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At least 37 records · Page 2

Chapter 10: Experimental Methods for the Determination of Parameters. In the book Multiphase Catalytic Reactors: Theory, Design, Manufacturing, and Applications.

The determination of kinetic parameters is a key element in catalyst research and multiphase catalytic process development. In this chapter, the experimental methods used to determine kinetic parameters, the nature of the parameters, and the areas of application and advantages of the different experimental approaches are discussed. Emphasis is placed on transient techniques and methods that provide intrinsic kinetic parameters, i.e., parameters that can be directly linked to the surface composition/structure of a heterogeneous catalyst.

02 PETROLEUM↗

Photoporomechanics: An Experimental Method to Visualize the Effective Stress Field in Fluid-Filled Granular Media

Effective stress governs the mechanical behavior of porous media. In this study, we use photoelasticimetry to visualize the evolving effective stress field in fluid-filled granular media in processes that couple fluid flow and mechanical deformation. We refer to this experimental method as photoporomechanics. We develop a fabrication process to produce millimeter-scale residual-stress-free photoelastic spheres with high geometric accuracy. We use color to quantify the forces acting on the particles over a wide range of forces, while using light intensity for a small range of forces. We then provide an application of photoporomechanics to illustrate the evolution of effective stress during one-dimensional consolidation: a process by which the stresses caused by a sudden load are gradually transmitted through a fluid-filled granular pack as the fluid drains and excess pore pressures dissipate. We report our technique provides a powerful experimental model system to study the grain-scale underpinning of coupled solid-fluid processes in granular media.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

A discussion on various experimental methods of impact ionization coefficient measurement in GaN

Impact ionization coefficients play a critical role in semiconductors. In addition to silicon, silicon carbide and gallium nitride are important semiconductors that are being seen more as mainstream semiconductor technologies. As a reflection of the maturity of these semiconductors, predictive modeling has become essential to device and circuit designers, and impact ionization coefficients play a key role here. Recently, several studies have measured impact ionization coefficients. We dedicated the first part of our study to comparing three experimental methods to estimate impact ionization coefficients in GaN, which are all based on photomultiplication but feature characteristic differences. The first method inserts an InGaN hole-injection layer, the accuracy of which is challenged by the dominance of ionization in InGaN, leading to possible overestimation of the coefficients. The second method utilizes the Franz–Keldysh effect for hole injection but not for electrons, where the mixed injection of induced carriers would require a margin of error. The third method uses complementary p–n and n–p structures that have been at the basis of this estimation in Si and SiC and leans on the assumption of a constant electric field, and any deviation would require a margin of error. In the second part of our study, we evaluated the models using recent experimental data from diodes demonstrating avalanche breakdown.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

A new experimental method for the accelerated characterization of composite materials

The use of composite materials for a variety of practical structural applications is presented and the need for an accelerated characterization procedure is assessed. A new experimental and analytical method is presented which allows the prediction of long term properties from short term tests. Some preliminary experimental results are presented.

Yeow, Y. T.↗

TiO{sub 2} synthesized by microwave assisted solvothermal method: Experimental and theoretical evaluation

In this study, a microwave assisted solvothermal method was used to synthesize TiO{sub 2} with anatase structure. The synthesis was done using Ti (IV) isopropoxide and ethanol without templates or alkalinizing agents. Changes in structural features were observed with increasing time of synthesis and evaluated using periodic quantum chemical calculations. The anatase phase was obtained after only 1 min of reaction besides a small amount of brookite phase. Experimental Raman spectra are in accordance with the theoretical one. Micrometric spheres constituted by nanometric particles were obtained for synthesis from 1 to 30 min, while spheres and sticks were observed after 60 min. - Graphical abstract: FE-SEM images of anatase obtained with different periods of synthesis associated with the order–disorder degree. Display Omitted - Highlights: • Anatase microspheres were obtained by the microwave assisted hydrothermal method. • Only ethanol and titanium isopropoxide were used as precursors during the synthesis. • Raman spectra and XRD patterns were compared with quantum chemical calculations. • Time of synthesis increased the short-range disorder in one direction and decreased in another.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Experimental methods for laboratory measurements of helium spectral line broadening in white dwarf photospheres

White Dwarf (WD) stars are the most common stellar remnant in the universe. WDs usually have a hydrogen or helium atmosphere, and helium WD (called DB) spectra can be used to solve outstanding problems in stellar and galactic evolution. DB origins, which are still a mystery, must be known to solve these problems. DB masses are crucial for discriminating between different proposed DB evolutionary hypotheses. Current DB mass determination methods deliver conflicting results. The spectroscopic mass determination method relies on line broadening models that have not been validated at DB atmosphere conditions. We performed helium benchmark experiments using the White Dwarf Photosphere Experiment (WDPE) platform at Sandia National Laboratories' Z-machine that aims to study He line broadening at DB conditions. Using hydrogen/helium mixture plasmas allows investigating the importance of He Stark and van der Waals broadening simultaneously. Accurate experimental data reduction methods are essential to test these line-broadening theories. In this paper, we present data calibration methods for these benchmark He line shape experiments. We give a detailed account of data processing, spectral power calibrations, and instrument broadening measurements. Uncertainties for each data calibration step are also derived. We demonstrate that our experiments meet all benchmark experiment accuracy requirements: WDPE wavelength uncertainties are <1 Å, spectral powers can be determined to within 15%, densities are accurate at the 20% level, and instrumental broadening can be measured with 20% accuracy. Fulfilling these stringent requirements enables WDPE experimental data to provide physically meaningful conclusions about line broadening at DB conditions.

