A comparative study of five methods measuring suspended sediment or solid concentrations in water–sediment mixtures indicated that, depending on the method used, broadly varying results can be obtained. For water–sediment mixtures containing sand size particles, the standard TSS method produced negatively biased results, accounting for 0 to 90% of the present solids; the negative bias directly depended on the magnitude of the sand fraction in the water–sediment mixture. The main reason for the differences between the TSS and the rest of the methods laid in the handling of samples; in the former methods, whole samples were analysed, whereas the TSS analysis was performed on sub-samples withdrawn from the water sample, the withdrawal process tending to exclude large particles. The methods using whole water–solid samples, rather than aliquots withdrawn from such samples, produced accurate estimates of solid concentrations, with a fairly good precision. Two whole-sample methods were studied in detail, a slightly modified standard SSC-B method and the newly proposed operational procedure referred to as the Multiple Filter Procedure (MFP), using three filters arranged in a series with decreasing pore sizes (25, 1.6 and 0.45 µm). Both methods assessed accurately concentrations of solids in a broad range of concentrations (200–8000 mg L⁻¹) and particle sizes (0.063–4.0 mm). The newly introduced MFP was in good agreement with the SSC procedure, the differences between the two procedures not exceeding the standard bias defined for the SSC-B method. The precision of both SSC and MFP was generally better than ±10%. Consequently, these methods should be used when the total mass of transported solids is of interest.