Development And Certification Of Explosive Candidate Reference Materialfor DAAF And DAOAF

3,3'-diamino-4,4'-azofurazan(DAAF)and 3,3'-diamino-4,4'-azoxyfurazan(DAOAF)are a novel high energy materials with high energy density.They have wide application prospect in initiation explosive at slapper detonator,high performance propellant and low signature propellant due to their fascinating properties.However,there is no reference material for DAAF and DAOAF on the market.Lack of reference material restricts the development of analytical technology,and corresponding product quality can not be effectively controlled.It is urgent to study the development and certification of explosive reference material in order to ensure the accuracy of value transmission and traceability in production and application for DAAF and DAOAF.The main contents in this thesis are summarized as below:3,4-diaminofurazan(DAF)was prepared with aqueous glyoxal,hydroxylamine and sodium hydroxide by only one step under atmospheric pressure.Crude product of candidate reference material for DAAF and DAOAF were prepared from DAF with oxidation reaction in the presence of oxidants.The effect of the reaction time,the reaction temperature,the ratio of the reactants and so on have been studied systematically and optimized,and optimal process parameters were obtained though technical studies.The structure of compound was characterized by IR,NMR spectra and MS.Impurities of crude product of candidate reference material for DAAF and DAOAF were characterized.A high performance liquid chromatography to analyze crude product of candidate reference material was established and characterization of impurities trapped in DAAF and DAOAF product were carried out by MS.The analytical method of trace ionic impurity was established using ion chromatography.Inductively coupled plasma was developed for inorganic metal impurity elements.Crude product of candidate reference material for DAAF and DAOAF were purified by using recrystallization technology.The purity of candidate reference material was determined by mass balance method,as well as the homogeneity and stability was estimated by high performance liquid chromatography method.The thermal property of candidate reference material for DAAF and DAOAF was studied.Thermal decomposition behavior of DAAF and DAOAF was studied by thermogravimetric/differential thermal gravity analysis(TG-DTG)and differential scanning calorimeter(DSC),and the kinetic parameters for thermal decomposition were calculated by Kissinger method and Flynn-Wall-Ozawa method.The specific heat capacity of DAAF and DAOAF was determined using continuous specific heat capacity modes of a DSC apparatus.The combustion energy of DAAF and DAOAF was measured by a precise IKA C5000 oxygen-bomb calorimeter.Standard molar enthalpy of combustion(?cH?m),standard molar enthalpy of formation(?fH?m)relative to the standard temperature 298.15 K were calculated.