On-line separation/preconcentration of V(IV)/V(V) in environmental water samples with CTAB-modified alkyl silica microcolumn and their determination by inductively coupled plasma-optical emission spectrometry.

A simple and selective method of flow injection microcolumn separation/preconcentration on-line coupled with inductively coupled plasma-optical emission spectrometry (ICP-OES) was developed for the speciation of V(V)/(IV). Various factors affecting the separation/preconcentration of V(IV) and V(V) by conical microcolumn packed with cetyltrimethylammonium bromide (CTAB)-modified alkyl silica have been systematically investigated. It is found that V(V) was quantitatively retained by the microcolumn at pH 2.0-7.0, while V(IV) was not retained by the microcolumn at pH 2.0-3.5 but quantitatively retained at pH 5.0-7.0. The two vanadium species adsorbed by the modified adsorbent were quantitatively desorbed by 0.10 mL of 1.0 mol L(-1) HNO(3). Therefore, V(V) and total vanadium could be determined by CTAB-modified alkyl silica packed microcolumn separation/preconcentration and on-line ICP-OES detection after adjusting sample solution to pH 2.5 and 6.0, respectively, and the assay of V(IV) was realized by subtracting V(V) from total V. The detection of limit (LOD) for V(V) was 0.03 microg L(-1) with an enrichment factor of 27.9 for a 3.0 mL sample consumption. The relative standard deviations (RSDs) (C(V(V))=C(V(IV))=5.0 microg L(-1), n=9) were 4.3% and 4.0% for V(V) and total V, respectively. The developed method was validated by the determination of V(IV) and V(V) in environmental water samples.