A novel method used to synthesize diacetone diperoxide (DADP) from acetone and hydrogen peroxide without the presence of a catalytic agent is presented. Previously reported syntheses used toluenesulfonic and m-sulfonic acid as catalyst. DADP was prepared with a purity of 99.99?%. The melting point range (128.5134.5?degrees C) is consistent with reported values. The success of the reported procedure depends on controlling the ratio between acetone and hydrogen peroxide as well as the temperature of the reaction mixture. The purified crystalline DADP samples were characterized using NMR, Raman, and IR spectroscopy, differential scanning calorimetry, gas chromatography and open atmosphere chemical ionization mass spectrometry (DART (TM)). The structure was compared to the well-known cyclic trimer triacetone triperoxide (TATP). The proposed synthetic scheme can be useful for preparing small amounts of the cyclic organic peroxide for characterization and fundamental studies and for formulation of gas chromatography, high performance liquid chromatography, and mass spectrometry standards.