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This standard is developed in accordance with the rules given in GB/T 1.1-2009.
This standard replaces GB/T 20155-2006 Determination of mercury, cadmium and lead in battery.
The following main changes have been made with respect to GB/T 20155-2006:
——The application scope of standard is modified (see Clause 1);
——The processing method of battery pack sample is added (see 6.2);
——The “Determination of mercury content [Cold atomic absorption spectrometric methods (AAS)]” is modified (see Clause 7, 2.1 of Edition 2006);
——The “Determination of cadmium/lead content [flame atomic absorption spectrometric methods (FAAS)]” is added (see Clause 9, 2.2 and 2.3 of Edition 2006).
This standard was proposed by China National Light Industry Council.
This standard is under jurisdiction of SAC/TC 176 National Technical Committee on Primary Battery of Standardization Administration of China.
The previous edition of this standard is as follows:
——GB/T 20155-2006.
Determination of Mercury, Cadmium and Lead in battery
Caution: the hydrochloric acid and nitric acid used in this standard are volatile and corrosive, so avoid inhalation or contact with skin when using them. Wash them with plenty of water immediately when splashing on the skin, and seek medical attention immediately if serious.
1 Scope
This standard specifies the detection methods of mercury, cadmium and lead in battery.
This standard is applicable to the determination of mercury, cadmium and lead in small sealed primary batteries which meet the standard of GB/T8897.2 and with single battery mass of not more than 200g.
Determination range: mercury content is 0.05 μg/g ~ 100 mg/g; cadmium content is 1.0 μg/g ~ 100 mg/g; lead content is 5.0 μg/g ~ 100 mg/g.
Note: The lower limit of the determination range of each element varies with the precision performance of the apparatus and the dilution multiple when preparing the sample solution. If the total volume of sample solution is reduced or the sample weighing amount is increased, the lower limit of the determination range of mercury, cadmium and lead may be reduced. For example, on the premise that the precision performance of the apparatus meets the requirements of this standard, when the total volume of the sample solution is half of that in “Table 1 Mass range, model example of battery and added reagent amount”, the lower limit of the determination range is: 0.025μg/g of mercury, 0.5μg/g of cadmium, 2.5μg/g of lead; the lower limit of the determination range is 0.01μg/g of mercury, 0.2μg/g of cadmium and 1.0μg/g of lead when the dilution multiple is 5 in case of preparing sample solution (when the battery sample mass is 20g, and the total volume of the sample solution is 100mL).
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
GB/T 603 Chemical reagent - Preparations of reagent solutions for use in test methods
GB/T 6682-2008 Water for analytical laboratory use - Specification and test methods
GB/T 8897.2 Primary batteries - Part 2: Physical and electrical specifications
3 Test method - General
After stripped, the battery is decomposed with nitric acid and hydrochloric acid and then filtered to prepare the sample solution. Method I cold atomic absorption spectrometric methods (AAS) or method II atomic fluorescence spectrometry is adopted to determine the content of mercury, and method III flame atomic absorption spectrometry or method IV inductively coupled plasma atomic emission spectrometry is adopted to determine the contents of lead and cadmium.
4 Test conditions
4.1 Ambient conditions
Except for special regulations, the inspection shall be carried out in the following environment:
Temperature: 15℃~35℃;
Relative humidity: 30%~90%;
Atmospheric pressure: 86kPa~106kPa.
4.2 Safety condition
Appropriate protective measures shall be taken to prevent personal injury.
It shall be determined by qualified and experienced technicians.
5 General reagents and apparatuses and equipment
Unless otherwise specified, reagents with a purity not lower than analytical purity and secondary water that meet the standard of GB/T 6682-2008 shall be used in the analysis, and guaranteed or spectrally pure reagents should be used for microscale and trace analysis. Unless otherwise specified, the preparations and products used in the test are prepared according to standard of GB/T 603.
