Determination of Trace Cadmium and Tin in Lead Alloys by Inductively Coupled Plasma-Mass Spectrometry
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摘要: 铅合金中的镉和锡由于含量较低，国家标准方法均为单一元素分析，步骤繁琐，检出限高，难以达到理想的检出要求。本文建立了应用电感耦合等离子体质谱法（ICP-MS）测定铅合金中微量级（μg/g级）杂质元素镉和锡的分析方法。采用单一的低浓度硝酸溶解铅合金，用低温慢溶的方式使样品溶解更加完全，减少了多离子对仪器的干扰；通过铅基体匹配和加入酒石酸保证了标准与样品介质的一致性，同时避免了锡的水解；以103Rh作为内标元素，111Cd和118Sn作为测量同位素克服了质谱干扰。方法检出限为镉0.05 ng/g、锡0.04 ng/g，比国家标准方法的检出限（1～6 μg/g）低，精密度小于4%。该方法试剂用量少，减少了处理样品的复杂性，实现了合金中微量级元素的准确测定。
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关键词:
- 铅合金 /
- 镉 /
- 锡 /
- 酒石酸 /
- 电感耦合等离子体质谱法
Abstract: Due to the low concentrations of cadmium and tin in lead alloys and the single element analysis performed by using the national standard method, the analytical protocol is very complex and the detection limit is not ideal. In this paper, a new analytical method for determining trace cadmium and tin in lead alloys by Inductively Coupled Plasma-Mass Spectrometry is reported. In this method, lead alloys are digested by low-concentration of nitric acid. The low temperature and slow digestion process assures the complete dissolution of samples and reduces the mass spectrometry interferences from multiple ions. Lead matrix matching and the addition of tartrate assure the medium consistency of the standard and sample and avoid hydrolysis of the tin content. Using 103Rh as an internal standard and 111Cd and 118Sn as the measuring isotopes, the mass spectrometry interferences are reduced. The detection limits of Cd and Sn are 0.05 ng/g and 0.04 ng/g, respectively, which are much lower than those of the national standard method (1-6 μg/g). The precision of this method is 4.0%. This method needs a relatively small sample weight, which simplifies the analytical process and can determine trace elements in alloys precisely and accurately.-
Key words:
- lead alloy /
- cadmium /
- tin /
- tartaric acid /
- Inductively Coupled Plasma-Mass Spectrometry
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表 1 基体效应试验结果
Table 1. Analytical results of the matrix effect
加入的铅量(g) Cd Sn 标准值(μg/g) 实测值(μg/g) 标准值(μg/g) 实测值(μg/g) 0 10.0 5.48 21.0 11.28 0.2 10.0 9.93 21.0 21.03 0 20.0 10.82 62.0 34.81 0.2 20.0 19.64 62.0 61.75 
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表 2 镉和锡的精密度和准确度实验
Table 2. The accuracy and precision tests for Cd and Sn
样品编号 Cd的精密度 Cd的准确度 标准物质编号 Sn的精密度和准确度 Cd的GFAAS测定值(μg/g) Cd的本法测定值(μg/g) RSD(%) Cd加标量(μg/g) Cd测定总量(μg/g) 加标回收率(%) Sn的标准值(μg/g) Sn的本法测定值(μg/g) RSD(%) 相对误差(%) 样品1 1.12 1.1 3.5 2 3.11 100.5 BYG-03-8-1 2.5 2.48 1.9 0.8 样品2 2.19 2.2 2.4 2 4.13 96.5 BYG-03-8-2 3.5 3.42 3.8 2.3 样品3 5.03 5.03 2.2 2 7.02 99.5 BYG-03-8-3 9 9.02 1.9 0.2 样品4 9.85 9.78 1.4 2 11.83 102.5 BYG-03-8-4 21 21.09 2.2 0.4 样品5 20.71 20.69 0.7 2 22.65 98 BYG-03-8-5 62 61.85 1.4 0.2
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表 3 铅合金样品中镉锡等10种杂质元素的分析
Table 3. Analytical results of ten impurity elements including Cd and Sn in the lead alloys
铅合金样品编号 杂质元素含量(μg/g) 各杂质元素含量总和(μg/g) Ag Cu Bi As Sb Sn Cd Zn Fe Ni 样品1 1.00 3.00 7.00 2.00 4.00 2.00 1.00 3.00 2.00 1.00 26.00 样品2 3.00 6.00 15.00 5.00 6.00 4.00 2.00 5.00 10.00 2.00 58.00 样品3 7.00 15.00 29.00 10.00 10.00 9.00 5.00 11.00 20.00 5.00 121.0 样品4 16.00 30.00 51.00 24.00 29.00 21.00 10.00 20.00 30.00 10.00 241.0 样品5 42.00 60.00 106.0 61.00 66.00 62.00 20.00 51.00 40.00 25.00 533.0
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