Development and applications of time-resolving electrochemical detector by means of the fast-scan differential pulse voltammetry using a microelectrode

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A novel short-pulse first-scan cyclic differential pulse voltammetry (FSDPV) using a microelectrode have been developed.The relationships between the electrode sizes and the pulse conditions have been examined in detail. It became clear that the available minimum pulse duration (tau_d)_<min> and rest time (tau_r)_<min> are related to the electrode size used ; i.e. (tau_d)_<min>=(tau_r)_<min>=20 and 50mus for 25- and 50-mum-radius Pt microelectrode, respectively.The FSCDPV of ferrocene in acetonitrile was measured at a potential scan-rate of 10 V/s and the pulse conditions of E_a (pulse height)=10 mV and tau_d=tau_r=20mus. The observed voltammogram is in good agreement with the simulated one based on reversible one electron transfer process.It became clear that the redox potential of ferrocene could be measured accurately with a relative standard deviation of 2% or better.In conclusion, the FSCDPV method appears to be an attractive tool not only for the accurate measurements of redox potentials in electrochemistry but rather for analytical applications, particularly, for time-resolving voltammetric detection in the flowing solutions.