Biomedical subjects
Gary M Hieftje
Publications and source records attributed to Gary M Hieftje.
Directly digital flow controller.
An improved directly digital flow controller is evaluated for its ability to modulate gas flow rates. As in the older device, the "GasDAC" (named for its similarity to a weighted-resistor digital-to-analog converter) is capable of controlling gas flow in a linear and reproducible manner with the advantage of having an adjustable range of flow rates. The new design incorporates venting to prevent "puffing" when the individual flow channels are opened. The temporal characteristics of the GasDAC are also examined; modulation frequencies of 10 Hz with various types of waveforms are possible with the new device.
Plasma-source mass spectrometry for speciation analysis: state-of-the-art.
Current and emerging capabilities of plasma-source mass spectrometry (PS-MS) as it is employed for elemental speciation analysis are reviewed. Fundamental concepts and their advantageous aspects, experimental conditions, and analytical performance are described and illustrated by recent examples from the literature. Novel instrumentation, techniques, and strategies for inductively-coupled plasma mass spectrometry (ICP-MS), microwave-induced plasma (MIP) mass spectrometry, glow-discharge (GD) mass spectrometry, and electrospray ionization (ESI), among others, are described. The use of ionization sources that provide tunable ionization, others that can be modulated between different sets of operating conditions, and others used in parallel is also examined.
Simultaneous multichannel mass-specific detection for high-performance liquid chromatography using an array detector sector-field mass spectrometer.
The use of a separation step, such as liquid chromatography, prior to inductively coupled plasma mass spectrometry (ICP-MS) has become a common tool for highly selective and sensitive analyses. This type of coupling has several benefits including the ability to perform speciation analysis or to remove isobaric interferences. Several limitations of conventional instruments result from the necessity to scan or pulse the mass spectrometer to obtain a complete mass spectrum. When the instrument is operated in such a non-continuous manner, duty cycle is reduced, resulting in poorer absolute limits of detection. Additionally, with scanning instruments, spectral skew can be introduced into the measurement, limiting quantitation accuracy. To address these shortcomings, a high-performance liquid chromatograph has been coupled to an ICP-MS capable of continuous sample introduction and simultaneous multimass detection. These features have been realized with a novel detector array, the focal plane camera. Instrument performance has been tested for both speciation analysis and for the elimination of isobaric interferences. Absolute limits of detection in the sub picogram to tens of picograms regime are obtainable, while the added mass dimension introduced by simultaneous detection dramatically increases chromatographic peak capacity.
Design and characterization of a directly polarized radioluminescent light source.
The properties of several directly polarized radioluminescent light (RL) sources are described. The RL sources are composed of a [small beta]-particle-emitting (90)Sr radioisotope coupled to polarization-oriented light-emitting plastic scintillators. The polarization of the scintillator molecules was achieved through a mechanical stress applied to the polymer matrix. The emission stability of the RL sources is described. It was found that the degree of polarization of light emitted by the sources varied from zero to 26%, depending on the matrix and scintillating material. The RL source with the highest degree of polarization was constructed from polystyrene and anthracene.
Characterization of a focal plane camera fitted to a Mattauch-Herzog geometry mass spectrograph. 2. Use with an inductively coupled plasma.
A novel charge-sensitive detector array, termed the focal plane camera (FPC), has been coupled to a Mattauch-Herzog mass spectrograph (MHMS) with an inductively coupled plasma ionization source. The FPC employs an array of gold Faraday cups, each with its own charge-integrating circuit that allows the simultaneous detection of several m/z ratios. The ion-sampling interface of the MHMS has been redesigned to provide better heat transfer away from the sampler and skimmer cones and to reduce the negative effects of turbulent gas flows around the plasma. The instrument has produced limits of detection in the tens to hundreds of parts per quadrillion regime and isotope ratio accuracy and precision of 5% error and 0.007% RSD, respectively. Limits of detection with the FPC are comparable to those obtained with a single-channel secondary electron multiplier (SEM). However, the isotope ratio accuracy and precision are better with the FPC than when the SEM is employed. The dynamic range has been shown to be linear over 7 orders of magnitude.
