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采用反相高效液相色谱法(HPLC),通过紫外检测,以氟硅烷衍生物形式测定总有机氟,对氟离子进行测定。

Determination of fluoride as fluorosilane derivative using reversed-phase HPLC with UV detection for determination of total organic fluorine.

机构信息

Department of Chemistry, University of Warsaw, Warsaw, Poland.

出版信息

J Sep Sci. 2010 Sep;33(17-18):2636-44. doi: 10.1002/jssc.201000179.

Abstract

A quantitative method for fluoride determination using RP HPLC and UV detection was developed. The method is based on the reaction of fluoride with triphenylhydroxysilane in highly acidic conditions and extraction of the reaction product into n-heptane. Chromatographic conditions as well as the derivatization parameters were optimized. LOQ for fluoride ion was evaluated as 0.25 μM (4.75 ppb) and linear range of response up to 75 μM (1.42 ppm) was obtained. The method was developed as a part of a procedure designed for the determination of total organic fluorine in natural waters, using SPE on a carbon sorbent and sodium biphenyl reagent for the defluorination reaction. LOD for a model compound, perfluorooctanoic acid, calculated for the complete procedure with 2000-fold preconcentration, is 20 ppt (n=4). Initial results show feasibility of total organic fluorine determination for environmental purposes.

摘要

开发了一种使用反相高效液相色谱法和紫外检测测定氟化物的定量方法。该方法基于氟化物在强酸性条件下与三苯基羟基硅烷的反应,以及将反应产物萃取到正庚烷中。优化了色谱条件和衍生化参数。氟离子的 LOQ 评估为 0.25 μM(4.75 ppb),响应线性范围可达 75 μM(1.42 ppm)。该方法是为了测定天然水中的总有机氟而开发的,在该方法中,使用碳吸附剂固相萃取和联苯钠试剂进行脱氟反应。对于模型化合物全氟辛酸,经过 2000 倍预浓缩后的完整程序计算的 LOD 为 20 ppt(n=4)。初步结果表明,该方法可用于环境目的的总有机氟测定。

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