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目的:建立测定水中镉的新反应体系的氢化物发生原子荧光法。方法:在酸性介质中,以铁氰化钾为氧化剂,草酸为掩蔽剂,氯化钴、硫脲提高挥发性镉物质的发生效率,2%盐酸溶液为载流,先将样品中Cd+、Cd2+氧化为Cd3+,Cd3+与硼氢化钾反应生成挥发性镉的氢化物CdH3,将氢化物导入原子化器,检测其荧光强度值。结果:方法的标准曲线最佳线性范围:0~10μg/L,相关系数为0.9999,方法检出限0.017μg/L,最低检出浓度为0.051μg/L,相对标准偏差1.4%~4.0%,回收率为95.7%~104.0%。对2个标准参考物质的分析结果令人满意。结论:用该法测定水中镉,操作简便、线性关系好、检出限低、重复性好、回收率高,能准确测定水中镉。
Objective: To establish a new hydride generation atomic fluorescence spectrometry method for the determination of cadmium in water. Methods: In an acidic medium, potassium ferricyanide as oxidant and oxalic acid as masking agent, cobalt chloride and thiourea were used to enhance the efficiency of volatile cadmium. The 2% hydrochloric acid solution was used as carrier. The contents of Cd +, Cd2 + Oxidation of Cd3 +, Cd3 + and potassium borohydride reaction of volatile cadmium hydride CdH3, the hydride into the atomizer to detect the fluorescence intensity value. Results: The optimal linear range of the standard curve was 0-10μg / L, the correlation coefficient was 0.9999, the detection limit was 0.017μg / L, the minimum detectable concentration was 0.051μg / L, the relative standard deviation was 1.4% -4.0% The recoveries ranged from 95.7% to 104.0%. The results of two standard reference materials were satisfactory. Conclusion: The method for the determination of cadmium in water has the advantages of simple operation, good linear relationship, low detection limit, good repeatability, high recovery and accurate determination of cadmium in water.