Breakout Session 2 A

The Biazzi continuous process is an industrial nitration procedure to produce mass quantity of explosives since mid-1930. PETN (Pentaerthyritol tetranitrate) is one of the high explosives and the Biazzi continuous process is used by the explosives industry to produce PETN even in modern-day.
This analytical study looks at the purity of PETN made from the Biazzi continuous process. According to various published papers, the overall yield of PETN synthesis is generally greater than 95 %. Common impurities are PE, PE-tri-N (Nitrate), PE-di-N, PE-mono-N, dipentaerytritol hexanitrate, (di-PEHN) and tripentaerythritol octanitrate (tri-PEON). Some organic salts are also identified by Klassen (et al.). The industrial standard nitration procedure for explosives synthesis in mass quantities, including PETN, is the Biazzi continuous process. The PETN analyzed in this study was purchased from Austin-Powder® in 2018, and dried prior to headspace analysis. Headspace samples were collected using SPME fiber analyzed on a GC/MS and GC-Q-TOF/MS. Acetone and acetone-related impurities and amine-related impurities were found. These impurities presumably result from the materials utilized in the the Biazzi continuous process. The excess acetone forms diacetone alcohol (4-methyl-4-hydroxy-2-pentanone) by aldol condensation; mesityl oxide (4-methyl-3-penten-2-one) is subsequently produced by a dehydration reaction. In addition, triacetonamine (2,2,6,6-tetramethyl-4-piperidone) was identified from the PETN product. In order to verify the aldol condensation and dehydration reaction, acetone (6 mL), sulfuric acid (10 drops) and ammonium hydroxide (2 mL) solution were placed in a 50 mL beaker, separately, and the beakers were placed in a reaction vessel at the given conditions. SPME headspace samples were analyzed and the expected chemicals were confirmed: acetone, diacetone alcohol, diacetonamine, mesityl oxide, triacetonamine, 2,2,6,6-tetramethyl-4-acetoxylimino piperdine, and N-[3-methyl-2-butenyl dene] methanamine. Indeed, the experimental results show that the solvent residue and gaseous ammonia could be reacted to create a set of new chemical species, reducing the purity of PETN and thereby it can interfere with the biological olfactory detection systems.