论文部分内容阅读
用自行改造的一种简单的连续氢化物发生系统,实现了与电感耦合等离子体质谱仪的联用。研究了该系统的分析性能,并以乙醇为信号增强剂建立了在折衷条件下同时测定As、Sb、Bi、Se和Te的分析方法以及在预还原剂体系中同时测定As、Sb、Bi和在高HCl体系中单独测定Se的方法。方法的主要特点是:①将乙醇作为信号增强剂首次用于氢化物发生ICP-MS系统,使As、Sb、Se和Te的灵敏度比溶液雾化法提高4~17倍。②氢化物发生系统简单实用,由于采用了带有多级撞击分离器的雾化室作为气液分离器,有效地分离了氢化物发生过程中的气液相,消除了ICP-MS中的Cl-对As、Se的多原子离子干扰问题。③将内标法用于氢化物ICP-MS,采用氢化物元素Ge为内标,显著地改善了分析精密度和准确度。在多元素同时分析的折衷条件下,As、Sb、Bi、Se和Te的仪器检出限(3σ,ng/L)分别为0.64,0.06,0.55,0.85,0.63;方法检出限(3σ,ng/L)分别为71,10,9,6,8。考察了该氢化物发生系统中的一些过渡元素的干扰情况,分析元素的价态影响以及碘化钾、硫脲和抗坏血酸的抗干扰效果。方法经水系沉积物标准物质以及生物和植?
A simple, continuous hydride generation system that has been modified by itself has been used in conjunction with an inductively coupled plasma mass spectrometer. The analytical performance of the system was studied. The analytical method of simultaneous determination of As, Sb, Bi, Se and Te under the compromise condition was established with ethanol as signal enhancer and the simultaneous determination of As, Sb, Bi and Method to measure Se separately in high-HCl system. The main features of the method are as follows: (1) For the first time, ethanol was used as a signal enhancer in the hydride generation ICP-MS system, and the sensitivities of As, Sb, Se and Te were increased by 4-17 times compared with the solution atomization method. ② hydride generation system is simple and practical, due to the use of a multi-stage impactor separator as a gas-liquid separator chamber, the effective separation of hydride during the gas-liquid phase, eliminating the ICP-MS Cl Polyatomic ion interference on As, Se. ③ The internal standard method for the hydride ICP-MS, the use of hydride Ge as an internal standard, significantly improved the analysis precision and accuracy. The detection limits (3σ, ng / L) of As, Sb, Bi, Se and Te were 0.64,0.06,0.55,0.85 and 0 respectively under the compromise of simultaneous analysis of multiple elements. .63; detection limit (3σ, ng / L) were 71,10,9,6,8. The interferences of some transition elements in this hydride generation system were investigated, the valence effects of elements and the anti-interference effect of potassium iodide, thiourea and ascorbic acid were analyzed. Methods The sediments of aquatic sediment reference material and biological and plant?