A novel solvent deficient precipitation (SDP) method to produce nanoparticles was studied for its potential in Fischer-Tropsch synthesis (FTS) catalysis. Using Fe(NO 3 ) 3 ⋅9H 2 O as the iron-containing precursor, this method produces ferrihydrite particles which are then dried, calcined, reduced, and carbidized to form the active catalytic phase for FTS. Six different drying profiles, including final drying temperatures ranging between 80 and 150 ∘ C, were used to investigate the effect of ammonium nitrate (AN), a major by-product of reaction between Fe(NO 3 ) 3 ⋅9H 2 O and NH 4 HCO 3 in the SDP method. Since AN has two phase-transitions within this range of drying temperatures, three different AN phases can exist during the drying of the catalyst precursors. These AN phases, along with physical changes occurring during the phase transitions, may affect the pore structure and the agglomeration of ferrihydrite crystallites, suggesting possible reasons for the observed differences in catalytic performance. Catalysts dried at 130 ∘ C showed the highest FTS rate and the lowest methane selectivity. In general, better catalytic performance is related to the AN phase present during drying as follows: phase III > phase II > phase I. However, within each AN phase, lower drying temperatures led to better catalytic properties.