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The Development and Application of Capillary Absorption Cells

Description: Abstract: "Various types of capillary absorption cells have been constructed from a variety of materials. These cells, having volumes as low as 160 microliters, have been used to increase the sensitivity of several colorimetrics methods as much as 1000 fold without appreciable loss of accuracy. Small volumes of solution must be used in order to concentrate the colored material present."
Date: 1951
Creator: Rosenfels, R. S.; Kirk, P. L.; Kitson, R. E.; Patton, R. L. & Curtis, R. E.
Partner: UNT Libraries Government Documents Department

Temperature Dependence of the Absolute Third-order Rate Constant for the Reaction between Na + O₂ + N₂ over the Range 571 - 1016 K Studied by Time-resolved Atomic Resonance Absorption Spectroscopy

Description: Article on temperature dependence of the absolute third-order rate constant for the reaction between Na + O₂ + N₂ over the range 571-1016 K studied by time-resolved atomic resonance absorption spectroscopy.
Date: 1985
Creator: Husain, David; Marshall, Paul & Plane, John M. C.
Partner: UNT College of Arts and Sciences

Measuring Atmospheric Ozone and Nitrogen Dioxide Concentration by Differential Optical Absorption Spectroscopy

Description: The main objective was to develop a procedure based on differential optical absorption spectroscopy (DOAS) to measure atmospheric total column of ozone, using the automated instrument developed at the University of North Texas (UNT) by Nebgen in 2006. This project also explored the ability of this instrument to provide measurements of atmospheric total column nitrogen dioxide. The instrument is located on top of UNT’s Environmental Education, Science and Technology Building. It employs a low cost spectrometer coupled with fiber optics, which are aimed at the sun to collect solar radiation. Measurements taken throughout the day with this instrument exhibited a large variability. The DOAS procedure derives total column ozone from the analysis of daily DOAS Langley plots. This plot relates the measured differential column to the airmass factor. The use of such plots is conditioned by the time the concentration of ozone remains constant. Observations of ozone are typically conducted throughout the day. Observations of total column ozone were conducted for 5 months. Values were derived from both DOAS and Nebgen’s procedure and compared to satellite data. Although differences observed from both procedures to satellite data were similar, the variability found in measurements was reduced from 70 Dobson units, with Nebgen’s procedure, to 4 Dobson units, with the DOAS procedure.A methodology to measure atmospheric nitrogen dioxide using DOAS was also investigated. Although a similar approach to ozone measurements could be applied, it was found that such measurements were limited by the amount of solar radiation collected by the instrument. Observations of nitrogen dioxide are typically conducted near sunrise or sunset, when solar radiation experiences most of the atmospheric absorption.
Date: December 2011
Creator: Jerez, Carlos J.
Partner: UNT Libraries

Detection and Quantification of Pu(III, IV, V, and VI) Using a1.0-meter Liquid Core Waveguide

Description: Detection and quantification of the aquo ions of Pu in 1 MHClO4 was carried out using a 1-meter liquid core waveguide (LCW) coupledto a fiber optic UV-Vis spectrometer. Detection limits of 7 x 10-7 M forPu(VI), 1.6 x 10-5 M for Pu(V), 5 x 10-6 M for Pu(IV) and 8 x 10-6 M forPu(III) were achieved. The limits of detection represent increases of 18to 33 times those achievable using a conventional 1-cm path length.Because of the much lower detection limits of the LCW, routineidentification of the oxidation states in dilute Pu solutions can bemade.
Date: February 15, 2005
Creator: Wilson, Richard E.; Hu, Yung-Jin & Nitsche, Heino
Partner: UNT Libraries Government Documents Department

Ultrafast and nonlinear optical characterization of optical limiting processes in fullerenes

