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EN71-3新法规标准更新,rosh19项检测报告方案

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扫一扫!EN71-3新法规标准更新,rosh19项检测报告方案扫一扫!
人气:-发表时间:2016-05-17 10:31【

该要求将于2013年7月21日生效,协调标准为EN71-3,目前还在过渡期。 

新EN71-3检测元素:铝、锑、砷、钡、硼、镉、铬(III)、铬(VI)、钴、铜、铅、锰、汞、镍、硒、锶、锡、有机锡、锌 ;XRF应用解决方案!

所需分析仪器:德国斯派克 荧光光谱仪

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

EN71-3: 2013 was officially released on June 5, the official version reduces the Ba (barium) limits. Specific limits are as follows(EN71-3:2013 已于6 月5 号正式发布,正式版本中降低了Ba(钡)的限值。具体的限值如

下:):

ROHS分析表

1.JPG

3. Chromium (III) and Chromium (VI) 关于三价铬和六价铬的检测

As a first action method, the migration of combined chromium can be determined. If the migration of

combined Chromium (i.e. Chromium (III) + Chromium (VI)) is below the maximum limit for Chromium (VI), it

can be inferred that the material complies with the requirements for both Chromium (III) and Chromium (VI).

标准中给出可溶性总铬的测试方法,如果测得可溶性铬(Cr (III) + Cr (VI))<0.2mg/kg(六价铬的高限值)时,

可以推断该材料符合三价铬和六价铬的要求。

For Chromium VI the method in Annex F the limit of quantification is higher than the migration limit for category

I and II toy materials. Compliance with the limits cannot be demonstrated by a migration test, however other

options are available:

—— determination of the content of combined chromium;

 —— safety assessment of the toy material.

附录F 中六价铬的定量限值高于第一类和第二类材料的迁移限值,不能按照附录F 的方法测试,但是可以通过

其它方式评估:

—— 铬的总含量

—— 玩具材料的安全评估

4. Organic tin(有机锡)

The migration of organic tin shall be calculated by adding the migration values for all the single organic tin

compound s that have been detected. The migration of organic tin is expressed as tributyltin. 10 kinds of

organic tin LOD, LOQ as follows:

有机锡的迁移通过计算检测出来的单个有机锡的总和。有机锡的迁移值通过三丁基锡来表达。10种有机锡的

LOD,LOQ如下:

Typical detection limits (LOD) and quantification limits (LOQ) expressed in mg/kg toy material (有机锡化合物

的的检测限(LOD)和定量限(LOQ))

分析ROHS

Annex F(附录F)

Methods of analysis for speciation of Chromium (III) and (VI)

铬(III) 和铬(VI)分析方法

F.1 Principle 原理

This method quantifies Chromium (III) and Chromium (VI) in the migration solution. This method is capable to

determine compliance with the migration limit for category III toy materials. The limit of quantification is higher

than the migration limits for category I and II toy materials . In I.2 guidance is given how compliance can be

demonstrated for category I and II toy materials .

这种方法定量铬(III) 和铬(VI)的迁移溶液。这种方法针对玩具材料的第III类材料。定量限值高于玩具材料的第I类

和第II类的迁移限值,不能按照附录F的方法测试,但是可以通过其它方式评估。

To prevent interconversion of Chromium (III) and Chromium (VI), the migration solution is neutralised directly

after the migration step. Experiments have shown that at a pH of 7.1 both species are stable. Mobile phase is

added, containing EDTA. EDTA reacts to form a complex with Chromium (III). Chromium (III) and Chromium

(VI) are then separated by liquid chromatography using an LC-ICP-MS technique.

为了防止三价铬和六价铬的相互转化,迁移溶液在样品迁移之后必须是中性的。实验表明pH值为7.1的时候两种

形态是稳定的。流动相要加入EDTA(乙二胺四乙酸)。EDTA反应生成三价铬的化合物。三价铬和六价铬通过

LC-ICP-MS技术分离。

When analysing Chromium (III) and (VI) in one run, a high peak of Chromium (III) may influence the peak of

Chromium (VI). This can be solved by skipping the complexation step with EDTA, thereby only showing the

Chromium (VI) peak in the chromatogram. Chromium (III) can then be determined by either analysing the

migration solution as well after the complexation step, or by determining the migration of combined Chromium:

Chromium (III) = total Chromium – Chromium (VI).

