微波消解-ICP-MS法测定硫磺中18种微量元素

建立了用微波消解-电感耦合等离子体质谱法(ICP-MS)同时测定硫磺中18种微量元素(锂、镁、铝、钙、钒、铬、锰、铁、钴、镍、铜、锌、镉、砷、硒、钡、铅和汞)的定量分析方法。通过对消解所用试剂及条件进行研究,确定最佳的样品处理条件；为了获得最佳的信噪比并降低光谱干扰,研究采用单变量方法,对ICP-MS的射频功率和雾化气体流量等因素进行了性能优化。结果显示：该方法各元素的校准曲线线性相关系数在0.999以上,所有元素的检出限(LODs) 在0.001-0.962 mg/Kg之间,测定下限范围在0.004-3.85 mg/Kg之间,回收率在82.9 %~115 %之间,相对标准偏差均小于3 %。

Determination of 18 Trace Elements in Sulfur by Microwave Digestion Coupled with Inductively Coupled Plasma Mass Spectrometry (ICP-MS)JIANG Jinhua 1, 4, ,XU Xinzhong 2, WANG Linlin 3, LV Xinming 2,*

A microwave digestion/inductively coupled plasma mass spectrometry (ICP-MS) method for simultaneous determination of 18 trace elements (lithium, magnesium, aluminum, calcium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, cadmium, arsenic, selenium, barium, lead and mercury) in sulfur has been developed. The optimal conditions of sample treatment were determined by studying the reagent and conditions used for digestion.In order to obtain the best signal-to-base ratio and remove spectral interference, a univariate method was used to optimize the performance of ICP-MS, such as RF power and atomizing gas flow rate.The results showed that the linear correlation coefficients of the calibration curves were all above 0.999, the limits of detection (LODs) of all elements ranged from 0.001 to 0.962mg/Kg, the limits of determination ranged from 0.004 to 3.85mg/Kg, the recoveries ranged from 82.9% to 115%, and the relative standard deviations were all less than 3%.