Determination of Selenium in Soil by Inductively Coupled Plasma-Mass Spectrometry with Aqua Regia Digestion in Water Bath
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摘要: 随着富硒产品关注度越来越高，对土壤中硒含量测定的研究也越来越受到人们的重视。应用传统电感耦合等离子体质谱法（ICP-MS）测定土壤样品中的硒时，受到的基体效应和多原子离子干扰比较显著，准确测定硒含量的难度较大。本文建立了采用50%王水-沸水浴消解体系，ICP-MS测定土壤样品中硒含量的方法，实验中采用动能歧视模式（KED）消除质谱干扰，选用103Rh元素作为在线加入内标以消除仪器信号漂移。用该方法对有证土壤标准物质进行分析，其结果均在不确定度范围内，测定值与认定值的相对误差介于-2.01%~2.99%之间，相对标准偏差（RSD）小于6.60%，检出限为0.012μg/g，测定下限为0.048μg/g。应用该方法与国家环境保护标准方法（HJ680—2013）对20个土壤实际样品进行比对分析，其结果基本一致。该方法适合于分析测定地质等行业大批量土壤样品中的硒。
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关键词:
- 水浴消解 /
- 土壤 /
- 硒 /
- 电感耦合等离子体质谱法 /
- 动能歧视模式
要点(1)将50%王水-沸水浴消解与ICP-MS法相结合测定土壤样品中的硒。
(2)样品前处理过程一步完成，提高了方法准确性和效率，适合大批量土壤样品中硒的分析。
(3) 应用动能歧视模式(KED)拓展了ICP-MS在地球化学分析领域的适用范围。
HIGHLIGHTS(1) The 50% aqua regia-boiling water bath digestion combined with ICP-MS method was used to determine selenium in soil samples.
(2) The sample pretreatment process was completed in one step to improve the accuracy and efficiency of the method and was suitable for the analysis of selenium in large numbers of soil samples.
(3) The application of kinetic energy discrimination mode (KED) expanded the application scope of ICP-MS in the field of geochemical analysis.
Abstract:OBJECTIVESWith more and more attention being paid to selenium-rich products, the study on the determination of selenium content in soil has become more significant. The accurate determination is difficult due to the serious interference of the matrix effect and polyatomic ion when determining selenium in soil samples by inductively coupled plasma-mass spectrometry (ICP-MS).OBJECTIVES To establish a method for accurate determination of Se in soil.METHODSThe content of selenium in soil samples was determined by ICP-MS with 50% aqua regia-boiling water digestion. Kinetic energy discrimination mode (KED) was adopted to eliminate mass spectrum interference, and the 103Rh element was selected as the internal standard for on-line addition to eliminate instrument signal drift.RESULTSThe results of the analysis of certified soil standard materials were consistent with those of certified standard materials within the uncertainty. The results showed that the relative errors (REs) of this method were between -2.01% and 2.99%, the relative standard deviation (RSD) was less than 6.60%, the detection limit was 0.012μg/g, and the minimum quantitative detection limit was 0.048μg/g. The method was applied to analyze 20 soil samples, and the results were consistent with those obtained by national environmental protection standard HJ680-2013.ConclusionThe study results are suitable for the determination of selenium in large numbers of soil samples from the geological industry. -
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图 1 碰撞气流速对78Se信号强度的影响
Figure 1. Effect of gas flow velocity on signal intensity of 78Se
表 1 不同消解时间下硒含量测定结果
Table 1 Analytical results of Se in different digestion time
土壤标准
物质编号Se认定值
(μg/g)不同消解时间Se测定值(μg/g) 0.5h 1.0h 1.5h 2.0h 2.5h 3.0h GBW07303 1.0±0.2 0.74 0.86 0.92 0.96 0.95 0.98 GBW07405 1.6±0.2 0.88 1.49 1.58 1.61 1.63 1.59 
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表 2 土壤标准物质中硒的测定结果
Table 2 Analytical results of Se in soil standard materials
土壤标准
物质编号Se认定值
(μg/g)12次Se测定值
(μg/g)测定平均值
(μg/g)相对误差
(%)RSD
(%)1.02 0.94 0.91 1.01 GBW07303 1.0±0.2 1.03 1.01 0.96 0.95 0.98 -1.67 3.76 1.00 1.01 0.97 0.99 0.26 0.32 0.28 0.28 GBW07304 0.29±0.08 0.26 0.29 0.27 0.28 0.28 -2.01 6.09 0.30 0.28 0.29 0.30 0.16 0.18 0.15 0.15 GBW07309 0.16±0.03 0.17 0.18 0.16 0.17 0.16 2.08 6.57 0.17 0.16 0.15 0.16 0.095 0.094 0.088 0.086 GBW07403 0.09±0.02 0.082 0.10 0.096 0.093 0.093 2.96 5.64 0.091 0.093 0.099 0.095 0.64 0.71 0.66 0.61 GBW07404 0.64±0.14 0.68 0.68 0.69 0.66 0.66 2.99 4.41 0.62 0.65 0.64 0.67 1.63 1.61 1.55 1.66 GBW07405 1.6±0.2 1.71 1.57 1.62 1.61 1.63 1.72 2.86 1.64 1.69 1.65 1.59
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表 3 实际样品中硒的检测结果与方法比对结果
Table 3 Analytical results of Se in real samples and comparison of different methods
样品编号 Se测定值(μg/g) 本方法 HJ 680—2013方法 SY-1 0.34 0.36 SY-2 0.13 0.12 SY-3 0.63 0.61 SY-4 0.48 0.49 SY-5 1.03 1.05 SY-6 0.41 0.39 SY-7 0.25 0.26 SY-8 0.17 0.16 SY-9 0.52 0.49 SY-10 0.51 0.51 SY-11 0.84 0.88 SY-12 0.69 0.72 SY-13 0.23 0.21 SY-14 0.14 0.14 SY-15 1.83 1.85 SY-16 0.74 0.71 SY-17 0.096 0.10 SY-18 1.85 1.83 SY-19 0.32 0.30 SY-20 0.21 0.20
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