S. Oszwaldowski et M. Jarosz, RP-HPLC STUDY OF REDOX EQUILIBRIA IN VANADIUM-PAR BINARY AND TERNARY-SYSTEMS - DIRECT DETERMINATION OF VANADIUM IN STEEL, Mikrochimica acta, 126(3-4), 1997, pp. 241-249
The reversed-phase high-performance liquid chromatographic (RP-HPLC) b
ehaviour of the binary chelates of V(V) and V(IV) with 4-(2-pyridylazo
) resorcinol (PAR) and ternary chelates of vanadium with PAR and auxil
iary ligands: hydrogen peroxide, hydroxylamine, tartrate and citrate w
ere studied using a C-18 column. The complex double-peak chromatograms
of V(IV)/V(V)-PAR systems were studied and the origin of each peak wa
s proved. Vanadium in ternary systems with PAR and hydrogen peroxide w
as found exclusively in V(V)-H2O2-PAR complex (single peak on the chro
matogram) despite its initial oxidation state. The double role of hydr
oxylamine (complex agent and reductor) in vanadium systems with PAR wa
s confirmed: in the V(V) system three species were identified (V(V)-PA
R, VM-NH2OH-PAR and V(IV)-PAR), but in the V(IV) system only two: V(IV
)-PAR and V(V)-NH2OH-PAR. Citrate and tartrate giving single peak were
found as auxiliary ligands in ternary V(V) systems of analytical impo
rtance. Due to its masking potential towards iron (III) ions, citrate
was chosen as the most suitable third component of a ternary vanadium
system with PAR, to form the basis of an RP-HPLC method for direct det
ermination of V in steel.