EN 71-3:2013+A2:2017

SLOVENSKI STANDARD
01-december-2017
1DGRPHãþD
SIST EN 71-3:2013+A1:2014
9DUQRVWLJUDþGHO0LJUDFLMDGRORþHQLKHOHPHQWRY]GRSROQLOLGRYNOMXþQR$
Safety of toys - Part 3: Migration of certain elements
Sicherheit von Spielzeug - Teil 3: Migration bestimmter Elemente
Sécurité des jouets - Partie 3 : Migration de certains éléments
Ta slovenski standard je istoveten z: EN 71-3:2013+A2:2017
ICS:
97.200.50 ,JUDþH Toys
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN 71-3:2013+A2
EUROPEAN STANDARD
NORME EUROPÉENNE
August 2017
EUROPÄISCHE NORM
ICS 97.200.50
English Version
Safety of toys - Part 3: Migration of certain elements
Sécurité des jouets - Partie 3 : Migration de certains Sicherheit von Spielzeug - Teil 3: Migration bestimmter
éléments Elemente
This European Standard was approved by CEN on 18 August 2014 and includes Amendment 2 approved by CEN on 18 April
2017.
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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2017 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 71-3:2013+A2:2017 E
worldwide for CEN national Members.

Contents Page
European foreword . 5
Introduction . 7
1 Scope . 8
2 Normative references . 8
3 Terms and definitions . 8
4 Requirements . 10
4.1 Toy material categories (see H.4) . 10
4.2 Specific requirements . 10
5 Principle . 11
6 Reagents and apparatus . 12
6.1 Reagents . 12
6.2 Apparatus . 12
7 Sampling and sample preparation . 12
7.1 Selection of test portions . 12
7.2 Standards preparation . 13
7.3 Sample preparation . 13
7.4 Migration procedure . 15
8 Methods of analysis . 18
9 Calculation of results . 18
9.1 General elements . 18
9.2 Chromium (III) and Chromium (VI) . 19
9.3 Organic tin . 19
10 Test report . 21
Annex A (informative) Significant technical changes between this European Standard and
the previous version . 22
Annex B (informative) Method performance . 24
B.1 Method performance . 24
B.2 Use of measurement uncertainty in compliance assessment . 24
B.3 Information on round robin test . 24
Annex C (normative) Sieve requirements . 26
Annex D (informative) Preparation and analysis of test portion . 27
Annex E (informative) Method of analysis for general elements. 28
E.1 Principle . 28
E.2 Working solutions . 28
E.2.1 Working solutions ICP-MS . 28
E.2.2 Working solutions ICP-OES . 29
E.3 Procedure . 31
E.4 Analysis . 31
E.4.1 General . 31
E.4.2 Limit of detection and quantification . 32
Annex F (informative) Methods of analysis for speciation of Chromium (III) and (VI) . 34
F.1 Principle . 34
F.2 Reagents . 34
F.3 Apparatus . 35
F.4 Procedure . 36
F.5 Analysis . 36
F.5.1 General . 36
F.5.2 LC-ICP-MS conditions . 36
F.5.3 Limit of detection and quantification . 37
Figure F.1 — Example of chromatogram of 0,6 ppb Chromium (III) and (VI) . 38
Annex G (informative) Method of analysis for organic tin (see H.10) . 39
G.1 Principle . 39
G.2 Terms and definitions . 40
G.3 Reagents . 40
G.4 Apparatus . 43
G.5 Procedure . 43
G.5.1 Sample derivatisation . 43
G.5.2 Calibration standards . 43
G.6 Analysis . 44
G.6.1 General . 44
G.6.2 Example of GC conditions . 46
G.6.3 Example of MS conditions . 47
G.6.4 Limit of detection and quantification . 47
G.6.5 Example of a GC/MS chromatogram . 48
Annex H (informative) Rationale . 49
H.1 General . 49
H.2 Mouthing behaviour of children (Scope) . 49
H.3 Skin contact (Scope) . 49
H.4 Toy categories (4.1) . 50
H.5 Test portions (7.1, 7.3.3.2, 7.3.3.3, 7.3.3.6) . 50
H.6 Size of test pieces (7.3.3.2, 7.3.3.3, 7.3.3.4). 50
H.7 Textile threads . 50
H.8 Chromium (VI) migration (7.4) . 50
H.9 Filtration of migration solutions (7.4.2.1, 7.4.2.2, 7.4.3.1, 7.4.3.3, 7.4.3.5) . 51
H.10 Organic tin (9.3) . 51
H.11 pH value . 51
H.12 De-waxing (see 7.3.2) . 52
Annex I (informative) Conformity assessment . 53
I.1 General . 53
I.2 Chromium VI . 53
Annex J (informative) List of other organic tin compounds . 54
Annex ZA (informative) Relationship between this European Standard and the Essential
Requirements of EU Directive 2009/48/EC . 55
Bibliography . 56

European foreword
This document (EN 71-3:2013+A2:2017) has been prepared by Technical Committee CEN/TC 52
“Safety of toys”, the secretariat of which is held by DS.
