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建立了氢化物发生-原子荧光光谱法(HG-AFS)测定经HNO3-HClO4-H2O2湿法消解的大米与圆白菜等样品中痕量铅的方法,系统地优化了灯电流等仪器参数条件,探讨了载流、还原剂、样品酸度、氧化剂的最佳浓度,考察了掩蔽剂去干扰的情况。实验表明:在选定载流浓度HCl 2%(V/V)、还原剂KBH4浓度2%(m/V)[KOH恒为0.5%(m/V)]、样品酸度HCl 1%(V/V)、氧化剂K3Fe(CN)60.4%(m/V)、掩蔽剂H2C2O40.2%(m/V)及优化设置灯电流等参数的最佳实验条件下,测定铅的检出限为0.07μg/L,在0.00—50.00μg/L范围呈良好的线性关系,样品测定变异系数小于等于6.22%。该方法简便、干扰少、灵敏度高,应用于大米、圆白菜等样品中Pb的测定,结果与参考值相符,是一种切实可行的方法。
A method for the determination of trace lead in rice and cabbage and other samples digested with HNO3-HClO4-H2O2 by hydride generation-atomic fluorescence spectrometry (HG-AFS) was established. Parameters such as lamp current were systematically optimized The carrier, reductant, sample acidity, the best concentration of oxidant, inspected masking agent to interfere with the situation. The experimental results show that when the concentration of HCl in the sample is 2% (V / V), the concentration of KBH4 is 2% (m / V) [KOH is 0.5% The detection limit of lead was 0.07μg under the optimum conditions of 60% (m / V) of K3Fe (CN), 40.2% (m / / L, in the range of 0.00-50.00μg / L showed a good linear relationship, the coefficient of variation of the sample was less than or equal to 6.22%. The method is simple, less interference, high sensitivity, and is applied to the determination of Pb in rice and cabbage samples. The result is in line with the reference value, which is a feasible method.