EN71-3-2013-元素的迁移

EN71-3 2013 Safety of toys - Part 3: Migration of certain elements
玩具安全-第3部分：元素的迁移
1 Scope（围）
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 compounds and zinc from toy materials and from parts of toys.
本欧洲标准规定了下列从玩具材料和玩具部件中转移的元素的详细要求和测试方法：铝、锑、砷、钡、硼、镉、铬（3+）、铬（6+）、钴、铜、铅、锰、汞、镍、硒、锶、锡、有机锡和锌。

Packaging materials are not considered to be part of the toy unless they have intended play value.
包装材料不包括在本标准围之类，除非它们属于玩具部分或者有娱乐价值。

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.
下列玩具种类的元素转移包括在本标准的要求之：
第一类：干燥，易碎，粉末状或柔软的玩具材料；
第二类：液体状/粘稠性玩具材料；
第三类：玩具表面刮出物。

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. Both the intended and foreseeable use has to be considered, bearing in mind the behaviour of children,
某些玩具和玩具零件，在考虑儿童正常的和可预见性的行为时，这些部分由于它
们的可接触性、功能、质量、大小或其它的特性，可明显排除因吮吸、舔食和吞咽造成的危害，这部分玩具不包括在EN 71标准的这一部分之。

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:
——All toys intended to be put in the mouth or to the mouth, cosmetics toys and writing instruments categorised as toys may be sucked, licked or swallowed;
——All the accessible parts and components of toys intended for children up to 6 years of age may 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;
备注2：为了执行本标准，下列标准适用于判断吮吸、舔食、吞咽的产品围：—所有供给食物或与嘴唇接触的玩具、化妆玩具和属玩具类的书写工具；
—供6 岁及以上儿童使用的玩具，即所有可能与嘴接触到的部分或零件，
对于大孩子来说，嘴与玩具部件的接触在大部分情况下被认为是不重要的。

2 Normative references（参考标准）
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)
EN 71-1:2011, 玩具的安全—第1部分: 物理机械性能
EN ISO 3696, 分析实验室用水—规格和测试方法(ISO 3696)
3. Terms and definitions（术语和定义）（略）
4. Requirements（要求）
4.1 Toy categories（玩具的分类）
Table 1 — Cross-reference table for determining category（表1 玩具材料分类的参照表）
4.2 Specific requirements（特殊要求）
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.
根据4.1对玩具材料做出分类，根据条款7和8检测出来的元素的迁移值不得超过表2给出的限值。

Table 2 — Migration limits from toy materials 表2玩具材料的迁移限量
5 Principle（原理）
Soluble elements are extracted from toy materials under the conditions which simulate the material remaining in contact with gastric simulant 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, Cobalt, Copper, Lead, Manganese, Mercury, Nickel, Selenium, Strontium, Tin and Zinc;
——Method for determining Chromium (III) and chromium (VI); ——Method for determining Organic tin.
模拟材料在吞咽后与胃酸持续接触一段时间，在此条件下，可溶性的元素被从玩具材料中萃取出来。

根据三种不同的方法对可溶性元素定量分析。

——标准元素(铝、锑、砷,钡,硼、镉、钴、铜、铅、锰、汞、镍、硒、锶、锡和锌);
——铬(III)和铬(VI);
——有机锡。

6 Reagents and apparatus（试剂和仪器）
6.1 Reagents（试剂）
All chemicals used for analysis shall be of analytical grade
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
7H
16
), 99%
6.1.7 Water, of at least grade 3 purity in accordance with EN ISO 3696.
6.1 试剂
在分析中，只能使用经过认可的分析纯试剂。

