Investigation of compound-independent calibration and partial molecular formula determination by gas chromatography–atomic-emission detection for characterisation of organophosphorus and organosulfur agents related to the chemical weapons convention
| Autor: | Yannick Juillet, Edmond Gibert, Arlette Bégos, Bruno Bellier |
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| Rok vydání: | 2005 |
| Předmět: |
Chemical Warfare
Analyte Chromatography Gas Molecular Structure Sulfur Compounds Chemistry Spectrophotometry Atomic Atomic emission spectroscopy Analytical chemistry Reproducibility of Results Guidelines as Topic Mass spectrometry Sensitivity and Specificity Biochemistry Analytical Chemistry Organophosphorus Compounds Reference Values Yield (chemistry) Calibration Molecule Chemical Warfare Agents Gas chromatography Organosulfur compounds Algorithms |
| Zdroj: | Analytical and Bioanalytical Chemistry. 383:848-856 |
| ISSN: | 1618-2650 1618-2642 |
| DOI: | 10.1007/s00216-005-0064-z |
| Popis: | Atomic-emission detection (AED) is a technique particularly-well suited to screening complex samples for multiple compounds containing heteroatoms such as phosphorus, sulfur, or nitrogen, which are especially relevant in verification of chemical disarmament. Among other GC detectors, AED has unique characteristics such as compound-independent calibration and possible raw-formula determination. Because contradictory results have been reported on these points, we set up a study with the objectives not only of applying these techniques to chemical weapons convention-related chemicals but of determining under which conditions they would yield satisfactory results. The extensive data collected in this study are evidence that the response of the detector, particularly for the phosphorus line, is very dependent on the molecular mass and concentration of the chemicals analysed whereas molecular structure seems to have less effect on the AED signal. Most interestingly, compound-independent calibration and subsequent partial molecular formula determination usually seem satisfactory when the reference compounds used to calibrate the system have GC retention times and molecular masses close to those of the unknown analytes (whose molecular mass may be determined by GC-CI-MS). We therefore suggest the use of a reference set of compounds covering a large chromatographic window, which enables the selection, within this set, of the most appropriate reference compound for calibration and for determination of the raw formula of an unknown analyte. For optimal performance, the use of a new discharge tube is also recommended. |
| Databáze: | OpenAIRE |
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