主题：【原创】EN 14372-2004 6.3 Chemical tests

谢谢楼主》。。。。。。。。

EN 14372-2004 Child use and care articles - Cutlery and feeding utensils - Safety requirements and tests

6.3 Chemical tests
6.3.1  Determination of the migration of certain elements
6.3.1.1 Principle
Soluble elements (antimony, arsenic, barium, cadmium, chromium, lead, mercury and selenium) are extracted from the individual components of the cutlery and feeding utensils which are accessible to the child. Conditions which simulate contact with stomach acid shall be used. The concentrations of the soluble elements are described quantitatively.
EN 14372-2004 儿童用护理用品—刀叉和喂养工具—安全要求和试验
6.3 化学试验
6.3.1 浸提液的测定
6.3.1.1 原理
刀叉和喂养工具会频繁与儿童接触，可以通过浸提具体产品组件的方法来提取可溶性物质（锑、砷、钡、镉、铬、铅、汞、硒）。浸提过程应模拟胃酸的接触条件。对可溶性物质的浓度进行定量分析。

6.3.1.2  Apparatus, reagents, procedure and determination
Tests shall be carried out according to EN 71-3.
6.3.2  Determination of phthalate content
6.3.2.1 Principle
The aim of the method is primarily to extract, identify and quantify monomeric phthalates (with wider application to other types of plasticisers) contained in PVC samples. The extraction method uses Soxhlet extraction apparatus with diethyl ether. The total diethyl ether extractable plasticiser content is calculated by weight with Gas Chromatography-Mass Spectroscopy (GC-MS) detection to identify and quantify individual phthalates.
NOTE  It is recommended that suitable qualitative methods be used to identify chlorine containing materials [10].
6.3.1.2 仪器、试剂、试验过程及测定
应依据EN 71-3进行试验。
6.3.2 邻苯二甲酸酯类含量的测定
6.3.2.1 原理
本法最初是用于提取、定性以及定量分析PVC样品中的邻苯二甲酸酯类单体（比其他类型的增塑剂应用更为广泛）。提取使用油脂索氏萃取器，乙醚作溶剂。经乙醚提取的增塑剂总量通过气质联用仪（GC-MS）对邻苯二甲酸酯类单体的定性及定量检测来计算得到。
注：推荐使用合适的定性方法对材料中含有的氯进行确定。

The total diethyl ether extractable plasticiser content is calculated by weight with Gas Chromatography-Mass Spectroscopy (GC-MS) detection to identify and quantify individual phthalates.
定性定量怎么用来计算含量？
NOTE  It is recommended that suitable qualitative methods be used to identify chlorine containing materials [10].
感觉不是对氯的含量进行确定，而是对含氯物质进行定性

6.3.2.2 Apparatus
6.3.2.2.1  Balance (accurate to 4 decimal points).
6.3.2.2.2  150 ml stoppered flat-bottomed flask. 
6.3.2.2.3  Soxhlet extractor with siphon cup.
6.3.2.2.4  Soxhlet cellulose thimble.
6.3.2.2.5  Water cooled condenser.
6.3.2.2.6  Spark proof heating mantle/water bath.
6.3.2.2.7 Steam bath.
6.3.2.2.8  Oven (105 ± 5) °C. 
6.3.2.2.9 Desiccator chamber.
6.3.2.2.10  (200 ± 0,15) ml volumetric flask.
6.3.2.3  Reagents (analytical grade)
6.3.2.3.1 Diethyl ether.
6.3.2.3.2 n-Hexane.
6.3.2.3.3  Di-isononyl phthalate (DINP), CAS No. 28553-12-0.
6.3.2.3.4  Di-(2-ethylhexyl) phthalate (DEHP), CAS No. 117-81-7.
6.3.2.3.5  Di-n-octyl phthalate (DNOP), CAS No. 117-84-0.
6.3.2.3.6  Di-iso-decyl phthalate (DIDP), CAS No. 26761-40-0.
6.3.2.3.7  Butyl benzyl phthalate (BBP), CAS No. 85-68-7.
6.3.2.3.8  Di-butyl phthalate (DBP), CAS No. 84-74-2.
6.3.2.2 仪器
6.3.2.2.1 天平（万分之一精度）。
6.3.2.2.2 150 ml具塞平底烧瓶
6.3.2.2.3 带虹吸气压计的索氏萃取器
6.3.2.2.4 索氏滤纸筒
6.3.2.2.5 水冷凝器
6.3.2.2.6 防火加热罩/水浴
6.3.2.2.7 蒸汽浴
6.3.2.2.8 烘箱（105 ± 5）°C
6.3.2.2.9 干燥箱
6.3.2.2.10 （200 ± 0.15）ml的容量瓶
6.3.2.3 试剂（分析纯）
6.3.2.3.1 乙醚
6.3.2.3.2 正己烷
6.3.2.3.3 邻苯二甲酸二异壬酯（DINP），CAS编号 28553-12-0。
6.3.2.3.4 邻苯二甲酸（2-乙基己基酯）（DEHP），CAS编号 117-81-7。
6.3.2.3.5 邻苯二甲酸二正辛酯（DNOP），CAS编号 117-84-0。
6.3.2.3.6邻苯二甲酸二异癸酯（DIDP），CAS编号 26761-40-0。
6.3.2.3.7 邻苯二甲酸丁苄酯（BBP），CAS编号 85-68-7。
6.3.2.3.8 邻苯二甲酸二丁酯（DBP），CAS编号 84-74-2。