6.1.1 盐酸溶液，c（HCl）=（0.07±0.005）mol/l
6.1.2 盐酸溶液，c（HCl）=（0.14±0.010）mol/l。

6.1.3 盐酸溶液，c（HCl）=约1mol/l。

6.1.4 盐酸溶液，c（HCl）=约2mol/l。

6.1.5 盐酸溶液，c（HCl）=约6mol/l。

6.1.6 正庚烷（C
7H
16
）：99%。

6.1.7 水：纯度至少达到ISO 3696 所规定的三级。

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 6.2.2 A means to measure the pH, with an accuracy of ± 0,2 pH units.
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.
6.2.5A selection of containers of gross volume, between 1,6 times and 5,0 times that of the volume of hydrochloric acid extract.
6.2.6 High retention filter-paper, ashless filter paper, particle retention in liquids 2.5µm.
6.2.7 Membrane filter, with a pore size of 0,45,0.22 and 0.02μm
6.2仪器
常规的实验仪器有：
6.2.1 平纹金属丝网不锈钢金属筛，筛网孔径大小为0.5mm
6.2.2 测量pH 值的设备，准确到±0.2 个pH 单位。

6.2.3 离心机，能高速分离固体。

6.2.4 搅拌混合物的装置，搅拌时温度为（37±2）℃。

6.2.5 一套容器，总体积为盐酸萃取剂体积的1.6-5.0 倍的容器。

6.2.6高效滤纸，无尘滤纸，在液体的粒子滞留为2.5 µm。

6.2.7 滤膜过滤器，滤孔为0.45, 0.22和0.02μm。

7 Sampling and sample preparation（样品和样品制备）
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 accessible toy material available is less than 10 mg test portions need not be prepared.
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. It must be assessed that the manufacturing process does not influence the migration of elements from the toy materials.
7.1 测试部位的选择
供测试的玩具样品应是销售状态的玩具，试样应从单个玩具样品上取下，即：单个玩具上同种材料可以结合起来作为同一测试试样，但不应采用其它玩具样品。

测试试样不应含一种以上材料或一种以上颜色，除非采用物理分离方法不能有效分离的样品，这种样品如点染色、印花纺织物或因重量限制的样品。

注：本要求不排除可以从能代表试样的材料及其附着的衬底材料上取下的测试试样。

对材料不足10mg的测试部分不进行测试。

以上不排除检测玩具材料的可能性，因为这些材料是用于制作玩具以证明符合最终玩具的要求。

在这种情况下，它应该被评估在制造过程中不影响玩具材料中元素的迁移。

7.2 Standards preparation（标准溶液的制备）
Prepare standard solutions in a proper working range according to the required limits for each element for the three categories.
在一个合适的工作围根据三类物质中每一种元素的限值准备标准溶液。

7.3 Sample preparation（样品的制备）
7.3.1 General
A blank solution shall be determined for any bias. The analytical results shall be corrected for this bias. For example for any contaminants that may be present in the filter paper or the gastric simulant.
测定一个空白溶液，有任何偏差分析结果应该被校正。

例如出现在滤纸上或者模拟液的污染
物。

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.
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 for 4 hours at 37°C. Weigh the filter pa per 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. Fold the filter paper carefully to enclose the test portion without loss. Extract the test portion within the filter paper with boiling n - heptane 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 hours 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°C ± 2 for 4 hours 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.
7.3.2 第一类：干燥，易碎，粉末状或柔软的玩具材料；第二类：液体或者粘性材料
从实验室样品上取下不少于 100mg 的测试材料。

