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程秀花, 黎卫亮, 郑民奇, 王海蓉. 自制氢化物发生装置与电感耦合等离子体质谱仪联用测定地质样品中的稀散元素锗和碲[J]. 岩矿测试, 2016, 35(3): 265-270. DOI: 10.15898/j.cnki.11-2131/td.2016.03.008
引用本文: 程秀花, 黎卫亮, 郑民奇, 王海蓉. 自制氢化物发生装置与电感耦合等离子体质谱仪联用测定地质样品中的稀散元素锗和碲[J]. 岩矿测试, 2016, 35(3): 265-270. DOI: 10.15898/j.cnki.11-2131/td.2016.03.008
CHENG Xiu-hua, LI Wei-liang, ZHENG Min-qi, WANG Hai-rong. Determination of Germanium and Tellurium in Geological Samples by A Self-developed Hydride Generation Device Paired with Inductively Coupled Plasma-Mass Spectrometer[J]. Rock and Mineral Analysis, 2016, 35(3): 265-270. DOI: 10.15898/j.cnki.11-2131/td.2016.03.008
Citation: CHENG Xiu-hua, LI Wei-liang, ZHENG Min-qi, WANG Hai-rong. Determination of Germanium and Tellurium in Geological Samples by A Self-developed Hydride Generation Device Paired with Inductively Coupled Plasma-Mass Spectrometer[J]. Rock and Mineral Analysis, 2016, 35(3): 265-270. DOI: 10.15898/j.cnki.11-2131/td.2016.03.008

自制氢化物发生装置与电感耦合等离子体质谱仪联用测定地质样品中的稀散元素锗和碲

Determination of Germanium and Tellurium in Geological Samples by A Self-developed Hydride Generation Device Paired with Inductively Coupled Plasma-Mass Spectrometer

  • 摘要: 氢化物发生与ICP-MS联用(HG-ICP-MS)可降低基体效应和多原子离子干扰,本文自制了一种与ICP-MS联用的氢化物发生装置,该装置采用三通将酸、碱和试样引入多接头的混合反应器中,再经自行设计的气液分离器随载气进入等离子体中,据此建立了HG-ICP-MS测定地质样品中稀散元素锗和碲的分析方法。实验中以20%盐酸+2%硼氢化钾(0.1%氢氧化钾介质)作为最佳氢化物发生反应体系,0.95 L/min为最佳载气流量,获得分析信号的灵敏度和稳定性较高,连续测定20次Ge和Te信号强度的相对标准偏差分别为8.3%和2.1%,残余在ICP-MS中的Ge和Te信号强度在200 s内基本清洗完毕。Ge和Te检出限分别为0.007 μg/g和0.006 μg/g,其中Te检出限比采用敞口四酸溶样ICP-MS直接测定的检出限(0.1 μg/g)更低,应用于分析实际样品可给出准确结果。

     

    Abstract: Hydride generation paired with Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) can reduce the matrix effect and interference of polyatomic ions. In this study, one self-made hydride generation device coupled with ICP-MS was developed for the determination of scattered elements, Ge and Te, in geological samples. A Y-shaped connection pipe is used to introduce acid, alkali and the sample into a multiple-joint reactor. After the reaction is complete, the mixture of liquid and gas is separated by self-designed gas-liquid separator. Finally, the gaseous hydrides along with the carrier gas enter the plasma. In this experiment, 20% HCl and 2% KBH4 (0.1% KOH medium) were used as the hydride generation reaction system and the carrier gas flow rate was set to 0.95 L/min to keep high sensitivity and stability. The relative standard deviations of Ge and Te signal intensity for 20 times continuous determination are 8.3% and 2.1%, respectively. The residual Ge and Te in ICP-MS can be cleaned up within 200 s. The detection limits of this method are 0.007 μg/g and 0.006 μg/g for Ge and Te, respectively. Moreover, the detection limit of Te for this method is lower than that of Te (0.1 μg/g) determined by ICP-MS directly after four-acid digestion. Therefore, this method can be used to gain accurate results for Ge and Te contents in geological samples.

     

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