原子荧光光谱法快速测定锑矿石中的汞、铋、硒

用王水直接水浴分解样品,硝酸、高氯酸湿法消解,酒石酸掩蔽锑,应用氢化物发生-原子荧光光谱法(HG-AFS)不经分离直接测定锑矿石中微量杂质元素汞、铋、硒的含量。汞、铋、硒的标准系列浓度分别在0.000 0~0.006 0、0.000~0.060、0.000~0.010 mg/L范围内与荧光强度具有良好的线性关系,线性相关系数分别为1.000 0、0.999 9、0.999 8,其加标回收率分别为95%~102%、99%~102%、99%~105%。相对标准偏差分别为0.82%~1.1%、1.1%~6.4%、1.6%~2.1%(n=8)。该方法对汞、铋、硒的检出限分别为2.0×10-11、4.1×10-11、4.0×10-10g/mL。

RAPID DETERMINATION OF MERCURY, BISMUTH, SELENIUM IN ANTIMONY ORE BY ATOMIC FLUORESCENCE SPECTROMETRY

A method for determination of the trace impurity elements such as mercury, bismuth, selenium in antimony ore by hydride generation -atomic fluorescence spectrometry（ HG- AFS） without separation was studied. The samples were decomposed with aqua regia in water bath, digested with nitric acid and perchloric acid, and bismuth in which was masked with tartrate. Mercury, bismuth, selenium concentrations of the standard series in the range of 0.000 0 - 0. 006 0, 0.000 - 0.060, 0. 000 - 0. 010 mg/L had a good linear relationship with the fluorescence intensity, and the correlation coefficient （r） were 1. 0000, 0. 999 9, 0.999 8, respective- ly. Mercury, bismuth, selenium recoveries of standard addition were 95% -102% , 99% -102% , 99% -105% , respectively. The relative standard deviations of Mercury, bismuth, selenium were 0.82% - 1.1% , 1.1% -6.4%, 1.6% -2.1% （n =8） ,repectively and the detection limits were 2.0×10^-11、4.1×10^-11、4.0×10ug/mL, respectively.