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目的建立钼、钨矿中汞含量的微波消解原子荧光光谱测定方法。方法向样品中加入6 ml硝酸、4 ml氢氟酸,2 ml盐酸,放置过夜,密闭后进行微波消解,冷却至室温,在样品测定液中加入200 g/L硫脲-抗坏血酸5 ml以掩蔽铁、砷、硒等杂质离子的干扰;以2%的硼氢化钾溶液作为还原剂,5%盐酸作为载流,采用氢化物-原子荧光法测定汞浓度。结果在1.0~10.0μg/L线性范围内,所得汞的回归方程为y=422.595 5x-98.649 0,r=0.999 4,呈良好的线性关系。方法的检出限为0.005 1μg/L,平均回收率为98.4%~100.1%,RSD为1.1%~3.2%。结论该方法具有快速、准确、灵敏度高、精密度好等特点,适用于钨矿及钼矿中汞的测定。
Objective To establish a method for determination of mercury in molybdenum and tungsten ore by microwave digestion and atomic fluorescence spectrometry. Methods Add 6 ml of nitric acid, 4 ml of hydrofluoric acid and 2 ml of hydrochloric acid to the sample. Place it in the oven overnight. After the solution is sealed, carry out microwave digestion and cool to room temperature. Add 5 ml of 200 g / L thiourea-ascorbic acid Iron, arsenic, selenium and other impurity ions; using 2% potassium borohydride solution as a reducing agent, 5% hydrochloric acid as a carrier, the determination of mercury concentration by atomic fluorescence spectrometry. Results In the linear range of 1.0 ~ 10.0μg / L, the regression equation of mercury was y = 422.595 5x-98.649 0, r = 0.999 4, showing a good linear relationship. The detection limit of this method was 0.005 μg / L with the average recovery of 98.4% -100.1% and RSD of 1.1% -3.2%. Conclusion The method is rapid, accurate, sensitive and accurate. It is suitable for the determination of mercury in tungsten ore and molybdenum ore.