微波消解-氢化物发生原子荧光光谱法同时测定化肥中砷、汞含量

Simultaneous Determination of As and Hg in Fertilizer by Microwave Digestion and Hydride Generation Atomic Fluorescence Spectroscopy

采用微波消解样品前处理手段以及双道原子荧光光度计,建立了微波消解-氢化物发生原子荧光光谱法同时测定化肥中砷、汞含量的方法。通过试验确定了样品前处理方法,对负高压、灯电流,载气、屏蔽气、原子化器高度、酸度等测试条件进行了优化。在优化的工作条件下,砷、汞含量分别在0～50 ng/mL和0～1.0 ng/mL范围内与荧光强度呈良好的线性关系,线性相关系数分别为0.9996,0.9996,检出限分别为0.085,0.008 ng/mL,回收率分别为88.8%～107.4%,90.0%～120%,测定结果的相对标准偏差均小于7%(n=6)。

A method was proposed for the simultaneous determination of As and Hg in fertilizer by microwave digestion and hydride generation atomic fluorescence spectroscopy. Sample pretreatement method, negative high pressure, burner current, carrier gas, shieding gas, atomizer height acidity and so on were optimized. On optimal conditions, As correlation coefficient was 0.9996 in the linear range of 0-50 ng/mL, while Hg correlation coefficient was 0.999 6 in the linear range of 0-1.0 ng / mL. The detection limits of As and Hg were 0.085,0.008 ng / mL, respectively, and recoveries were 88.8%-107.4%,90.0%-120%,respectively. The relative standard deviations of As and Hg detetion results were less than 7%（n=6）.