In this paper, the adsorption process of methylene blue has been investigated on microcline particles as a function of particle size and temperature. The characterization of microcline in the particle size ranges of 1−71 μm and 71−315 μm gained by sieving was proved using X-ray diffraction (XRD) and scanning electron microscopy combined with energy-dispersive detector (SEM-EDS) in powder form, over laser diffraction measurements in aqueous suspension. The optimum dosage of adsorbent was 13.5 g/L in dye adsorption and the adsorption isotherms on both microcline size fractions were determined at this adsorbent concentration. The maximum adsorption capacities were in the range of 1.5–3.1 mg g−1 on microcline particles with supplementing evaluation of isotherms using the Langmuir model. Considering the problems of linearization of equations, the non-linear least-squares estimation can be strongly recommended for modeling adsorption-equilibrium. The adsorption isotherm determined at elevated temperature of 60−65 °C represents a breakpoint at around 20 mg L−1 of equilibrated dye concentration due to performing of a potential process of dye self-association. According to our experiments, the increase in temperature has an adverse effect on adsorption.