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 February 2018, and conflicting national standards
shall be withdrawn at the latest by February 2018.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent
rights.
This document supersedes ! EN 71-3:2013+A1:2014".
This document includes Amendment 1 approved by CEN on 2014-08-18.
The start and finish of text introduced or altered by amendment is indicated in the text by tags !".
This document includes Amendment 2 approved by CEN on 2017-05-31.
The start and finish of text introduced or altered by amendment is indicated in the text by tags #$.
This document has been prepared under a mandate given to CEN by the European Commission and the
European Free Trade Association, and supports essential requirements of EU Directive 2009/48/EC.
For relationship with EU Directive 2009/48/EC, see informative Annex ZA, which is an integral part of
this document.
The significant changes from the previous edition of this standard are detailed in Annex A.
EN 71, Safety of toys, consists of the following parts:
— Part 1: Mechanical and physical properties;
— Part 2: Flammability;
— Part 3: Migration of certain elements;
— Part 4: Experimental sets for chemistry and related activities;
— Part 5: Chemical toys (sets) other than experimental sets;
— Part 7: Finger paints — Requirements and test methods;
— Part 8: Activity toys for domestic use;
— Part 9: Organic chemical compounds — Requirements;
— Part 10: Organic chemical compounds — Sample preparation and extraction;
— Part 11: Organic chemical compounds — Methods of analysis;
— Part 12: N-Nitrosamines and N-nitrosatable substances;
— Part 13: Olfactory board games, gustative board games, cosmetic kits and gustative kits;
— Part 14: Trampolines for domestic use.
NOTE 1 In addition to the above parts of EN 71, the following guidance documents have been published: CEN
Technical Report CEN/TR 15071, Safety of toys — National translations of warnings and instructions for use in
EN 71, CEN Technical Report CEN/TR 15371, Safety of toys — Replies to requests for interpretation of EN 71-1,
EN 71-2, and EN 71-8 and CEN/TR 15371-2, Safety of toys — Replies to requests for interpretation of the chemical
standards in the EN 71-series.
NOTE 2 Words in italics are defined in Clause 3 (Terms and definitions).
According to the CEN-CENELEC Internal Regulations, the national standards organisations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Introduction
The Toy Safety Directive (2009/48/EC) [1] specifies maximum migration limits for three categories of
toy materials. The limits for the migration of certain elements are expressed in milligram per kilogram
toy material and are detailed in Table 2. The purpose of the limits is to minimise children’s exposure to
certain potentially toxic elements.
1 Scope
This European Standard specifies requirements and test methods for the migration of aluminium,
antimony, arsenic, barium, boron, cadmium, chromium (III), chromium (VI), cobalt, copper, lead,
manganese, mercury, nickel, selenium, strontium, tin, organic tin and zinc from toy materials and from
parts of toys.
Packaging materials are not considered to be part of the toy unless they have intended play value.
NOTE 1 See guidance document of the European Commission guidance document no. 12 [2] on the application
of the Directive on the safety of toys – packaging.
The standard contains requirements for the migration of certain elements from the following categories
of toy materials:
— Category I: Dry, brittle, powder like or pliable materials;
— Category II: Liquid or sticky materials;
— Category III: Scraped-off materials.
