The application of biopolymers such as chitosan is one of the emerging sorption methods for the removal of metal ions, even at low concentrations. A rapid, sensitive and selected method is de- scribed for preconcentrative determination of vanadium(V) using the synthesized 3-Hydroxyben- zaldehyde-4 Amino antipyrine (HBAP), which was chemically immobilized on chitosan. This is easy to prepare in comparison to many other sorbents. The synthesized sorbent material was se- lective to vanadium(V) within a better response time of 30 min. The method was selective in presence of other foreign ions like Cl-, F-, , , Na+, Ca2+, Zn2+, Fe3+, Fe2+, Cu2+, Cr3+, EDTA, Mn2+, Co2+ and Ni2+. The calibration plots were linear over the concentration range of 0.5 μg·L-1 to 7 μg·L-1 of vanadium(V). These values are 100 times lower than by the direct determination of vanadium by FAAS. The developed procedure was reproducible with a relative standard deviation of 2.84%. The developed sorbent was successfully applied for the determination of vanadium(V) in real water and soil samples. Unlike most preconcentration procedures, the present enrichment method allowed for a rapid and reliable determination of vanadium(V) in environmental samples by the simple and routinely available flame atomic absorption spectrometry technique.