Description: The authors present recent results of broadband femotosecond (fs) transient absorption (TA) and broadband nanosecond (ns) optical limiting (OL) studies of C{sub 60} and derivatized C{sub 60}. Improvements in measurement techniques for fs TA spectra provide sensitivity to 10{sup {minus}5} in differential transmission, allowing detailed comparison of excited-state spectra with established energy level diagrams, as well as comparison of the ratio of triplet to singlet excited-state absorption cross sections from TA spectra with those obtained by modeling time transients at different wavelengths. For derivatized fullerenes, which provide enhanced solubility and a ground-state absorption extended into the infrared compared with C{sub 60} there is no spectral region where the triplet absorption cross section dominates the singlet as strongly as demonstrating broadband limiting in all 6, 6 mono-adducts and neat C{sub 60}. The authors report new approaches to processing sol-gel encapsulated fullerenes to improve the OL performance of solid-state materials to approach the response of solution limiters.
Date: October 1, 1997
Creator: Kohlman, R.; Klimov, V. & Shi, X.
Partner: UNT Libraries Government Documents Department

Recent advances in the measurement of high temperature bimolecular rate constants

Description: Recent advances in the measurement of high temperature reaction rate constants are discussed. The studies carried out by shock tube methods are particularly considered because these results are important not only in theoretical chemical kinetics but also in practical applications. The work on 5 chemical reactions are reviewed in detail. These are: D + H{sub 2}, Cl + H{sub 2}, H + O{sub 2}, CH{sub 3} + CH{sub 3}, and H + NO{sub 2}.
Date: July 1, 1995
Creator: Michael, J.V.
Partner: UNT Libraries Government Documents Department

Probing Compositional Variation within Hybrid Nanostructures

Description: We present a detailed analysis of the structural and magnetic properties of solution-grown PtCo-CdS hybrid structures in comparison to similar free-standing PtCo alloy nanoparticles. X-ray absorption spectroscopy is utilized as a sensitive probe for identifying subtle differences in the structure of the hybrid materials. We found that the growth of bimetallic tips on a CdS nanorod substrate leads to a more complex nanoparticle structure composed of a PtCo alloy core and thin CoO shell. The core-shell architecture is an unexpected consequence of the different nanoparticle growth mechanism on the nanorod tip, as compared to free growth in solution. Magnetic measurements indicate that the PtCo-CdS hybrid structures are superparamagnetic despite the presence of a CoO shell. The use of X-ray spectroscopic techniques to detect minute differences in atomic structure and bonding in complex nanosystems makes it possible to better understand and predict catalytic or magnetic properties for nanoscale bimetallic hybrid materials.
Date: June 22, 2010
Creator: Yuhas, Benjamin D.; Habas, Susan E.; Fakra, Sirine C. & Mokari, Taleb
Partner: UNT Libraries Government Documents Department

Effects of backlight structure on absorption experiments

Description: The impact of spectral details in the backlight of absorption spectroscopy experiments is considered. It is shown that experimentally unresolved structure in the backlight spectrum can introduce significant errors in the inferred transmission. Furthermore, it is shown that a valuable experimental procedure previously used to test the accuracy of the data fails to reveal these errors.
Date: November 8, 2004
Creator: Iglesias, C A
Partner: UNT Libraries Government Documents Department

Effect of Mn Substitution for Multiferroic BiFeO3 Probed by High-Resolution Soft-X-Ray Spectroscopy

Description: The electronic structures of BiFeO{sub 3} (BF) and Mn-doped BiFeO{sub 3} (BF(Mn)) have been studied by X-ray absorption spectroscopy (XAS) and soft-X-ray emission spectroscopy (SXES). The BF and BF(Mn) have the mixed valence state of Fe{sup 2+} and Fe{sup 3+}. The valence band is mainly composed of O 2p state hybridized with the majority-spin t{sub 2g} and e{sub g} orbitals of Fe 3d state. The conduction band is composed of the minority-spin t{sub 2g} and e{sub g} orbitals of Fe 3d. The band gaps of BF and BF(Mn) are estimated to be 1.3 eV and 2.7 eV, respectively. The increase of band gap with Mn substitution contributes to the change of bandwidth of valence band.
Date: July 11, 2008
Creator: Higuchi, Tohru; Higuchi, T.; Hattori, T.; Sakamoto, W.; Itoh, N.; Shimura, T. et al.
Partner: UNT Libraries Government Documents Department

Electronic Structure of the ID Conductor K0.3MoO3 studied using resonant inelastic x-ray scattering and soft x-ray emission spectroscopy

