Novel monolithic disks were prepared via ring opening metathesis polymerization (ROMP) from norborn-2-ene (NBE), a crosslinker, i.e., 1,4,5,8,8a-hexahydro-1,4,4,5,8, exo, endo-dimethanonaphthalene (DMN-H6) and tris(norborn-5-ene-2-ylmethylenoxy)methylsilane, respectively, 2-propanol and toluene (25:25:41:9, all %, w/w) using RuCl2(PCy3)2(CHPh) (Cy=cyclohexyl) as initiator and triphenylphosphine (PPh3) as modulator. Disks 1-2 mm thick were prepared by polymerization in a mold, disks thinner than 1mm were prepared by impregnation of nylon or other porous filters prior to the polymerization step. These disks were evaluated for the preconcentration of iodine and selected organic solutes from dilute aqueous samples by solid-phase extraction (SPE). Quantitative measurement of the extracted solutes was achieved by diffuse-reflectance spectroscopy (DRS) directly on the surface of the disk.