This paper presents a study involving the development of a new mini polytetrafluoroethylene (PTFE) vessel project for biological sample preparation in micro scale in closed system with microwave radiation for subsequent determination of Cd, K, Mg and Na by atomic spectrometry techniques. All experiments were carried out in micro quantities of samples (up to 20 mg) and reagents (300 µL of HNO 3 ) for 5 min at 350 W. Certified reference materials of biological samples (bovine muscle and liver) were used to evaluate the accuracy of the proposed system and the results obtained were in agreement with the certified value at 95% of confidence (t-test). Relative standard deviations (RSD) were lower than 8.0% for all elements. The proposed method is not only easy and fast, but it is also based on the use of an inexpensive system for sample digestion.