This thesis is focused on analysis of reduction of ammonium perrhenate using less frequent reducing agents. Ascorbic acid and acetylhydrazine were chosen as less common reducing agents. Reductions were observed leveraging capillary zone electrophoresis and UV/Vis spectroscopy. Measurements were carried out both in acidic and in basic environments. Reduction of peak area of ammonium perrhenate was observed using capillary zone electrophoresis after addition of reducing agent. Rate of absorption of ammonium perrhenate was monitored with UV/Vis spectroscopy. Furthermore, the possibility of shifting the equilibrium of the reaction to the benefit of the reduction products was monitored by the addition of the complexing agent. Py- rogallol (benzene-1,2,3-triol) was used as the ligand and acetylhydrazine was selected as the reducing agent. The reduction was monitored by capillary zone electrophoresis. The identity of the resulting complex was confirmed with ESI/MS. Keywords rhenium, rhenium complexes, ascorbic acid, acetylhydrazine, capillary zone electrophore- sis, UV/Vis spectroscopy, mass spectrometry