The experiment described here for advanced inorganic chemistry undergraduate students includes a solvolysis reaction of [CoCl(NH[subscript 3])[subscript 5]][superscript 2+] in nonaqueous (H[subscript 3]PO[subscript 4]) medium, followed by an alternative way of using ion-exchange chromatography based on the capability of changing the charges of the species by a pH-shift ([Co(H[subscript 2]PO[subscript 4])(NH[subscript 3])[subscript 5]][superscript 2+]/[Co(PO[subscript 4])(NH[subscript 3])[subscript 5]]). The complex is then hydrolyzed in acidic medium to produce the corresponding aquocomplex ([Co(H[subscript 2]O)(NH[subscript 3])[subscript 5]][superscript 3+]). Time monitoring of the latter process with UV-vis and [to the thirty-first power]P NMR spectroscopies is conducted and comparison of the two techniques indicate the validity of the results obtained despite the different spectroscopic response to the reaction mixtures. (Contains 1 scheme, 1 table and 1 figure.)