In this paper, the natural sand grains were modified by wet modification with acetic acid, and the modified sand grains obtained were used as sorbent in the micro solid-phase adsorption column. The atomic absorption spectrometry (AAS) as the detection method was connected to the micro-column, and the adsorption behavior of lead ions on the modified sand grains in the column was analyzed. At the same time the adsorption conditions were optimized. Identification of the surface modification characterized and performed based on FTIR and SEM. The results showed that the saturated adsorption of the modified sand grains for lead ions was superior to that of natural sand grains. The saturated adsorption of the modified sand grains reached 28.7 mg·g-1 under the following condition, including the size of the grains was 38～74 μm, the sample pH was about 6, the loading flow rate of the solution through the micro-column was 1.5 mL·min-1, the adsorption temperature was room temperature. The adsorption capacity of lead ions on modified sand grains increased by 13%, and the adsorption rate could reach 92.6%. Different concentrations of HCl, H2SO4, and HNO3 dilute solutions were selected for desorption experiments, and the experimental results showed that the desorption effect of 0.01 mol·L-1 hydrochloric acid solution is good, so that 0.01 mol·L-1 HCl solution was selected as the best desorption agent. The desorption rate reached 97.3% under optimal conditions.