Cross-linked poly(orthocarbonate)s were prepared by condensation of the tetraethyl orthocarbonate with different length of aliphatic diols. The synthesized polymers have been characterized by Fourier-transform infrared spectroscopy, solid-state C-13 cross-polarization magic angle spinning (CPMAS) nuclear magnetic resonance, thermal gravimetric analysis, and elemental analysis. The cross-linked polymers were evaluated for organic solvent absorbency application. The effect of diol type on swelling properties of cross-linked polymers was studied through the solvent absorption tests. The swelling parameters such as maximum solvent absorbency, saturation time, and retention of the solvent were evaluated for the synthesized sorbents. All of the cross-linked polymers had moderate thermal stability and good regenerable solvent uptake abilities. POLYM. ENG. SCI., 53:2102-2108, 2013. (c) 2013 Society of Plastics Engineers