摘要
采用三电极系统,在HCI条件下,利用氟对锆(Ⅳ)-水杨基荧光酮(SAF)二元络合体系的竞争抑制及聚乙二醇的增敏作用,用单扫描极谱法测定多样品中各含量的氟。最佳底液组成是:1.2mg/L Zr(Ⅳ)-0.24mol/L HCI-1.4×10^-4mol/L的水杨基荧光酮-1.6mg/L的聚乙二醇(20000)。其起始电位为-0.30V,峰电位在-0.68V(vs.SCE)左右,测氟的线性范围为16.0-800.0μg/L,线性回归方程为Ip″(×10^-4nA)=1.3551+0.0048c(μg/L)(n=21,r=0.9996),检出限为12.2μg/L。本法适用于土壤、水样、蔬菜及人发中各含量氟的测定。用单扫描极谱法研究了氟的极谱行为,证明了电极反应物为水杨基荧光酮而非ZrFp^4-p,极谱波为不可逆还原吸附波,讨论了电极反应机理。
A method for the determination of fluorine by single sweep polarography has been established. It was based on the inhibitory effect of fluorine on the formation of binary complex between Zr(Ⅳ) and salicyl fluomnl (SAF) under acidic conditions, and the sensitization of Polyethylene glycol. The optimal determination conditions are 2.0 mg/L Zr(Ⅳ) -0.24 mol/L HCI- 1.4×10^-4mol/L SAF-1.6 mg/L polyethylene glycol (20000). The peak potential is -0.68V(vs. SCE). The peak height is linearly proportional to the concentration of fluorine over the range of 16.0-800.0μg/L with the linear regression equation as Ip"(×10^-4nA) = 1.3551+0.0048c (μg/L) ( n = 21, r = 0.9996), and the detection limit is 12.2μg/L. The method is rapid, sensitive, simple, economical and has good selectivity. The results are satisfactory when it was used to analyze soil, water, vegetable and hair. It was proved by sin-gle-sweep polarogrophy that the reaction of fluorine at the electrode had the characteristic of irreversible adsorptive reduction wave and the electro-active complex was salieyl fluomnl (SAF) not ZrFp^4-p, a brief discussion of the electrode reaction was also given.
出处
《分析试验室》
CAS
CSCD
北大核心
2009年第5期11-15,共5页
Chinese Journal of Analysis Laboratory
基金
高等学校博士学科点专项基金(20050616009)
“广东省珠江三角洲经济区农业地质与生态地球化学调查”专题基金(1212010511216)项目资助
关键词
氟
单扫描极谱
电极反应机理
Single-sweep polarography
Fluorine
Electrode reaction mechanism