毛细管电泳柱内在线还原化学发光测定V(Ⅳ)和V(Ⅴ)-陕西师范大学学报期刊社网站

陕西师范大学学报（自然科学版）

化学与材料科学

毛细管电泳柱内在线还原化学发光测定V(Ⅳ)和V(Ⅴ)

杨维平1,章竹君2

（1 陕西师范大学民族教育学院；2 陕西师范大学化学与材料科学学院，陕西西安 710062）

杨维平，男，教授,博士，主要从事毛细管电泳及发光分析方面的研究. E-mail: wpy@snnu.edu.cn.

摘要:

利用毛细管柱内在线还原方法，结合毛细管电泳-化学发光同时分离与检测V(Ⅳ)和V(Ⅴ).V(Ⅴ)在毛细管内在电场作用下被酸性H2O2在线还原为V(Ⅳ)，根据两种V(Ⅳ)离子到达检测窗口的迁移时间的不同，从而达到分离与检测的目的.按照样品混合液、HCl和H2O2依次进样，以002 mol/L HAc-NaAc (pH=47)为缓冲液，分离电压为15kV.V(Ⅳ)和V(Ⅴ)的检测限分别为68×10-12mol/L和2.1×10-10mol /L (3σ).对1×10-10mol/L V(Ⅳ)和1×10-9mol/L V(Ⅴ)进行5次测定，迁移时间的RSD(%)分别为12%和14%, 峰高的RSD(%)分别为48%和45%.V(Ⅳ)和V(Ⅴ)的线性范围分别为：25×10-11~10×10-9 mol/L、50×10-10~50×10-8 mol/L.

关键词：

化学发光；毛细管电泳；钒形态；柱内还原

收稿日期：

2010-01-10

中图分类号：

O6573

文献标识码：

文章编号：

1672-4291(2010)04-0051-04

基金项目：

国家自然科学基金资助项目（30470886）

Doi:

Determination of V(Ⅳ) and V(Ⅴ) using online reduction chemiluminescence occured in capitlary electrophoresis

YANG Wei-ping1，ZHANG Zhu-jun2

(1 Education School of Nationalities, Shaanxi Normal University;2 College of Chemistry and Materials Science，Shaanxi Normal University, Xi′an 710062, Shaanxi, China）

Abstract:

Based on in-capillary reduction, the separation and determination of vanadium(Ⅳ) and vanadium(Ⅴ) can be achieved using capillary electrophoresis with chemiluminescence method. V(Ⅴ) can be reduced by acidic H2O2 to form V(Ⅳ) in case of sample running through the capillary, and the separation and detection of V(Ⅳ) and V(Ⅴ) can be achieved according to migration time difference of both V(Ⅳ) ions. The sample solution, HCl and H2O2 were successively injected. Running buffer was composed of 0.02mol/L HAc-NaAc (pH=47). 15kV was applied as separation voltage. The limits of detection for vanadium (Ⅳ) and vanadium (Ⅴ) (3σ) were 68×10-12 mol /L and 21×10-10 mol/L, respectvely. The linear ranges of vanadium (Ⅳ) and vanadium (Ⅴ) were 2.5×10-11～10×10-9 mol/L and 50×10-10～50×10-8mol/L, respectvely.

KeyWords:

chemiluminescence; capillary electrophoresis; vanadium speciation; in-capillary reaction