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The composition effect of carbon supported Ni x M 1−x (M = Bi, Pd, and Au) nanomaterials toward glycerol electrooxidation (GEOR) was evaluated in alkaline media. Ni-rich catalysts with different atomic ratios (M atomic ratio ≤20%) were synthesized by the heatless coreduction method and characterized by various physicochemical and electrochemical techniques. All structures of the Ni x M 1−x /C catalysts were composed of a rich phase of Ni(OH) 2 , as evidenced by TDA-TGA and XPS. Among the different nanomaterials, the Ni 0.9 Au 0.1 /C catalyst provided the lowest onset potential (+0.12 V vs Hg/HgO) and the highest peak current density. In situ infrared spectroscopy experiments combined with electrochemical measurements exhibited the formation of formate for all catalysts, thus indicating the breakage of C− C bonds of glycerol. GEOR led to 100% selectivity for formate after 1 h electrolysis and 100% conversion of glycerol after 24 h at +1.55 V. Furthermore, when these inexpensive catalysts were tested in tandem with cathodic CO 2 electroreduction, the anodic Ni 0.9 Au 0.1 /C catalyst displayed the highest partial current density for CO and the lowest onset potential.