The requirements of this standard do not apply to toys or parts of toys which, due to their accessibility,
function, volume or mass, clearly exclude any hazard due to sucking, licking or swallowing or prolonged
skin contact when the toy or part of toy is used as intended or in a foreseeable way, bearing in mind the
behaviour of children.
NOTE 2 For the purposes of this standard, for the following toys and parts of toys the likelihood of sucking,
licking or swallowing toys is considered significant (see H.2 and H.3):
− All toys intended to be put in the mouth or to the mouth, cosmetics toys and writing instruments
categorised as toys can be considered to be sucked, licked or swallowed;
− All the accessible parts and components of toys intended for children up to 6 years of age can be
considered to come into contact with the mouth. The likelihood of mouth contact with parts of toys
intended for older children is not considered significant in most cases (see H.2).
2 Normative references
The following documents, in whole or in part, are referenced in this document and are necessary 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.
EN 71-1:2011, Safety of toys — Part 1: Mechanical and physical properties
EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
base material
material upon which coatings may be formed or deposited
3.2
coating
layer of material formed or deposited on a base material which can be removed by scraping
Note 1 to entry: Coatings can include paints, varnishes, lacquers, inks, polymeric coatings or other substances of
a similar nature, whether they contain metallic particles or not, and irrespective of the manner of application.
3.3
limit of detection
minimum single result which, with a stated probability, can be distinguished from a suitable blank
value; the result, c , is given by the formula:
L
c x+⋅ks
L bl bl
where
is the mean of the blank values,
!x
bl
sbl is the standard deviation of the blank values and"
k is a numerical factor chosen according to the confidence level desired

Note 1 to entry: The use of k=3 will usually suffice.
3.4
limit of quantification
lowest amount of analyte in a sample that can be quantitatively determined with a suitable precision
and accuracy
Note 1 to entry: For the purpose of this standard, the limit of quantification is twice the limit of detection.
3.5
other material, whether mass coloured or not
material such as wood, leather or other porous substances which may absorb colouring matter without
forming a coating
3.6
paper
sheet formed by irregularly intervened fibres with a mass per unit area of 400 g/m or less
3.7
paper board
sheet formed by irregularly intervened fibres with a mass per unit area over 400 g/m
Note 1 to entry: The term paperboard also includes materials commonly referred to as card or cardboard with a
mass per unit area over 400 g/m .
3.8
scraping
mechanical removal of coatings down to but not including the base material
3.9
toy material
material present in toys and accessible as determined in accordance with EN 71-1:2011, 8.10
=
4 Requirements
4.1 Toy material categories (see H.4)
Table 1 shows the categories of common toy materials. Toys not listed in Table 1 shall be classified into
one of the categories.
Table 1 — Cross-reference table for determining category
Toy Material Category I Category II Category III
Coatings of paints, varnishes, lacquers, printing
X
inks, polymers, foams and similar coatings
Polymeric and similar materials, including
laminates, whether textile reinforced or not,   X
but excluding other textiles
Paper and paper board   X
Textiles, whether natural or synthetic   X
Glass, ceramic, metallic materials   X
Other materials whether mass coloured or not
(e.g. wood, fibre board, hard board, bone and   X
leather)
Compressed paint tablets, materials intended
to leave a trace or similar materials in solid
X
form appearing as such in the toy (e.g. the cores
of colouring pencils, chalk, crayons)
Pliable modelling materials, including
X
modelling clays and plaster [3]
Liquid paints, including finger paints,
varnishes, lacquers, liquid ink in pens and
X
similar materials in liquid form appearing as
such in the toy (e.g., slimes, bubble solution)
Glue sticks  X
4.2 Specific requirements
The migration of elements from toy materials categorised in accordance with 4.1 shall not exceed the
migration limits given in Table 2 when tested in accordance with Clauses 7 and 8.
