Two novel environmentally friendly fluorinated surfactants, disodium monofluoroalkyl phosphates were synthesized using phosphorus pentoxide, i.e. H(CF 2 ) 6 CH 2 OPO(ONa) 2 and H(CF 2 ) 6 CH 2 OCH 2 CH 2 OPO(ONa) 2 . The novel synthesized fluorinated surfactants have a high thermal stability on the basis of Thermogravimetric Analysis. Their surface properties were also examined with the aim to have similar surface tensions of dilute aqueous solutions when compared with the conventional fluorocarbon surfactants, ammonium perfluorooctanoate. The two synthesized monofluoroalkyl phosphates can respectively reduce the surface tension of water to 23.73 mN/m at 78.3 mmol/L and 21.38 mN/m at 20.93 mmol/L. In addition, the Krafft points are both below 0°C.