Preparation of dinitro pentamethylene tetramine (DPT) through the action of nitrating mixture formed of ammonium nitrate and fuming nitric acid on hexamine in presence of acetic acid, acetic anhydride and p-formaldehyde has been carried out. DPT was also prepared from hexamine dinitrate which is an important intermediate appears through preparation of DPT from hexamine directly. Prepared DPT was purified and then characterized through the determination of melting point, element test, FTIR spectrometry, UV spectrometry, and high performance liquid chromatography "HPLC". The obtained results were reliable and consistent with the literature.