This study centered on the quantitative analysis of about 27 trace elements including toxic ones using instrumental neutron activation analysis of fine ambient particulate matter in the third and fourth industrial complex area of Daejeon city, Korea. For analytical quality control, the certified reference material (NIST, the National Institute of Standards and Technology, U.S.A., SRM 2783, air particulate on filter media) was used. The errors relative to SRM values of Sb, Mn, V, Mg, Na, K, Ti, Co, Zn, and Sm fell below 5%, while those of Cr, Fe, Ba, Th, Ce, Al, and Cu were less than 10%. From the results of the quantitative analysis, the concentration of toxic metals such as As, Mn, Se, V, and Zn were $3.26{\pm}2.72$, $9.86{\pm}4.71$, $2.18{\pm}1.25$, $4.91{\pm}2.41$, $158{\pm}78ng/m^3$, respectively. And the results of factor analysis indicated that there are no more than six factors of sources of fine ambient particulate with statistical significance in the study area.