ynchrotron radiation X-ray absorption near-edge structure(XANES) spectroscopy is a powerful method for nondestructive quantitative determination of elemental speciation.Sulfur K-edge XANES spectroscopy has been successfully used to characterize sulfur species in atmospheric particulate matter(PM).We tried to analyze the concentration of sulfur in PM using XANES combined with ion chromatography(IC).Different sulfur states and their percentage to total sulfur element in PM were conformed by analyzing the sulfur K-edge XANES spectra.The sulfur concentration under different states was obtained using the sulfur concentration in soluble SO42? divided by the percentage of +6 sulfur in PM.The XANES and IC analyses of atmospheric PM2.5 collected at five coastal sites in Shanghai revealed that sulfates(about 90%) was the dominating sulfur compound in the samples,while a few sulfonates(4.8%–6.5%) and di-and polysulfides(0%–6.8%) were detected.The concentration of total sulfur in the atmospheric PM2.5 is 3.60–6.38 μg.m?3.