An HPLC Method For Analysis Of HBIW In Its Crude Product

Energetic compoundhexanitrohexaazaisowurtzitane (HNIW) has been employed inseveral applications, propellants compositions, energetic binder explosive.Hexabenzylhexaazaisowurtzitane(HBIW)is the first precursor of synthesizing HNIWand directly affects the efficacy of the hydrogenolysis reaction. So for laboratory workas well as for production control it is of great importance to establish analyticalmeasures to determine the concentration of HBIW.The synthesis of hexabenzylhexaazaisowurtzitane(HBIW) is performed by thefacile condensation of glyoxal with benzylamine. An important step in the synthesisof HNIW is the hydrogenolysis of the chemical intermediate. An improvement to thehydrogenolysis of HBIW would represent an improvement in the overall synthesis ofHNIW.Many by-products in HBIW can cause catalyst poisoning which reduces thehydrogenolysis reaction efficiency and even inhibits it run. The HBIW concentrationof the crude products directly affects the efficacy of the hydrogenolysis reaction.A new high performance liquid chromatography (HPLC) method was developed toquantify Hexabenzylhexaazaisowurtzitane (HBIW) utilizing different HBIW crudeproducts obtained from independent distributors. Chromatographic separation of thetarget ingredient was achieved by reversed phase C18column and isocratic elution oftetrahydrofuran and distilled water. Quantification of the analyte was achieved usingultraviolet detection at a wavelength of241nm.The plot of concentration versus peakarea was linear over the range of0.2-1.0mg/mL with correlation coefficient (r2=0.999).The precisions were achieved with RSD values lower than1.99%and the accuracyvalues(RE) were lower than4.54%for HBIW of the quality control samples at0.2,0.6,1.0mg/mL.The analysis of four selected HBIW crude products was performed in this study.The results of the analysis exhibit variability in HBIW content of its crudeproducts.The content of HBIW ranged from84.55%to95.28%which is consistentwith the results obtained by speculating according to the samples’ melting point.The ability to determine the concentration of HBIW is helpful in understanding theefficiency of synthesizing HBIW and determining whether the next reaction ofcatalytic hydrogenolysis, an important step in the synthesis of (hexanetrohexaazaiso-wurtzitane) HNIW, will go.