In this study, we investigated the composition of an electrolytic Fe phosphide at different synthesis temperatures. We found that the ratio of Fe in the electrodeposit increases with synthesis temperature, whereas the oxygen content introduced into the electrodeposit by the atmospheric oxidation of Fe decreases. The aim of this study was to identify the reason for this effect. For this purpose, the ratio of Fe and P in the electrodeposits prepared at different temperatures was analyzed in depth. In addition, the types and ratios of Fe phosphide phases were considered. It was proved that with increase in temperature, a significant amount of Fe reacted with P to form Fe phosphide phases, and consequently, the amount of residual pure Fe that would react directly with oxygen decreased.