5.1 Hydrochloric acid (ρ 1.19g/mL).
5.2 Hydrochloric acid 1+1.
5.3 Nitric acid (ρ 1.42g/mL).
5.4 Nitric acid, 1+1.
5.5 Nitric acid, 1+99.
5.6 Potassium dichromate solution: 50g/L.
5.7 Standard mercury storage solution, 0.1000mg/mL: weigh 0.1354g of mercury chloride (HgCl2) that has been fully dried and put in a silica gel desiccator overnight, dissolve it in 10mL of potassium dichromate solution, add 100mL of nitric acid (5.4), and transfer into a 1,000mL volumetric flask, dilute to the scale with water and mix well. Or purchase standard mercury solution with a mass concentration of 0.1000mg/mL of commercially available certified national standard material.
5.8 Mercury standard solution, 0.1000μg/mL: pipette 10.00mL of mercury standard storage solution (5.7), put it in a 100mL volumetric flask, add 1mL of potassium dichromate solution (5.6) and 10mL of nitric acid (5.4), dilute to the scale with water, and mix well to obtain standard mercury intermediate solution (I) with concentration of 10.00μg/mL; pipette 10.00mL of standard mercury intermediate solution (I), put it in a 100mL volumetric flask, add 1mL of potassium dichromate solution (5.6) and 10mL of nitric acid (5.4), dilute to the scale with water, and mix well to obtain standard mercury intermediate solution (II) with concentration of 1.000μg/mL; pipette 10.00mL of standard mercury intermediate solution (II), put it in a 100mL volumetric flask, add 1mL of potassium dichromate solution (5.6) and 10mL of nitric acid (5.4), dilute it to the scale with water, and mix well to obtain the standard mercury solution with the concentration of 0.1000μg/mL.
Foreword I 1 Scope 2 Normative references 3 Test method - General 4 Test conditions 5 General reagents and apparatuses and equipment 6 Sample 7 Method I Determination of mercury content [cold atomic absorption spectrometric methods (AAS)] 8 Method II Determination of mercury content [atomic fluorescence spectrometry (AFS)] 9 Method III Determination of cadmium/lead content [flame atomic absorption spectrometric methods (FAAS)] 10 Method IV Determination of cadmium or lead contents [inductively coupled plasma atomic emission spectrometric method (ICP-AES)] 11 Quality assurance and control 12 Test report Annex A (Informative) Reference working conditions for apparatus Bibliography
除有特殊规定外 ，检验应在以下环境中进行 ： a) 温度 ：15 ℃ 35 。c; b) 相对湿度 ：30 % 90 % ; c) 大气压力 ：86 k Pa 106 kPa 。 4.2 安全条件
