In environmental analysis, some samples may be dissimilar to previously characterized materials. These samples may contain elemental concentrations that are difficult to determine by X-ray fluorescence due to the unavailability of appropriate certified reference materials. This work reports the elemental analysis of aquatic plants by X-ray fluorescence without suitable certified reference materials. Synthetic calibration standards were prepared that approximated the concentrations in the samples. The suitability of this approach was characterized by comparison of X-ray fluorescence results with atomic absorption spectrometry measurements. The concentrations of magnesium, aluminum, silicon, calcium, titanium, chromium, manganese, iron, nickel, copper, and strontium were determined in aquatic plants from the Bratsk Reservoir, Irkutsk, Russia. The concentrations were high and exceeded typical values in terrestrial plants.