The folic acid (F) gel, prepared in a 1 : 1 dimethyl sulfoxide (DMSO)–water mixture (v/v), at 0.2% (w/v) concentration has a nano-fibrous network morphology. FTIR spectra indicate the presence of intermolecular H-bonding interactions in the gel. The folic acid–chitosan (C) hybrid (FC) gel (prepared by mixing 0.1 ml of 1% (w/v) C solution with 2 ml 0.2% (w/v) F solution) appears as a yellow transparent semi-solid mass consisting of a nano-fibrous network with a higher density of branches. The fibrillar diameter of the FC hybrid gel (10.5 nm) is much lower than that of F gel (17.3 nm). The FTIR band at 3390 cm−1 of F gel shows a shift to 3435 cm−1 in the FC hybrid gel indicting a hydrogen bonding interaction between C and F. The fluorescence intensity of the FC hybrid gel is enhanced by 2.75 times than that of F gel. The shear viscosity of FC hybrid gel is 3 orders higher than that of the F gel and both gels exhibit shear thickening at a low shear rate (<10−3 s−1) but above that, shear-thinning occurs. In the creep phase, the FC hybrid gel exhibits strain recovery but the F gel does not. The complex modulus (G*) of both systems initially exhibit a sharp increase, followed by a slow increase with time (t) and dG*/dt varies with C concentration in the FC hybrid gel showing a maximum. The WAXS pattern of the FC hybrid xerogel does not exhibit any crystalline peak, suggesting that the additive (C) inhibits the crystallization of F. The dye absorption by the hybrid gel material is maximum for Eosin Yellow, (83.5%), however, Methyl Orange and Methylene Blue are absorbed to a lesser extent (∼40%). The FC hybrid gel absorbs 55% of Cu2+, 67.2% of Cr3+ and 49% of Co2+ from their respective solutions.