Optimization of focused ultrasonic extraction of propellant components determined by gas chromatography/mass spectrometry

Fryš, Ondřej; Česla, Petr; Bajerová, Petra; Adam, Martin; Ventura, Karel

doi:10.1016/j.talanta.2012.05.058

Cited by 13 publications

(6 citation statements)

References 24 publications

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“…The effect of the liner type and inlet temperature were evaluated and, therefore, varied between the experiments (as described in the corresponding section below). All other instrumental parameters were consistent and based on common practices in the field [ 5 , 22 – 24 ]. Injection was carried out in split mode, with a 25:1 split ratio, and the injection volume was set to 1 μL.…”

Section: Methodsmentioning

confidence: 99%

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Forensic profiling of smokeless powders (SLPs) by gas chromatography–mass spectrometry (GC-MS): a systematic investigation into injector conditions and their effect on the characterisation of samples

Kesic,

McCann,

Bowerbank

et al. 2024

Anal Bioanal Chem

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Smokeless powders (SLPs) are composed of a combination of thermolabile and non-thermolabile compounds. When analysed by GC-MS, injection conditions may therefore play a fundamental role on the characterisation of forensic samples. However, no systematic investigations have ever been carried out. This casts doubt on the optimal conditions that should be adopted in advanced profiling applications (e.g. class attribution and source association), especially when a traditional split/splitless (S/SL) injector is used. Herein, a study is reported that specifically focused on the evaluation of the liner type (Ltype) and inlet temperature (Tinj). Results showed that both could affect the exhaustiveness and repeatability of the observed chemical profiles, with Ltype being particularly sensitive despite typically not being clarified in published works. Perhaps as expected, degradation effects were observed for the most thermolabile compounds (e.g. nitroglycerin) at conditions maximising the heat transfer rates (Ltype = packed and Tinj ≥ 200 °C). However, these did not seem to be as influential as, perhaps, suggested in previous studies. Indeed, the harshest injection conditions in terms of heat transfer rate (Ltype = packed and Tinj = 260 °C) were found to lead to better performances (including better overall %RSDs and LODs) compared to the mildest ones. This suggested that implementing conditions minimising heat-induced breakdowns during injection was not necessarily a good strategy for comparison purposes. The reported findings represent a concrete step forward in the field, providing a robust body of data for the development of the next generation of SLP profiling methods. Graphical abstract

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Section: Methodsmentioning

confidence: 99%

“…The ASTM guideline E2999, for instance, explicitly suggests the use of a S/SL injector with an inlet temperature between 190 and 220 °C, as well as acetone or dichloromethane as injection solvents [ 17 ]. Similar conditions were adopted by many research works, often by further reducing the inlet temperature down to 170 °C [ 22 ].…”

Section: Introductionmentioning

confidence: 99%

Forensic profiling of smokeless powders (SLPs) by gas chromatography–mass spectrometry (GC-MS): a systematic investigation into injector conditions and their effect on the characterisation of samples

Kesic,

McCann,

Bowerbank

et al. 2024

Anal Bioanal Chem

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“…RSM can also be effective in finding the combination of factors that produce the optimum response [ 1 ]. The main advantage of this technology is that fewer experimental trials are needed to evaluate multiple factors, and their interactions, making it less laborious and time-consuming than other optimization techniques (e.g., the “one-variable-at-a-time” optimization) [ 2 ]. Recently, He et al optimized the protein yield, total phenolic contents (TPC), and lecithin content of black turtle bean extract using RSM [ 3 ].…”

Section: Introductionmentioning

confidence: 99%

Rapid High Performance Liquid Chromatography Determination and Optimization of Extraction Parameters of the α-Asarone Isolated from Perilla frutescens L.

et al. 2017

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Response surface methodology (RSM), based on a central composite design, was used to determine the best liquid-to-raw material ratio (10:3–15 mL/g), extraction time (1–3 h), and ethanol concentration (50%–100%) for maximum content of α-asarone from Perilla frutescens (PF) extract. Experimental values of α-asarone were 9.51–46.36 mg/g; the results fitted a second-order quadratic polynomial model and correlated with the proposed model (R2 > 0.9354). The best conditions were obtained with extraction time of 1.76 h, liquid-to-raw material ratio of 10:13.5 mL/g, and ethanol concentration of 90.37%. Under these conditions, the model predicted extraction content of 40.56 mg/g, while experimental PF content of α-asarone was 43.84 mg/g dried plant. Optimized conditions determined for maximum content of α-asarone were similar to the experimental range. Experimental values agreed with those predicted, thus validating and indicating suitability of both the model and the RSM approach for optimizing extraction conditions. In addition, a reliable, reproducible and accurate method for the quantitative determination of α-asarone by High Performance Liquid Chromatography (HPLC) analysis was developed with limit of detection (LOD), limit of quantitation (LOQ) values of 0.10 and 0.29 µg/mL and excellent linearity (R2 > 0.9999).

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“…Additionally, unlike many other experimental designs, CCDs are capable of modelling curvilinear variable effects [26,27]. Recent studies have successfully utilised CCDs to optimise the extraction and instrumental analysis parameters of propellant or nitroaromatic explosive residues [28][29][30]. In spite of these findings, the broader capability of experimental design to investigate initial factors such as appropriate sampling and storage methods remains unexplored.…”

Section: Introductionmentioning

confidence: 99%

Optimisation of recovery protocols for double-base smokeless powder residues analysed by total vaporisation (TV) SPME/GC-MS

Sauzier

Bors

Ash

et al. 2016

Talanta

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The investigation of explosive events requires appropriate evidential protocols to recover and preserve residues from the scene. In current protocols however, there is a lack of scientifically rigorous investigation concerning their validity. In this study, a central composite design was used to determine statistically validated optimum recovery parameters for double-base smokeless powder residues on steel, analysed using total vaporisation (TV) SPME/GC-MS. It was found that maximum recovery was obtained using isopropanol-wetted swabs stored under refrigerated conditions for a minimum period, then extracted for 15 minutes into acetone. These parameters were applied to the recovery of post-blast residues deposited on steel witness surfaces following a PVC pipe bomb detonation, resulting in detection of all target components across the majority of samples. Higher overall recoveries were obtained from plates facing the sides of the device, consistent with the point of first failure occurring in the pipe body as observed in previous studies. The methodology employed here may be readily applied to a variety of other explosive compounds, and thus assist in establishing 'best practice' procedures for explosive investigations.

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Optimization of focused ultrasonic extraction of propellant components determined by gas chromatography/mass spectrometry

Cited by 13 publications

References 24 publications

Forensic profiling of smokeless powders (SLPs) by gas chromatography–mass spectrometry (GC-MS): a systematic investigation into injector conditions and their effect on the characterisation of samples

Forensic profiling of smokeless powders (SLPs) by gas chromatography–mass spectrometry (GC-MS): a systematic investigation into injector conditions and their effect on the characterisation of samples

Rapid High Performance Liquid Chromatography Determination and Optimization of Extraction Parameters of the α-Asarone Isolated from Perilla frutescens L.

Optimisation of recovery protocols for double-base smokeless powder residues analysed by total vaporisation (TV) SPME/GC-MS

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