高分辨电感耦合等离子体质谱法测定FCC催化剂中微量元素

DETERMINATION OF TRACE ELEMENTS IN FLUID CATALYTIC CRACKING CATALYST BY HR-ICP-MS

建立了高分辨电感耦合等离子体质谱(HR-ICP-MS)法测定流化催化裂化(FCC)催化剂样品中Na、Mg、Al、P、Ca、V、Fe、Ni、Cu、As、Sb、Pb 12种微量金属元素的方法。样品用HNO3+HCl经微波消解后,试液直接采用HR-ICP-MS法同时测定上述12种元素,在高分辨质谱测量模式下避免了大量的谱干扰。研究了样品消解液所产生的基体效应,以Sc、Y、In、Bi作为内标元素校正了基体效应,讨论和确定了实验的最佳测定条件。结果表明,12种微量元素的检出限为0.022-62μg/l,加标回收率为91.8%-109.2%,相对标准偏差(RSD)小于3.5%。

An analytical method using high resolution inductively coupled plasma mass spectrometry （HR-ICP-MS） for rapid simultaneous determination of Na, Mg, Al, P, Ca, V, Fe, Ni, Cu, As, Sb and Pb elements in fluid catalytic cracking （FCC） catalyst was described. The sample was dissolved in HNO3 and HCl by microwave digestion then the above 12 elements in the solution were analyzed directly by HR-ICP-MS. Most of the spectral interferences could be avoided by measuring in the high resolution mode （HRM）. The matrix effect due to the digested solution was evaluated. Correction for matrix effects was made by using Sc, Y, In and Bi as internal standards. The optimum conditions for the determination were tested and discussed. The result showed that the detection limit of the method was in the range of 0. 022-62 μg/l, the relative standard deviation （RSD） was less than 3.5% and the recovery of the sample was in the range of 91. 8%-109. 2%. This method can be used to determine the trace elements in FCC catalyst with the features of accuracy, rapid determination and convenience.