湿法消化法测定蜂花粉中铅的研究

Determination of lead in bee pollen by wet digestion method

本文建立了湿法消化-原子吸收光谱法测定蜂花粉中铅的方法。实验优化表明,最佳消化程序为:70℃0.5 h→140℃1 h→180℃6~10 h(至溶液变浅黄);石墨炉最佳温升:干燥温度120℃,灰化温度500℃,原子化温度1900℃,清残余温度2200℃;最佳称样量0.25 g^0.30 g。该方法条件下,线性范围在5~80 ng/ml之间,线性方程为y=0.0024x-0.0009,R^2=0.9988,线性关系良好。方法回收率在95.2~100.1%之间,n=3。精密度RSD为3.05%,n=6。结合实际检测结果,为GB 2762蜂花粉中铅的指标限量提出了合理指标建议。

A wet digestion atomic absorption spectrometry method was established for the determination of lead in bee pollen. The results showed that the optimal extracting technological conditions were as follows： the best digestion procedures used for 70℃--0.5 h, 140℃-1 h, 180℃-6-10 h （until solution became pale yellow）. The optimal temperature rise of graphite furnace was that dried at 120℃, ashed at 500℃, atomized at 1900℃, and clear residual temperature was 2200℃. The best sample weight was 0.25 to 0.30 g. Under the condition of the method, the linear range was range from 5 ng/ml to 80 ng/ml, the linear equation was y=0.0024x-0.0009, R2=0.9988, showed a good linear correlation. The recovery of the method was 95.2-100.1%, n=3. The precision of the results showed that RSD was 3.05%, n=6. Based on the actual test results, the reasonable index of the lead in the GB 2762 bee pollen was put forward.