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

Quantitative Detection of Trace Explosive Vapors by Programmed Temperature Desorption Gas Chromatography-Electron Capture Detector

“…Recently, quantitation methods using thermal desorption systems with a cooled inlet system (TDS-CIS), coupled to a GC-ECD have been developed for TNT and RDX vapors. 24,25 The losses associated with the TDS-CIS-GC-ECD instrumentation for trace explosive vapors were characterized and accounted for in example calibration curves using a direct liquid deposition method onto sorbent-filled thermal desorption sample tubes. However, the literature focused on instrumentation characterization and method development but never actually sampled,…”

“…2,[18][19][20][21][22][23] In order to detect explosive vapors, alternative sampling protocols must be used, such as vapor collection with sorbent-filled thermal desorption sample tubes, but quantitative detection remains difficult due to lack of vapor standards and calibration methods that do not account for sample tube and instrumentation losses.Recently, quantitation methods using thermal desorption systems with a cooled inlet system (TDS-CIS), coupled to a GC-ECD have been developed for TNT and RDX vapors. 24,25 The losses associated with the TDS-CIS-GC-ECD instrumentation for trace explosive vapors were characterized and accounted for in example calibration curves using a direct liquid deposition method onto sorbent-filled thermal desorption sample tubes. However, the literature focused on instrumentation characterization and method development but never actually sampled,…”

“…Use the twenty tube autosampler and the previously described TNT and RDX TDS-CIS-GC-ECD method to run and analyze all eighteen tubes O/N. 24,25 A summary of the TDS-CIS-GC-ECD parameters for the method is provided in Table 1.…”

Minimizing thermal degradation in gas chromatographic quantitation of pentaerythritol tetranitrate

“…Other published laboratory methods for analysis of trace explosive vapors such as trinitrotoluene (TNT) and hexamethylenetetramine (RDX) involve collection on sorbent-filled tubes during active sampling [5][6][7][8][9][10]. The analyte is then thermally desorbed and refocused on a cryogenically cooled gas chromatograph (GC) inlet, followed by gas chromatographic analysis.…”

“…Thus, FAPA ionization coupled to a high-resolution mass spectrometer (HRMS) is used here as an alternate detection strategy for the GC separation to minimize fragmentation compared to EI and conclusively identify the PETN molecular ion via the high mass accuracy of the mass analyzer (∼1 ppm). This approach enabled methodology from the GC-FAPA-HRMS instrument to be transferred to a conventional gas chromatograph equipped with a thermal desorption system and electron capture detection (ECD) [9,10,21] to provide simple, direct analysis of sorbent-trapped PETN on a routine basis.…”