Table 2 — Migration limits from toy materials
Migration limit
Element
Category I Category II Category III
mg/kg mg/kg mg/kg
Aluminium 5 625 1 406 70 000
Antimony 45 11,3 560
Arsenic 3,8 0,9 47
Barium 1 500 375 18 750
Boron 1 200 300 15 000
Cadmium 1,3 0,3 17
Chromium
37,5 9,4 460
(III)
Chromium
0,02 0,005 0,2
(VI)
Cobalt 10,5 2,6 130
Copper 622,5 156 7 700
Lead 13,5 3,4 160
Manganese 1 200 300 15 000
Mercury 7,5 1,9 94
Nickel 75 18,8 930
Selenium 37,5 9,4 460
Strontium 4 500 1 125 56 000
Tin 15 000 3 750 180 000
Organic tin 0,9 0,2 12
Zinc 3 750 938 46 000
5 Principle
Soluble elements are extracted from toy materials using conditions which simulate the material
remaining in contact with gastric juices for a period of time after swallowing. The concentrations of the
soluble elements are determined quantitatively by three different methods:
— method for determining general elements: Aluminium, Antimony, Arsenic, Barium, Boron,
Cadmium, Chromium, Cobalt, Copper, Lead, Manganese, Mercury, Nickel, Selenium, Strontium, Tin
and Zinc;
— method for determining Chromium (III) and Chromium (VI);
— method for determining organic tin.
6 Reagents and apparatus
6.1 Reagents
All reagents used for analysis shall be of analytical grade or, if unavailable, technical grade reagents
which have been determined to have acceptably low levels of impurity to allow the analysis to be
performed.
6.1.1 Hydrochloric acid solution, c(HCl) = (0,07 ± 0,005) mol/l.
6.1.2 Hydrochloric acid solution, c(HCl) = (0,14 ± 0,010) mol/l.
6.1.3 Hydrochloric acid solution, c(HCl) = approximately 1 mol/l.
6.1.4 Hydrochloric acid solution, c(HCl) = approximately 2 mol/l.
6.1.5 Hydrochloric acid solution, c(HCl) = approximately 6 mol/l.
6.1.6 n-Heptane, (C H ), 99 %.
7 16
6.1.7 Water, of at least grade 3 purity in accordance with EN ISO 3696.
6.2 Apparatus
Standard laboratory equipment and the following shall be used.
6.2.1 Plain weave wire cloth stainless steel sieve, of nominal aperture size 0,5 mm and tolerances
as indicated in Table C.1.
!
6.2.2 Equipment for measuring pH, calibrated and sufficiently accurate for the purposes of this
European Standard."
6.2.3 Centrifuge, capable of centrifuging at high speed to separate the solids.
6.2.4 A means to agitate the mixture, at a temperature of (37 ± 2) °C.
An orbital or linear shaker, wrist action shaker, shaking water bath or magnetic stirrer can be used. It is
important that the migration solution is in constant motion relative to the sample.
6.2.5 A selection of containers of gross volume, between 1,6 times and 5,0 times that of the volume
of hydrochloric acid extract.
NOTE It is important to be aware the use of borosilicate glass ware may result in high blank values for Boron.
6.2.6 High retention filter-paper, ashless filter paper, particle retention in liquids 2,5 µm.
6.2.7 Membrane filters with pore sizes of 0.45, 0.22 and 0.02 µm.
7 Sampling and sample preparation
7.1 Selection of test portions
A laboratory sample for testing shall consist of one toy in the form in which it will be marketed. Test
portions shall be taken from toy materials of the single toy sample. Identical materials in the toy may be
combined and treated as a single test portion but additional toy samples shall not be used to prepare
larger test portions. Test portions are taken from each colour of each toy material. Test portions may be
composed of more than one toy material or colour only when discrete specimens cannot be separated
physically, e.g. dot printing, patterned textiles, etc.
NOTE This requirement does not preclude the preparation of test portions which represent the material and
any base material upon which it is deposited.
If the total weight of available toy material is less than 10 mg test portions are disregarded (see H.5).
The above does not preclude the possibility of testing toy materials before they are used to manufacture
a toy in order to prove compliance of the final toy. In this case, it shall be assessed that the
manufacturing process does not influence the migration of elements from the toy materials.
7.2 Standards preparation
Prepare standard solutions covering a suitable working range appropriate to the required limits for
each element for the three categories. Examples for ICP-MS and ICP-OES are included in Annex E.
