This study investigates unique weathering crust samples from the most altered sections (30-43 m) of the weathering profile within the Souktal Plutonic Complex, Northern Kazakhstan. The samples, obtained from two drill cores, consist of quartz, kaolinite, microcline, muscovite, and plagioclase, as identified through polarized light microscopy and confirmed by X-ray diffraction analysis. Sequential extraction of rare earth elements (REE) was performed using inductively coupled plasma mass spectrometry (ICP-MS) following a two-step leaching procedure with hydroxylamine hydrochloride (0.2 mol NH₂OH·HCl) and sodium hydroxide (1 mol NaOH) solutions. The extraction process effectively recovered REE, indicating their presence in an ion-exchangeable form, with total extraction rates (REE + Sc + Y) ranging from 4.1 to 7.8 ppm. The total light REE content varies from 3.5 to 5.9 ppm, while heavy REE content ranges from 0.2 to 0.7 ppm across all samples. Petrological and geochemical analyses suggest that the studied area represents an ion-adsorption-type REE weathered deposit. These findings enhance the understanding of ionic-adsorbed REE within weathering crusts and highlight the effectiveness of sequential extraction methods for REE determination. Moreover, the study suggests that this area holds promising potential as a future REE ion-adsorption site, contributing to the development of Kazakhstan’s national REE industry.