The electrochemistry component of this laboratory was the first time that most students were exposed to cyclic voltammetry and the bulk electrolysis technique. An Amel System 5000 Potentiostat was used for all measurements. For cyclic voltammetry, the electrochemical cell was a 100 mL beaker equipped with a Ag/AgCl reference electrode (student prepared), a BAS (West Lafayette, IN) platinum-disk working electrode (2 mm diameter) and a large (1 cm2) platinum flag counter electrode. After having verified a flat background of tetrabutylammonium hexafluorophosphate (0.01 M) supporting electrolyte in acetonitrile in the range 0.0 to 1.0 V vs. Ag/AgCl, cyclic voltammograms of ferrocene and acetylferrocene (approximately 3.2 x 10-3 M) were obtained at scan rates of 100 500 mV/sec. A typical cyclic voltammogram of ferrocene showed a reversible oxidation at E1/2 = +0.35 V vs. Ag/AgCl with Ep/2 = 0.057V. A typical cyclic voltammogram of acetylferrocene also showed a reversible oxidation at E1/2 = +0.58 V vs. Ag/AgCl with Ep/2 = 0.044V. Small peaks for ferrocene were also visible in the acetylferrocene cyclic voltammogram. These results are comparable to the reported E of acetylferrocene at +0.27 V vs. the ferrocene/ferrocenium couple (6).
A second new electrochemical component that was recently introduced into this laboratory is the bulk electrolysis of ferrocene to ferrocenium. The electrochemical cell was a 100 mL beaker equipped with an Ag/AgCl reference electrode (student prepared), a BAS (West Lafayette, IN) reticulated vitreous carbon (RVC) working electrode and an extremely large platinum flag counter electrode. After having verified a flat background of tetrabutylammonium hexafluorophosphate (0.01 M) supporting electrolyte in acetonitrile in the range 0.0 to 1.0 V vs. Ag/AgCl, the bulk electrolysis of ferrocene (approximately 7.5 x 10-4 M) was achieved on several occasions. As expected, a new peak in the UV-Vis was observed at 620 nm and the solution changed color from orange to blue. Unfortunately to date, these experimental conditions are not reproducible.