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M B Denton

Publications and source records attributed to M B Denton.

10 recordsLinked to original sources

Read-noise characterization of focal plane array detectors via mean-variance analysis.

Mean-variance analysis is described as a method for characterization of the read-noise and gain of focal plane array (FPA) detectors, including charge-coupled devices (CCDs), charge-injection devices (CIDs), and complementary metal-oxide-semiconductor (CMOS) multiplexers (infrared arrays). Practical FPA detector characterization is outlined. The nondestructive readout capability available in some CIDs and FPA devices is discussed as a means for signal-to-noise ratio improvement. Derivations of the equations are fully presented to unify understanding of this method by the spectroscopic community.

Algorithms↗

Fluorescence quenching high-performance thin-layer chromatographic analysis utilizing a scientifically operated charge-coupled device detector.

A scientifically operated charge-coupled device detector combined with fluorescence quenching high-performance thin-layer chromatographic plates was employed for the detection of organic compounds, The plates were excited with 254 nm light from a mercury lamp, and quantitative information was obtained from organic compounds that absorbed the optimum conditions for detection. The linear dynamic range, sensitivity, and reproducibility of the system were evaluated by quantitative analysis of famotidine, acetaminophen, caffeine, and acetylsalicylic acid. The detection limits of the system were found to be in the nanogram range.

Acetaminophen↗

Structural basis of the antagonism between inorganic mercury and selenium in mammals.

Mercuric chloride toxicity in mammals can be overcome by co-administration of sodium selenite. We report a study of the mutual detoxification product in rabbit plasma, and of a Hg-Se-S-containing species synthesized by addition of equimolar mercuric chloride and sodium selenite to aqueous, buffered glutathione. Chromatographic purification of this Hg-Se-S species and subsequent structural analysis by Se and Hg extended X-ray absorption fine structure (EXAFS) spectroscopy revealed the presence of four-coordinate Se and Hg entities separated by 2.61 A. Hg and Se near-edge X-ray absorption spectroscopy of erythrocytes, plasma, and bile of rabbits that had been injected with solutions of sodium selenite and mercuric chloride showed that Hg and Se in plasma samples exhibited X-ray absorption spectra that were essentially identical to those of the synthetic Hg-Se-S species. Thus, the molecular detoxification product of sodium selenite and mercuric chloride in rabbits exhibits similarities to the synthetic Hg-Se-S species. The underlying molecular mechanism for the formation of the Hg-Se-S species is discussed.

Animals↗

Utilization of a scientifically operated charge-coupled device detector for high-performance thin-layer chromatographic analysis of tetracyclines.

A high-performance thin-layer chromatography (HPTLC) method using a scientifically operated charge-coupled device detector is described for the assay of tetracycline pharmaceutical products. Quantitative information can be obtained for all samples on a TLC plate within a few seconds. The separation efficiency and detection limits were determined on both normal phase and reverse phase TLC plates. Fluorescence detection mode offers higher sensitivity than fluorescence quenching mode. The dynamic range, sensitivity, accuracy and precision of the system were evaluated. Detection limits of the impurities are in the range of 0.1 to 0.5 ng or 0.3 to 1% of tetracycline, depending on the compound, with a recovery percentage over 85%. The existing impurities in tetracycline capsules were determined using both HPLC and HPTLC techniques. All of the impurities were below the regulation level.

Anti-Bacterial Agents↗

Stability studies of tetracycline in methanol solution.

The stability of tetracycline in methanol solution was investigated by UV-visible spectroscopy, HPLC and TLC methods. After dissolution in methanol, tetracycline decomposed rapidly under the influence of light and atmospheric oxygen, forming more than fourteen different degradation products. None of the previously reported degradation products, such as the epi- and anhydro-compounds, were detected as the final degradation products. The molecular structures for eight of the compounds were suggested by their product-ion mass spectra. A degradation sequence was proposed for the reactions of tetracycline with methanol. A new HPLC-MS mobile phase was developed, which solved the clogging problem at the interface between the HPLC and MS chamber and enabled a high separation efficiency.

Chromatography, High Pressure Liquid↗

Application of energy-resolved measurements to Laue diffraction: determination of unit-cell parameters, deconvolution of harmonics and assignment of systematic absences.

