Compared with the existing methods of analyses a quick and more reliable procedure has been developed to determine the bitumen, solvent, water and solids content of mineral wastes, in order to serve efficiently both plant operations and research needs. Bitumen and hydrocarbon solvent in the samples are extracted using solvents that do not absorb in the CH₃ group region of the ¹H NMR spectrum. Bitumen is then determined spectrophotometrically, and the process solvent by quantitative ¹H NMR. Water is dissolved in methanol and subsequently determined using a Karl Fischer titrator. Solids are measured gravimetrically. This procedure was used to analyse mineral tailings from the centrifuge stage of the hot water process for the extraction of bitumen from oil sands. Results for all four components; bitumen, process solvent, water and solids, had relative standard deviations much lower than the ones obtained using a modified Dean-Stark method. Mineral agglomerates obtained after the extraction of bitumen from oil sands using the solvent extration-spherical agglomeration method, were also analyzed by both methods. As a result of compaction occurring during solids agglomeration, complete extraction of bitumen by the Dean-Stark method could not be achieved. Extraction of bitumen and precision of results were much improved for agglomerated samples using the proposed method of analysis which is amenable to wastes containing solids, water, bitumen and solvent in any proportion.