In this research, insoluble poly (3-mercaptopropylsiloxane) was prepared by hydrolyzing mixture of tetraethoxysilane (TEOS) with 3-mercaptopropyl trimethoxysilane (MPTS) in the presence of a tin catalyst. Many products were pre pared using different mole ratios of TEOS to MPTS (i.e., 5:1, 2:1, 1:1, 1:2, and 1:5).The best mole ratio, which gives the highest metal uptake for the ligand was chosen for further evaluation. Then, the capability of this ligand in extraction of heavy metal ions (i.e., Pb 2+,Cu 2+,Ni 2+,Zn 2+,Hg 2+,and Cd 2+) from their solutions was determined at different pHs (2 ≤ pH ≤ 8). Atomic absorption and complexometric titrations were used for determination of metal content in metal ion solution.