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Bio-matrix of rice husk and Mobil Composition of Matter No. 41 (MCM-41) was modified with alizarin red S for preconcentration of Pd2+ prior flame atomic absorption spectrometric determination. The prepared bio-matrix (RH@MCM-41@ARS) was characterized by Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), transmission electron microscope (TEM), scanning electron microscope, energy dispersive X-ray spectrometer (SEM/EDX) and surface area studies. The impact of different parameters (solution pH, amount of sorbent, contact time, sample volume, initial Pd2+ concentration and diverse ions) on the uptake of Pd2+ were evaluated. The maximum adsorption capacity of Pd2+ onto RH@MCM-41@ARS was 198.2 mg g−1 at optimum conditions. Applying the optimized procedure as a preconcentration step led to limit of detection of 0.13 μg L−1 and dynamic analytical range up to 500 μg L−1. The sorbent was regenerated by 0.5 mol L−1 thiourea for at least 10 cycles without significant reduction of adsorption capacity. The method was applied for preconcentration of Pd2+ from real samples.