A bismuth pre-concentration and determination system implemented with inductively coupled plasma atomic emission spectrometry (ICP-AES) associated with a flow-injection (FI) method with an ultrasonic nebulization system was studied. For the retention and on-line pre-concentration of bismuth, quinolin-8-ol and Amberlite XAD-7 were used at pH 5.0. The bismuth complex was removed from the micro-column with nitric acid. The detection limit for the pre-concentration of 100 ml of aqueous solution was 0.03 ng ml ^–1 with a relative standard deviation (RSD) of 2.5%, calculated with the peak heights obtained. The RSD for the human urine samples were between 1 and 5%. This reflects the cumulative imprecision of all the process. The calibration graph using the pre-concentration system for bismuth was linear with a correlation coefficient of 0.9991 at levels near the detection limits up to at least 100 ng ml ^–1 . The method was succesfully applied to the determination of bismuth in human urine samples digested previously with a mixture of H ₂ O ₂ and HNO ₃ .