For the first time this theses full evaporation technique was combined with single-drop micro extraction using air-agitated liquid-liquid microextraction based on solidification floating organic droplet as pre-concentration For determination of low molecular weight chlorobenzenes in effluent sample by gas chromatography-electron capture detector (GC-ECD) . In full evaporation technique, analytes are completely transferred to gas phase so the influences of salt, buffer and stirring speed as extraction parameters are eliminated. This technique results in reducing memory effect and getting moresimple. The preconcentration step is intended to reduce the limit of detection, both by removal of interferences and by increasing of the concentration of the analytes. The proposed method was initially optimized and the optimum experimental conditions found were: 250?l cyclohexane was injected rapidly into aqueous sample then the mixture was 8 times aspirated and dispensed using a syringe, and by enlarging the surface area between the donor and acceptor phases, after preconcentration 2.5 ?l hexadecane micro drop exposed for 25 minutes into steam phase of a 7.5 ?l sample in 8ml vial with at 50?.The calculated calibration curves gave a high level of linearity for all target analytes with correlation coefficients ranging between 0.9993 and 0.9996. The repeatability of the proposed method, expressed as relative standard deviation varied between 7.2 and 9.3% (n = 3). The limits of detection ranged between 0.003 and 0.006 ?g/l using GC–ECD
