A new, simple and cheap dispersive liquid-liquid microextraction (DLLME) procedure was optimized for the preconcentration of trace amounts of Ni(II) as a prior step to its determination by flame atomic absorption spectrometry (FAAS). It is based on the microextraction of nickel, where appropriate amounts of the extraction solvent (CHCl3), disperser solvent (ethanol) and chelating agent, name 5-[(Z)-isoxazol-3-yl-diazenyl]-2-methyl-quinolin-8-ol (MMD), were firstly synthesized/characterized and used. Various parameters that affect the extraction procedure such as pH, centrifugation rate and time, the chelating agent (MMD) concentration and sampling volume on the recovery of Ni(II) were investigated. The preconcentration of a 20 ml sample solution was thus enhanced by a factor of 80. The resulting calibration graph was linear in the range of 0.24-10 mg L-1 with a correlation coefficient of 0.9998. The limit of detection (3 s/b) obtained under optimal conditions was 1.00 mu g L-1. The relative standard deviation for certified reference material determinations was 1.2%. The accuracy of the method was verified by the determination of Ni(II) in the certified reference material of wastewater (Waste water CWW TMD). The proposed procedure was successfully applied to the determination of Ni(II) in some fake jewelry and cosmetics samples.