微波密闭消解-ICP-MS－标准加入法测定矿石中金和银

建立了微波密闭消解-电感耦合等离子体质谱法(ICP-MS)采用标准加入法测定矿石中痕量元素金和银。考察了微波试样消解、基体效应、质谱干扰，并进行了ICP离子源以及质谱仪检测条件和微波消解参数的最优化。以标准加入法消除复杂多变的矿石基体对分析信号的影响，干扰校正方程消除多原子离子等质谱重叠影响。本法测定矿石中金银结果表明:回收率为197Au 106%～113%、107Ag 95%～105%、 109Ag 93%～103%，相对标准偏差RSD <6%（n=8），检测限197Au为10 ng/g、107Ag为3 ng/g、109Ag为6 ng/g。方法适用性强，可满足不同类型矿石中超痕量金银的测定,分析步骤少，操作简便，快捷准确

Closed Microwave Digestion- Inductively Coupled Plasma Mass Spectrometry with Standard Addition for the Determination of Gold and Silver in the Ores

A new method for simultaneous and directional determination of trace Ag and Au in the ore by inductively coupled plasma mass spectrometry (ICP-MS) with microwave digestion has been established. The operating condition of microwave sample digestion preparation, the affection of matrix and the influences of Mass have been investigated, and the operating parameter of the ICP ionization source and mass spectrometry and the microwave furnace for digestion were optimized. The standard addition method to eliminate the complex ore matrix effects on analysis of signal , and then adopt interference correction equations to eliminate polyatomic ion mass overlapping effects on the determination of gold and silver. Applied to the determination of gold and silver in the ore results show that: recovery of 197Au 106% ~ 113%, 107Ag 95% ~ 105%, 109Ag 93% ~ 103%, relative standard deviation RSD <6% (n = 8), detection limit 197Au of 10 ng / g, 107Ag to 3 ng / g, 109Ag to 6 ng / g. Method applicability, meet the needs of determination of ultra-trace gold and silver in the different types of ores , analysis the step small, simple, fast and accurate.