这个应该没有疑问

6.3.2.4  Reagents (standard solutions) 
Prepare a series of individual stock standard solutions of the individual phthalate esters in n-Hexane as shown in Table 3.
Table 3 — Stock solutions
Phthalate ester    DIDP    DINP    DBP    BBP    DNOP    DEHP
Concentration μg/ml    5 000    5 000    200    200    200    200

Where appropriate from the stock standard solutions prepare two sets of five phthalate esters GC-MS calibration solutions in n-Hexane to the maximum linear concentration shown in Table 4 (Calibration Set 1), and Table 5 (Calibration Set 2).
Table 4 — Calibration Set 1
Phthalate ester    DINP    DBP    BBP    DEHP
Concentration μg/ml    5 000    20    20    20

Table 5 — Calibration Set 2
Phthalate ester    DIDP    DNOP
Concentration μg/ml    5 000    20


6.3.2.4 试剂（标准溶液）
用正己烷为溶剂分别制备各类邻苯二甲酸酯类的标准储备液，如表3所示。
表3 — 标准储备液
邻苯二甲酸酯类    DIDP    DINP    DBP    BBP    DNOP    DEHP
浓度 μg/ml    5 000    5 000    200    200    200    200
分别用各邻苯二甲酸酯类的标准储备液制备2套GC-MS测试用标定溶液，每套5个浓度成线性关系，其最大线性浓度见表4（标定浓度1）及表5（标定浓度2）。
表4 — 标定浓度1
邻苯二甲酸酯类    DINP    DBP    BBP    DEHP
浓度 μg/ml    5 000    20    20    20

表5 — 标定浓度2
邻苯二甲酸酯类    DIDP    DNOP
浓度 μg/ml    5 000    20


Where appropriate from the stock  啥意思？语法上看不懂

6.3.2.5  Sampling, extraction and gravimetric analysis for phthalate plasticisers
Place the sample in a pre-weighed 150 ml flat bottomed flask and heat in an oven at (105 ± 5) °C for (30 ± 5) min. Allow to cool in a desiccator. Weigh the flask and sample. Use a scalpel or other appropriate cutting utensils to cut a representative portion from the sample into small pieces (< 5 mm Ø). Weigh accurately (2 ± 0,2) g of the pieces into a Soxhlet thimble and add cotton wool to the top of the thimble.
Add approximately (50 ± 10) ml of diethyl ether into the flask. Reflux gently for 6 h ± 30 min. Allow sufficient time for the diethyl ether to cool. Completely evaporate the diethyl ether by means of a steam bath. Place the flask in an oven at (105 ± 5) °C for (30 ± 5) min. Allow to cool in a desiccator and weigh. Repeat the drying and cooling cycles until the difference between two consecutive weighings are not more than 0,0005 g. A blank solution shall be run consecutively.
6.3.2.5邻苯二甲酸酯类的取样、浸提和重量分析
将样品放入已预先称重的150 ml具塞平底烧瓶中，然后将烧瓶放在（105 ± 5）°C烘箱内烘（30 ± 5）min。结束后取出置于干燥箱中放冷。再次称重烧瓶及样品。使用手术刀或其他适宜的剪切工具将样品具有代表性的部分剪切成小块状（< 5 mm Ø）。精确称量（2 ± 0.2）g块状物放入索氏滤纸筒，然后用脱脂棉塞住滤纸筒上口。
将约（50 ± 10）ml乙醚加入烧瓶。缓慢回流6 h ± 30 min。然后让乙醚完全冷却。之后用蒸气浴使乙醚完全挥发。再将烧瓶放入（105 ± 5）°C烘箱内烘（30 ± 5）min。结束后取出置于干燥箱中放冷并称重。重复上述烘干并冷却的操作步骤，直至两次连续的称重之差不超过0.0005 g。同法制备空白溶液。

