Tandem capillary column gas chromatography-mass spectrometric determination of the organophosphonate nerve agent surrogate dimethyl methylphosphonate in gaseous phase
| Autor: | George P. Cobb, Nicholas A. Romero, Gopal Coimbatore, Jonathan W. Boyd, Les N. McDaniel |
|---|---|
| Rok vydání: | 2009 |
| Předmět: |
Acetonitriles
Chromatography Gas Time Factors Calibration curve Analytical chemistry Standard solution Mass Spectrometry Analytical Chemistry chemistry.chemical_compound Organophosphorus Compounds Limit of Detection Chemical Warfare Agents Acetonitrile Detection limit Air Pollutants Chromatography Chemistry Dimethyl methylphosphonate Repeatability Organophosphates Calibration Central Nervous System Stimulants Gas chromatography Gases Gas chromatography–mass spectrometry Environmental Monitoring |
| Zdroj: | Talanta. 81(4-5) |
| ISSN: | 1873-3573 |
| Popis: | A procedure based on capillary column gas chromatographic-mass spectrometric (GC-MS) confirmation was developed for the verification of the ubiquitous and versatile chemical and nerve agent simulant, dimethyl methyl phosphonate (DMMP; CAS# 756-79-6), from gaseous samples. This method was developed to verify low nanogram DMMP concentrations during testing of a nerve agent detection system. Standard solutions of 1, 5, 10, 50, 100, 500, and 1000ng/ml DMMP in acetonitrile were employed. Through 15 calibration curves using the 5 lowest concentrations, coefficient of determination (r(2)) values showed a mean of 0.998 (0.992-1.000). An additional 15 calibration curves likewise containing 5 concentrations of DMMP spanning 3 orders of magnitude (1, 50, 100, 500, and 1000ng/ml) yielded a mean r(2) of 0.997 (0.991-1.000). Sixty-five nitrogen diluted gaseous samples varying from 1.0 to 10.0microl in volume were analyzed and concentrations of DMMP ranging from 1 to 1000ng/ml were confirmed. An additional 35 vapor samples in UHP N(2) ranging in DMMP concentration from 5.8microg/m(3) to 1.0mg/m(3) were analyzed by increasing sample volume range to between 10.0 and 100microl. For gaseous samples with volumes1.0microl, the lowest concentration observed was 5.8microg/m(3). The method detection limit (Appendix B of Title 40 CFR, United States) for 1.0microl autoinjected standards in acetonitrile was determined to be 0.331ng/ml. Method precision for 15 independently analyzed standards of 25ng/ml had a relative standard deviation of 1.168. This method demonstrated high linearity across a wide range of concentrations, as well as excellent sensitivity and repeatability, and proved applicable to other lower alkyl-phosphonates. |
| Databáze: | OpenAIRE |
| Externí odkaz: |
|
Full Text from ScienceDirect