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Edgar D Lee

Publications and source records attributed to Edgar D Lee.

6 recordsLinked to original sources

New interface plate for microspray ionization mass spectrometry.

A new interface plate was employed in microspray ionization mass spectrometry (microESI-MS) to improve ion transmission from the sprayer into the sampling nozzle of the mass spectrometer at atmospheric pressure. Using a time-of-flight mass spectrometer (TOFMS), a fivefold increase in ion intensity and a sevenfold reduction in method detection limit were observed. The interface plate attenuated the dependence of the ion intensity on the sprayer position. Even when the distance between the sprayer tip and sampling nozzle was 15.0 mm, ion signals were still stronger than when the sprayer tip was positioned 3.0 mm in front of the sampling nozzle with the original interface plate. This enhancement in the performance of microESI-MS was due to the improved shapes of the equipotential lines near the sprayer tip and the long desolvation distance between the sprayer and the sampling nozzle of the MS.

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Miniature toroidal radio frequency ion trap mass analyzer.

A miniature ion trap mass analyzer is reported. The described analyzer is a 1/5-scale version of a previously reported toroidal radio frequency (rf) ion trap mass analyzer. The toroidal ion trap operates with maximum rf trapping voltages about 1 kVp-p or less; however despite the reduced dimensions, it retains roughly the same ion trapping capacity as conventional 3D quadrupole ion traps. The curved geometry provides for a compact mass analyzer. Unit-mass resolved mass spectra for n-butylbenzene, xenon, and naphthalene are reported and preliminary sensitivity data are shown for naphthalene. The expected linear mass scale with rf amplitude scan is obtained when scanned using a conventional mass-selective instability scan mode combined with resonance ejection.

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Superimposition of a magnetic field around an ion guide for electron ionization time-of-flight mass spectrometry.

A new electron ionization source was developed for orthogonal acceleration time-of-flight mass spectrometry (TOFMS) based on the superimposition of a magnetic field around a radio frequency-only (rf-only) ion guide. The cylindrically symmetric magnetic field compresses the electron beam from the electron source into a long narrow volume along the ion guide axis. The magnetic field also helps to maintain a narrow energy distribution of electrons that penetrate the full length of the ion guide despite the influence of the radial rf field. Ionization occurs inside the ion guide with improved efficiency resulting from efficient use of electrons, prolonged interaction time, and nontraditionally large ionization volume. At the same time, the rf field effectively focuses ions radially and confines them to the axis of the ion guide by collisional focusing, leading to high ion transmission efficiency. Furthermore, the source can also be operated in a trap-and-pulse mode to improve the ion sampling duty cycle of orthogonal acceleration TOFMS. To validate the design concept of this new ion source, a simple prototype using a single set of cylindrical rods was constructed and retrofitted to an orthogonal acceleration TOFMS. A significant increase in ion signal intensity was observed by operating the source in a pulsed ion extraction mode. Low detection limits (for example, 12 fg for toluene) were determined at 12.5 spectra s(-1) in the full spectrum mode.

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Electron ionization in superimposed magnetic and radio frequency quadrupolar electric fields.

An improved design of a novel electron ionization source for orthogonal acceleration time-of-flight mass spectrometry is described, based on the superimposition of an axial magnetic field with cylindrical symmetry around a radio frequency-only quadrupole. A tubular permanent magnet was designed to generate the required strong magnetic field and field profile. An axial electric field along the ion guide for efficient ion extraction was introduced using segmented quadrupole rods. Details of the source design and the effects of various operating parameters are described. The source produces high-quality mass spectra with regard to fragmentation, relative abundances, and isotopic ratios. Preliminary results have shown excellent sensitivity, with limits of detection in the subfemtogram range (octafluoronaphthalene, full spectrum acquisition) in gas chromatography/mass spectrometry operation.

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Prediction of gas-phase reduced ion mobility constants (K0).

A method of predicting reduced ion mobility values, K0, for use in ion mobility spectrometry is described. While the method is very similar to a previously reported method based on a neural network, the method described in this paper uses a purely statistical regression approach. Furthermore, it has been applied to a wider class of compounds, including chemical agents. Various molecular parameters were evaluated in the predictive model to determine the qualitative dynamics that have the greatest effect on K0. An R2 value of 80.1% was obtained when calculated K0 values were plotted against measured K0 values for 162 compounds for which experimental K0 values were available. However, when chloroacetophenone and 3-xylyl bromide (3-methylbenzyl bromide) were removed from the set due to their large residual values, the predictability increased to an R2 value of 87.4%. This compares well with the value of 88.7%, which was obtained in a regression step of a previous neural network study for a less diverse set of 168 compounds.

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Incorporation of a venturi device in electrospray ionization.

Electrospray ionization has grown to be one of the most commonly used ionization techniques for mass spectrometry, and efforts continue to improve its performance. Typically, the sprayer tip must be very close to the entrance orifice of the mass spectrometer in order to maximize the conduction of ions from the sprayer into the mass spectrometer. However, because of space-charge repulsion, most ions never reach the sampling orifice. In this work, an industrial air amplifier, for which the working mechanism is based on venturi and coanda effects, was added between an electrospray ionization source and a time-of-flight mass spectrometer. When a series of reserpine solutions (0.5, 1.0, 5.0, and 10.0 microM) were monitored using mass spectrometry, an over 5-fold increase in m/z 609.3 ion intensity was measured for a separation distance of 14 mm between the electrospray tip and interface capillary inlet, as compared to when the electrospray tip was in its normal position 1 mm in front of the inlet without the amplifier. When a voltage was applied to the air amplifier to further assist in focusing the electrosprayed ions, an approximately 18-fold increase in m/z 609.3 ion intensity was obtained. In addition, a 34-fold reduction in method detection limit was observed.

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