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色膏EN732013元素的迁移

作者:高考题库网
来源:https://www.bjmy2z.cn/gaokao
2021-01-22 07:31
tags:

keyboard-

2021年1月22日发(作者:reasons)
,.
EN71-3 2013






Safety of toys - Part 3: Migration of certain
elements
玩具安全
-

3
部分:元素的迁移

1 Scope
(范围)

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范围之类,
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内:

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,< br>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
标准的这一部分之内。

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、吞咽的产品范
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




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

具材料分类的参照表)

Toy Material
玩具材料

Category
Category
I
种类Ⅰ

Coatings

of paints, varnishes, lacquers,
printing inks, polymers, foams and
similar coatings
涂层:
油漆、
清漆、
生漆、
印刷油墨、
聚合物、
海绵和类 似的涂层


II
种类Ⅱ


Category
III
种类Ⅲ

X
,.
Polymeric and similar materials,
including

laminates, whether textile reinforced or
not, but

excluding other textiles
高分子材料和类似的材料,
包括不论是否有纺
织物增强的层压材料,
但不包括其它的 纺织物

Paper and paper board
纸张和纸板

Textiles, whether natural or synthetic
天然或合成纺织物

Glass, ceramic, metallic materials
玻璃,陶瓷,金属材料

Other materials whether mass coloured
or not

(e.g. wood, fibre board, hard board, bone
and

leather)
其它材料,不管是否被染色(例如:木材、纤
维板、硬质板、骨头和皮革)

Compressed paint tablets, materials
intended to



X


X


X


X


X
X


,.
leave a trace or similar materials in solid
form

appearing as such in the toy (e.g. the
cores of

colouring pencils, chalk, crayons)
压缩漆,
会留下痕迹的或类似的以固体形式出
现在玩具上的材料< br>(例如:
彩色铅笔芯,
粉笔、
蜡笔)

Pliable modelling materials, including
modelling

clays and plaster
软性造型材料,包括造型粘土和石膏

Liquid paints, including finger paints,
varnishes,

lacquers, liquid ink in pens and similar
materials in liquid form appearing as
such in the toy (e.g. slimes, bubble
solution)
液体油漆,包括指画颜料、清漆、生漆、笔里
面 的液体油墨和在玩具上呈液态的类似材料
(例如煤泥、泡泡水)

Glue sticks
固体胶


X


X

X


,.
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

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


2
玩具材料的迁移限量

Element

元素

Category I
种类Ⅰ
(mg/kg)
Aluminium


Antimony


Arsenic


Barium


Boron


Cadmium


Chromium (III)
铬(
3+


Chromium (VI)
铬(
6+


Cobalt


Copper


Lead


10.5
622.5
13.5
2.6
156
3.4
130
7700
160
0.02
0.005
0.2
5625
45
3.8
1500
1200
1.3
37.5
Category


种类Ⅱ
(mg/kg)
1406
11.3
0.9
375
300
0.3
9.4
Category


种类Ⅲ
(mg/kg)
70000
560
47
18750
15000
17
460
,.
Manganese


Mercury


Nickel


Selenium


Strontium


Tin


1200
7.5
75
37.5
4500
15000
300
1.9
18.8
9.4
1125
3750
0.2
938
15000
94
930
460
56000
180000
12
46000
Organic tin
有机锡

0.9
Zinc



5 Principle
(原理)

3750
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< br>,
硼、镉、钴、铜、铅、锰、汞、镍、硒、锶、锡和
,.

);
——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
7
H
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
±
0.0 05

mol/l
6.1.2
盐酸溶液,
c

HCl

=

0.14
±
0.010

m ol/l


6.1.3
盐酸溶液,
c

HCl

=

1mol/l


6.1.4
盐 酸溶液,
c

HCl

=

2mol/l


6.1.5
盐酸溶液,
c

HCl

=

6mol/l


6.1.6
正庚烷(
C
7
H
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 2.5?m.

6.2.7 Membrane filter, with a pore size of 0,45,0.22 and 0.02
μ
m
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

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 ?m。

6.2.7
滤膜过滤器,滤孔为
0.45, 0.22

0.02
μ
m


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.
在一个合适的工作范围内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 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. 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

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< br>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
10 h
)。

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)


Wfp2
计算
7.4.2.1

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
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

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

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< br>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< br>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

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、陶瓷和金属材料





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< br>/
陶瓷
/
金属材料,
必须先按
7.3.3.1
的程< br>,.
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
/
陶瓷
/
金属材料的玩具和部件无须按< br>7.4.3.5
的程序进
行测试。可接触的玻璃
/
陶瓷
/< br>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



7.3.3.2

7.3.3.3

7.3.3.4

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< br>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

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< br>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< br>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
μ
m
or 0,22
μ
m 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
,.
?m or 0,22 ?m 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 ?m. Or where the ref iltration cannot be performed, repeat the
migration and separation steps finally using a membrane filter of pore
size 0,02 ?m.





