<p>In this study, we employ an optimization approach for removing cadmium (Cd) and lead (Pb) from aqueous solutions using clay, nanoclay, and magnetic nanocomposite adsorbents. The experimental design was based on the Taguchi method by considering 5 factors: 1- adsorbent type (TA), 2- initial concentration (C) of contaminating metals, 3- adsorbent dosage (D), 4- pH (P), and 5- temperature (T), each of which was considered at 4 levels in the experiment. Based on the results of the ANOVA analysis, the adsorption capacity of Cd and Pb ions was mainly influenced by the initial concentration (56–57%) and the adsorbent dose (35–36%), while pH and temperature had a minimal effect of less than 2%, and the type of adsorbent contributed a small percentage of 4%. By optimizing the metal ion adsorption process the best conditions for Cd were as follows: TA = nanoclay, C = 200 mg L⁻¹, D = 1.6 g L⁻¹, P = 10, and T = 45 °C, and for Pb: TA = clay, C = 200 mg L⁻¹, D = 1.6 g L⁻¹, P = 10, and T = 35 °C. Based on the studied properties of the adsorbents, including FTIR spectra, measurements of specific surface area and SEM and TEM images, clay and nanoclay have been identified as two promising adsorbents for the adsorption of Cd and Pb from solution.</p>