Direct liquid deposition calibration method for trace cyclotrimethylenetrinitramine using thermal desorption instrumentation

► Cryo-focusing improves reproducibility for liquid and vapor samples. ► Losses are observed using a commercial thermal desorption unit. ► Calibration curves are established using direct liquid deposition of RDX. ► Calibration curves can be established simultaneously for TNT and RDX. A simple method...

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Bibliographic Details
Published in:Journal of Chromatography A 2013-03, Vol.1282, p.178-182
Main Authors: Field, Christopher R., Lubrano, Adam L., Rogers, Duane A., Giordano, Braden C., Collins, Greg E.
Format: Article
Language:English
Subjects:
Analytical chemistry
Applied sciences
Chemical industry and chemicals
Chemistry
Chromatographic methods and physical methods associated with chromatography
Cryo-focusing
desorption
Exact sciences and technology
Explosives
Gas chromatographic methods
gas chromatography
GC–ECD
glass
Industrial chemicals
instrumentation
Powders, propellants, explosives
Quantitation
RDX
Thermal desorption
trinitrotoluene
vapors
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Summary:► Cryo-focusing improves reproducibility for liquid and vapor samples. ► Losses are observed using a commercial thermal desorption unit. ► Calibration curves are established using direct liquid deposition of RDX. ► Calibration curves can be established simultaneously for TNT and RDX. A simple method for establishing calibration curves with sorbent-filled thermal desorption tubes has been demonstrated for nitroaromatic and nitramine vapor samples using a thermal desorption system with a cooled inlet system (TDS–CIS), which was coupled to a gas chromatograph (GC) with an electron capture detector (ECD). The method relies upon the direct liquid deposition of standard solutions onto the glass frit at the head of sorbent-filled thermal desorption tubes. Linear calibration results and ideal system conditions for the TDS–CIS–GC–ECD were established for mixtures containing both cyclotrimethylenetrinitramine, a.k.a. RDX, and 2,4,6-trinitrotoluene (TNT). Because of the chemical characteristics of RDX, a higher TDS–CIS flow rate relative to the optimized approach for TNT was required for efficient RDX desorption. Simultaneous quantitation of TNT and RDX using the direct liquid deposition method with optimized instrumentation parameters for RDX were compared to results from a standard split/splitless GC inlet and a CIS.
ISSN:0021-9673
DOI:10.1016/j.chroma.2013.01.051