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Detection of the Alpha and Gamma Polymorphs of HMX in Beta-HMX by Raman Spectroscopy.

DE88012867

Publication Date	1988
Personal Author	Holy, J. A.; Firsich, D. W.; Walters, R. R.
Page Count	7
Abstract	HMX (octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine) is an important military explosive which exhibits four polymorphic forms- alpha, beta, gamma, and delta. Commercial lots of this compound are analyzed for polymorphic composition in order to achieve predictable firing characteristics. This analysis may be done qualitatively with powder diffraction, while quantitative results are typically obtained through infrared spectroscopy performed of a nujol mull. The grinding action inherent in the preparation of a nujol mull causes changes in two of the polymorphs. These changes are caused by the pressure generated during the grinding process. Larger errors result when significant amounts of the gamma or delta form are present due to the composition-altering effects of sample grinding. Delta-HMX is normally absent from samples that have been solution processed because this form is thermodynamically favored only at high temperatures ( >/approx gt/140/degree/ C). In addition, small amounts of delta-HMX that might be present can readily transform morphology under the mechanical action of normal handling. It is for both these reasons that it is impractical to pursue the quantitative analysis of this form, and we will not do so here. The Raman spectra of beta-HMX have previously been measured and shown to have many intense peaks. The Raman spectra have been used to measure the transformations between polymorphs as a function of pressure and temperature. The results reported here show that Raman spectroscopy can be used to detect the alpha and gamma phases in beta-HMX at concentrations well under 1%. 13 refs., 6 figs. (ERA citation 13:049471)
Keywords	Chemical Explosives Raman Spectra Grinding Infrared Spectra Phase Transformations Pressure Effects Temperature Effects Meetings HMX Chemical analysis ERDA/450100 Tetrazocine/oxtahydro-tetranitro
Source Agency	Technical Information Center Oak Ridge Tennessee
NTIS Subject Category	79A - Ammunition, Explosives, & Pyrotechnics 99A - Analytical Chemistry
Corporate Authors	Monsanto Research Corp., Miamisburg, OH. Mound.; Department of Energy, Washington, DC.
Supplemental Notes	American Defense Preparedness Association Compatibility symposium, New Orleans, LA, USA, 18 Apr 1988.
Document Type	Conference Proceedings
NTIS Issue Number	198904
Contract Number	AC04-76DP00053

Detection of the Alpha and Gamma Polymorphs of HMX in Beta-HMX by Raman Spectroscopy.

Detection of the Alpha and Gamma Polymorphs of HMX in Beta-HMX by Raman Spectroscopy.
DE88012867

Publication Date	1988
Personal Author	Holy, J. A.; Firsich, D. W.; Walters, R. R.
Page Count	7
Abstract	HMX (octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine) is an important military explosive which exhibits four polymorphic forms- alpha, beta, gamma, and delta. Commercial lots of this compound are analyzed for polymorphic composition in order to achieve predictable firing characteristics. This analysis may be done qualitatively with powder diffraction, while quantitative results are typically obtained through infrared spectroscopy performed of a nujol mull. The grinding action inherent in the preparation of a nujol mull causes changes in two of the polymorphs. These changes are caused by the pressure generated during the grinding process. Larger errors result when significant amounts of the gamma or delta form are present due to the composition-altering effects of sample grinding. Delta-HMX is normally absent from samples that have been solution processed because this form is thermodynamically favored only at high temperatures ( >/approx gt/140/degree/ C). In addition, small amounts of delta-HMX that might be present can readily transform morphology under the mechanical action of normal handling. It is for both these reasons that it is impractical to pursue the quantitative analysis of this form, and we will not do so here. The Raman spectra of beta-HMX have previously been measured and shown to have many intense peaks. The Raman spectra have been used to measure the transformations between polymorphs as a function of pressure and temperature. The results reported here show that Raman spectroscopy can be used to detect the alpha and gamma phases in beta-HMX at concentrations well under 1%. 13 refs., 6 figs. (ERA citation 13:049471)
Keywords	Chemical Explosives Raman Spectra Grinding Infrared Spectra Phase Transformations Pressure Effects Temperature Effects Meetings HMX Chemical analysis ERDA/450100 Tetrazocine/oxtahydro-tetranitro
Source Agency	Technical Information Center Oak Ridge Tennessee
NTIS Subject Category	79A - Ammunition, Explosives, & Pyrotechnics 99A - Analytical Chemistry
Corporate Authors	Monsanto Research Corp., Miamisburg, OH. Mound.; Department of Energy, Washington, DC.
Supplemental Notes	American Defense Preparedness Association Compatibility symposium, New Orleans, LA, USA, 18 Apr 1988.
Document Type	Conference Proceedings
NTIS Issue Number	198904
Contract Number	AC04-76DP00053