A novel extraction device, capillary microextraction of volatiles (CMV) was coupled to a TRIDION-9 GC–MS with a needle trap (NTD) and evaluated for the analysis of ignitable liquids fire debris. The performance of the TRIDION-9 was compared to a benchtop GC–MS using CMV. A system detection limit of ~10 ng for each of 20 key ignitable liquid residue (ILR) compounds was determined for the T9 GC–MS. Dynamic headspace sampling of simulated ILRs was performed in closed and open-air systems. Closed system evaluations the CMV/NTD technique resulted in extraction performance similar to the CMV alone; however, ILR analysis on the T9 was impacted by limited chromatographic resolution. Compound identification was possible for 14 out of the 20 selected compounds on the T9 when 1 μL of a 1% standard accelerant mixture (SAM) was sampled, compared to 17 compounds on the benchtop GC–MS for the same mass loading. Open-air sampling with a modified vapor source resulted in the retention of most compounds with as low as 5 min. sampling, and equilibrium concentrations were reached after 10 min. No significant differences were observed between CMV and CMV/NTD sampling suggesting that the combined technique does not suffer from affinity bias. While the potential of the CMV/NTD extraction coupled to a T9 GC–MS for fire debris analysis was limited by the chromatographic resolution of the instrument, this study serves as proof of concept for the CMV’s potential for the extraction of ILRs in combination with portable GC–MS systems.
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Recovery and detection of ignitable liquid residues from the substrates by solid phase microextraction – direct analysis in real time mass spectrometry
In this study, direct analysis in real time mass spectrometry (DART-MS) was coupled to the solid phase microextraction (SPME) to extract and analyze the ignitable liquid residues (ILR) present in the sample matrices. The SPME extraction parameters, such as extraction temperature and extraction time, were optimized using a two factor central composite design. The SPME-DART-MS setup was utilized to analyze the substrates and fire debris matrices spiked with gasoline. The results indicate that the less volatile marker compounds from gasoline were recovered from the substrates and fire debris, and their profiles matched well with the gasoline liquid samples analyzed directly by DART-MS. As expected, the effective extraction of marker compounds in gasoline required a relatively high temperature, i.e., 150 ℃. In the presence of a matrix, a higher extraction temperature and longer extraction time could benefit the extraction efficiency. The desorption of ILR on SPME fiber was performed by inserting the fiber into the DART-MS helium gas stream at 300 ℃ for 1 min with no carry-over residues being observed between successive samples. The chemical information attained with this method is typically not observed in the current GC/MS-based practice. The SPME-DART-MS was also extended to reanalyze less volatile components of ILR on substrates after the ASTM E1412 activated charcoal method, which indicates its possible application subsequent to the traditional GC/MS ILR analysis. The SPME-DART-MS has shown promise in ILR detection as an important complementary tool.
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- Award ID(s):
- 2216092
- PAR ID:
- 10650054
- Publisher / Repository:
- Elsevier
- Date Published:
- Journal Name:
- Forensic Chemistry
- Volume:
- 41
- Issue:
- C
- ISSN:
- 2468-1709
- Page Range / eLocation ID:
- 100611
- Format(s):
- Medium: X
- Sponsoring Org:
- National Science Foundation
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