离子对反相色谱法同时测定钢铁及合金中锆和铪  

Simultaneous determination of zirconium and hafnium in iron and steel by ion pair reversed-phase liquid chromatography

作　　者：彭霞[1] 胡晓燕[1] 

机构地区：[1]钢铁研究总院,北京100081

出　　处：《冶金分析》2005年第1期23-26,共4页Metallurgical Analysis

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。An analytical method based on re versed-phase high performance liquid chromatography, with ultraviolet/visible detection at 583 nm was studied. The ternary metal complexes with fluoride and 2-(5-bro-mo-2-pryidylazo)-5-diethylaminophenol (5-Br-PADAP) were used as a basis of the method for the simultaneous determination of Zr(IV) and Hf(IV). 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(IV) and 1.3-200 μg/L for Hf(IV), respectively. The detection limits of Hf(IV) and Zr(IV) 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.

关 键 词：流动相 反相色谱 离子对 5-BR-PADAP 同时测定 样品浓度 混合液 分离柱 显色反应 色谱分离 

分 类 号：TG115[金属学及工艺—物理冶金]