如果不能获得100mg或者100mg以上的测试材料，测试材料必须从每种不同玩具材料上获得大于 10mg 的质量。

如果材料为10mg至100mg 之间，测试部分的质量必须注明（见条款10h），同时有关元素的含量必须按使用的测试试样为100mg 计算。

如果玩具材料含有油脂、油类、蜡或类似材料，应执行去蜡程序。

有机锡的测试样品不用执行去蜡测试。

将高效滤纸在37℃烘4个小时。

称取滤纸的重量，精确到0.1mg (Wfp1)。

为了在去蜡的过程中减少样品的损失，滤纸应尽可能的小。

称量样品，精确到0.1mg。

将测试试样包在高效滤纸中，使用沸腾的正庚烷去油脂直至完全清除。

如果执行去油程序应注明（见条款10h）。

证明显示，用正庚烷进行6小时的索氏提取能彻底清除蜡质玩具材料的非极性成分。

用其它方法验证表明他们有能力完全去除有关玩具材料的非极性成分。

移去非极性物质后，含有油脂检测样品的折叠滤纸在37±2℃烘4个小时确保移除残留物质，称量干燥的滤纸包，精确到0.1 mg (Wfp2)。

用Wfp2 计算7.4.2.1中HCL溶液的体积。

7.4.3 Category III: Scraped-off（第三类：玩具表面刮出物）。

7.4.3.1 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.
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. When possible coatings on textiles may 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 plasticized layers), the coating can be cut off and tested as polymeric material (7.3.2.2).
7.3.3.1 油墨、清漆、生漆、印刷墨水、聚合物涂层和类似的涂层
在室温下采用机械方法（通常是刮）从试样上获取涂层。

从能通过孔径为0.5mm的金属筛网的筛分材料中获取不少于100mg 的测试试样。

如果粉碎后的同一种涂层仅能得到 10mg 至100mg，测试部分的质量必须注明（见条款10h）。

有关元素的含量应按使用的测试试样为100mg 计算。

纺织品上的涂层可以作为粉末刮下来（见条款10h）。

如果涂层比较厚而且很难刮下来，则可以做为聚合物材料直接剪切下来（7.3.2.2）。

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 a maximum dimension of no more than approximately 6 mm. 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.
7.3.3.2 聚合物材料和类似材料，包括用或不用纺织物增强的层压材料，但不包括其它纺织物
从聚合物或类似材料上取下不少于 100mg 的测试部分，具体方法如下：
从材料截面厚度最小处剪下测试部分。

每个试样的所有尺寸要小于6mm。

视觉尺寸可以与事先准备好的材料相比较。

如果不能获得100mg或者100mg以上的测试材料，测试材料必须从每种不同玩
具材料上获得大于 10mg 的质量。

如果材料为10mg至100mg 之间，测试部分的质量必须注明（见条款10 h），同时有关元素的含量必须按使用的测试试样为100mg 计算。

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 a maximum dimension of no more than approximately 6mm. 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.
If the paper or paper board to be tested is coated with a coating of paint, varnish, lacquer, printing ink, adhesive or similar coating, 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.
7.3.3.3 纸或纸板
从纸或纸板上取下不少于 100mg 的测试部分。

每个试样的所有尺寸在不受压的状态下必须小于6mm。

视觉尺寸可以与事先准备好的参考材料相比较。

如果不能获得100mg或者100mg以上的测试材料，测试材料必须从每种不同玩具材料上获得大于 10mg 的质量。

如果材料为10mg至100mg 之间，测试部分的质量必须注明（见条款10h），同时有关元素的含量必须按使用的测试试样为100mg 计算。

如果待测试的纸或纸板上有油漆、清漆、生漆、油墨、胶粘剂涂层或类似涂层，涂层的测试试样不应分开移取。

在这种情况下，测试试样从材料上直接取下，使测试试样同时包括含涂层部位的代表性试样。

7.3.3.4 Textiles, whether natural or synthetic
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 a maximum dimension of no more than approximately 6mm. 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 100 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.
Samples taken from patterned textiles shall be representative of the whole material.
7.3.3.4 天然或合成的纺织物
从纺织材料上通过剪切的方式取下不少于 100mg 的测试试样。

每个试样的所有尺寸要小于6mm。

视觉尺寸可以与事先准备好的参考材料相比较。

如果不能获得100mg或者100mg以上的测试材料，测试材料必须从每种不同玩具材料上获得大于 10mg 的质量。

如果材料为10mg至100mg 之间，测试部分的质量必须注明（见条款10 h），同时有关元素的含量必须按使用的测试试样为100mg 计算。

从印花纺织物取下的试样必须能代表整个材料。

7.3.3.5 Glass, ceramic and metallic materials
If the toy or any of its removable components fit 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 any coating in accordance with 7.3.3.1. NOTE Inaccessible glass, ceramic and metallic toy materials, like other
inaccessible materials, are not tested according to clause 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.
7.3.3.5 玻璃、瓷和金属材料
应先按 EN 71-1 对玩具和部件进行有关的测试。