Description: The electronic structure of the quasi-one dimensional conductor K{sub 0.3}MoO{sub 3} has been measured using high resolution resonant inelastic x-ray scattering and x-ray absorption spectroscopy. The data is compared to that from the related two dimensional insulator {alpha}-MoO{sub 3}. Scattering features are observed from both oxides that are explained in terms of the band momentum selectivity of the scattering process, allowing a comparison of the scattering data to recent band structure calculations.
Date: September 24, 2008
Creator: Learmonth, T.; Glans, P.-A.; McGuinness, C.; Plucinski, L.; Zhang, Y.; Guo, J.-H. et al.
Partner: UNT Libraries Government Documents Department

X-ray absorption spectroscopy on the calcium cofactor to the manganese cluster in photosynthetic oxygen evolution

Description: Along with Mn, calcium and chloride ions are necessary cofactors for oxygen evolution in Photosystem II (PS II). To further test and verify whether Ca is close to the Mn cluster, the authors substituted strontium for Ca and probed from the Sr point of view for any nearby Mn. The extended X-ray absorption fine structure (EXAFS) of Sr-reactivated PS II indicates major differences between the intact and NH{sub 2}OH-treated samples. In intact samples, the Fourier transform of the Sr EXAFS shows a Fourier peak that is missing in inactive samples. This peak II is best simulated by two Mn neighbors at a distance of 3.5 Angstrom, confirming the proximity of Ca (Sr) cofactor to the Mn cluster. In addition, polarized Sr EXAFS on oriented Sr-reactivated samples shows this peak II is dichroic: large magnitude at 10 degrees (angle between the PS II membrane normal and the x-ray electric field vector) and small at 80 degrees. Analysis of the dichroism yields the relative angle between the Sr-Mn vector and membrane normal (23 degrees {+-} 4 degrees), and the isotropic coordination number for these layered samples. X-ray absorption spectroscopy has also been employed to assess the degree of similarity between the manganese cluster in PS II and a family of synthetic manganese complexes containing the distorted cubane [Mn{sub 4}O{sub 3}X] core (X = benzoate, acetate, methoxide, hydroxide, azide, fluoride, chloride or bromide). In addition, Mn{sub 4}O{sub 3}Cl complexes containing three or six terminal Cl ligands at three of the Mn were included in this study. The EXAFS method detects the small changes in the core structures as X is varied in this series, and serves to exclude these distorted cubanes of C3v symmetry as a topological model for the Mn catalytic cluster. The sulfur K-edge x-ray absorption near-edge structure (XANES) spectra for ...
Date: December 16, 1999
Creator: Cinco, Roehl M.
Partner: UNT Libraries Government Documents Department

DOE/SC0001389 Final technical report: Investigation of uranium attenuation and release at column and pore scales in response to advective geochemical gradients

Description: Experimental approach Column experiments were devised to investigate the role of changing fluid composition on mobility of uranium through a sequence of geologic media. Fluids and media were chosen to be relevant to the ground water plume emanating from the former S-3 ponds at the Oak Ridge Integrated Field Research Challenge (ORIFC) site. Synthetic ground waters were pumped upwards at 0.05 mL/minute for 21 days through layers of quartz sand alternating with layers of uncontaminated soil, quartz sand mixed with illite, quartz sand coated with iron oxides, and another soil layer. Increases in pH or concentration of phosphate, bicarbonate, or acetate were imposed on the influent solutions after each 7 pore volumes while uranium (as uranyl) remained constant at 0.1mM. A control column maintained the original synthetic groundwater composition with 0.1mM U. Pore water solutions were extracted to assess U retention and release in relation to the advective ligand or pH gradients. Following the column experiments, subsamples from each layer were characterized using microbeam X-ray absorption spectroscopy (XANES) in conjunction with X-ray fluorescence mapping and compared to sediment core samples from the ORIFC, at SSRL Beam Line 2-3. Results U retention of 55 – 67 mg occurred in phosphate >pH >control >acetate >carbonate columns. The mass of U retained in the first-encountered quartz layer in all columns was highest and increased throughout the experiment. The rate of increase in acetate- and bicarbonate-bearing columns declined after ligand concentrations were raised. U also accumulated in the first soil layer; the pH-varied column retained most, followed by the increasing-bicarbonate column. The mass of U retained in the upper layers was far lower. Speciation of U, interpreted from microbeam XANES spectra and XRF maps, varied within and among the columns. Evidence of minor reduction to U(IV) was observed in the first-encountered quartz layer in ...
Date: May 13, 2013
Creator: Savage, Kaye S.; Zhu, Wenyi & Barnett, Mark O.
Partner: UNT Libraries Government Documents Department

