Studies have shown that sonochemical synthesis (as effect of ultrasound cavitation) is extremely effective. The power of ultrasound has expanded outside of chemical synthesis since scientists and industry found wider applications for ultrasound technologies. Due to this reason, today it is completely understandable that application of ultrasound is widely represented (for example: in physics, biology, chemistry, pharmacy, medical diagnostics and surgery, as well in the food-processing industry and cosmetic industries). In this experimental work, hydroxyquinolinic acid reactions with zinc(II) and cobalt(II) cations have been explored and studied. Series of hydroxyquinolinic acid and transition metal salts water solutions were prepared within certain pH value in order to obtain metal complexes. Synthesized compounds were characterized by infrared spectroscopy and thermogravimetric analysis. The structures of the compounds are suggested based on the obtained results.