当分析三价铬和六价铬的时候,三价铬有一个高峰可能会影响六价铬的峰。可以用EDTA络合解决这个问题,因

此色谱图上只显示六价铬的峰。三价铬络合后可F.2 Reagents 试剂

Use reagents of highest purity. 所用试剂需要优级纯

F.2.1 Water, Milli Q 18.2 M?.cm

F.2.1 水,Milli Q超纯水系统生产的电阻率18.2 M?.cm的水

F.2.2 Hydrochloric acid, HCl (30% d = 1,15 g/ml or equal)

F.2.2 盐酸,HCl (30% d = 1,15 g/ml or 等同)

F.2.3 Tetrabutylammonium hydroxide (TBAH), 40 wt % in water, [CH3(CH2)3]4NOH, CAS# 2052-49-5

F.2.3 TBAH,水中的质量分数40%,[CH3(CH2) 3]4NOH, CAS# 2052-49-5

F.2.4 Potassium Ethylenediamine tetraacetic acid, C10H14K2N 2O 8 * 2H2O, CAS# 7379-27-3

F.2.4 乙二胺四乙酸钾,C10H14K2N 2O 8 * 2H2O, CAS# 7379-27-3

F.2.5 Ammonia, NH3 (25 % in water)

F.2.5 氨NH3 (25 %在水中)

F.2.5.1 Ammonia solution c(NH3 (aq)= (0,07 ± 0.005) mol/L

F.2.5.1氨水溶液 c(NH3 (aq)= (0,07 ± 0.005) mol/L

F.2.6 Acetic acid (glacial), 100 %

F.2.6 冰醋酸,100%

F.2.7 Methanol, CH3OH

F.2.7 甲醇, CH3OH

F.2.8 Hydrochloric acid solution, c(HCl) = (0,07 ± 0,005) mol/L

F.2.8 盐酸溶液,c(HCl) = (0,07 ± 0,005) mol/L

F.2.9 Chromium (III) 1000 mg/l in water

F.2.9 1000 mg/l三价铬溶液

F.2.10 Chromium (VI)1000 mg/l in water

F.2.10 1000 mg/l六价铬溶液

F.2.11 Stock solution Chromium (M1)

Prepare a stock solution (M1) diluting 0,5 mL of the commercial available stock solutions of the individual

elements (concentration = 1 000 mg/kg) in mobile phase to a volume of 50 mL. Allow the final solution to stand

for 1 hour at 50 °C.

F.2.11 铬储备溶液(M1)

制备一个储备溶液(M1),在流动相中稀释0.5ml从商家购买的单种元素浓度为1000mg/L的标液到50ml。

终的溶液在50 °C下保存一小时。

F.2.12 Diluted stock solution (M2)

Dilute 0,5 mL of stock solution M1 in mobile phase to 50 mL.

F.2.12 稀释的储备溶液(M2)

在流动相中稀释0.5ml储备溶液M1到50ml。

F.2.13 Working solutions (Calibrating Standards)

Sequentially dilute diluted stock solution (M2) with mobile phase, after addition of 2,5 mL ammonia and 2,5 mL

hydrochloric acid, in order to obtain standards to be used for calibration according to the scheme in Table B.1.

Allow the working solutions to stand for 1 h at 50 °C.

F.2.13工作溶液(校准溶液)

将稀释后的储备溶液(M2)加入流动相继续稀释,然后添加2.5ml氨水和2.5ml盐酸根据表F.1以获得校准溶

液。允许工作溶液在50 °C下保存一小时。

Table F.1 — Preparation scheme working solutions

ROHS分析表

dissolve in water. Adjust the pH with acetic acid to 7.1.

F.2.14 流动相

称取647mgTBAH 和243 mg EDTA,加水稀释,定容到1000ml。用醋酸调pH 到7.1。

F.3 Apparatus 设备

F.3.1 Volumetric flasks, glass

F.3.1 玻璃容量瓶

F.3.2 Variable pipettes with disposable tips, variable range

F.3.2 可调节移液枪:带一次性吸头,可变容积范围

F.3.3 ICP-MS, equipped with HPLC module

F.3.3 ICP-MS,需配备HPLC 组件

F.3.4 pH-meter

F.3.4 pH 计

F. 4 Procedure

Use 1 ml of migration solution. Add 1 mL ammonia to 1 mL migration solution. Additionally 8 mL mobile phase

solution is added. Allow the final solution to stand for 1 h at 50 °C.

NOTE 1 When the pH was adjusted, the amount of ammonia added must be equivalent to the total amount of

HCl. The pH of 7.1 is established after addition of 8 ml of mobile phase.

NOTE 2 It has been shown that presence of manganese will lead to oxidation of Chromium (III) into Chromium

(VI).

F. 4 程序

加1ml 氨水到1ml 迁移溶液中,继续加入8ml 流动相溶液。混合后的溶液在50 °C 下保存1 h。

备注1:当调pH 值的时候,添加氨水的量和盐酸的总量相同。在添加8ml 流动相后pH 值为7.1。

备注2:锰的存在会导致三价铬氧化为六价铬

F.5 Analysis 分析

F.5.1 General 概要

Inject samples and calibration solutions into the LC - ICP - MS system.

注入样品和校准溶液到LC-ICP-MS系统中。

F.5.2 Limit of detection and quantification 检测限值和定量限值

In Table F.2 typical limits of detection (LOD )and quantification (LOQ) are given.

Table F.2 — Typical detection limits (LOD) and quantification limits (LOQ) expressed in mg/kg toy material

ROHS分析

此文关键字:rosh分析仪 ROHS检测仪

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