氢化物发生-原子荧光光谱法测定铁矿石中的痕量锌

Determination of Trace Zinc in Iron Ore by Hydride Generation-Atomic Fluorescence Spectrometry

研究氢化物发生-原子荧光光谱法测定铁矿石样品中的痕量锌,使用硝酸、盐酸、氢氟酸和高氯酸对铁矿石样品进行消解,以盐酸溶液为载流,硼氢化钾为还原剂,氯化钴溶液和1,10-菲啰啉为荧光增强剂,对锌的氢化物发生条件进行了试验,确定了锌最优氢化物发生条件;对仪器参数进行了条件试验,选择了最佳仪器工作条件。用铁矿石有证标准物质和加标回收试验对分析方法准确度进行了验证,有证标准物质结果均在误差允许范围内,加标回收率在90.1%~104%,结果准确可靠,满足规范要求;选取铁矿石有证标准物质,按照分析方法流程进行10次测定,方法精密度RSD为2.7%,方法精密度良好;按照分析方法流程制备11个空白溶液,按照仪器设定条件进行测定,方法检出限为0.10 mg/kg。

The determination of trace zinc in iron ore samples by hydride generation-atomic fluores-cence spectrometry was studied.Iron ore samples were digested by nitric acid,hydrochloric acid,hydrofluor-ic acid and perchloric acid.The zinc hydride generation conditions were tested by using hydrochloric acid so-lution as carrier current,potassium borohydride as reducing agent,cobalt chloride solution and 1,10-phen-anthroline as fluorescence enhancers.The optimal conditions of zinc hydride generation were determined.The instrument parameters were tested and the best working conditions of the instrument were selected.The accuracy of the analysis method was verified by the certified reference material of iron ore and the recovery test of standard addition.The results of certified reference materials were within the error allowable range,and the recovery rate of standard addition was 90.1%~104%.The results were accurate and reliable,which met the requirements of the specification.The certified reference material of iron ore was determined 10 times according to the analysis method process.The precision RSD of the method was 2.7%,and the preci-sion of the method was good.According to the analytical method,11 blank solutions were prepared and deter-mined according to the conditions set by the instrument.The detection limit of the method was 0.10 mg/kg.