Three liquid crystals (LCs) of different polarities were prepared, characterized and applied as stationary phase in gas chromatography by their coating on chromosorb pink acid washed (P AW) with thickness film 20%. The prepared liquid crystals are Triton x 100-CH3COOH (H1), Triton x 100-KCl (H2) and CTAB-KCl (I1). LCs was characterized by thermal analyzer via differential thermal analysis (DTA) and thermo gravimetric analysis (TGA), in addition to scanning electron microscope (SEM). It has been found that, their maximum recommended temperatures are 200°C. The chromatographic characterization, polarity through McReynolds scheme, selectivity through criterion scheme and efficiency of separation through resolution were studied via inverse gas chromatography. H1 exhibits highest polarity and most selective toward polar compounds compared with the other two LCs, this was compatible with its high efficiency of gas chromatographic separation of alcohol compounds. I1 shows the lowest polarity and less selective stationary phase toward polar solutes than other two LCs, but it has high criterion value using saturated hydrocarbons as solutes, this was reflected on the separation of saturated hydrocarbons giving good separation followed by aromatic hydrocarbons.