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

Abstract: 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. [Copyright &y& Elsevier]