An experiment on water discharge gauging and suspended sediment sampling performed in the Amazon River basin on 24 March 1995, during a rising-water period is described. The experiment involved different devices, including an Acoustic Doppler Current Profiler (ADCP) for water discharge measurements. From the different samplers used, one specially built for the HiBAm project was tested successfully. An attempted use of the relationship between the ADCP signal and the total suspended sediment (TSS) was performed for sediment yield calculations. Different calculation methods were used with the TSS data obtained by the samplers and the results are discussed. The mean water discharge (Q) and TSS sediment yield (Qs) results were 172 400 m3 s-1 and 3.15 × 106 t day-1, respectively. A relationship between the Qs value at depth and the surface Qs value is also proposed.