The amperometric detection with two polarized indicating electrodes (also named as biamperometic detection) is based on the measurement and the intensity of current passing through the two identical, usually inert, electrodes, to which a small potential difference from few tens to few hundreds milli volts was applied. The current flowing in the detection cell is observed only, when solution contacting the electrodes contains two forms of reversible redox couple, it means such one for which at the same potential the oxidation of the reduced form or the reduction of oxidized form can occur. This behaviour is observed for such couples as Br 2 /Br-; I 2 /I-; Fe 3+ / Fe 2+ ; Ce 4+ /Ce 3+ ; Ag + /Ag; AgI/Ag, I-; AgBr/Ag, Br-; AgCl/ Ag,Cl-; quinine/hydroquinine; Cu 2+ /Cu + (in some nonaqueous media), etc. 1-3. In biamperometric detection, in the presence of an excess of one form of reversible redox couple, the magnitude of the current measured is linearly proportional to the concentration of the second form in the solution as long as concentration over potential is not involved. When the polarizing potential difference applied to the electrodes is increased, an extension of the linear range of response is observed, however, it is associated with possible interference for other redox species present in solution. When the system detected in the solution is irreversible, the oxidation and reduction processes have activation potentials much larger, even up to 1 V. Such a large