摘要
本工作利用一种改进型旋流雾室雾化氢化物发生装置,建立同时测定铅、砷、锑、铋、锗、锡及非氢化物元素的ICP-AES法。溶液中的Pb(Ⅱ)首先以H_2O_2-(NH_4)_2S_2O_8溶液氧化为Pb(Ⅳ),然后再与NaBH_4溶液反应产生氢化物,与由气动雾化产生的样品气溶胶一起被导入等离子体中。Pb,As,Sb,Bi,Sn,Ge的检出限分别为1.4,7.6,2.8,1.3,2.4和15μg/L,较通常的气动雾化法低20-60倍,硒、碲在氧化剂存在下不能产生氢化物。研究了共存元素的干扰及消除方法。实际样品(沉积物)分析结果与推荐值吻合。
A method for simultaneous determining Pb, As, Sb, Bi, Sn, Ge and nonhydrideforming elements has been developed with a modified cyclone nebulizer-hydride generator. Lead(Ⅱ) is oxidized firstly to Pb(Ⅳ) using 2% (V/V) hydrogen peroxide 8%(W/V)-ammonium persulfate as oxid ing agent. The sample solution is mixed with 3% NaBH4 solution, and the mixture is pumped into the chamber by a peristaltic pump. Hydrides formed and the sample aerosol produced by a Meinhard nebulizer are introduced into ICP with carrier gas. Detection limits of Pb, As, Sb, Bi, Sn, Ge are 1.4, 7.6, 2.8, 1.3, 2.4 and 15 μg/L respectively, and are improved 62, 20, 66, 12, 18 and 24 times respectively comparing with pneumatic nebulization method. Interferences of coexisting elements have been studied, and 0.4%(W/V) KCNS-0.6% (W/V)H_2C_2O_4 solution was used to eliminate the Interferences of Fe, Cu, Co and Ni.Spectral interferences of interelements were corrected using interference factor method. The method has been used to analyze sediment samples, and satisfactory results have been obtained.
出处
《光谱学与光谱分析》
SCIE
EI
CAS
CSCD
北大核心
1990年第5期36-40,49,共6页
Spectroscopy and Spectral Analysis