如果玩具或部件可以完全进入小零件测试圆筒并含有可触及的玻璃/瓷/金属材料，必须先按7.3.3.1的程序移取玩具上的涂层，然后按7.4.3.5的程序对玩具进行测试。

注：不含可触及的玻璃/瓷/金属材料的玩具和部件无须按7.4.3.5 的程序进行测试。

可接触的玻璃/瓷/金属材料如果不满足小零件圆筒的要求，这些大部件由于不能吞咽也不需要测试。

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.
7.3.2.6 其它材料，不管是否大量着色
按 7.3.3.2、7.3.3.3、7.3.3.4 或7.3.3.5 中适用的程序从材料上取下不少于100mg 的测试试样。

如果不能获得100mg或者100mg以上的测试材料，测试材料必须从每种不同玩具材料上获得大于 10mg 的质量。

如果材料为10mg至100mg 之间，测试部分的质
量必须注明（见条款10 h），同时有关元素的含量必须按使用的测试试样为100mg 计算。

如果待测试的玩具材料上有油漆、清漆、生漆、油墨或类似涂层应按照7.3.3.1的程序测试。

7.4 Migration procedure（迁移程序）
7.4.1 General
The migration solution shall be used for the determination of elements. For the determinations of Chromium species and organic tin the migration solutions shall be stabilized and/or otherwise treated immediately after their preparation.
For other elements, if the migration solutions are to be retained for more than 24 hours prior to analysis, they shall be stabilized 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).
7.4.1概述
最后的迁移溶液可以用作某些元素的检测。

铬的化合物和有机锡的迁移溶液应稳定或者立即测试（相关的测试方法见附录）。

对于其它元素来说，如果配制好的溶液在分析前的保存时间超过24h，必须加入浓度约1mol/l盐酸加以稳定。

并在10h项中注明。

7.4.2 Category I: Dry, brittle, powder like or pliable and Category II: Liquid or sticky（第一类：干燥，易碎，粉末状或柔软的玩具材料；第二类：液体或者粘性材料）
7.4.2.1 Samples containing grease, oil, wax or similar material Weigh, to the nearest 0, 05g, Wfp2 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 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 ,05ml. Record the weights
or volumes of water and hydrochloric acid used (V
H2O and V
HCl
).
Shake the mixture for at least 1 minute and measure the pH of the mixture. If the pH exceeds 1, 5 add a solution of 2mol/L hydrochloric acid drop - wise whilst mixing until the pH is between 1, 0 and 1, 5. Close the container and agitate the mixture at 37 ± 2 °C for 1 hour. Stop the agitation and leave the containers to stand for a further 1 hour a t 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 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 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 ). 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 ref iltration cannot be performed, repeat the migration and separation steps finally using a membrane filter of pore size 0,02 µm.
7.4.2.1含油脂、油类、蜡或类似材料的样品
称量0.05g左右，Wfp2*25g的20℃水导入含有滤纸包的萃取容器中。

为了不损失样品，滤纸应完全浸透。

添加同等质量的0.14mol/l的盐酸溶液混和。

假定添加的水和盐酸溶液的密度是1.0g/ml，那么溶液可以按体积添加，精确到0.05ml。

纪录所用的水和盐酸的体积。

混合物摇动1分钟，测混合物的pH 值，如果pH 值大于1.5，逐滴加入盐酸溶液C（HCl）=约2mol/l，直到pH 值达到1.0 至1.5 之间，密封容器，在温度为（37±2）℃时搅拌混合物，持续1小时，然后使混合物在（37±2）℃下放置1 小时。

