1、 ISO 2015 Safety of toys Part 5: Determination of total concentration of certain elements in toys Scurit des jouets Partie 5: Dtermination de la concentration totale de certains lments dans les jouets INTERNATIONAL STANDARD ISO 8124-5 First edition 2015-06-01 Reference number ISO 8124-5:2015(E) ISO
2、8124-5:2015(E)ii ISO 2015 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2015, Published in Switzerland All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocop
3、ying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Ch. de Blandonnet 8 CP 401 CH-1214 Vernier, Geneva, Switzerland Tel. +41 22 74
4、9 01 11 Fax +41 22 749 09 47 copyrightiso.org www.iso.org ISO 8124-5:2015(E)Foreword iv Introduction v 1 Scope . 1 2 Normative references 1 3 T erms 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
5、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 mat
6、erials, 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,
7、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
8、 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.
9、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 reser
10、ved iii Contents Page 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 b
11、ody 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 Electro
12、technical 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
13、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
14、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
15、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 ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT), see the fol
16、lowing 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
17、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 childrens products Part 7: Requirements and test methods
18、for finger paints Part 8: Age determination guidelinesiv ISO 2015 All rights reserved 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 decid
19、e 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 th
20、e 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, decis
21、ions 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
22、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 Safety of toys
23、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 mater
24、ials 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
25、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 m
26、aterials, 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 leathe
27、r); 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;
28、 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
29、 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 lates
30、t 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 INTERNATIONAL ST ANDARD ISO 8124-5:2015(E) ISO 2015 All rights reserved 1 ISO 8124-5:2015(E) ISO 8124-3, Safety of toys Part 3: Mig
31、ration of certain elements ISO 3696, Water for analytical laboratory use Specification and test methods 3 T erms a nd definiti ons 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
32、 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 defini
33、tion 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 mater
34、ial 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.
35、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.
36、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 mater
37、ials, 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 2 ISO 2015
38、 All rights reserved 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
39、 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 fina
40、l 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
41、/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 Aceton
42、e/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 eq
43、uipped 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
44、 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 a
45、nd 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
46、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-(-trifluoromethyl- ,-difluorovinyl)-1,3,5-enzenetricarboxylate, or PTFE/PFA (perfluoroalkoxyethylene) or another ISO 2015 All right
47、s reserved 3 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
48、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 wi
49、th carbide burr grinders. 5.2.6 Centrifuge, capable of centrifuging at (5 000 500) g 1) , with compatible tubes. 5.2.7 Analytical balance, capable of measuring accurately to 0,000 1 g. 5.2.8 P ol ypr op y lene or PFTE micr ofilt ers, pore size 0,45 m. 5.2.9 V olumetric 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 s