Collision Broadening in the Microwave Rotational Spectrum of Gaseous Monomeric Formaldehyde

Description: A source-modulation microwave spectrograph was utilized to measure line width parameters for several spectral lines in the pure rotational spectrum of formaldehyde (H₂CO). The spectrograph featured high-gain ac amplification and phase-sensitive detection, and was capable of measuring microwave lines having absorption coefficients as small as 10⁻⁷ cm⁻¹ with a frequency resolution on the order of 30 kHz. Center frequencies of the measured lines varied from 4,830 MHz to 72,838 MHz; hence, most of the observations were made on transitions between K-doublets in the rotational spectrum. Corrections were applied to the measured line width parameters to account for Doppler broadening and, where possible, for deviations due to magnetic hyperfine structure in some of the K-doubled lines. Low modulation voltages and low microwave power levels were used to minimize modulation and saturation broadenings; other extraneous broadenings were found to be insignificant. The primary broadening mechanism at low gas pressure is pressure broadening, and a review of this topic is included. Line width parameters for the several observed transitions were determined by graphing half-widths versus pressure for each spectral line, and performing a linear least-squares fit to the data points. Repeatability measurements indicated the accuracy of the line width parameters to be better than ±10 percent. The reasons for this repeatability spread are discussed, Broadening of each line was measured for self- and foreign-gas broadening by atomic helium and diatomic hydrogen. Effective collision diameters were calculated for each broadening interaction, based on the observed rates of broadening.
Date: December 1973
Creator: Rogers, David Valmore
Partner: UNT Libraries

Electron transfer of carbonylmetalate radical pairs: femtosecond visible spectroscopy of optically excited ion pairs

Description: Charge transfer excitation at 640 nm of the cobaltocenium tetracarbonylcobaltate ion pair, [Cp{sub 2}Co{sup +}{vert_bar}Co(CO){sub 4}{sup -}], was monitored in 1,2- dichloroethane solution by femtosecond transient visible absorption spectroscopy. The absorption prepares a neutral radical pair that can undergo spontaneous back electron transfer, and which shows a double peaked spectrum with features at 760 and 815 nm at 3 ps delay time. Transient decay times of 5.8{+-}0.5 ps were measured by monitoring the decay of Co(CO){sub 4} at 757 nm and 780 nm, and these are assigned to the back electron transfer step. The ET kinetics are consistent with the previously reported rates of electron transfer that were measured for specific vibrational states by picosecond transient IR.
Date: February 1, 1997
Creator: Wen, X.; Spears, K.G.; Wiederrecht, G.P. & Wasielewski, M.R.
Partner: UNT Libraries Government Documents Department

Diffuse reflectance FTIR of stains on grit blasted metals

Description: Diffuse reflectance mid-infrared Fourier transform (DRIFT) spectroscopy has been applied to the detection of oil contamination on grit-blasted metals. The object of this application is to detect and discriminate between silicone and hydrocarbon oil contamination at levels approaching 10 mg/m{sup 2}. A portable FTIR spectrometer with dedicated diffuse reflectance optics was developed for this purpose. Using translation devices positioned by instructions from the spectrometer operating system, images of macroscopic substrates were produced with millimeter spatial resolution. The pixels that comprise an image are each a full mid-infrared spectrum with excellent signal-to-noise, each determined as individual files and uniquely saved to disc. Reduced spectra amplitudes, based on peak height, area, or other chemometric techniques, mapped as a function of the spatial coordinates of the pixel are used to display the image. This paper demonstrates the application of the technique to the analysis of stains on grit-blasted metals, including the calibration of the method, the inspection of substrates, and the migration of oil contamination.
Date: August 9, 1997
Creator: Powell, G.L.; Hallman, R.L. Jr. & Cox, R.L.
Partner: UNT Libraries Government Documents Department