A home made cryotrap device for the isolation of volatile organic sulphur compounds from aqueous solutions by means of purging followed by cryogenic preconcentration before introducing analytes into a chromatographic column has been tested. The system was optimized for a selection of sulphur compounds at ppb level with reference to type of cooling agent (suspension of CO2 in air or vapours of liquid nitrogen), purge time and film thickness of trap. The procedure was used for the determination of sulplur compounds in some environmental samples at ppt level. The stability of sulphur compounds investigated in water solutions was also evaluated.