硒形态流动注射催化光度法分析

基于在pH7的柠檬酸磷酸氢二钠缓冲溶液中,硒(Ⅳ)对Na2S还原天青Ⅰ有强催化作用,建立了流动注射催化光度法测定硒的新方法。考察了不同流路的影响,分别研究了试剂和试样的流速、反应介质及酸度、反应温度、共存物质的影响。利用单纯形优化法选择了各种试剂的最佳用量以及采样体积、反应管长的最佳实验条件。方法的线性范围为01～20mg·L-1,检出限为0015mg·L-1,相对标准偏差小于31%,进样频率为120个·h-1。该方法用于大蒜和硒酵母中有机硒和无机硒的测定,结果发现大蒜对硒有强的富集作用,有机硒的转化率随环境硒浓度的增加而下降。测定的回收率在971%～1043%。

Speciation Analysis of Selenium by Flow-Injection Catalytic Spectrophotometry

A new flow-injection catalytic spectrophotometric method was proposed for the determination of Se(IV) based on its catalytic effect on the reduction reaction of azure I by Na2S in pH 7.0 citric-acid sodium-hydrogen-phosphate buffer solution. Some different schematic diagrams of FIA were compared. Effects of the flow rates of reagents and sample, the medium and its acidity, the temperature, and coexistent substances were studied respectively. The amount of used reagents and the experimental conditions for sampling volume and coil length were optimized by using the controlled and weighed centroid simplex method. The Linear range of the determination is 0.1-2.0 mg x L(-1), the detection limit is 0.015 mg x L(-1), the relative standard deviation is less than 3.1%, and the sampling frequency is 120 samples per hour. The method has been applied to the determination of organic selenium and inorganic selenium in garlic and selenium-yeast. It was found that garlic had a strong enriching effect for selenium, and the conversion ratio of organic selenium decreased with increasing the concentration of selenium in the environment. The recovery of this method is 97.1%-104.3%.