7.4.2.1
含油脂、油类、蜡或类似材料的样品

称量
0.05 g
左右,
Wfp2*25g

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

=

2mol/l
,直到
pH
值达到
1.0

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

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 ?m或者0,02 ?m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 ?m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 ?m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

?m or 0 ,22 ?m 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
?m or 0,22 ?m 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 ?m. Or where the ref iltration cannot be performed, repeat the
migration and separation steps finally using a membrane filter of pore
s
ize 0,02 ?m.

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

C

HCl

=0.07mol/l
与测试试样混合。如果测试试样的质量为
10mg

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


6mol/l
,.

pH
值调整到
1.0

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

=

2mol/l
,直到
pH
值达到
1.0

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 .45?m或者0.22?m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 ?m或者0,02 ?m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 ?m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 ?m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 light. 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
μ
m or 0,22
μ
m 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
?m or 0,22 ?m 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 ?m. Or where the ref iltration cannot be performed, repeat the
migration and separation steps finally using a membrane filter of pore
size 0,02 ?m.

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

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

=

2mol/l
的水溶液直到
pH
值达到
1.0

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 ?m或者0,02 ?m
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 ?m或者0,02 ?m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 ?m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 ?m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


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 ?m or 0,22 ?m
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
?m or 0,22 ?m 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 ?m. Or where the ref iltration cannot be performed, repeat
the
migration and separation steps finally using a membrane filter of pore
size 0,02 ?m.

,.
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

=

2mol/l
的溶液直到
pH
值达到
1.0

1.5

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 ?m或者
0,02
?m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 ?m或者0,02 ?m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 ?m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 ?m的膜过滤器过滤。

7.4.3.4 Textiles, whether natural or synthetic

Follow the procedure in 7.4.3.1.
7.4.3.4
天然或合成的纺织物







7.4.3.1
的程序进行

7.4.3.5 Glass, ceramic and metallic materials

Weight the toy or component in a 50 mL glass container with nominal
dimensions: height 60 mm, diameter 40 mm. Add sufficient volume of an
,.
aqueous solution of 0,07 mol/L HCl at approximately 20
°
C to just cover
the toy or component. Cover the container, protect the contents from
light and allow the contents to stand for 2 h at (37
±

2)
°
C.

NOTE 1 This type of container will take all components/toys that fit
inside the small parts cylinder.

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
μ
m or 0,22
μ
m 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
?m or 0,22 ?m 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 ?m. Or where the ref iltration cannot be performed, repeat the
migration and separation steps finally using a membrane filter of pore
size 0,02 ?m.

,.
7.4.3.5
玻璃、陶瓷和金属材料





将玩具或部件放入

50ml
的玻璃容器,尺寸为: 高
60mm
,直径
40mm


20
°
C
下加入足量的盐酸溶液
C

HCl

=0.07 mol/ l
,以使能正好覆盖玩具或
部件。将容器盖上,使内容物避光并在温度(
37
±
2
)℃下放置
2
小时。

备注
1
:这 类容器可容纳所有能够进入小零件测试圆筒的部件
/
玩具。

接着立刻将混合 物中的固体物有效地分离出来,
先进行倾析,
然后使用
0,45
?m或者0,02 ?m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
项下列
明。

有可能一些小的颜料粒子通过0,45 ?m或者0,02 ? m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 ?m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 ?m的膜过滤器过滤。

7.4.3.6 Other materials, whether mass coloured or not

The materials shall be tested by the most appropriate method of 7.4.3.2,
7.4.3.3, 7.4.3.4 or 7.4.3.5. The method used shall be reported under 10 h.
7.4.3.6
其它材料,不管是否大量着色





必须按
7.4.3.2

7.4.3.3

7.4.3.4

7.4.3.5
中最适用的方法对材料进行测
试。采用的方法必须在
10h
项中列明。

8 Methods of analysis
(分析方法)

For all types of sample preparation, the final extract is analysed for
presence of elements by ICP-MS, ICP-OES, CVAAS,

GC- MS or other
,.
suitable techniques.

