 % (v/v), “analytical” grade.

5.1.2 Nitric acid, 10 % (v/v): Add 100 ml concentrated nitric acid (5.1.1) to 500 ml water (5.1.4). Dilute

to 1 000 ml with water (5.1.4).

5.1.3 Hydrochloric acid, concentrated, 1,19 g/ml, 37 % (v/v), “analytical” grade.

5.1.4 Water, of at least grade 3 purity, in accordance with ISO 3696.
5.1.5 Hydrogen peroxide, 30 % (v/v).

NOTE Hydrogen peroxide which is not stabilized must be stored at cold (4 °C or less) temperatures.

5.1.6 Methylene chloride, “analytical” grade.

5.1.7 Acetone/ethanol solution, 1:1 mixture of absolute ethanol and acetone (“analytical” grades).

5.2 Apparatus

All glassware shall be soaked in 10 % (v/v) nitric acid (5.1.2) for at least 2 h and then rinsed in deionised

water before use.
5.2.1 Microwave digestion system

Microwave sample preparation system equipped with a sample holder and high-pressure microwave

digestion vessels (5.2.2, high pressure microwave digestion vessel).

NOTE 1 Some newer models of microwave digestion systems do not utilise high-pressure digestion vessels and

these systems are considered as a suitable alternative provided they give an equivalent performance.

NOTE 2 There are many safety and operational recommendations specific to the model and manufacturer of the

microwave equipment used in individual laboratories. The analyst is required to consult the specific equipment

manual, manufacturer, and literature for proper and safe operation of the microwave equipment and vessels (see

A.3, precautions relating to the use of microwave digestion).
5.2.2 High pressure microwave digestion vessel

Closed-top vessel specifically designed for microwave digestion, of suitable capacity. It is recommended

to use a vessel capable of withstanding a temperature of at least 225 °C and an internal pressure of at least

3 000 kPa. The liner of the vessel shall be PTFE (polytetrafluoroethylene)/TFM [tris-(α-trifluoromethyl-

β,β-difluorovinyl)-1,3,5-enzenetricarboxylate], or PTFE/PFA (perfluoroalkoxyethylene) or another

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ISO 8124-5:2015(E)

chemically inert material. Vessels shall also be equipped with a safety relief valve or disc that will

prevent vessel rupture or ejection of the vessel cap.

NOTE 1 The inner liners shall be inspected regularly to check for any chemical or physical degradation.

NOTE 2 Internal pressures in excess of 3 000 kPa can occur with some samples, e.g. crayons, and so a suitable

pressure-rated vessel, e.g. 5 000 kPa, should be used in these cases.
5.2.3 Scalpel, or other suitable scraping or cutting tools.
5.2.4 Laboratory grinding mill.
5.2.5 Rotary grinder, preferably with carbide burr grinders.

5.2.6 Centrifuge, capable of centrifuging at (5 000 ± 500) g , with compatible tubes.

5.2.7 Analytical balance, capable of measuring accurately to 0,000 1 g.
5.2.8 Polypropylene or PFTE microfilters, pore size 0,45 µm.
5.2.9 Volumetric flasks, 25 ml or 100 ml capacity with stopper.
5.2.10 Pipettes, such as 1 ml, 5 ml, 10 ml, 20 ml, etc.
5.2.11 Beakers, various capacities including 25 ml, 50 ml, 100 ml, etc.

5.2.12 Electric hot plate, suitable for operation at surface temperatures up to at least 140 °C.

NOTE Provided that the hot plate is capable of handling the extra heating required, use of a 12 mm to 25 mm

thick heat-resistant glass plate placed on the hot plate can help reduce the presence of hot spots common to

electric hot plates.
5.2.13 Filter paper and funnel.

5.2.14 Hot block digester, heated metal block with variable temperature settings up to at least 140 °C

(optionally can have programmable settings and temperature ramps) with compatible digestion vessels

of suitable capacity.
6 Selection and composition of test portions

See A.1.2 (practical considerations in deciding whether to composite test portions).

6.1 Selection of test portions

Test portions shall be taken from accessible parts (see ISO 8124-1) of the laboratory sample in accordance

with Clause 7 (preparation of test portions). When appropriate, the laboratory sample shall be subjected

to relevant tests in accordance with ISO 8124-1, before the accessibility is considered. Identical materials

in the laboratory sample can be combined and treated as a single test portion, but the use of additional

laboratory samples is not permitted. If it is not possible to obtain at least 10 mg, no further testing shall

be conducted and this shall be reported under Clause 11 c) (test report).

It is recommended that the test portion mass be in the region of 100 mg where sufficient material is available.

1) g=9,806 65 m/s
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ISO 8124-5:2015(E)
6.2 Compositing of test portions

Up to three test portions can be combined to form a composite test portion provided that the required

detection limit can still be achieved (see A.1.2, practical considerations in deciding whether to composite

test portions) and the combined materials are similar in nature.

The compositing of dissimilar materials is not permitted, e.g. compositing textiles and paint coatings.

