Chemical composition of fine (PM2.5) aerosol samples collected for the 5 years period (2001- 2005) using Gent Stacked filter unit sampler at Klang Valley (3 o 10 ’ 30 ’’ N, 101 o 43 ’ 24 ’’ E) were analysed using Neutron Activation Analysis (NAA) and Proton Induced X-ray Emission (PIXE). Results of the study show that the major component of the fine aerosol was black carbon and sulfur with the mass concentration ranged from 4.4 - 6.7µg m -3 and 1.2 - 1.9µg m -3 , respectively. The total fine aerosol mass concentration were in the ranged of 25 - 31µg m -3 with the reconstructed mass was about 50% as relative to the gravimetric mass. Statistical method, factor analysis with varimax approach has been applied to the aerosol composition data for the fingerprint identification. The analysis produces five identified fingerprint represent soil, industry, motor vehicles/biomass burning and Pb and Zn sources. There is also an unidentified source that could be related to unknown industrial activities.