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样品以盐酸、过氧化氢进行溶解,以铁氰化钾作氧化剂,用氢化物发生-原子荧光光谱法测定金属镁中痕量铅。研究了氢化物发生的介质和酸度、硼氢化钾溶液的浓度、氢氧化钠的浓度、铁氰化钾的浓度对测定结果的影响,确定了最佳的测定条件。同时对仪器的操作参数进行了最佳选择。在最佳条件下,铅浓度在0~20μg/L范围内与荧光强度呈良好的线性关系,相关系数大于0.9995,方法的检出限为0.37μg/L。样品中铅的加标回收率在91%~102.7%之间,相对标准偏差为4.2%。
The samples were dissolved with hydrochloric acid and hydrogen peroxide. Potassium ferricyanide was used as oxidant to determine trace lead in metallic magnesium by hydride generation - atomic fluorescence spectrometry. The effects of medium and acidity, the concentration of potassium borohydride solution, the concentration of sodium hydroxide and the concentration of potassium ferricyanide on the determination results were studied, and the optimal determination conditions were determined. At the same time the instrument operating parameters of the best choice. Under the optimal conditions, the concentration of lead in the range of 0 ~ 20μg / L showed a good linear relationship with the fluorescence intensity, the correlation coefficient was greater than 0.9995, the detection limit of the method was 0.37μg / L. The spiked recoveries of lead in the samples ranged from 91% to 102.7% with relative standard deviations of 4.2%.