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目的建立饮用水中砷、锑的氢化物发生—原子荧光测定方法。方法在盐酸介质中,以硼氢化钠为还原剂,使砷、锑离子生成原子态砷、锑蒸气,由氩气带入原子荧光光谱仪中进行检测。同时还研究了仪器条件、酸度、介质、硼氢化钠浓度等分析条件对测定砷、锑的影响。结果在优化的条件下,砷、锑在0～100μg/L浓度范围内线性关系良好(r>0.9995),检出限为:砷0.0587μg/L、锑0.0529μg/L。分别取2.0、4.0、6.0μg/L3种浓度标准溶液连续测定11次,测定的荧光值统计相对标准偏差,分别为:砷4.4%、1.8%、0.8%,锑4.1%,2.8%,0.9%;加标值为0.8、1.0、2.0μg/L3个等级,回收率为95.0%～105.5%。结论该方法简便,快速,检出限低,重现性好,结果准确可靠,适用于饮用水中砷、锑的同时测定。
Objective To establish a hydride generation - atomic fluorescence spectrometry method for determination of arsenic and antimony in drinking water. Methods Arsenic and antimony ions were generated from arsenic and antimony ions in a hydrochloric acid medium by using sodium borohydride as a reducing agent to generate atomic-state arsenic and antimony vapor, and the argon atoms were taken into an atomic fluorescence spectrometer for detection. At the same time also studied the instrument conditions, acidity, medium, sodium borohydride concentration and other analytical conditions for the determination of arsenic, antimony. Results Under the optimal conditions, arsenic and antimony had a good linear relationship (r> 0.9995) in the range of 0-100 μg / L with the detection limits of 0.0587 μg / L for arsenic and 0.0529 μg / L for antimony. The standard deviations of 2.0, 4.0 and 6.0 μg / L were determined continuously for 11 times. The relative standard deviations of the measured fluorescence were 4.4%, 1.8%, 0.8%, 4.1%, 2.8%, 0.9% The spiked values were 0.8, 1.0 and 2.0 μg / L, and the recoveries ranged from 95.0% to 105.5%. Conclusion The method is simple, rapid, low detection limit, reproducible, accurate and reliable. It is suitable for simultaneous determination of arsenic and antimony in drinking water.