【摘要】 选用Zr(Hf)-F-5 Br PADAP体系进行锆和铪的高灵敏度显色反应,确定了柱前衍生、色谱分离及测定的最佳条件。考察了5 Br PADAP的浓度、pH值、流动相、流动相的组成及显色时间对锆和铪络合物及色谱分离的影响。选用乙腈和水的混合液为流动相,流动相中对离子试剂NaF的浓度为1 5×10-4～3×10-4mol/L,pH4 2±0 2;用C18作为分离柱,峰面积与样品浓度线性范围为Zr:1 6～200μg/L,Hf:1 3～200μg/L,分离度1 84。方法的检测限为Zr:12 1μg/g,Hf:9 92μg/g。此方法用于合成钢样中锆和铪的直接测定,结果令人满意。更多还原

【Abstract】 An analytical method based on reversed-phase high performance liquid chromatography,with ultraviolet/visible detection at 583 nm was studied.The ternary metal complexes with fluoride and 2-（5-bromo-2-pryidylazo）-5-diethylaminophenol （5-Br-PADAP） were used as a basis of the method for the simultaneous determination of Zr*$ and Hf*$.Optimum conditions for the determination of zirconium and hafnium were investigated,including the concentration of 5-Br-PADAP,the pH of forming complexes,the mobile phase and its composition and the time of color development.5-Br-PADAP complexes were eluted with mobile phase,which was acetonitrile-water containing fluoride(1.5×10^-4-3×10^-4 mol/L,pH 4.2±0.2).The separation was performed by a C₁₈ reversed-phase column.The calibration curves were linear in the ranges of 1.6-200 μg/L for Zr*$ and 1.3-200 μg/L for Hf*$,respectively.The detection limits of Hf*$ and Zr*$ were 9.92 μg/g and 12.1 μg/g respectively.The results of analyzing Zr and Hf in steel and iron by the developed method were satisfactory.更多还原