The article presents the results of hydrochemical and geochemical sampling of 10 solonchaks in the western Aral Sea region, with determination of lithium concentrations. The methodology used to investigate surface brines involves identifying salt flat areas through visual interpretation of remote sensing data, fieldwork, and laboratory analyses for lithium detection. Lithium content was determined by atomic emission spectroscopy and atomic absorption analysis. A total of 68 brine samples were analyzed: in 41 samples, the lithium concentration ranged from 1 to 10 mg/L, and in 27 samples, from 10 to 20 mg/L. Additionally, 63 samples of salts, silt, and loams were analyzed, in which the lithium content ranged from 1 to 30 g/t; only in 12 samples did this value exceed 30 g/t. Based on the sampling results, the Kitbay and Eastern Koshkarata solonchaks were identified as having relatively elevated lithium concentrations, substantiating the need for further exploration and appraisal studies in the Aral Sea region to identify a new hydromineral type of lithium raw material. This study is relevant to Kazakhstan in the context of assessing the lithium resource potential of brines in the Aral Sea region and opens up new prospects for their further investigation.