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Sample introduction in gas chromatography using a coiled wire filament
Authors:Tai V Truong  Aaron N Nackos  Jacolin A Murray  Jon A Kimball  Jason E Hawkes  Donald J Harvey  H Dennis Tolley  Richard A Robison  Calvin H Bartholomew  Milton L Lee
Institution:1. Department of Chemistry and Biochemistry, Brigham Young University, Provo, UT 84602, USA;2. Department of Chemical Engineering, Brigham Young University, Provo, UT 84602, USA;3. Department of Microbiology and Molecular Biology, Brigham Young University, Provo, UT 84602, USA;4. Department of Statistics, Brigham Young University, Provo, UT 84602, USA
Abstract:A simple device for field sampling and concentration of analytes for subsequent introduction into an injection port for gas chromatographic (GC) analysis has been developed. It consists of a tiny, coiled platinum wire filament (CWF) that is attached to a retractable plunger wire, which fits inside a syringe needle housing. Sampling is accomplished by dipping the end of the CWF in a liquid sample, which is drawn into the wire coil by capillary action, and introducing it into the injection port either before or after allowing the solvent to evaporate. The CWF can be used with or without a nonvolatile chemical coating. A major advantage of this sampling device is that nonvolatile sample matrix components remain on the wire coil, reducing the required injection port and liner cleaning frequency and contamination of the head of the chromatographic column. The coil itself can be easily cleaned between analyses by rinsing and/or burning off residual material in a small flame. The sampling coil facilitates specifically designed chemical reactions in the injection port, such as thermochemolysis and methylation. Applications demonstrated in this work include: (1) direct introduction of samples with little or no pre-treatment, (2) simultaneous thermochemolysis and methylation of lipid-containing samples such as bacteria and bacterial endospores for analysis of biomarkers, and (3) solid phase micro-extraction (SPME) using temporary wire coatings. The CWF allowed for significant reduction in sample preparation time, in most cases to less than a few minutes. The peak shapes examined for polycyclic aromatic hydrocarbon analytes (PAHs) were significantly better (asymmetry factors <1.3) when using the CWF sampling technique compared to splitless and on-column injection techniques (asymmetry factors >1.3). Extraction efficiencies for SPME (especially for high boiling point components such as PAHs) improved by an average of 2.5 times when using the CWF compared to the performance of commercially available SPME fibers. Coiled wire filaments and GC injection port liners were used for more than 100 Bacillus endospore thermochemolysis methylation analyses without the need for cleaning or replacement.
Keywords:Sample introduction  Gas chromatography  Solvent-less injection  Coiled wire filament  Solid phase micro-extraction  Bacillus endospores  Fatty acid methyl esters  Polycyclic aromatic hydrocarbons
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