接着立即将混合物中的固体有效地分离出来，先使用滤膜过滤器过滤，然后根椐需要离心分离。

分离必须在上述放置时间结束后尽快完成，离心分离不能超过10 分钟，同时必须在10h项中列明。

有可能一些小的颜料粒子通过0,45 µm或者0,02 µm的膜过滤器。

在某种情况下这可能导致迁移值是不正确的，它不仅包括元素的迁移值还包括悬浮颗粒的元素值。

当发生这种情况的时候立即用0,02 µm的膜过滤器重新过滤。

如果不能重新过滤，则重复迁移和分离步骤，最后用0,02 µm的膜过滤器过滤。

7.4.2.2 Samples not containing grease, oil, wax or similar material Using the appropriate sized container, mix the test portion so prepared with 50 times its mass of an aqueous solution at of 0,07 mol/L HCl at approximately 20 °C. If appropriate, pliable materials suchs 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 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 between 1,0 and 1,5 with approximately 6 mol/L HCl in order to avoid over-dilution. The amount of hydrochloric acid used in relation to the amount of solution shall be reported under 10 h). If only small quantities of alkaline material are present and the pH of the mixture is greater than 1,5 add drop-wise, while shaking the mixture, an aqueous solution of approximately 2 mol/L HCl until the pH is between 1,0 and 1,5. Protect the mixture from light. Agitate the mixture at (37 ± 2) °C 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 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 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 ). 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 ref iltration cannot be performed, repeat the migration and separation steps finally using a membrane filter of pore size 0,02 µm.
7.4.2.2不含油脂、油类、蜡或类似材料的样品
使用尺寸合适的容器，将相当于测试试样质量50 倍、温度为20℃的盐酸溶液C（HCl）=0.07mol/l与测试试样混合。

如果测试试样的质量为10mg 至100mg 之间，用上述溶液5ml 与测试试样混合。

摇动1分钟，然后检查混合液的酸度。

如果测试试样含大量通常为碳酸钙的碱性材料，使用盐酸C（HCl）约6mol/l 将pH 值调整到1.0 至1.5 之间以避免稀释过度。

使用的盐酸与溶液之比必须在10g 项中列明。

如果碱性材料数量不大，混合物的pH 值又大于1.5，一边摇动混合物一边逐滴加入盐酸水溶液C（HCl）=约2mol/l，直到pH 值达到1.0 至1.5 之间，使混合物避光，在温度为（37±2）℃时搅拌混合物，持续1小时，然后使混合物在（37±2）℃下放置1 小时。

接着立即将混合物中的固体有效地分离出来，使用0 .45µm或者0.22µm滤膜过滤器过滤，然后根椐需要离心分离。

分离必须在上述放置时间结束后尽快完成，离心分离不能超过10 分钟，同时必须在10h项中列明。

有可能一些小的颜料粒子通过0,45 µm或者0,02 µm的膜过滤器。

在某种情况下这可能导致迁移值是不正确的，它不仅包括元素的迁移值还包括悬浮颗粒的元素值。

当发生这种情况的时候立即用0,02 µm的膜过滤器重新过滤。

如果不能重新过滤，则重复迁移和分离步骤，最后用0,02 µm的膜过滤器过滤。

7.4.3 Category III: Scraped-off（第三类：玩具表面刮出物）。

7.4.3.1 Coatings of paint, varnish, lacquer, printing ink, polymer and similar coatings
Using the appropriate sized container, mix the test portion so prepared with 50 times its mass of an aqueous solution of 0,07 mol/L HCl solution 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 at. Shake for 1 min. Check the acidity of the mixture. If the pH is greater than 1,5 add drop-wise, while shaking the mixture, an aqueous solution of approximately 2 mol/L HCl until the pH is between 1,0 and 1,5. Protect the mixture from lig ht. Agitate the mixture at (37 ± 2) °C for 1 h continuously and then allow to stand for 1 h at (37 ± 2) °C. 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 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 ). 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 ref iltration cannot be performed, repeat the migration and separation steps finally using a membrane filter of pore size 0,02 µm.
7.4.3.1油墨、清漆、生漆、印刷墨水、聚合物涂层和类似的涂层
使用合适的容器，在20℃将相当于测试试样质量50倍的0.07mol/l盐酸溶液与测试试样混合。