7.3 Sample preparation
7.3.1 General
A blank solution shall be determined for any bias. The analytical results shall be corrected for any bias
due, for example, to contaminants present in the filter paper (6.2.6) or the gastric simulant.
When there is a significant bias the method should be checked.
7.3.2 Category I: Dry, brittle, powder like or pliable and Category II: Liquid or sticky
If possible obtain a test portion of not less than 100 mg of the material from the laboratory sample.
If a test portion of 100 mg or more cannot be obtained, a test portion shall be obtained from each toy
material present in the laboratory sample in a mass greater than 10 mg. If the weight of the test portion
obtained is between 10 mg and 100 mg, that weight shall be reported (see Clause 10 h)). In this case the
analytical results shall be calculated as though 100 mg of the test portion had been used (see H.5).
If the toy material contains any grease, oil, wax or similar material, material shall be de-waxed. De-
waxing shall not be carried out on test portions being analysed for organic tin. Dry a high retention
filter paper (see 6.2.6) for 4 h at 37 °C ± 4°C. Weigh the filter paper to the nearest 0,1 mg (Wfp1). The
filter paper used should be as small as possible without risking loss of the test portion during the de-
waxing procedure. Weigh the test portion, to the nearest 0,1 mg, onto the pre-dried and weighed filter
paper. Calculate the mass of the test portion. Use this mass for the calculation of the results of the test.
Fold the filter paper carefully to enclose the test portion without loss. Extract the test portion within the
filter paper with boiling n-heptane (6.2.5) using suitable laboratory apparatus. The use of a de-waxing
step shall be reported (see Clause 10 h)).
It has been shown that Soxhlet extraction with n-heptane for 6 h is usually sufficient to completely
remove non-polar ingredients from waxy toy materials. Alternative methods should be validated to
show that they are capable of completely removing the non-polar ingredients from relevant toy
materials.
After removal of non-polar ingredients, dry the folded filter paper containing the dewaxed test portion
in an oven at (37 ± 2) °C for 4 h to ensure the removal of residual solvent. Weigh the dried filter paper
parcel, to the nearest 0,1 mg (Wfp2). Use Wfp2 for the calculation under 7.4.2.1 on the volume of 0,07 M
HCl.
7.3.3 Category III: Scraped-off
7.3.3.1 Coatings of paint, varnish, lacquer, printing ink, polymer and similar coatings
Remove the coating from the laboratory sample by mechanical means (usually scraping) at room
temperature. If possible obtain a test portion of not less than 100 mg passing through a metal sieve of
aperture 0,5 mm (see 6.2.1).
If the weight of the test portion obtained is between 10 mg and 100 mg, that weight shall be reported
(see Clause 10 h)). In this case the analytical results shall be calculated as though 100 mg of the test
portion had been used (see H.5). When possible, coatings on textiles are to be scraped off as a powder
(and report this under Clause 10 h)). In case of a thick layer or one which is difficult to remove (e.g.
pliable or plasticised layers), the coating can be cut off and tested as polymeric material (7.3.3.2).
7.3.3.2 Polymeric and similar materials including laminates and reinforced textiles, but
excluding other textiles
If possible obtain a test portion of not less than 100 mg of the polymeric or similar material, according
to the following directions.
Cut out test portions from the areas having the thinnest material cross section. Each test piece shall
have at least one dimension of approximately 6 mm when possible (see H.6). The use of pre-prepared
reference materials for visual size comparison is recommended.
If a test portion of 100 mg or more cannot be obtained, a test portion shall be obtained from each toy
material present in the laboratory sample in a mass greater than 10 mg. If the weight of the test portion
obtained is between 10 mg and 100 mg, that weight shall be reported (see Clause 10 h)). In this case the
analytical results shall be calculated as though 100 mg of the test portion had been used (see H.5).
7.3.3.3 Paper and paper board
If possible obtain a test portion of not less than 100 mg of the paper or paper board. Each test piece shall
have at least one dimension of approximately 6 mm when possible (see H.6). The use of pre-prepared
reference materials for visual size comparison is recommended.
