Quantitative Real-Time Monitoring of Chemical Reactions by Autosampling Flow Injection Analysis Coupled with Atmospheric Pressure Chemical Ionization Mass Spectrometry
| Autor: | Liguo Song, Kelsey D. Cook, Zhenqian Zhu, Mary Ellen P. McNally, John E. Bartmess, Ron M. Hoffman |
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| Rok vydání: | 2012 |
| Předmět: |
Flow injection analysis
Spectrometry Mass Electrospray Ionization Molar concentration Chromatography Acrylonitrile Propylamines Capillary action Chemistry Analytical chemistry Atmospheric-pressure chemical ionization Injector Mass spectrometry Chemical reaction Analytical Chemistry law.invention Automation Atmospheric Pressure law Calibration Flow Injection Analysis Phenethylamines Solvents |
| Zdroj: | Analytical Chemistry. 84:7547-7554 |
| ISSN: | 1520-6882 0003-2700 |
| DOI: | 10.1021/ac3017136 |
| Popis: | Although qualitative and/or semiquantitative real-time monitoring of chemical reactions have been reported with a few mass spectrometric approaches, to our knowledge, no quantitative mass spectrometric approach has been reported so far to have a calibration valid up to molar concentrations as required by process control. This is mostly due to the absence of a practical solution that could well address the sample overloading issue. In this study, a novel autosampling flow injection analysis coupled with an atmospheric pressure chemical ionization mass spectrometry (FIA/APCI-MS) system, consisting of a 1 μL automatic internal sample injector, a postinjection splitter with 1:10 splitting ratio, and a detached APCI source connected to the mass spectrometer using a 4.5 in. long, 0.042 in. inner diameter (ID) stainless-steel capillary, was thus introduced. Using this system together with an optional FIA solvent modifier, e.g., 0.05% (v/v) isopropylamine, a linear quantitative calibration up to molar concentration has been achieved with 3.4-7.2% relative standard deviations (RSDs) for 4 replicates. As a result, quantitative real-time monitoring of a model reaction was successfully performed at the 1.63 M level. It is expected that this novel autosampling FIA/APCI-MS system can be used in quantitative real-time monitoring of a wide range of reactions under diverse reaction conditions. |
| Databáze: | OpenAIRE |
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