微波消解-冷原子吸收光谱法测定电池中汞

Determination of Mercury in Battery by Microwave Digestion Cold Atomic Absorption Spectrometry

建立了微波消解 冷原子吸收光谱快速测定电池中汞的分析方法。采用密闭微波酸湿法消解电池样品 ,优化了微波消解条件和仪器测定条件。以HNO3 H2 SO4(φ =4∶1)混合酸作消解液、微波加热 3min ,以0 5mol·L-1H2 SO4为反应介质在室温下测定。方法的特征浓度为 0 2 5 μg·L-1。测定了 5种电池样品 ,回收率在 99 9%～ 113%之间 ,相对标准偏差为 4 9%～ 11 9%。与传统法相比 ,该法具有快速、省试剂、消解完全、汞丢失少等优点。

In this paper, a method of microwave digestion followed by cold atomic absorption spectrometry (CAAS) for the determination of mercury in battery was developed. Microwave digestion conditions and operational conditions of CAAS were optimized. The digestive solution was a mixture of hydrochloric acid-sulfuric acid (4:1, volume ratio) and the digestive time was 3 min at a microwave power of 1.0 MPa. The reaction medium was 0.5 mol (.) L-1 sulfuric acid at room temperature. The characteristic concentration was 0.25 mug(.) L-1. Five battery samples were determined, the recoveries were from 99.9% to 113%, and the relative standard deviations were from 4.85% to 11.9% (n = 6). The analytical results were satisfactory. The method is fast, simple, accurate and solvent-saving.