There are no unified MPCs for wastewater; therefore, we analyzed more than 70 wastewater samples with high concentrations of nitrogen to evaluate the possibility of determining the actual concentrations of alkylamines. Additional peaks interfering with the identification of the target components were not found in any of the cases. At the same time, methylamine and dimethylamine were detected in several wastewater samples (Table 2). Figure 2 demonstrates a typical electropherogram of a wastewater sample after the distillation of analytes with water steam. To assess the accuracy of the results, the standard addition method was used. A known volume of a reference solution of a mixture of alkylamines was added to test samples of potable water and wastewater. Then, the described sample preparation was performed followed by the analysis of the resulting solution by capillary electrophoresis. The results of determination of alkylamines without additions and with additions of reference solutions (Table 3) show the high accuracy of the results obtained.