Recent workhas established that second harmonic ac polarographic measurements may be utilized advantageously in the determination of rate parameters of fast electrode processes (1-3). Excellent agreement between experiment and theory has been observed for several examples of the socalled quasi-reversible case (1-3). Similar success has been realized with one system characterized by a fast follow-up chemical reaction (4). Rate parameters obtained in these studies agree favorably with those yielded by more familiar techniques, such as fundamental harmonic ac polarographic measurements (5, 6). The sensitivity of second harmonic ac polarographic currents to kinetic parameter variations led in one case to the suggestion that the charge transfer coefficient may be determined with three significant figure accuracy (1).These and earlier investigations (see references 1-6 for a more complete bibliography) have been confined almost solely to measurement of the second harmonic current amplitude. Only brief reports of semi-quantitative attempts at second harmonic phase angle measurements may be found in the literature (7,8).In conventional (fundamental harmonic) ac polarography,
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