A validated method should be used. The sensitivity of the used method
must be such that the quantification limit is below the migration limits in
Table 2.

The obtained migration solution (7.4) is analysed by three different
methods (one f or general elements, one for Chromium (III) and
Chromium (VI) and one for

organic tin ) . Each method requires an
amount of the migration solution. For general elements 4 ml of
migration solution is required, for Chromium (III) and (VI) 1 ml; for
organic tin 5 ml. In order to determine all of the required elements, it
may be necessary to perform an additional dilution of the migration
solution. In this case, the limits of detection and the limits of
quantification of the relevant analyses shall be reported under 10 h.



对于不同类型的样品的制备,最后用
ICP-MS

ICP- OES

CVAAS

GC- MS

其它合适的技术萃取分析存在的元素。

使用的方法应该进行方法确认 。
所用方法的定量限值应该低于表
2
中的迁移限值。

迁移溶液的分 析通过三种不同的方法(一种是一般元素,一种是铬
(III)
和铬
(VI)
,还有一种是有机锡)。每个方法需要一定量的迁移溶液。对于一般元素需

4ml
的 迁移溶液
,

(III)
和铬
(VI)
需要
1ml ;
有机锡需要
5ml
。如果三种测试都测
,
有必要稀释迁移溶液。< br>在这种情况下相关分析的检出限和定量限应在
10h
项中注
明。

9 Calculation of results
(结果的计算)

,.
9.1 Standard elements
(标准元素)

9.1.1 Calibration curve
(校准曲线)

Prepare calibration curves of each element of interest by plotting the
concentration of the standards of the element of interest (see 7.2)
against the measuring signal. For quantification the calibration curve
shall have a correlation coefficient better or equal to 0,990.





通过测试每一个元素标准溶液的浓度绘制一个校准曲线来检测仪器的反 应。
校准曲线定量化的校正因子为
0.990
或者更好。

9.1.2 Calculation of migration
(迁移的计算)

Calculate the amount of an element in the sample by



where


Migration : release of an element from the sample (mg/kg)

C : sample solution concentration (mg/L)

V : volume of simulant added (mL)

A : amount of test portion (mg)
f: dilution factor
Report the results to the number of significant figures justified by the
precision of the measurement .
样品中某一元素含量的计算公式:

迁移量(
mg/kg
=
C
?
V
?
1000
?
f

A
,.
迁移:某一元素从样品中释放出来(
mg/kg


C:
样品溶液浓度
(mg/L)
V:
模拟添加的体积(
ml


A:
样品质量(
mg


f:
稀释因子

报告结果的有效数字应根据测量的精密度来确定。

9.1.3 Interpretation of results
结果分析

The measurement uncertainty, ut,r, shall be used to interpret an
analytical result in relation to compliance assessment. Laboratories are
required to determine their own performance data, including
measurement uncertainty (see Annex B).
测量不确定度,
Ut,r
,应被用来解释相关符合性评估的分析 结果。实验室必须确
定自己的性能数据,包括测量的不确定度。

9.2 Chromium (III) and Chromium (VI) Cr(3+)

Cr(6+)
9.2.1 Calibration curve
(校准曲线)

Prepare calibration curves of each element of interest by plotting the
concentration of the standards of the element of interest (see 7.2)
against the measuring signal. For quantification the calibration curve
shall have a correlation coefficient better or equal to 0,990.





通过测试每 一个元素标准溶液的浓度绘制一个校准曲线来检测仪器的反应。
校准曲线定量化的校正因子为
0 .990
或者更好。

9.2.2 Calculation of migration
(迁移的计算)

,.
Calculate the amount of an element in the sample by

where

Migration : release of an element from the sample (mg/kg)

C : sample solution concentration (mg/L)

V : volume of simulant added (mL)

A : amount of test portion (mg)
f: dilution factor
NOTE

For calculation of C take the dilution factor into account caused
by the neutralisation step and the complexation step.
Report the results to the number of significant figures justified by the
precision of the measurement .
样品中元素含量的计算公式:

迁移量 (
mg/kg

=
C
?
V
?
1000?
f

A
迁移:一种元素从样品中释放出来(
mg/kg


C:
样品溶液浓度
(mg/L)
V:
模拟添加的体积(
ml


A:
样品质量(
mg


f:
稀释因子

备注:计算
C
要考虑到稀释因素所引起的中和和络合作用。

报告结果的有效数字应根据测量的精密度来确定。

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