Preparation and characterization of micro-bore wall-coated open-tubular capillaries with low phase ratios for fast-gas chromatography–mass spectrometry: Application to ignitable liquids and fire debris

Fast Gas Chromatography (GC) allows for analysis times that are a fraction of those seen in traditional capillary GC. Key modifications in fast GC include using narrow, highly efficient columns that can resolve mixtures using a shorter column length. Hence, a typical fast GC column has an inner diameter of 100–180 μm. However, to maintain phase ratios that are consistent with typical GC columns, the film thickness of fast GC stationary phases are also low (e.g., 0.1–0.18 μm). Unfortunately, decreased film thickness leads to columns with very low sample capacity and asymmetric peaks for analytes that are not sufficiently dilute. This paper describes micro-bore (50 μm i.d.) capillary columns with thick films (1.25 μm), and low phase ratios (10). These columns have greater sample capacity yet also achieve minimum plate heights as low as 110 μm. Hence, separation efficiency is much higher than would be obtained using standard GC columns. The capillary columns were prepared in-house using a simple static-coating procedure and their plate counts were determined under isothermal conditions. The columns were then evaluated using temperature programming for fast GC–MS analysis of ignitable liquids and their residues on fire debris exemplars. Temperature ramps of up to 75 °C min−1 could be used and separations of ignitable liquids such as gasoline, E85 fuel, and lighter fluid (a medium petroleum distillate) were complete within 3 min. Lastly, simulated fire debris consisting of ignitable liquids burned on carpeting were extracted using passive headspace absorption-elution and the residues successfully classified

Differentiation of Structurally Similar Phenethylamines via Gas Chromatography - Vacuum Ultraviolet Spectroscopy (GC – VUV)

The vacuum ultraviolet region includes wavelengths shorter than 200 nm. Electronic transitions of sigma and pi bonds lie in this region, which have the potential to yield structural information. Thus, a VUV detector should be able to detect nearly any molecule analyzable by gas chromatography. This study sought to determine the extent to which structurally similar phenethylamines are differentiated using their VUV spectra. Phenethylamines are a common drug class including pseudoephedrine and illicit drugs such as methamphetamine. Several phenethylamines are difficult to analyze by electron impact mass spectrometry due to their fragmentation giving the same mass to charge ratio fragments at similar ratios. While phenethylamines are generally differentiable by retention time, an extra layer of specificity is preferred in forensic analyses. A vacuum ultraviolet (VUV) spectrophotometer coupled to a gas chromatograph was used to collect VUV spectra at high frequency between 125 and 430 nm. Eight phenethylamines were analyzed for this work using GC/VUV. A calibration curve and limit of detection study was performed that indicates a limit of detection around 10 μg mL−1 and an upper limit of linearity around 1000 μg mL−1. The spectra, analyzed by Principal Component Analysis and Discriminant Analysis, indicate the ability to reliably differentiate each of the drugs from one another including structural isomers and diastereomers. Lastly, five “street” samples containing amphetamines were analyzed to demonstrate “real world” performance