In this study, we tried to put the super-hydrophobic surfaces as stationary phase in the packed column. methyl isobutyl ketone (MIBK) and 4-Heptanone (4-HEP) that both in ion mobility spectrometer with corona ionization source (CD-IMS) has overlapping peaks, was used as the analyte. To prepare column, Teflon tube with a length of 20 cm and to fill it copper particles with 40-20 mesh prepared by grinding methods were used. To prepare a packed column, the Teflon tube and copper particles prepared by grinding method was used. Alkaline and oxidizing solution of the sodium hydroxide (NaOH) and ammonium persulfate (NH 4 S 2 O 8 ) in deionized water were used to produce nanostructured surface on copper particle. Oxidizing solution by a syringe pump at a rate of 800 ?/min was passed through the column. After washing the nanostructure surface with deionized water and drying under nitrogen gas flow,by passing ethanol solution of stearic acid through the column, nano-structure surface was functionalized and super-hydrophobic surface was obtained. Column to connect to the device and perform separation insert between the injection port and IMS cell. Separation process to a single temperature and at 150 ° C was performed. Then, filler particle size and column length was optimized. Finally to validate the method, a solution of a mixture of two compounds with known concentrations, injected to CD-IMS device and column connected to it. The percentage of error for measuring analytes in two different solutions was below 5%.