This study aims to determine the temporal distribution and composition of suspended particulate matter in different sizes PM2.5–10 (Coarse Particle, CP) and PM2.5 (Fine Particle, FP) for source apportionment analysis. CP and FP samples were collected using the Gent PM10 stacked filter unit (SFU) sampler at an urban coastal city of Kuala Terengganu, in Malaysia, from August 2006 to December 2007. Samples were analyzed for elemental concentrations using Inductive Coupled Plasma-Mass Spectrometry (ICP-MS) and Inductive Coupled Plasma-Optical Emission Spectrometry (ICP-OES). Water-soluble ionic species were determined using Ion Chromatography. The results show that the concentration range of the CP and FP fractions varied from 1.17 to 28.45 μg/m3 and from 3.82 to 35.58 µg/m3 with mean concentrations (n = 80) of 10.41 ± 5.40 µg/m3 and 14.31 ± 6.53 µg/m3, respectively. On average, the measured chemical species accounted ca. 54% of the coarse particles and 32% of the fine ones. Na+, SO42–, Cl–, NO3–, Al, Ca, Fe, K and Na were mainly in the coarse particle size range and accounted for ca. 52% of the coarse particle mass, while SO42–, NH4+, K+, Al, Ca, K and Na were mainly in fine particle size range and accounted for ca. 28% of the fine particle mass. The data sets were then analyzed using Principle Component Analysis (PCA) to identify the possible sources of these fine and coarse particles based on their chemical species. For both fractions, the sources were soil dust, marine aerosol, vehicle exhaust, secondary aerosol, road dust and biomass burning. In addition, crustal enrichment factors (cEF) were calculated, and the results were consistent with those of the PCA analysis.