ICP-AES测定湖泊沉积物中微量元素的样品微波消解研究

Study on Microwave Digestion of Sediment of Poyang Lake Determined by ICP-AES

为正确测定鄱阳湖沉积物中微量元素而研究样品消解方法,采用密闭式微波消解系统处理样品,以ICP-AES法测定多种微量元素。分别从不同的消解液、用酸量、消解工序以及样品消解量等方面进行研究和优化,最终确定了一个最适合消解鄱阳湖沉积物的前处理消解体系为:消解样用量为0.5 g,180℃电热板上预处理约15 min,消解体系选择酸比例为4∶4∶2的HNO3-HF-H2O2体系和HNO3-HF-HClO4体系均可,消解工序为5 atm/3 min—10 atm/2 min—15 atm/5 min—20 atm/10 min的逐步加热工序。这种消解方法简单快速、效率高、劳动强度低,为以后鄱阳湖沉积物的测定做了样品准备工作。

in order to determine the sediment of Poyang Lake correctly, digestion methods for the samples were studied in the present paper. Microwave digestion was used to digest the samples, and ICP-AES was used to determine the samples. Different digestion solutions, the amount of acids, digestion procedure and the amount of sample were investigated and optimized. Finally, an optimal digestion method was established to carry out the further analysis of all sediment samples： weigh up 0. 5 g sample, take a pretreatment by heating on the electric plate for about 15 min at 180℃, and add HNO3-HF-HClO4 or HNO3-HF-H2O2 in the proportions of 4 t 4, 2. The microwave digestion procedure was 5 arm/3 min-10 arm/2 min-15 atm/5 min-20 atm/10 min. This method was simple, fast, effective with low work intensity.