Citation: FU Liang, SHI Shu-Yun, CHEN Xiao-Qing. Accurate Determination of Trace Toxic Elements in Activated Clay Using Inductively Coupled Plasma Tandem Mass Spectrometry. Chinese Journal of Analytical Chemistry, 2018, 46(8): 1253-1260. doi: 10.11895/j.issn.0253-3820.181258 [复制]
Accurate Determination of Trace Toxic Elements in Activated Clay Using Inductively Coupled Plasma Tandem Mass Spectrometry
建立了不同样品消解方式下，检测活性白土中痕量毒理性元素的电感耦合等离子体串联质谱（ICP-MS/MS）分析方法。分别采用微波和密闭压力对活性白土样品进行消解，利用ICP-MS/MS法测定其中Cr、Ni、As、Cd、Sn、Sb、Hg和Pb共8种毒理性元素。在MS/MS模式下，分别以O2和NH3/He为反应气消除了测定过程中的质谱干扰。各元素具有良好的线性关系（R2 ≥ 0.9999），检出限为0.35~5.20 ng/g。应用与活性白土基质组成相似的国家标准参考物质水系沉积物（GBW07306）验证了分析方法的准确性和精密度，结果显示，采用微波消解和密闭压力消解对样品进行前处理的测定值与标准参考物质的证实值基本一致，相对标准偏差（RSD）≤ 5.2%，验证了分析结果准确可靠、精密度高。本方法具有分析速度快、检出限低且无干扰的优点，适用于活性白土中痕量毒理性元素的高通量分析。
An analytical method was established for accurate determination of trace toxic elements in activated clay by inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) with different digestion processes. The activated clay was digested by microwave and closed pressurized acid, respectively. Eight kinds of toxic elements including Cr, Ni, As, Cd, Sn, Sb, Hg and Pb were measured by ICP-MS/MS. In the MS/MS mode, O2 and NH3/He were employed as reaction gases to eliminate the interference during the determination process. The analysis results shown good linearity (R2 ≥ 0.9999), and the limit of detection was 0.35-5.20 ng/g. The accuracy and precision of the analytical method were evaluated by the national standard material stream sediment (GBW07306) that is similar to the matrix composition of activated clay. The results shown that the measured values of microwave digestion and closed pressurized acid digestion were in good agreement with the certified values of the standard reference materials with the relative standard deviation (RSD) less than or equal to 5.2%, which proves that the analysis results are accurate, reliable and high precision. The method is considered to be suitable for high-throughput analysis of trace toxic elements in activated clay by advantages of fast analysis, low limit of detection and interference-free.