应采取适当防护措施 ，防止造成人身伤害 。
应由有资格 、有经验的技术人 员进行测定。
5 通用试剂与仪器设备
除非另有说明 ，在分析中应使用纯度不低于分析纯的试剂和符合 GB/T 6682-2008 的二级水 微 量 、痕量分析时宜使用优级纯或光谱纯试剂 。除非另有说明，试验中所用制剂和制品均按照 GB/T 603 制备。 5.1 盐酸（ρ 1.19 g/ m L） 。 5.2 盐酸 ，1+ 1。 5.3 硝酸（ρ 1.42 g/ m L） 。 5.4 硝酸 ，1+ 1。 5.5 硝酸 ，1+ 99 。 5.6 重铭酸钊l溶液，50 g/ L。 5.7 乘标准储存溶液 ，0.100 0 mg/ n1L ：称取置于硅胶干燥器中放置过夜已充分干 燥的氯化乘＜ HgCl 2 ) 0.135 4 g ti于 10 m L 重馅酸御榕液，加入 100 m L 硝酸（ 5.的，移入 1000 m L 容量瓶中 ，用水稀 释至刻 度，混匀 。或购买市售 有证国家标准物质质量浓度为 0.100 0 mg/ mL 的束标准j容液 。 5.8 隶标准溶液，0. 100 0 /Lg/ m L：移取 10.00 m L 来标准储存溶液（ 5.7），置 于 100 m L 容量瓶中，加入 1 mL 重馅酸例溶液（ 5.6） 、10 m L 硝酸（5.的，用水稀释至刻度 ，混句得到浓度为 10.00 1.1g/ m L 柔标准 中 间溶液＜ I ＞ ；移取 10.00 m L 隶标准中 间溶液 cI＞ ，置 于 100 m L 容量瓶中 ，加入 1 n1L 重络酸佣溶液 ( 5.6 ） 、10 m L 硝酸（5.的，用水稀 释至刻度 ，？昆匀得到浓度为 1.000 µg/ m L 束标准中间溶液 ＜ II ) ；移取 10.00 n1L 乘标准中间榕液（ lI) ＇置 于 1 00 m L 容量瓶中 ，加入 1 m L 重络酸押溶液（ 5.6） 、10 m L 硝酸 ( 5.,n 注1 g .称量精确至 0001 g（小型扣式电池可 称量数只电池，使总质量达到 l g 以上〉 。 6. 1 .2 电池组样晶
对于由11 个（ n 为 2 个或 2 个以上〉 单体电池构成的电池组，称量并记录电池组质 量为 Mo (g） ，将电 池组拆分为 n 个单体电池 和电池组塑料或金属外壳及极柱零件两个测试样品 ，称量并记录样品 1 目11 n 个单体电池的总质量 M 1 C g） 稍 量并 记 录样品 2 即电池组 塑料或金 属外壳及极柱零件的总质量 J\t12 (g） 。称量 1个单体电池井；记录其质量 1n ( g) , (M1 η . 111 ) ' 100 g二三m 二月O g，称量精确至 0.01 g ; 10 g>,n 注1 g，称量精确至 0.001 g；将电池组塑料或 金属外壳及极柱零件用清洁的剪钳 、剪刀或其他适 当工具剪切为 尺寸 3 m m 以下的颗粒试料 ，称量全部颗粒试料并记录其质 量 m ，精确至 0 .001g。样品 1 单体电池的隶或销或铅单个元素含量的测定结果为 W 1 (µg/ g） ，样品2 即电池组塑料或金属外壳及极柱 零件的隶或俑或铅单个元 素含量 的测定结果为 W 2 ( /J,g／剖，则电池组 的柔政铺或铅单个元素含 量的测 定结果 w (µg/g） 为：w =JVJ 't且J』, +M ? W ? ‘ ." • •
7.2. 1 氯化亚锡 （ SnCl2 • 2 H2 0） 溶液 ，200 g/ L ：称取 20 g 氧化亚锡 C SnCl2 • 2 H2 0） 加热溶于盐酸 (5.2 ） 中，冷却后再加入盐酸 （ 5.2 ） 至1容 液总体积为 100 m L. 7.2.2 测来仪或原子吸收分光光度计（ 附亲测定装置和最空心阴极灯） 。
7.3 试验步骤
7.3. 1 仪器调试 按照仪器说明书进行调试 。 7.3.2 工作 曲线
分别移取宋标准洛液（ 5.8)0.00 mL 、0.50 m L 、.00 m L 、2.00 m L 、5.00 、10.00 m L 于一组 100 m L 容 量瓶中 加入 lm L 重错酸钊l溶液（5.6 ） 、10 m L 硝酸 （ 5.川，用水稀释至刻度混匀．即得隶质量浓度分别 为 0.00 /-lg/ m L 、0. 50 ×10-3 11.g/ m L 、1.00 ×10-3 µg/ m L 、2 .00 ×10-3 µg/ m L、5.00 ×10-3 µg/ m L 、 10.00 ×10-3 附／m L 的标准系列溶液 。将标准系列洛液由低浓 度到高浓度依次引人仪器反应装 置中 ， 加入 l m L 氯化亚锡溶液（7.2.1），以 O µg/ m L 溶液调零，测量吸光度 ；以隶质量浓度（11.g/ mL） 或亲量 (µg） 为横坐标 ，吸光度为纵坐标 ，做工作曲线。
分别移取来标准洛液（5.8)0.00 m L 、1.00 m L 、2.00 m L、5.00 m L、10.00、20.00 m l 于一组 100 m L 容量瓶中 ，用载流液（ 8.2.1） 稀释至刻度混匀，即得来质量浓 度分别为 0.00 ,ug/ m L 、1.00 ×10-3 ,ug/ m L 、 2 .00 ×10-3 ,ug/ n1L 、5.00 ×10-3 ,ug/ m L 、10.00 ×10-3 ,ug/ m L 、20.00 ×10-3 ,ug/ m L 的标准系列溶液 。在 仪器调节至最佳工作条件（参见附录 A ） 下 ，在还原剂（ 8.2.
