微波消解-原子荧光光谱法测定乳与乳制品中的砷

Microwave digestion-atomic fluorescence spectrometry of arsenic content in milk and dairy products

建立用氢化物原子荧光法测定乳与乳制品中的砷,研究前处理方法和原子荧光仪器对实验结果的影响,最后确定消解试剂为3∶2的硝酸和双氧水,微波消解最高温度为180℃,消解时间为25 min,且无需赶酸直接定容上级检测;原子荧光的还原剂为15 g/L的硼氢化钾,载流液为5%的盐酸。用以上最优化条件对乳与乳制品进行测定,得到砷的检出限为0.029μg/L,相对标准偏差为1.2%,回收率范围为93%～108%。

Established using hydride generation atomic fluorescence spectrometry determination of arsenic in milk and dairy products,to study the pre-treatment methods and atomic fluorescence instruments for the impact of experimental results studied pre-treatment methods and experimental results of atomic fluorescence instruments for the impact of the finalization of the digestion reagent 3∶2 nitric acid and hydrogen peroxide microwave digestion maximum temperature of 180 ℃,digestion time of 25 min;atomic fluorescence of the reducing agent for the 15 g/L of potassium borohydride,carrier liquid for 5% hydrochloric acid.Using the above optimum conditions,the reaction essence was measured to be the detection limit of mercury 0.029 μg/L,the relative standard deviation of 1.2% and the recovery ranges from 93%～108%.