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In the search of better catalysts for fuel cells, synthesis of several intermetallic compounds and alloys as nanoparticles has been investigated. In order to obtain these materials as catalysts for fuel cells, chemical co-reduction of precursors in the absence of surfactants with suitable reducing agents has been chosen as the method of synthesis. This work was done in collaboration with combinatorial groups and electrochemists for identifying potential catalysts and electrochemically evaluating them. Starting with PtPb, the scope of this method has been extended to obtain Pt intermetallic compounds and alloys with metals across the periodic table with sodium naphthalide as the reducing agent. The sodium napthalide method has been compared side by side with the sodium borohydride method for metals which can be reduced by both. Other reducing agents have also been explored. PtPb synthesis using sodium naphthalide has been investigated in detail as a case study. Factors affecting room temperature crystallization of PtPb and contributing to low activity observed previously have been identified and addressed by changing th