如果测试试样的质量在10mg 与100mg 之间，用上述溶液5.0ml
与测试试样混合。

摇动1分钟，然后检查混合液的酸度。

如果pH 值大于1.5，一边摇动混合物，一边逐滴加入盐酸C（HCl）=约2mol/l的水溶液直到pH 值达到1.0 至1.5 之间，使混合物避光。

在温度为（37±2）℃时持续搅拌混合物一小时，然后使混合物在（37±2）℃下放置一小时。

接着立刻将混合物中的固体物有效分离出来，先使用0,45 µm或者0,02 µm 的滤膜过滤器过滤，然后根椐需要离心分离。

分离必须在上述放置时间结束后尽快完成，离心分离不能超过10 分钟，同时必须在10h项中注明。

有可能一些小的颜料粒子通过0,45 µm或者0,02 µm的膜过滤器。

在某种情况下这可能导致迁移值是不正确的，它不仅包括元素的迁移值还包括悬浮颗粒的元素值。

当发生这种情况的时候立即用0,02 µm的膜过滤器重新过滤。

如果不能重新过滤，则重复迁移和分离步骤，最后用0,02 µm的膜过滤器过滤。

7.4.3.2 Polymeric and similar materials including laminates and reinforced textile, but excluding other textiles
Follow the procedure in 7.4.3.1.
7.4.3.2 聚合物材料和类似材料，包括用或不用纺织物增强的层压材料，但不包括其它纺织物
按7.4.3.1的程序进行
7.4.3.3 Paper and paper board
Macerate the test portion so prepared with 25 times its mass of water so that the resulting mixture is homogeneous. Quantitatively transfer the mixture to the appropriate sized container. Add to the mixture an aqueous solution of 0,14 mol/L HCl at approximately 20 °C at 25 times the mass of the test portion.
Shake for 1 min. Check the acidity of the mixture. If the pH is greater than 1,5 add drop-wise, while shaking the mixture, an aqueous solution of approximately 2 mol/L HCl until the pH is between 1,0 and 1,5. Protect the mixture from light. Agitate the mixture at (37 ± 2) °C for 1 h continuously and than allow to stand for 1 h at (37 ± 2) °C. Without delay, efficiently separate the solids from the solution, firstly
by filtration using a 0,45 µm or 0,22 µm membrane filter, and if necessary, centrifuge at high speed 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 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 ). 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 ref iltration cannot be performed, repeat the migration and separation steps finally using a membrane filter of pore size 0,02 µm.
7.4.3.3 纸或纸板
用相当于测试试样质量 25 倍的水将测试试样浸泡，使得到的混合物均匀。

将混合物定量转移到尺寸合适的容器中。

20 °C下在混合物中加相当于测试试样质量25 倍的盐酸溶液C（HCl）=0.14mol/l。

摇动 1 分钟，然后检查混合液的酸度。

如果pH 值大于1.5，一边摇动混合物，一边逐滴加入盐酸C（HCl）=约2mol/l的溶液直到pH 值达到1.0 到1.5 之间，使混合物避光，在温度为（37±2）℃时搅拌混合物，持续一小时，然后使混合物在（37±2）℃下放置一小时。

接着立刻将混合物中的固体物有效地分离出来，先使用0,45 µm或者0,02 µm滤膜过滤器过滤，然后根椐需要离心分离。

分离必须在上述放置时间结束后尽快完成，离心分离不能超过10分钟，同时必须在10 h项中列明。

有可能一些小的颜料粒子通过0,45 µm或者0,02 µm的膜过滤器。

在某种情况下这可能导致迁移值是不正确的，它不仅包括元素的迁移值还包括悬浮颗粒的元素值。

当发生这种情况的时候立即用0,02 µm的膜过滤器重新过滤。

如果不能。