Determination of trace amounts of niobium in steel by reversed-phase high-performance liquid chromatography with methyl isobutyl ketone extraction and pre-column derivatization

A method for the determination of trace amounts of niobium in steel samples by reversed-phase high-performance liquid chromatography (RP-HPLC) was dev eloped, The iron matrix was removed from sample solution by using methyl is obutyl ketone as an extraction agent. 2-(5-Bromo-2-pyridylazo)-5-diethylan- tino phenol (5-Br-PADAP) was used as a pre-column chelating agent to form t ernary complex with Nb(V) and tartaric acid. The Nb(V) complex was eluted w ithin 3 min with a mobile phase of methanol-water (56:44 (v/v)) containing 10 mmol/l acetate buffer (pH 3.5) on a C-18 column and determined with spec trophotometric detection at 600 nm. The detection limit of this method for Nb in iron or/and steel sample was 0.015 mug/g. The proposed method was app lied to the analysis of trace amounts of niobium. in cast iron. (C) 2001 El sevier Science B.V. All rights reserved.