Fluorinated methylsiloxanes are modified methylsiloxanes and include tris(trifluoropropyl)trimethylcyclotrisiloxane (D3F) and tetrakis(trifluoropropyl)tetramethylcyclotetrasiloxane (D4F). Here, we report fluorinated methylsiloxanes (D3F and D4F) in surface water and sediment samples collected near a fluorinated methylsiloxane manufacturing plant in Weihai, China. The concentrations of D3F and D4F in surface water ranged from 3.29-291 ng/L and from 7.02-168 ng/L, respectively. The concentrations of D3F and D4F in sediment ranged from 11.8-5478 ng/g and from 17.2-6277 ng/g, respectively. In simulation experiment, the half-lives of D3F and D4F at different pH values (5.2, 6.4, 7.2, 8.3, and 9.2) varied from 80.6-154 h and from 267-533 h, respectively. CF3(CH2)2MeSi(OH)2 was identified as one of the main hydrolysis products of fluorinated methylsiloxanes. It was also detected in the river samples at concentrations of 72.1-182.9 ng/L. In addition, the slow rearrangement of D3F (spiked concentration = 500 ng/L) to D4F (concentration = 11.0-22.7 ng/L) was also found during 336h hydrolysis experiment.