University of North Florida
Browse the Citations
-OR-

Contact Info

Stuart Chalk, Ph.D.
Department of Chemistry
University of North Florida
Phone: 1-904-620-1938
Fax: 1-904-620-3535
Email: schalk@unf.edu
Website: @unf

View Stuart Chalk's profile on LinkedIn

Mass spectrometry

Classification: Mass spectrometry -> particle beam

Citations 6

"Effect Of Mobile Phase Composition On The Electrochemical Cell Conversion Efficiency In Electrochemistry/mass Spectrometry"
Anal. Chim. Acta 1998 Volume 369, Issue 3 Pages 253-262

Notice (8): Undefined variable: uid [APP/View/Elements/citation.ctp, line 40]
Merle Regino, Carol Weston and Anna Brajter-Toth*

Abstract: A new electrochemical flow-through cell has been recently developed and characterized for online EC/MS experiments with thermospray and particle beam LC-MS interfaces. It was discovered in this work that the mobile phase composition had a significant effect on the sensitivity in the online EC experiments with the new flow-through electrochemical cell. An application of hydrodynamic EC methods is illustrated in the optimization of EC/MS measurements using different mobile phases including aqueous, non-aqueous, and mixed mobile phases.
Interface Apparatus

"Eluent Jet Interface For Combining Capillary Liquid Flows With Electron-impact Mass-spectrometry"
Anal. Chem. 1996 Volume 68, Issue 4 Pages 675-681

Notice (8): Undefined variable: uid [APP/View/Elements/citation.ctp, line 40]
Charles E. Kientz, Albert G. Hulst, Ad L. De Jong, and Eric R. J. Wils

Abstract: A new interface based on an eluent jet in combination with a conventional gas chromatography momentum separator for use with electron impact mass spectrometry is described. The formation of the eluent jet is based on radio frequency inductive heating. The aerosol formation in the; interface is discussed in relation to commercial particle beam (PB) interfaces. The interface is tested in combination with electron impact mass spectrometry using flow injection analysis at now rates in the range of 5-15 µL/min commonly encountered in microcolumn liquid chromatography. Electron impact spectra at 1-10 ng levels are found to be comparable with reference spectra. In the single-ion mode, 50 pg of caffeine is detectable with a signal-to-noise ratio of 3:1. Contrary to many other PB systems, linear calibration plots are obtained in the tested range of 3-200 ng of caffeine.
Caffeine Interface

"Comparative Investigation Of UV, Electrochemical And Particle Beam Mass Spectrometric Detection For The High Performance Liquid Chromatographic Determination Of Benzoic And Cinnamic Acids And Of Their Corresponding Phenolic Acids"
J. Chromatogr. A 1996 Volume 753, Issue 2 Pages 157-170

Notice (8): Undefined variable: uid [APP/View/Elements/citation.ctp, line 40]
C. Bocchi, M. Careri*, F. Groppi, A. Mangia, P. Manini and G. Mori

Abstract: The capabilities of different detection techniques, UV, controlled-potential coulometry and particle-beam electron-impact mass spectrometry (PB-EI-MS) for the HPLC analysis of phenolic acids were studied; fifteen benzoic and cinnamic acid derivatives were considered. For the electrochemical detector (ED) a reversed-phase LC method was set up, whereas normal-phase partition chromatography, on a CN column, was used for UV and MS. Library-searchable EI mass spectra were obtained using the PB-MS technique with flow injection analysis. UV detection was performed at 280 nm, whereas measurements with the LC-coulometric system were carried out using a porous graphite electrode. The detector responses were compared in terms of linearity, precision and limits of detection; for this purpose, the mass spectrometer was operated under selected-ion monitoring conditions. A linear dynamic range of at least 10^-3 was found for the HPLC method with electrochemical detection, with detection limits ranging from 1 to 5 pg injected; the relative standard deviation (RSD) was typically 0.6-3.0% at the 0.1 ng level (n=4). Using UV or PB-EI-MS detection, minimum amounts in the 5-50 and 2-5 ng ranges, respectively, could be detected. Calibration curves were linear from the limit of detection to at least 15 µg for most of the analytes detected by UV; the RSD of the peak areas obtained in UV mode ranged from 1.2 to 3.1% at the 500 ng level (n=4). Non-linear behavior over the entire amount range studied (from 10 ng to 10 µg) was observed using the LC-PB-MS technique, so that two different calibration fittings at low and high levels were calculated. Precision of the LC-PB-MS system was generally good (RSD between 0.5 and 1.8% at the 100 ng level, n=4) except for caffeic acid (RSD 7.5% at the 50 µg level, n=4).
Linear dynamic range

