Currently there is a need for specialized pyrotechnic materials to combat the threat of biological weapons. Materials have been characterized based on their potential to produce heat and molecular iodine gas (I2) to kill spore‐forming bacteria (e. g. anthrax). One formulation, already proven to kill anthrax simulants, is diiodine pentoxide with aluminum; however, it suffers from poor stability and storage problems. The heat and iodine gas output from this mixture and candidate replacement mixtures were measured with bomb calorimetry and extraction and analysis of I2 by UV‐Vis. Of the mixtures analyzed, calcium iodate and aluminum was found to be the highest producer of I2. The heat output of this mixture and others can be tuned by adding more fuel, with the cost of some iodine. Products of combustion were analyzed by thermal analysis (SDT), XPS, XRD, and LC/MS. Evidence for various metal iodides and metal oxides was collected with these methods.

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The hexanitrates of the six‐carbon sugars mannitol and sorbitol were prepared and studied to gain insight in their relative stabilities. Synthesis and characterization of these materials resulted in the identification of two new crystalline polymorphs, one for each hexanitrate. Mannitol hexanitrate (MHN) exposed to elevated temperatures exhibited a different structure when measured by x‐ray diffraction (XRD) and Raman spectroscopy; however, no differences were observed in the thermal behavior. Sorbitol hexanitrate (SHN) has two distinct crystalline polymorphs that result in different melting behavior and differences in Raman and XRD. Thermal stability of these hexanitrates was also examined; despite being isomers, SHN and MHN differ in their long‐term thermal stability.