A new separation method based on a combination of coagulation and colum flotation was used to treat fine sphalerite in the range 90 per cent - 15 pm with a relative high superfical gas velocity and a thick froth layer. Minerals studied include sphalerite, calcite, kaolinite and baryte. A new developed sedimentometer was used for sedimentation analysis to characterise hetercoagulation of mixture and coagulation after addition of active ions or reagents. A comparison between use of selective frother and depressant (SHMP) was made to deactivate activated minerals. Selectivity of frother for sphalerite was found in flotation test. The depression function of Flotanol for activated minerals was confirmed in sedimentation alalysis. The use of small quantities of HPAM can improve the flotation of fine sized sphalerite particle and reduce recovery of activated gangue minerals in the neutral or alkaline pulp. A satisfactory separation of fine sphalerite from its gangue was achieved by using alkylpolyglycolether (Flotanol) and copolymer polyacrylamide (HPAM hydrolysed polyacrylamide) as frothing and flocculating agents Respectively.