1,3,3-Trinitroazetidine (TNAZ) has been prepared at a laboratory scale in HEMRL. The structure of the compound has been confirmed by IR, NMR. mass. elemental analysis and by X-ray crystallography. HPLC technique has been employed to confirm the purity of TNAZ (>99%). The compound is further characterized by thermal techniques and is found to undergo limited decomposition at its melting point. Small scale sensitivity tests have also been carried out and the results show that TNAZ is significantly more sensitive to mechanical stimuli than TNT. (C) 2004 Elsevier B.V. All rights reserved.