title: Post-Blast Analysis of Hexamethylene Triperoxide Diamine using Liquid Chromatography-Atmospheric Pressure Chemical Ionization-Mass Spectrometry.
abstract: A qualitative method using liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (LC/APCI-MS) has been developed and validated for the identification of trace hexamethylene triperoxide diamine (HMTD) using three structurally-specific ions. Residues are extracted with deionized water (DI) and identified using a gradient mobile phase program and positive ion full scan mode on a Thermo Finnigan LCQ Ion Trap Mass Spectrometer. This method was validated according to several performance characteristics for the qualitative identification of an analyte using the characteristic ions, demonstrating the method's reliability for use on forensic applications. The method's limit of detection (LOD) can identify HMTD in an extract from a cotton matrix to which 20 μg of HMTD has been applied (equivalent to 10 ppm in extract). Previous scientific publications using LC/MS have not demonstrated post-blast HMTD residue analyses and suffer from a lack of chromatographic retention, sufficient number of mass spectral ions with validation, or require more complex/expensive instrumental methods (accurate mass or MS/MS). Post-blast analyses were successfully conducted with two syringe detonations that verified the efficacy of the method on the analysis of debris and residues following detonation.
authors.affiliation: Counterterrorism and Forensic Science Research Unit, Federal Bureau of Investigation Laboratory Division, Visiting Scientist Program (administered by Oak Ridge Institute for Science and Education), 2501 Investigation Parkway, Quantico, VA, 22135, United States. Electronic address: Christine.Marsh@ic.fbi.gov.
authors.forename: Christine M
authors.initials: CM
authors.lastname: Marsh
authors.affiliation: Explosives Unit, Federal Bureau of Investigation Laboratory Division, 2501 Investigation Parkway, Quantico, VA, 22135 United States. Electronic address: Robert.Mothershead@ic.fbi.gov.
authors.forename: Robert F
authors.initials: RF
authors.lastname: Mothershead
authors.affiliation: Counterterrorism and Forensic Science Research Unit, Federal Bureau of Investigation, Laboratory Division, 2501 Investigation Parkway, Quantico, VA, 22135 United States. Electronic address: Mark.L.Miller@ic.fbi.gov.
authors.forename: Mark L
authors.initials: ML
authors.lastname: Miller
keywords: Atmospheric Pressure Chemical Ionization; HMTD; Mass Spectrometry; Peroxide Explosives; Post-Blast Residues