Speciation of Vanadium(IV) and Vanadium(V) Using Ion-exchange Chromatography and ICP-AES.

A speciation method for vanadium(IV) and vanadium(V) is presented that uses a combination of HPLC and ICP-AES. In this method, 1 mM HNO3 solution and 100 mM HNO3 solution were applied in sequence as eluent. A vanadium(IV) and vanadium(V) mixture was injected into a HPLC anion-exchange column; and vanadium(IV) cation was then eluted by 1 mM HNO3, while vanadium(V) oxoacid anion was trapped on the column. After this separation, vanadium(V) was eluted as a cation from the column by 100 mM HNO3. Vanadium was detected by ICP-AES. In this separation, about 15% of vanadium(V) interfered with vanadium(IV), and trace vanadium(IV) interfered with vanadium(V). This interference could be estimated by simple calculation based on standard observations, and the speciation of vanadium(IV) and vanadium(V) was performed. The lower determination limit was 1 microgram/mL, which is insufficient to speciate vanadium sampled by conventional sampling methods in a working environment. However, impurity of the other valent vanadium species in a vanadium(V) reagent can be determined by the present method, which should be valuable in precisely assessing the toxicities of vanadium species.