Solid Au and Ag microelectrodes for both,model,and in situ voltammetric measurements, have been designed andtested. Amalgamation procedure and the parameters of measurement procedure are discussed. Differences betweengold and silver electrodes were studied. Silver electrodes showed more stable behavior and were used prevalently for calibration and in situ measurements.Calibration of a 30-µm diameter Ag electrode for Mn(II), Fe(II), I(-I) andS(-II) showed good linearity with reasonable confidence intervals, necessary for quantification of the signalsobtained in situ, with average sensitivity of 0.05, 0.01, 0.16 and 1.10 nA/(µmol L-1) and minimal detection limit of 3.5, 28, 0.3 and 0.05 µmol L-1, respectively. Additional checking of the electrode sensitivity with the reduction peaks of oxygen is proposed.
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