Analytical procedures for the analyses of organic and inorganic compounds in air particulates collected on a single cellulose fiber filter were investigated using analytical facilities commonly available in a chemical laboratory. For the analysis of inorganic compounds, a DC are emission spectrometer coupled with a photo-diode array detector was used to quantify the metal contents, including Cd, Cr, Cu, Fe, Mg, Mn, Ni, Pb, Si and V. The sample treatment method included pulverizing a portion of the filter and mixing if with thermochemical agents, which could enhance the sensitivity if the method for subsequent analyses. The recovery of the method was checked against SRM 1648 Urban Particulate Matters. The performance of various thermochemical agents was compared. The emission-time profiles show the possibility of differentiating refractory elements from the more volatile ones and thereby providing valuable information for use in the apportionment of mahor air pollution sources.