微波消解ICP-MS法同时测定大气颗粒物中多种痕量元素

Simultaneous Determination of Trace Elements in Atmospheric Particulates by ICP-MS with Microwave Digestion

采用微波消解电感耦合等离子体质谱法同时测定大气颗粒物中13种元素,选择硝酸体系消解20 min,硝酸加入体积为8 mL。Cu、Ni、Cr、Pb、Al、Mg、Mn、Ca在0μg/L～100μg/L,Ag、Ba、Co、Cd、Sn在0μg/L～5.00μg/L范围内线性良好,除Al、Mg、Ca检出限较高外,其他10种元素的检出限为0.07 ng/m3～1.82 ng/m3(按采样体积0.688 m3、定容体积50 mL计),滤膜样品平行测定3次的RSD≤1.2%,加标回收率在92%～108%之间。

13 kinds of elements concentrations in atmospheric particulates were determined by inductively coupled plasma mass spectrometry with microwave digestion. Nitric acid digestion system was taken to digest sample 20 minutes, and 8 mL nitric acid was added. The calibration curves showed a good linearity from 0 μg/L to 100μg/L for Cu, Ni, Cr, Pb, Al, Mg, Mn and Ca, and from 0 μg/L to 5.00 μg/L for Ag, Ba, Co, Cd and Sn. The detection limits of the elements ranged from 0.07 ng/m3 to 1.82 ng/m3 except A1, Mg, and Ca had higher detection limits （ air sampling volume 0. 688 m3 , formulated into a volume 50 mL）. Membrane samples were analyzed by duplicated tests three times, giving value of RSD ≤ 1.2%. Spiked recoveries ranged from 92% to 108%.