This study presents a new method for the determination of nickel in aqueous samples by slotted quartz tube-flame atomic absorption spectrometry (SQT-FAAS) after a dispersive assisted simultaneous complexation and extraction (DASCE) process. Synthesized ligand was directly dissolved in the extraction solvent to eliminate the complex formation step prior to the extraction. All parameters of the SQT-FAAS and DASCE method were systematically optimized to improve the detection power of nickel for trace determinations. Under the optimum experimental conditions, the optimized method (DASCE-SQT-FAAS) recorded 137-fold enhancement in detection power over the conventional FAAS. The limits of detection and quantification were determined to be 1.6 mu g/L and 5.2 mu g/L, respectively. The calibration plot was linear over a wide concentration range and the precision for replicate measurements was appreciably high. Nickel was not detected in five different water samples but spiked recovery tests for three samples yielded results that were close to 100%, confirming the method's accuracy and applicability to the matrices tested.