The synthesis of pyrophoric nanoparticles from Fe(II)-oxalate precursor will be presented. The precursor was synthesized using a solution based controlled nucleation process. In this, the solution of oxalic acid was added drop wise to the FeCl₂.2H₂.O solution under continuous stirring at 60-70^oC. The solution mixture was cooled down to 25^oC and centrifuged to recover the precipitate. In another approach, Fe(II)-oxalate nanorod synthesis was attempted using polyethylene glycol (PEG-600) surfactant template. Oxalic acid, FeCl₂.2H₂.O and PEG-600 were homogeneously mixed together and diluted with de-ionized water and sonicated for 4 h. Finally, the contents were centrifuged to recover the precipitate. In both synthesis methods, the precipitate was thoroughly washed with de-ionized water and ethanol and dried at 95^oC. As-synthesized oxalates were characterized using thermogravimetric analyzer/differential scanning calorimetry, Fourier Transform Infrared (FTIR) spectrometry, and transmission electron microscopy (TEM). Microstructure of the oxalate prepared using PEG-600 shows nanorod morphology with porous structure. Decomposition of oxalates into pyrophoric nanoparticles was accomplished in an isothermal flow reactor under reducing environment. Next, the particles were oxidized in air and the temperature change during their oxidation was recorded using a pyrometer. For both lab-synthesized and commercial Fe(II)-oxalates, the temperature reaches to their respective maximum of 850^oC and 670^oC in less than 1 second. Furthermore, no degrading effect on pyrophoric action was noticed on storing α-Fe for 16-24 h. Thus, Fe(II)-oxalate shows promise to produce pyrophoric nanomaterial, which may be useful for several applications.