The post-synthesis treatment of AlZSM-5 and GaZSM-5 zeolites by etching with buffer solution of ammonium fluoride and 0.25 M HF acid was carried out. The treatment is applied in order to obtain secondary pores in crystals and to provide easier access to the catalytically active zeolite centers. Hydrothermal synthesis of these zeolites was performed from systems containing tetrapropylammonium bromide as a template. The reaction parameters of synthesis conditions for both zeolites were optimized in order to obtain pure crystalline phases. The zeolites obtained were characterized by X-ray diffraction, IR spectroscopy, scanning electron microscopy, physical adsorption-desorption of nitrogen and solid-state NMR spectroscopy. It has been found that the result materials remain with high crystallinity while new mesoporous are created in their structure. The volume due to the presence of mesopores increases by up to 67% from the total volume, which is a drastic increase compared with the parent solids. The investigations with FTIR spectroscopy of low-temperature CO adsorption and solid-state NMR spectroscopy show that the treatment is slightly selective toward dissolution of heteroatom (aluminum or gallium). This phenomenon is observed for the first time for gallium-substituted zeolites. In order to study the influence of the metal atom in zeolite structure and the efficacy of the acid attack on the catalytic activity, the samples obtained were tested in reaction of m-xylene and toluene transformation. [GRAPHICS] .