Hybrid nanomaterials have attracted considerable interest in environmental science, analytical chemistry and atomic spectroscopy. In the present study, a column solid phase extractioo procedure was developed for the separation and preconcentration of indium in various matrixes by using hybrid nanomaterial B2O3/ZrO2 (HNMBZ). Various experimental and analytical parameters such as sample solution pH, sample solution volume, flow rate of sample solution and eluent, volume and concentration of eluent and amount of HNMBZ, effect of common matrix ions and capacity of sorbent were investigated. The adsorbed metal ions on HNMBZ were eluted with 6 mL of 1 mol . L-1 HNO3 solutions and their concentrations were determined by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Under the optimized conditions, detection limits for indium for 3 pixels and 5 pixels were found as 0. 20 and 0. 16 mu g . L-1, respectively. The accuracy of the procedure was checked by spiked water samples. The developed procedure was successfully applied to real samples for the separation and determination of indium.