A review of the different methodologies employed to fractionate and characterize riverine suspended particulate matter is presented. The importance of size-based metal speciation is underlined and the possibility of studying it by the Sedimentation Field Flow Fractionation (SdFFF) technique is illustrated. The studies on the metal load in river Suspended Particulate Matter (SPM) performed over the last ten years are critically reviewed focusing on the different methods employed to collect, concentrate and size-fractionate samples. The fact that there is no homogeneity in methods and data collection in this field is underlined. Among the different fractionation techniques, Field Flow Fractionation (FFF) methodologies have proved to be a good approach to study the role of SPM in metal load and transport. The possibility of studying size-based metal speciation using the SdFFF technique is presented and the importance of metal speciation in rivers is underlined.