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1.
Anal Chem ; 90(11): 6885-6892, 2018 06 05.
Article in English | MEDLINE | ID: mdl-29694027

ABSTRACT

Two differential mobility analyzers (DMAs) acting as narrow band mobility filters are coupled in series, with a thermal fragmentation cell placed in between, such that parent ions selected in DMA1 are fragmented in the cell at atmospheric pressure, and their product ions are analyzed on DMA2. Additional mass spectrometer analysis is performed for ion identification purposes. A key feature of the tandem DMA is the short residence time (∼0.2 ms) of ions in the analyzer, compared to tens of milliseconds in drift tube ion mobility spectrometers (IMS). Ion fragmentation within the analyzer and associated mobility tails are therefore negligible for a DMA but not necessarily so in conventional IMS. This advantage of the DMA is demonstrated here by sharply defined product ion mobility peaks. Ambient pressure ion fragmentation has been previously demonstrated by both purely thermal means as well as rapidly oscillating intense electric fields. Our purely thermal fragmentation cell here achieves temperatures up to 700 °C measured inside the heating coil of a cylindrical ceramic heater, through whose somewhat colder axis we direct a beam of mobility-selected ions. We investigate tandem separation of chloride adducts from the explosives EGDN, nitroglycerine (NG), PETN, and RDX and from deprotonated TNT. Atmospheric pressure fragmentation of the first three ions yields one or several previously reported fragments, providing highly distinctive tandem DMA channels for explosive identification at 1 atm. RDX ions had not been previously fragmented at ambient pressure, yet [RDX + Cl]- converts up to 7% (at 300 °C) into a 166 m/ z product. The known high thermal resilience of TNT is confirmed here by its rather modest conversion, even when the ceramic is heated to 700 °C. At this temperature some previously reported fragments are found, but their mobilities are fairly close to each other and to the one of the far more abundant parent ion, making their identification by mobility alone problematic. We anticipate that moderately higher fragmenter temperatures will produce smaller fragments with mobilities readily separated from that of [TNT - H]-.

2.
J Am Soc Mass Spectrom ; 20(2): 287-94, 2009 Feb.
Article in English | MEDLINE | ID: mdl-19013080

ABSTRACT

We determine the sensitivity of several commercial atmospheric pressure ionization mass spectrometers towards ambient vapors, ionized by contact with an electrospray of acidified or ammoniated solvent, a technique often referred to as secondary electrospray ionization (SESI). Although a record limit of detection of 0.2 x 10(-12) atmospheres (0.2 ppt) is found for explosives such as PETN and 0.4 ppt for TNT (without preconcentration), this still implies the need for some 10(8)-10(9) vapor molecules/s for positive identification of explosives. This extremely inefficient use of sample is partly due to low charging probability ( approximately 10(-4)), finite ion transmission, and counting probability in the mass spectrometer (1/10 in quadrupoles), and a variable combination of duty cycle and background noise responsible typically for a 10(3) factor loss of useful signal.


Subject(s)
Explosive Agents/analysis , Spectrometry, Mass, Electrospray Ionization/methods , Atmospheric Pressure , Pentaerythritol Tetranitrate/analysis , Trinitrotoluene/analysis , Uncertainty
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