tThe increasing use of platinum group metals, PGMs (e.g. platinum, palladium and rhodium) in catalyticconverters and the increasing mining activities for these metals in South Africa, has increased the presenceof these metals in the aquatic environment. For this reason, the developments of sensitive detection tech-niques for metal ions in environmental samples have been investigated in this study. The work reportedin this paper describes the development of an adsorptive differential pulse stripping voltammetric proce-dure for the determination of palladium (Pd), platinum (Pt) and rhodium (Rh) in environmental samplescollected from rivers in close proximity to mining activities in South Africa. A screen-printed carbonelectrode coated with a bismuth film, SPCE/BiF was constructed. The optimisation of the experimentalconditions performed, included an appropriate buffer solution for coating and the supporting electrolytesolution. The voltammetric procedure included pre-concentration of the metals using dimethylglyoxime(DMG) as chelating agent, followed by adsorptive differential pulse stripping voltammetry (AdDPSV)at appropriate deposition potentials for each of Pd, Pt and Rh. Other essential stripping voltammet-ric parameters optimised included the DMG concentration, composition of the supporting electrolyte,pH, deposition time, and deposition potential. Interference studies in the presence of Ni and Co havealso been conducted and showed promising results. The results obtained for this investigation haveshown that the detection limits of 0.008 �g/L, 0.006 �g/L and 0.005 �g/L were obtained for Pd(II), Pt(II)and Rh(III) determination respectively, using the SPCE/BiF sensor. The results obtained for Pd(II) deter-mination of freshwater samples have shown that the concentration of Pd(II) in these samples rangedbetween 2.56–5.17 ± 0.41 ppb (n = 3). The results obtained for the Pt(II) concentrations ranged between0.41–0.71 ± 0.17 ppb (n = 3). In the case of the Rh(III) determination, it was found to be 0.14–0.38 ± 0.07ppb (n = 3). It was therefore concluded that the performance of the SPCE/BiF sensor was found to be moresensitive than the GCE/BiF sensor constructed in our laboratory in a previous study. It was further estab-lished that the SPCE/BiFE sensor delivers more sensitive results in ammonia buffer (pH = 9.2) solution,compared to acetate buffer (pH = 4.8) solution.