The use of energy-resolved area detection of Laue diffraction patterns for the determination of unit-cell parameters and systematic absences is demonstrated. Seven different crystals having previously known unit cells were re-examined using Laue diffraction methods. These crystals included four different crystal systems including cubic, orthorhombic, tetragonal and monoclinic cells. The crystals had cell sizes ranging from 179.4 to 4588.3 A(3). Comparison of known and re-determined cells showed good agreement (ratio of known to measured cells = 0.987 +/- 0.18). A single procedure was suitable for all unit-cell determinations. The accuracy of the method is presently limited by the quality of the available energy measurements. Some of the crystals represent space groups containing systematic absences normally obscured by harmonic overlap when using the Laue method. These include absences due to 2(1) screw axes (h, k or 1 = 2n + 1) and cell centering (h + k = 2n + 1). All systematic absences were identified using a combination of multiple linear regression with either stepwise elimination or stepwise inclusion and an F test for assignment of systematic absence. The methods are discussed in detail and simulations are used to evaluate critical tolerances for future systems.

Journal Article↗

A foil-mask spectrometer for laue pattern imaging: simultaneous position, intensity and energy.

An X-ray spectrometer for simultaneous position, intensity and energy determinations suitable for Laue diffraction applications is described. The foil-mask spectrometer consists of a series of metal foils of varying composition and thickness which are used to modulate the energy distribution of an incident X-ray source. Three modes of operation are described: a high-resolution spectrometer for measurement of nearly monochromatic X-rays, an intensity discriminator for partitioning the intensity from a small number of spatially overlapped monochromatic X-ray sources, and a low-resolution spectrometer for polychromatic X-rays with broad spectral features. The first mode of operation is designed to allow the energy of monochromatic Laue reflections to be measured with a resolution suitable for determination of unit-cell parameters. The second mode of operation is designed to allow the intensity of each component in a spatial region containing overlapping orders or spatially overlapped reflections to be discriminated for use in refinements or space-group assignment. The third mode of operation is described for completeness. The theory behind each mode of operation is described. The energy resolution of the spectrometer improves with the square root of the intensity of the incident beam. It also increases linearly with the change in energy with respect to transmission efficiency of a particular foil. In theory, the resolution of the spectrometer can readily exceed 50 eV over a wide range of energies depending on the foils used and the incident X-ray photon flux. Determinations of the energies of Mo Kalpha and Cu Kalpha radiation using a first-generation ten-foil spectrometer gave values of 17.5 +/- 0.1 and 8.08 +/- 0.05 keV, respectively. Treatment of random error shows good correspondence with a Poisson model. The use of this spectrometer is demonstrated using a sample of tetraphenylphosphonium tetrachlorooxomolybdenum(V). Comparison of predicted and observed energies shows good agreement over a wide range of energies. The ratio of predicted to measured energy for the first 50 measurements was 0.9918+/-0.0344. Up to three components of a position having harmonic overlap were separated. This work demonstrates the feasibility of using Laue diffraction to completely determine the crystal structure of a molecule without recourse to monochromatic methods.

Journal Article↗

Evaluation of charge-injection devices for use in laue diffraction imaging.

Charge-injection devices (CIDs) are versatile detectors having a number of features which recommend them for use in the imaging of X-ray diffraction patterns. They have a flexible nondestructive readout allowing for analysis of image quality during data collection and rapid readout of selected portions of the device. CIDs have full-well capacities in the range of 10(6) charge carriers giving them a high dynamic range for both direct and indirect imaging of X-rays. CIDs have peak quantum efficiencies in the optical region over 50% allowing for their incorporation into indirect detection systems. Rapid random single-pixel address allows for their use as single X-ray photon counters with energy discrimination. Three types of position-sensitive detectors for X-rays have been developed using CIDs. Two CID formats, the CID 17PPRA (388 x 256) and the CID 38SG (512 x 512), were incorporated into systems performing indirect imaging, direct imaging and single X-ray photon counting with energy discrimination. Indirect images of the Laue diffraction patterns from tetraphenylphosphonium tetrachlorooxomolybdenum(V) and natural MoS(2) were collected using a phosphor sheet to convert X-rays into optical photons which were detected with the CID 38SG. Directly detected images of spots from the Laue diffraction pattern of MoS(2) were recorded with the CID 17PPRA. Single photon counting with energy discrimination is demonstrated with the CID 17PPRA using a reflection from the Laue diffraction pattern of MoS(2). Useful information could be obtained from a single pixel at read rates over 7 kHz. Complete energy-dispersive analysis suitable for determination of space groups from Laue diffraction is currently limited due to incomplete charge collection and/or split events.

Journal Article↗