Simultaneous Determination of Trace As, Sb, Bi and Hg in Soils by Hydride Generation-Inductively Coupled Plasma-Atomic Emission Spectrometry
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摘要: 土壤样品用水浴加热王水溶解1 h，在10%的盐酸介质下，用0.5 L/min的载气流量，10 g/L的硼氢化钠-氢氧化钠作为还原剂，将自行设计的一种新型氢化物发生器与电感耦合等离子体发射光谱法(ICP-AES)联用测定痕量砷、锑、铋、汞，一次溶样即可实现多元素在同母液同条件下同时测定。方法检出限为0.01~0.06 ng/g，加标回收率为92.0%~102.0%，精密度(RSD)低于5%。此方法通过加入抗坏血酸-硫脲溶液预先将砷和锑还原，汞的测定不受还原剂的影响，同时解决了目前多元素分次测量带来的不便和试剂消耗多等问题，样品前处理及测量过程快速、简单，无记忆效应的影响，适合环境样品中痕量砷、锑、铋、汞的同时测定。Abstract: A method for the simultaneous determination of the trace contents of As, Sb, Bi and Hg in the same solution by Hydride Generation-Inductively Coupled Plasma-Atomic Emission Spectrometry (HG-ICP-AES) was established by using 10% hydrochloric acid as the dissolved medium. The soil sample was dissolved in water bath with aqua regia for one hour, and then ascorbic acid-thiourea solution was added to reduce As and Sb in advance without influence on the content of Hg. The elements were determined by a new type self-designed hydride generator coupled with ICP-AES with 10% hydrochloric acid, 0.5 L/min carrier gas and 10 g/L NaHB4-NaOH as reductants. This method solved the problems of the inconvenience of multi-element determination and more reagent consumption. The sample pre-treatment and determination were easy, rapid and had no memory effect. The detection limits of the method were 0.01-0.06 ng/g, the recoveries of standard materials were between 92.0% and 102.0%, and RSD was less than 5%. This method is suitable for the simultaneous determination of the trace contents of As, Sb, Bi and Hg in environmental samples.
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Key words:
- soil /
- As /
- Sb /
- Bi /
- Hg /
- hydride generation /
- Inductively Coupled Plasma-Atomic Emission Spectrometry
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表 1 还原剂对Hg测定的影响
Table 1. Effect of reductant on Hg determination
汞标准溶液的浓度
ρ(Hg)/(μg·L-1)Hg的测定强度/(Cts·S-1) 不加还原剂 加还原剂 4.0 1121 1127 10.0 2660 2680 20.0 5115 5097 100.0 26182 26208 
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表 2 NaHB4浓度的影响
Table 2. Effect of NaHB4 concentration
元素的测定强度/
(Cts·S-1)ρ(NaHB4)/(g·L-1) 5.0 10.0 15.0 Hg 5080 5425 4954 As 1353 1572 1282 Sb 2112 2326 1740 Bi 1397 1489 1172
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表 3 地质标准样品分析结果
Table 3. Analytical results of elements in National Standard Reference Materials
标准物质编号 分析元素 wB/(μg·g-1) 准确度RE/% RSD/%
(n=4)标准值 测定值 GBW 07402 As 13.70 13.43 98.0 1.53 Sb 1.30 1.25 96.2 1.04 Bi 0.38 0.36 94.7 2.33 Hg 0.015 0.014 94.0 4.28 GBW 07404 As 58.00 62.05 107.0 2.13 Sb 6.30 6.39 101.4 1.96 Bi 1.04 1.06 101.9 1.22 Hg 0.59 0.61 103.4 2.09 GBW 07408 As 12.70 12.30 96.8 3.40 Sb 1.00 0.99 99.0 0.82 Bi 0.30 0.28 93.3 3.38 Hg 0.017 0.015 88.2 3.28 GBW 07104 As 2.10 1.92 91.4 3.43 Sb 0.12 0.11 91.7 4.62 Bi 0.081 0.079 97.5 2.17 Hg 0.012 0.011 91.7 4.11 GBW 07111 As 0.40 0.37 92.5 4.64 Sb 1.34 1.31 97.8 0.98 Bi 0.05 0.05 100.0 2.66 Hg 0.035 0.032 91.4 3.97
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表 4 实际样品分析结果
Table 4. Analytical results of elements in real samples
实际样品 分析元素 wB/(μg·g-1) 回收率/% 测定值 加标量 测得总量 鲫鱼肉 As 0.108 0.100 0.202 94.0 Hg 0.069 0.100 0.171 102.0 鲫鱼肝 As 0.065 0.100 0.160 95.0 Hg 0.027 0.050 0.073 92.0
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