If a test portion of 100 mg or more cannot be obtained, a test portion shall be obtained from each toy
material present in the laboratory sample in a mass greater than 10 mg. If the weight of the test portion
obtained is between 10 mg and 100 mg, that weight shall be reported (see Clause 10 h)). In this case the
analytical results shall be calculated as though 100 mg of the test portion had been used (see H.5).
If the paper or paper board to be tested has paint, varnish, lacquer, printing ink, adhesive or similar
material applied to its surface, test portions of the coating shall not be taken separately. In such cases
test portions shall be taken from the toy material so that they also include representative parts of the
coated area.
7.3.3.4 Textiles, whether natural or synthetic (see H.7)
If possible obtain a test portion of not less than 100 mg of the textile material by cutting into test pieces.
Each test piece shall have at least one dimension of approximately 6 mm when possible (see H.6). The
use of pre-prepared reference materials for visual size comparison is recommended.
If a sample is not uniform in its material or colour, a test portion shall be obtained from each different
material present in a mass greater than 100 mg. A test portion present in a mass between 10 mg and
100 mg shall not be tested separately but shall be tested together with the material to which it is
attached. Test portions taken from patterned textiles shall be representative of the whole material.
7.3.3.5 Glass, ceramic and metallic materials
If the toy or any of its removable components fits entirely within the small parts cylinder (see EN 71-1)
and contains accessible glass, ceramic or metallic materials then the toy or component shall be tested in
accordance with 7.4.3.5 after removal of all accessible coatings in accordance with 7.3.3.1.
NOTE Inaccessible glass, ceramic and metallic toy materials, like other inaccessible materials, are not tested
according to 7.4.3.5. Neither are accessible glass, ceramic and metallic toy components which do not fit within the
small parts cylinder. The exposure to certain elements from these larger components, which cannot be swallowed,
is not considered significant.
7.3.3.6 Other materials, whether mass coloured or not
If possible obtain a test portion of not less than 100 mg of the toy material according to 7.3.3.2, 7.3.3.3,
7.3.3.4 or 7.3.3.5 whichever is appropriate.
If a test portion of 100 mg or more cannot be obtained, a test portion shall be obtained from each toy
material present in the laboratory sample in a mass greater than 10 mg. If the weight of the test portion
obtained is between 10 mg and 100 mg, that weight shall be reported (see Clause 10 h)). In this case the
analytical results shall be calculated as though 100 mg of the test portion had been used. If the toy
material to be tested is coated with a coating of paint, varnish, lacquer, printing ink or similar coating
follow the procedure in 7.3.3.1.
7.4 Migration procedure
7.4.1 General
The migration solution shall be used for the determination of elements. For the determinations of
Chromium species (see H.8) and organic tin the migration solutions shall be stabilised and/or otherwise
treated immediately after their preparation (see relevant analytical methods in Annex F and G).
For other elements, if the migration solutions are to be retained for more than 24 h prior to analysis,
they shall be stabilised by addition of hydrochloric acid so that the concentration HCl of the stored
solution is approximately 1 mol/l. The stabilisation by hydrochloric acid shall be reported (see Clause
10 h).
7.4.2 Category I: Dry, brittle, powder like or pliable and Category II: Liquid or sticky
7.4.2.1 Samples containing grease, oil, wax or similar material
Weigh, to the nearest 0,05 g, Wfp 2 x 25 g of water at approximately 20 °C into the extraction container
containing the filter paper parcel. Macerate carefully without loss so that the filter paper is thoroughly
soaked. Then add the same mass of 0,14 mol/l hydrochloric acid solution (6.1.2) at approximately 20 °C
and mix. For the purposes of these measured additions the density of the water and hydrochloric acid
solution can be assumed to be 1,0 g/ml and the solutions may be added volumetrically using suitable
dispensers accurate to the nearest 0,05 ml. Record the weights or volumes of water and hydrochloric
acid used (V and V ).
H2O HCl
!Shake the mixture for at least 1 min and measure the pH of the mixture. If the pH exceeds 1,30 add a
solution of 2 mol/l hydrochloric acid (6.1.4) drop-wise whilst mixing until the pH is 1,2 ± 0,1. Close the
container and agitate the mixture at (37 ± 2) °C (see 6.2.4) for 1 h. Stop the agitation and leave the
containers to stand for a further 1 h at (37 ± 2) °C."
