微波消解-电感耦合等离子体质谱法测定煤矸石中镉铬铅

以氢氟酸,硝酸和过氧化氢作为消解试剂,采用逐步升温消解程序,建立了微波消解-电感耦合等离子体质谱法测定煤矸石中镉、铬、铅的方法。选择10 μg/L的Rh溶液作为内标溶液,以²⁰⁸Pb 、⁵²Cr和¹¹⁴Cd分别作为铅、铬、镉的测定同位素,在选定的仪器工作参数下,应用建立的方法对不同地区的煤矸石样品进行测定,测定值与石墨炉原子吸收光谱法(GF-AAS)和电感耦合等离子体原子发射光谱法(ICP-AES)的测定值一致,相对标准偏差(RSD,n=5)均小于7%。方法检出限分别为:0.013 μg/g(镉)、2.00 μg/g(铬)、0.20 μg/g(铅)。

Determination of cadmium,chromium, lead in coal gangue by microwave digestion-inductively coupled plasma mass spectrometry

The hydrofluoric acid, nitric acid and hydrogen peroxide were used as digestion reagent. The gradual temperature rising procedure was adopted. Then, a method for the determination of cadmium, chromium and lead in coal gangue by microwave digestion-inductively coupled plasma mass spectrometry was established. 10 μg/L Rh solution was used as internal standard. ²⁰⁸Pb, ⁵²Cr and ¹¹⁴Cd was used as the determination isotope of lead, chromium and cadmium, respectively. Under the selected instrumental working conditions, the proposed method was applied to the determination of coal gangue samples from different areas. The determination results were consistent with those obtained by graphite furnace atomic absorption spectrometry (GF-AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES). The relative standard deviation (RSD, n=5) was less than 7 %. The detection limit of method was 0.013 μg/g, 2.00 μg/g and 0.20 μg/g for cadmium, chromium and lead, respectively.