In the present work, a ultrasound-assisted emulsification dispersive liquid-liquid microextraction based on solidification of floating organic droplet method has been developed as a sample preparation method prior to flame atomic absorption spectrometry determination of trace amounts of gold in the standard, wastewater and river water samples. In the proposed method, 1-dodecanol and 5-(4-dimethylamino-benzylidene) were used as extraction solvent and chelating agent, respectively. Several factors that may be affected on the extraction process, such as type and volume of the extraction solvent, ionic strength, pH of the aqueous solution, extraction temperature and extraction time were studied and optimized. Under the best experimental conditions, the calibration curve exhibited linearity over the range of 8.0 ng·mL −1 -3.0 µg·mL −1 with a correlation coefficient of 0.9978 and detection limit based on three times the standard deviation of the blank signal was 1.5 ng·mL −1 . Eight replicate determinations of 0.2 and 1.0 g·mL −1 of gold gave a mean absorbance of 0.051 and 0.253 with relative standard deviations of ±2.3% and ±1.5%, respectively. Finally, the developed method was successfully applied to the extraction and determination of gold ions in a silica ore, wastewater, river water and standard samples and satisfactory results were obtained.