The decrease in Aral Sea area, which started in the 1960s, caused considerable changes in the hydrological, chemical, and biological structure of sea water. Regular observations of Aral water chemistry ceased in the early 1990s. There were no observations of the concentrations of biogenic element compounds in water (the so-called "first-day analyses"). During expeditions of the Institute of Oceanology, RAS, in September 2012 and October 2013, integrated hydrochemical observations were carried out, including measuring the concentrations of biogenic element compounds, dissolved oxygen, hydrogen sulfide, and carbonate equilibrium components. An objective of this study was to develop methods of hydrochemical studies under high water salinity (mineralization). In addition to the standard hydrochemical complex, water samples were taken to determine total water mineralization and the concentration of dissolved and suspended metal forms. The results of these studies are given.