Without delay separate the solid matter from the solution by filtration through a membrane filter to
remove visible solid material. Use filters with a pore size of 0,45 µm or 0,22 µm as necessary. In
addition, if necessary, centrifuge at high speed (6.2.3) to remove remaining visible solid materials.
Separation shall be completed as soon as possible after completion of the standing time; centrifuging
shall take no longer than 10 min and shall be reported under Clause 10 h).
There is the possibility of small pigment particles passing through a 0,45 µm or 0,22 µm membrane
filter (indicated by e.g. a cloudy solution, a Tyndall beam or a coloured filtrate) (see H.9). This could lead
– in certain cases – to an incorrect determination of the migration value as the result measured will
include not just the migrated element but also element chemically bound to the suspended particles.
Where this occurs either refilter the solution immediately using a membrane filter of pore size 0,02 µm.
Or where the refiltration cannot be performed, repeat the migration and separation steps finally using a
membrane filter of pore size 0,02 µm.
7.4.2.2 Samples not containing grease, oil, wax or similar material
!Using the appropriate sized container (see 6.2.5), mix the test portion so prepared with 50 times its
mass of an aqueous solution of 0,07 mol/l HCl (see 6.1.1) at approximately 20 °C. If appropriate, pliable
modelling materials such as clay or doughy materials shall be suspended completely (e.g. by stirring).
For a test portion mass of between 10 mg and 100 mg, mix the test portion with 5,0 ml of this solution.
Shake for at least 1 min. Check the acidity of the mixture.
If the test portion is likely to contain large quantities of alkaline materials, generally in the form of
calcium carbonate, adjust the pH to 1,2 ± 0,1 with approximately 6 mol/l HCl (see 6.1.5) in order to
avoid over-dilution. The amount of hydrochloric acid used in relation to the amount of solution shall be
reported under Clause 10 h). If only small quantities of alkaline material are present and the pH of the
mixture is greater than 1,3 add drop-wise, while shaking the mixture, an aqueous solution of
approximately 2 mol/l HCl (see 6.1.4) until the pH is 1,2 ± 0,1. Protect the mixture from light. Agitate
the mixture at (37 ± 2) °C (see 6.2.4) for 1 h continuously and then allow to stand for 1 h at (37 ± 2)
°C."
Without delay separate the solid matter from the solution by filtration through a membrane filter to
remove visible solid material. Use filters with a pore size of 0,45 µm or 0,22 µm as necessary. In
addition, if necessary, centrifuge at high speed (6.2.3) to remove remaining visible solid materials.
Separation shall be completed as soon as possible after completion of the standing time; centrifuging
shall take no longer than 10 min and shall be reported under Clause 10 h).
There is the possibility of small pigment particles passing through a 0,45 µm or 0,22 µm membrane
filter (indicated by e.g. a cloudy solution, a Tyndall beam or a coloured filtrate) (see H.9). This could lead
– in certain cases – to an incorrect determination of the migration value as the result measured will
include not just the migrated element but also element chemically bound to the suspended particles.
Where this occurs either refilter the solution immediately using a membrane filter of pore size 0,02 µm.
Or where the refiltration cannot be performed, repeat the migration and separation steps finally using a
membrane filter of pore size 0,02 µm.
7.4.3 Category III: Scraped-off
7.4.3.1 Coatings of paint, varnish, lacquer, printing ink, polymer and similar coatings
!Using the appropriate sized container (see 6.2.5), mix the test portion thus prepared with 50 times
its mass of an aqueous solution of 0,07 mol/l HCl solution (see 6.1.1) at approximately 20 °C. Where the
test portion has a mass of between 10 mg and 100 mg, mix the test portion with 5,0 ml of this solution.
Shake for at least 1 min. If necessary, check the acidity of the mixture. If the pH is greater than 1,3 add
drop-wise, while shaking the mixture, an aqueous solution of approximately 2 mol/l HCl (see 6.1.4)
until the pH is 1,2 ± 0,1. Protect the mixture from light. Agitate the mixture at (37 ±
...