This study aimed to introduce non-parametric tests and guard bands to assess the compliance of some river water properties with Brazilian environmental regulations. Due to the heterogeneity of the measurands pH, Biochemical Oxygen Demand (BOD), manganese molar concentration, and Escherichia coli, which could be wrongly treated as outliers, as well as the non-Gaussian data, robust methods were used to calculate the measurement uncertainty. Next, based on guard bands, the compliance assessment was evaluated using this previous uncertainty information. For these four measurands, partial overlaps between their uncertainties and the specification limit could generate doubts about compliance. The non-parametric approach for calculating the uncertainty connected to the guard bands concept classified pH and BOD as “conform”, with a risk to the consumer of up to 4.0% and 4.9%, respectively; in contrast, manganese molar concentration and Escherichia coli were “not conform”, with a risk to the consumer of up to 25% and 7.4%, respectively. The methodology proposed was satisfactory because it considered the natural heterogeneity of data with non-Gaussian behavior instead of wrongly excluding outliers. In an unprecedented way, two connected statistical approaches shed light on the measurement uncertainty in compliance assessment of water analysis.