8─羟基喹啉─5─磺酸柱前衍生反相HPLC分离测定痕量Al（Ⅲ）、Co（Ⅲ）、Fe（Ⅲ）和Pd（Ⅱ）

Separation and determination of microamounts of aluminum,cobalt,iron and palladium by high performance liquid chromatograpny

本文采用８－羟基喹啉－５－磺酸（ＨＱＳ）为柱前衍生试剂，用含有１０ｍｍｏｌ·Ｌ－１的四丁基溴化铵（ＴＢＡ＋Ｂｒ－）、７．５×１０－５ｍｏｌ·Ｌ－１的ＥＤＴＡ和２０ｍｍｏｌ·Ｌ－１的ｐＨ５．６乙酸－乙酸钠缓冲溶液的甲醇－水（４５：５５，Ｖ／Ｖ）溶液为流动相，以Ｃ１８硅烷化载体为固定相，１６ｍｉｎ内分离测定了Ｃｏ（Ⅲ）、Ｆｅ（Ⅲ）、Ａｌ（Ⅲ）和Ｐｄ（Ⅱ）的ＨＱＳ的配合物、信噪比为３时，检出限分别为：Ｃｏ（Ⅲ）０．９ｐｐｂ、Ｆｅ（Ⅲ）１．５ｐｐｂ和Ｐｄ（Ⅱ）５．４ｐｐｂ，方法灵敏度高，干扰少，用于测定试剂级盐酸，硝酸和中国红茶样品中的这些离子，结果良好。

The reversed-phase high performance liquid chroma to graphy-spectrophotometric determination of aluminum, cobalt, iron and palladium using 8-hydroxyquinoline-5-sulfonic acid(HQS)as precolumn chelate reagent on ODS column has been investigated.The mobile phase is methanol-water(45:55,V/V) containing 20mmol/L pH5. 6 acetate buffer and 10mmol/Ltetrabutylammonium bromide(TBABr).The four complexes can be separated completely within 16 min.The detection limits are 0.9,1.5 and 5.4 ng for cobalt(Ⅱ),iron (Ⅲ)and palladium(Ⅱ)respectively when the ratio of signal to noise is 3.This method has been applied to the determination of cobalt and iron in samples.