Use of a novel array detector for the direct analysis of solid samples by laser ablation inductively coupled plasma sector-field mass spectrometry.
The use of laser ablation (LA) as a sample-introduction method for inductively coupled plasma mass spectrometry (ICP-MS) creates a powerful tool for trace elemental analysis. With this type of instrument, high analyte spatial resolution is possible in three dimensions with ng/g limits of detection and minimal sample consumption. Here, simultaneous detection is used to eliminate the correlated noise that plagues the ablation process. This benefit allows analyses to be performed with single laser pulses, resulting in improved depth resolution, even less sample consumption, and improved measurement precision. The new instrument includes an LA sample-introduction system coupled to an ICP ionization source and a Mattauch-Herzog mass spectrograph (MHMS) fitted with a novel array detector. With this instrument, absolute limits of detection are in the tens to hundreds of fg regime and isotope-ratio precision is better than 0.02% RSD with a one-hour integration period. Finally, depth-profile analysis has been performed with a depth resolution of 5 nm per ablation event.
Our remembrances of Howard Malmstadt.
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Simultaneous or scanning data acquisition? A theoretical comparison relevant to inductively coupled plasma sector-field mass spectrometers.
The benefits of simultaneous multichannel detection over single-channel scanning detection are well established in analytical chemistry. Multichannel detection increases duty cycle, which leads to enhanced sensitivity, detection limits, and reduced analysis time. Also, multichannel detection used with either isotope-ratio or internal-standard techniques provides a mechanism to reduce the effect of multiplicative or flicker noise prevalent in plasma sources. An additional benefit of simultaneous detection is superior analysis of short-lived transient signals. Presented here is a theoretical comparison between simultaneous/continuous multichannel acquisition and single-channel scanning acquisition. To conduct this comparison, reported sensitivity, single-channel precision, and background values for commercial inductively coupled plasma sector-field mass spectrometers (ICP-SFMS) are used to generate theoretical figures of merit for both acquisition methods. Among the figures of merit that will be considered are detection limits, precision, and analysis time, particularly for multi-element or multi-isotope analysis.
Characterization of a focal plane camera fitted to a Mattauch-Herzog geometry mass spectrograph. 1. Use with a glow-discharge source.
A Mattauch-Herzog geometry mass spectrograph (MHMS) has been equipped with a novel array detector, the focal plane camera (FPC). The FPC consists of an array of gold Faraday cups, each coupled to its own integrator, with interrogation of the integrators performed by a multiplexer. The initial coupling of this instrument with a pin-type glow discharge source has provided limits of detection in the single to hundreds of nanograms per gram regime; isotope ratio accuracy and precision better than 5% error and 0.2% RSD, respectively; and a linear dynamic range of at least 6 orders of magnitude. A current weakness of the FPC is its pixel size, which limits both sensitivity and baseline resolution (to R = 130). The minimum data acquisition time for multiple images at present is 1 ms/image, with a dead time of 3.2 ms between images, which will limit the ability of the FPC to monitor extremely short transient signals.
Incorporation of an electro-optic ion detector into an improved plasma-source mass spectrograph.
Throughout the history of mass spectrometry, array detectors have been used to conduct simultaneous and continuous mass-spectrographic studies. The benefits of acquiring multichannel data through the use of an array detector are well known and include greater duty cycle, improved precision through ratioing and internal-standardization techniques, and better quantitative analysis of fast signal transients. Because of these benefits, numerous types of array-detector-based instrumentation have been developed, including optical and mass spectrometers. Presented here is the improved performance of a plasma-source Mattauch-Herzog mass spectrograph fitted with a multichannel electro-optic ion detector. A glow-discharge source is used for all measurements. Previously reported array-detector-based data for this mass spectrograph were severely limited in quality and featured extremely poor peak shapes and resolution. Several figures of merit relevant to array detectors will be presented, including sensitivity, resolution, peak shape, and abundance sensitivity, all of which have been significantly improved. Remaining negative aspects of the array-detector performance include susceptibility to a magnetic field and the absence of uniform sensitivity across the array surface.