When calculating the concentration of a target element in a material, it is assumed that all of that

element found in the digested sample originated from any one of the composited materials. Using this

assumption and the masses of the individual materials, the total concentration of the target element is

calculated for each individual material in the composite test portion.
7 Preparation of test portions

Materials from the laboratory sample are selected for testing in accordance with Clause 6 (selection and

composition of test portion) and removed using cutting tools such as scalpels, razor blades, scissors,

and grinding and milling tools as described in the subclauses below. If a grinding apparatus [such as a

mill (5.2.4) or rotary grinding tool (5.2.5) with disposable grinding bits] is used, then any contaminated

parts shall be thoroughly cleaned or disposed of between uses to prevent cross-contamination. Ensure

that the device itself cannot contaminate the material being prepared.

In 7.1 to 7.9, collect sufficient material to obtain a test portion of between 10 mg and 100 mg. In cases

where less than 10 mg of material is available (see 6.1, selection of test portions) no further testing is

required and this is reported under Clause 11 c) (test report).

Digest the prepared test portion according to the procedures described in 8.1 (microwave digestion) or

8.2 (hot plate and hot block digestion of test portion).

7.1 Coatings of paint, varnish, lacquer, printing ink, polymer and similar coatings

Remove each different coating from the laboratory sample by scraping down to the base material, taking

care to avoid the inclusion of the base material. Where lithographic coatings (dot printing) are present,

it is impractical to separate the individual colours and so remove these coatings in such a way that a

representative test portion is obtained.

For some coatings deposited on a non-polymeric base material, it is permissible to add a few drops of

solvent, such as acetone/ethanol (5.1.7) mixture or methylene chloride (5.1.6), to soften the paint and

aid in its removal from the base material.

In the first instance, acetone/ethanol (5.1.7) should be used. If this treatment is not effective in aiding

removal, methylene chloride can be used under a fumes hood.

If a solvent treatment is used, ensure that all traces of solvent have been removed by evaporation prior to

microwave digestion (see 8.1, microwave digestion). Divide removed coatings into small pieces having a

maximum length in any direction of 2 mm in order to facilitate efficient digestion.

7.2 Polymeric and similar materials, including laminates, whether textile-reinforced or

not, but excluding other textiles

Scrape-off, cut, or grind the clean, dry material into pieces having a maximum length in any dimension

of 2 mm using a scalpel or other suitable scraping or cutting tool.
7.3 Paper, paperboard and cardboard
See A.2.2 (paper, paperboard and cardboard).

Cut the material into pieces with a maximum length in any dimension of 2 mm using a suitable cutting tool.

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ISO 8124-5:2015(E)

If the paper or paperboard to be tested is coated with paint, varnish, lacquer, printing ink, adhesive,

or similar coating, test portions of the coating shall not be taken separately. In such cases, take test

portions from the material so that they also include representative parts of the coated area.

Material that is printed, where the ink has become part of the base material, is prepared as though they

are unprinted.
7.4 Natural or synthetic textiles

Cut the material into pieces having a maximum length in any dimension of 2 mm using a suitable cutting tool.

If the sample is not of a uniform material or colour, where possible, obtain a test portion from each

different material or colour present in a mass greater than 100 mg. Materials or colours present in

amounts between 10 mg and 100 mg shall form part of the test portion obtained from the main material.

Test portions taken from patterned textiles shall be representative of the whole material.

7.5 Other materials, whether mass-coloured or not

Cut, scrape, or grind the material into pieces having a maximum length in any dimension of 2 mm using

a suitable cutting tool.
7.6 Materials intended to leave a trace

Obtain test portions from each different material in the laboratory sample, in the form that it appears

in the laboratory sample, ensuring that the material is cut into pieces having a maximum length in any

dimension of 2 mm.
7.7 Pliable modelling materials, including modelling clays, and gels

Obtain test portions from each different material or colour of material in the form that it appears in the

laboratory sample, i.e. without allowing the material to dry out. Cut the material into pieces having a

maximum length in any dimension of 2 mm.

7.8 Paints, including finger paints, varnishes, lacquers, and similar materials, in solid

or liquid form
7.8.1 Materials in solid form

Using a suitable tool, grind, crush, or cut the sample into particles having maximum length in any

dimension of 2 mm.

Finger paint supplied in the form of powder shall be diluted with water (5.1.4) in accordance with the

manufacturer’s instructions and then prepared according to 7.8.2 (materials in liquid form).

7.8.2 Materials in liquid form

Ensure that all settled material has been incorporated into the sample by scraping and long-term

mechanical shaking. Immediately prior to sampling, ensure the liquid is homogenised by stirring or

shaking for 5 min. Obtain a test portion of between 10 mg and 100 mg. In cases where less than 10 mg of

material is available (see 6.1, selection of test portion) no further testing is required and this is reported

under Clause 11 c) (test report). Digest the prepared test portion according to 8.1 (microwave digestion)

or 8.2 (hot place and hot block digestion of test portion).

If the liquid is intended to solidify or dry during intended use, it shall be coated onto a clean glass plate

and dried to constant weight before taking test portions as described in 7.1 (coatings of paint, varnish,

lacquer, printing ink, polymer and similar coatings).
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ISO 8124-5:2015(E)

Report under Clause 11 g) (test report) whether the material was tested in the dry or liquid state.

7.9 Metallic materials whether or not partly coated

Where practical, obtain the test portion from an uncoated part of the metallic material. If the metal

part is partiall
...

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