Fibrous polymers having an excellent heat resistance were successfully introduced as the stationary phase in capillary gas chromatography (GC) and the basic separation performance has been investigated. Poly( p phenylene 26 benzobisoxazole); Zylon, fibers were selected as the stationary phase taking into account the chemical structure, heat resistance, solvent resistance and the physical strength. About 330 filaments of the polymer were packed longitudinally into fused silica capillaries of 0 32 mm i.d. , and the GC separation of several test mixtures, such as n alkylbenzenes and n alkanes was carried out with these fiber packed capillary columns. From the results it has been demonstrated that the fiber packed capillary columns have a great potential as the separation media for volatile compounds. Polymer coating onto the surface of the packed filaments has been also studied, and the results clearly showed that the retentivity was significantly improved over a conventional capillary columns of the same length and that the selectivity can be tuned by selecting different types of coating materials selected for the purposes. The applications of polymer coated fiber packed capillary as a miniaturized sample preparation device was also investigated for the analysis of environmental pollutants in river water samples. Fibrous polymers having an excellent heat resistance were successfully introduced as the stationary phase in capillary gas chromatography (GC) and the basic separation performance has been investigated. Poly (p phenylene 26 benzobisoxazole); Zylon, fibers were selected as the stationary phase taking into account the chemical structure, heat resistance, solvent resistance and the physical strength. About 330 filaments of the polymer were packed longitudinally into fused silica capillaries of 0 32 mm id, and the GC separation of several test mixtures, such as n alkylbenzenes and n alkanes was carried out with these fibers packed capillary columns. From the results it has been demonstrated that the fiber packed capillary columns have a great potential as the separation media for volatile compounds. Polymer coating onto the surface of the packed filaments has been also studied, and the results clearly showed that the retentivity was significantly improved ove ra conventional capillary columns of the same length and that the selectivity can be tuned by selecting different types of coating materials selected for the purposes. The applications of polymer coated fiber packed capillary as a miniaturized sample preparation device was also investigated for the analysis of environmental pollutants in river water samples.