原文由 redanqi 发表:
6.3.2.5  Sampling, extraction and gravimetric analysis for phthalate plasticisers
Place the sample in a pre-weighed 150 ml flat bottomed flask and heat in an oven at (105 ± 5) °C for (30 ± 5) min. Allow to cool in a desiccator. Weigh the flask and sample. Use a scalpel or other appropriate cutting utensils to cut a representative portion from the sample into small pieces (< 5 mm Ø). Weigh accurately (2 ± 0,2) g of the pieces into a Soxhlet thimble and add cotton wool to the top of the thimble.
Add approximately (50 ± 10) ml of diethyl ether into the flask. Reflux gently for 6 h ± 30 min. Allow sufficient time for the diethyl ether to cool. Completely evaporate the diethyl ether by means of a steam bath. Place the flask in an oven at (105 ± 5) °C for (30 ± 5) min. Allow to cool in a desiccator and weigh. Repeat the drying and cooling cycles until the difference between two consecutive weighings are not more than 0,0005 g. A blank solution shall be run consecutively.
6.3.2.5邻苯二甲酸酯类的取样、浸提和重量分析
同法制备空白溶液。

是邻苯二甲酸增塑剂的取样、浸提和重量分析吧
A blank solution shall be run consecutively 空白溶液同法制备，还是连续跑几次？
run可以翻译为制备吗？

6.3.2.6  Preparation of sample extract solution for Gas Chromatography-Mass Spectroscopy (GC-MS)
To the weighed extract (6.3.2.5) add (50 ± 2) ml of n-Hexane. Stopper the flask and swirl to completely dissolve the extract. Decant the solution into a 200 ml volumetric flask, repeatedly rinsing the flask with n-hexane. Make up to the mark. Prepare (if necessary) further diluted solutions using n-hexane such that the final concentration in solution is within the linear calibration concentration for phthalate present. Transfer a portion of the n-hexane solution into a capped vial for GC-MS analysis.
Suitable GC-MS column and method and data on the repeatability of the method are described in Annex A.

6.3.2.6用于气质联用仪（GC-MS）的样品浸提溶液的制备
在已称重的浸提物（6.3.2.5）中加入（50 ± 2）ml的正己烷。塞紧烧瓶然后来回晃动使浸提物完全溶解。然后将溶液缓缓倒入一200 ml的容量瓶中，再用正己烷将上述步骤重复一遍。定容至刻度线。如需要，再用正己烷对上述制备液进行稀释，使得其最终浓度在邻苯二甲酸酯类储备液的线性标定浓度范围内。移取适量该正己烷溶液至封口瓶内，进行GC-MS分析。
附录A中给出了适宜的GC-MS柱、检测方法以及方法重现性方面的数据。

repeatedly rinsing the flask with n-hexane.  Prepare (if necessary) further diluted solutions using n-hexane such that the final concentration in solution is within the linear calibration concentration for phthalate present. Transfer a portion of the n-hexane solution into a capped vial for GC-MS analysis.
Suitable GC-MS column and method and data on the repeatability of the method are described in Annex A.

再用正己烷将上述步骤重复一遍。定容至刻度线。如需要，再用正己烷对上述制备液进行稀释，使得其最终浓度在邻苯二甲酸酯类储备液的线性标定浓度范围内。移取适量该正己烷溶液至封口瓶内，进行GC-MS分析。
附录A中给出了适宜的GC-MS柱、检测方法以及方法重现性方面的数据。

第一句，我觉得是用正己烷重复洗涤烧瓶。repeatedly这里是重复多次的意思，我们洗烧瓶讲究的就是少量多次。
Prepare (if necessary) further diluted solutions using n-hexane such that the final concentration in solution is within the linear calibration concentration for phthalate present.很拗口，
a portion of是部分的还是适量的？

6.3.2.7 Calculation of results
Compare the obtained GC-MS spectra to known spectra or phthalate ester standards to allow qualitative identification of phthalate ester plasticisers or any other compounds. Plot a calibration graph of the response against the known standard concentrations.
From the calibration graph determine the response of phthalate ester found in the blank/sample and interpolate the concentration of phthalate ester in μg/ml correcting for any dilutions.

6.3.2.7 结果计算
对测得的GC-MS图谱与已知的图谱或邻苯二甲酸酯类的标准图谱进行比较，得到该邻苯二甲酸酯类增塑剂或其他化合物的定性确定。绘制已知浓度的标准溶液的光谱标准曲线图。
从该曲线图上即可找到邻苯二甲酸酯类的响应峰对应的空白/样品以及稀释范围内的浓度。