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目的:研制顺序注射式原子荧光测汞仪和进行批量样品预处理的微型恒温消解仪,及食品中微量汞的测定方法。方法:测汞仪将程控注射泵、程控多通道顺序注射阀与串联的容积相差十倍的汞蒸气翻泡瓶联接,在微机控制下,完成汞蒸气发生、浓缩、二次快速爆气,采用精密控制步进电机驱动12通道选择阀,联接测汞仪的光池与样品溶液、还原剂、汞吸收液,实现自动化操作,提高分析速度。结果:测量汞的线性范围0.0006861μg/L~10μg/L,线性误差6.63%,检测限0.000681μg/L。鲤鱼中汞的标准差4.01800、回收率97.8%,乳粉中汞的标准差0.18688、回收率96.5%。结论:建立了顺序注射汞测定方法,提高了分析速度、灵敏度和准确度。
OBJECTIVE: To develop a method for the determination of trace mercury in food by the sequential injection atomic fluorescence mercury analyzer and the batch thermostat digestion instrument. Methods: The mercury-measuring instrument was connected to a programmable syringe pump and a programmed multi-channel sequential injection valve with a mercury vapor turn-over bottle with a difference of ten times the capacity in series. Under the control of a microcomputer, mercury vapor generation, concentration and rapid second- Precise control of the stepper motor drives the 12-way selector valve, which couples the cell and sample solutions, reducing agents, and mercury absorbers of the mercury analyzer to automate operations and increase analysis speed. Results: The linear range of mercury was 0.0006861μg / L ~ 10μg / L, the linearity error was 6.63% and the limit of detection was 0.000681μg / L. The standard deviation of mercury in carp was 4.01800, the recovery rate was 97.8%, the standard deviation of mercury in milk powder was 0.18688, and the recovery rate was 96.5%. Conclusion: A sequential injection method for mercury determination was established to improve the analysis speed, sensitivity and accuracy.