均匀设计在优化原子荧光法测砷条件中的应用  

Application of Uniform Design in Optimizing the Condition of Arsenic Determination by Atomic Fluorescence Spectrometry

作　　者：杨启霞[1] 韩吉衢[2] 常显波[1] 杜旭昌 

机构地区：[1]烟台大学环境与材料学院,山东烟台264005 [2]烟台大学光电技术学院,山东烟台264005 [3]莱州市锅炉检验所,山东莱州261400

出　　处：《光谱学与光谱分析》2009年第2期526-529,共4页Spectroscopy and Spectral Analysis

基　　金：国家海洋局海洋生态环境科学与工程重点实验室项目(MESE-2007-02)资助

摘　　要：采用均匀设计U1＊0（108）优化氢化物发生-原子荧光光谱法测定水萝卜和菠菜中砷的条件,借助UD3.0软件,建立了数学模型并进行了回归分析,求得最优解。结合空心阴极灯灯丝的使用寿命和噪声水平及其他影响因素,得出优化的实验条件,负高压280-360V,灯电流50-70 mA,载气流量500-700mL.min^-1,硼氢化钾浓度15.0-20.0 g.L-1,盐酸浓度0.6-1.2 mol.L^-1,进样量0.5-1.0 mL。在该条件范围内测定了两个蔬菜样品,相对标准偏差（RSD）低于3.6%,加标回收率为94.1%-101.3%,检出限0.042μg.L^-1。文章将均匀设计作为一种有效的试验设计方法引入有多种因素影响的原子荧光光谱分析中,为实验条件优化提供了一个很好的方法和思路。In the present paper, uniform design U10 （10^8） was used to optimize the condition of arsenic determination in vegetable samples by hydride generation-atomic fluorescence spectrometry. Mathematical model was established and regression analysis was done, and the optimized solutions to those equations were obtained by making use of the UD3.0 software. Combining the life-span of hollow cathode filament, noise of negative voltage and other factors, the optimal condition was obtained as follows： negative voltage was 280-360 V; lamp current was 50-70 mA; carrier gas flow rate was 500-700 mL · min^-1 ; KBH4 concentration was 15. 0-20. 0 g · L^-1 ; HCL concentration was 0. 6-1.2 mol · L^-1 ; sample size was 0. 5-1.0 mL. Two samples of vegetable were analyzed under the optimized condition. The results showed that the relative standard deviation was less than 3. 6 %, and the recovery was within 94. 1%-101.3% ,with their detection limits of 0. 42 ug· L^-1. In this paper, as an effective method of experiment design, uniform design was introduced to hydride generation-atomic fluorescence spectrometry analysis with multifactors, which offered a good idea for the optimization of experiment conditions.

关 键 词：均匀设计 氢化物发生-原子荧光光谱法 砷 优化实验条件 

分 类 号：O657.3[理学—分析化学]