FIELD: electrochemistry.
SUBSTANCE: disclosed is a method for controlling formation and stability of organonickel sigma complexes. In order to implement the method, a working solution prepared for electrolysis by dissolving the complex [NiBr2 (bpy)] and organic bromide in dimethylformamide is loaded into the cuvette of a spectroelectrochemical cell to control formation and stability of organonickel sigma complexes. Then, the electrodes fixed in the holder are immersed in the working solution in such a way that the working electrode is installed perpendicular to the optical path of the spectrophotometer beam, and the auxiliary electrode is set at the maximum distance from the working electrode, at the opposite wall of the cuvette around the optical path of the detecting radiation, respectively. Further, a DC source is connected to the terminals of the working and auxiliary electrodes while observing the polarity. After that, the cuvette with the assembly of the working and auxiliary electrodes installed in the holder is placed in the closed cuvette compartment of a standard spectrophotometer. Then, voltage is applied to the terminals of the working and the auxiliary electrodes, and electrolysis is carried out at a constant current strength of 15 mA at the ambient temperature for 5 minutes. Formation of organonickel sigma complexes in the working solution is detected by appearance of an absorption band in the visible range of 400–700 nm. Also disclosed is a spectroelectrochemical cell for monitoring the formation and stability of organonickel sigma complexes.
EFFECT: expansion of the monitoring capability for the formation reaction and stability of nickel-organic sigma complexes using the optical spectroelectrochemistry method with the exclusion of the effect of anodic reaction products on the spectrum of the electrochemically generated nickel-organic sigma-complexes, achieved by monitoring formation and stability of nickel-organic sigma-complexes and the new design of the electrochemical cell for its implementation, with capability to obtain higher quality organonickel sigma complexes both due to the features of the claimed cell design and by eliminating the mixing process in the near-electrode zone of the claimed cell, thereby increasing the quality of generating organonickel sigma complexes.
13 cl, 8 dwg, 4 ex
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Authors
Dates
2023-07-19—Published
2022-12-20—Filed