高分辨等离子体质谱法直接测定高纯镓中的痕量元素

Direct Determination of Trace Elements in High Purity Gallium by High Resolution-Inductively Coupled Plasma-Mass Spectrometry

建立高分辨电感耦合等离子体质谱法（HR-ICP．MS）测定高纯镓样品中Be、Mg、Al、Si、Ti、V、Cr、Mn、Fe、Co、Ni、cu、zn、Ge、As、Mo、Ag、Cd、In、Sb、Ba、Ph、Bi等痕量元素的方法。样品用HNO，＋HCl经微波消解后，试液直接进样用HR-ICP-MS法同时测定上述元素，在高分辨质谱测量模式下避免了大量的质谱干扰。详细地研究了HCl和高纯镓所产生的基体效应，以Sc、Rh、Tl作为内标元素校正了基体效应．讨论和确定了实验的最佳测定条件。结果表明，23种痕量元素的检出限在0．001．0．21μg／L之间；回收率在89．8％～111．6％之间，相对标准偏差（RSD）小于3．3％。

An analytical method using high resolution inductively coupled plasma mass spectrometry （HR- ICP-MS） for rapid simultaneous determination of Be, Mg, Al, Si, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ge, As, Mo, Ag, Cd, In, Sb, Ba, Pb and Bi elements in high purity gallium was described. The sample was dissolved in HNO3 and HCI by microwave digestion then the above 22 elements in the solution was analyzed directly by HR-ICP-MS. Most of the spectral interferences could be avoided by measuring in the high resolution mode （HRM）. The matrix effects due to the presence of excess HC1 and Ga were evaluated. Correction for matrix effects was made using Sc, Rh and TI as internal standards. The optimum condition for the determination was tested and discussed. The result showed that the detection limit of the method was in the range of 0.001-0. 21 μg/L, the relative standard deviation （RSD） was less than 3.3% and the recovery of the samples was in the range of 89.8% - 111.6%.