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Arnold, A. F. (1963) Studies in the electrolytic reduction of some aromatic nitro-compounds. Doctoral thesis, Sir John Cass College.
Discussions of the bases of classical and linear sweep polarography are given, followed by a description of double layer phenomena and their influence on polarograms. Particular emphasis is placed on the discussion of kinetic waves. Polarographic maxima, and reports of polarographic behaviour of aromatic nitro-compounds are reviewed in short chapters.
The apparatus used in the present work is described and details of modifications to a linear-sweep polarograph including a method for variation of sweep speeds are discussed.
Experiments are described which were done to test the behaviour of some typical systems (i.e. reduction of Tl+, Zn(NH3)4++ , Ni(H2O)6++ and o-nitrophenol) in linear sweep polarography with variable sweep speed. Discussion of the results indicated that the theories noted previously were not applicable to a high accuracy, particularly for estimation of peak potentials.
Classical polarograms for ranges of pH values, different alcohol and background electrolyte concentrations are recorded for picric acid, styphnic acid, and trinitrophloroglucinol. The linear sweep polarography of the same compounds is reported in some detail. A discussion in a separate chapter relates the abnormally large current peaks to adsorption of the electroactive species.
Some characteristics of the maximum of styphnic acid, taken as an example, are reported and reviewed as symptoms of surface phenomena.
Reduction mechanisms of the trinitrocompounds are discussed in a final chapter.
Appendices describing some problems of technique are included: these deal with irregularities in performance of dropping mercury electrodes, and an electrode of novel design with forced streaming of solution.
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