"Identification Of Pesticides By Liquid Chromatography Particle Beam Mass Spectrometry Using Electron Ionization And Chemical Ionization"
J. Chromatogr. A 1998 Volume 805, Issue 1-2 Pages 127-135

Notice (8): Undefined variable: uid [APP/View/Elements/citation.ctp, line 40]
C. Aguilar*, F. Borrull and R. M. Marcé

Abstract: Liquid chromatography-mass spectrometry (LC-MS) with a particle beam (PB) interface is used to separate and identify a group of pesticides. The mass spectra obtained under the different ionization modes, electron ionization (EI) and positive and negative chemical ionization (PCI and NCI) are compared. The operating conditions under each mode, determined by studying the influence on the ion abundance of the ion source temperature of the EI mode, and the gas pressure and ion source temperature in the methane CI were optimized. EI was more sensitive than PCI and NCI and of the latter two modes, NCI gave higher responses, especially for organophosphorus compounds. When online solid-phase extraction-LC-PB-MS was applied to real samples, limits of detection in full scan mode were in the range of 0.5 and 10 µg L-1 for EI. The analysis of real samples by online solid-phase extraction-LC-PB-MS enabled EI detection of one of the pesticides studied and confirmation by PCI and NCI. The combined EI/CI information also enabled the detection of some non-target compounds.
Pesticides Solid phase extraction

"Identification Of Carbamates By Particle Beam/mass Spectrometry"
J. Mass Spectrom. 1997 Volume 32, Issue 1 Pages 43-54

Notice (8): Undefined variable: uid [APP/View/Elements/citation.ctp, line 40]
Jaroslav Slobodník, Maria E. Jager, Sacha J. F. Hoekstra-Oussoren, Maarten Honing, Ben L. M. van Baar*, Udo A. Th. Brinkman

Abstract: The possibility of analyzing 33 carbamate pesticides and 14 of their transformation products was investigated utilizing flow injection particle beam/mass spectrometry (PBMS) with electron impact (EI) ionization and ammonia and methane positive and negative chemical ionization (CI). Optimum operating conditions of the interface and mass spectrometer in each mode were determined, with special attention given to spectrum quality; variables investigated included ion source temperature and ion source pressure in CI experiments. Ammonia, as a reagent gas, provided less fragmentation and better quantitative results than methane. The CI response was generally higher with positive ion detection (PCI) than with negative ion detection (NCI), but NCI was found to be highly selective for compounds such as aminocarb, asulam and thiophanate-methyl. As regards analyte detectability, EI performed best for most compounds, with the spectra providing relevant structure information. The response of more polar degradation products is generally larger by 2-3 orders of magnitude compared with the parent compounds. When analyzing real samples, the combined use of CI for molecular mass determination and EI for structure elucidation is required. The spectral information from this study and additional chromatographic data were used for the determination of low- and sub µg L-1 levels of the test carbamates in surface water.
Carbamates Surface

"Structural Alteration Study Of α-chloro-α-oximino-4-hydroxyacetophenone By Particle Beam Liquid Chromatography Mass Spectrometry"
Rapid Commun. Mass Spectrom. 1998 Volume 12, Issue 15 Pages 1031-1033

Notice (8): Undefined variable: uid [APP/View/Elements/citation.ctp, line 40]
S. K. Huang

Abstract: The structure of -chloro--oximino-4-hydroxyacetophenone (COHAP) can be fully characterized by electron ionization and desorption chemical ionization mass spectrometry through a probe introduction of the sample or by the flow injection of particle beam liquid chromatography/mass spectrometry with tetrahydrofuran/hexane elution. With reversed-phase liquid chromatography, or when a normal-phase diol or silica column was employed with nonaqueous mobile phase for the separation of COHAP from its reaction mixture, however, the compound was detected as its dehydrochlorinated product by particle beam liquid chromatography/mass spectrometry. Our studies show that the liquid chromatographic peak which is regarded as COHAP is actually the p-hydroxybenzoyl hydroxamic acid and p-hydroxybenzoyl nitrile oxide under reversed-phase and normal-phase liquid chromatographic conditions, respectively.