79 ASTRONOMY AND ASTROPHYSICS↗

Sorbent, Sublimation, and Icing Modeling Methods: Experimental Validation and Application to an Integrated MTSA Subassembly Thermal Model

This paper details the validation of modeling methods for the three core components of a Metabolic heat regenerated Temperature Swing Adsorption (MTSA) subassembly, developed for use in a Portable Life Support System (PLSS). The first core component in the subassembly is a sorbent bed, used to capture and reject metabolically produced carbon dioxide (CO2). The sorbent bed performance can be augmented with a temperature swing driven by a liquid CO2 (LCO2) sublimation heat exchanger (SHX) for cooling the sorbent bed, and a condensing, icing heat exchanger (CIHX) for warming the sorbent bed. As part of the overall MTSA effort, scaled design validation test articles for each of these three components have been independently tested in laboratory conditions. Previously described modeling methodologies developed for implementation in Thermal Desktop and SINDA/FLUINT are reviewed and updated, their application in test article models outlined, and the results of those model correlations relayed. Assessment of the applicability of each modeling methodology to the challenge of simulating the response of the test articles and their extensibility to a full scale integrated subassembly model is given. The independent verified and validated modeling methods are applied to the development of a MTSA subassembly prototype model and predictions of the subassembly performance are given. These models and modeling methodologies capture simulation of several challenging and novel physical phenomena in the Thermal Desktop and SINDA/FLUINT software suite. Novel methodologies include CO2 adsorption front tracking and associated thermal response in the sorbent bed, heat transfer associated with sublimation of entrained solid CO2 in the SHX, and water mass transfer in the form of ice as low as 210 K in the CIHX.

Bower, Chad↗

On the Use of Experimental Methods to Improve Confidence in Educed Impedance

Results from impedance eduction methods developed by NASA Langley Research Center are used throughout the acoustic liner community. In spite of recent enhancements, occasional anomalies persist with these methods, generally at frequencies where the liner produces minimal attenuation. This investigation demonstrates an experimental approach to educe impedance with increased confidence over a desired frequency range, by combining results from successive tests with different cavity depths. A series of tests is conducted with three wire-mesh facesheets, for which the results should be weakly dependent on source sound pressure level and mean grazing flow speed. First, a raylometer is used to measure the DC flow resistance of each facesheet. These facesheets are then mounted onto a frame and a normal incidence tube is used to determine their respective acoustic impedance spectra. A comparison of the acoustic resistance component with the DC flow resistance for each facesheet is used to validate the measurement process. Next, each facesheet is successively mounted onto three frames with different cavity depths, and a grazing flow impedance tube is used to educe their respective acoustic impedance spectra with and without mean flow. The no-flow results are compared with those measured in the normal incidence tube to validate the impedance eduction method. Since the anti-resonance frequency varies with cavity depth, each sample provides robust results over a different frequency range. Hence, a combination of results can be used to determine the facesheet acoustic resistance. When combined with the acoustic reactance, observed to be weakly dependent on the source sound pressure level and grazing flow Mach number, the acoustic impedance can be educed with increased confidence. Representative results of these tests are discussed, and the complete database is available in electronic format upon request.

Jones, Michael G.↗

Experimental Methods in Reduced-gravity Soldering Research

The National Center for Microgravity Research, NASA Glenn Research Center, and NASA Johnson Space Center are conducting an experimental program to explore the influence of reduced gravity environments on the soldering process. An improved understanding of the effects of the acceleration environment is important to application of soldering during current and future human space missions. Solder joint characteristics that are being considered include solder fillet geometry, porosity, and microstructural features. Both through-hole and surface mounted devices are being investigated. This paper focuses on the experimental methodology employed in this project and the results of macroscopic sample examination. The specific soldering process, sample configurations, materials, and equipment were selected to be consistent with those currently on-orbit. Other apparatus was incorporated to meet requirements imposed by operation onboard NASA's KC-135 research aircraft and instrumentation was provided to monitor both the atmospheric and acceleration environments. The contingent of test operators was selected to include both highly skilled technicians and less skilled individuals to provide a population cross-section that would be representative of the skill mix that might be encountered in space mission crews.

Pettegrew, Richard D.↗

MnNiO 3 revisited with modern theoretical and experimental methods

MnNiO 3 is a strongly correlated transition metal oxide that has recently been investigated theoretically for its potential application as an oxygen-evolution photocatalyst. However, there is no experimental report on critical quantities such as the band gap or bulk modulus. Recent theoretical predictions with standard functionals such as LDA+U and HSE show large discrepancies in the band gaps (about 1.23 eV), depending on the nature of the functional used. Hence there is clearly a need for an accurate quantitative prediction of the band gap to gauge its utility as a photocatalyst. In this work, we present a diffusion quantum Monte Carlo study of the bulk properties of MnNiO 3 and revisit the synthesis and experimental properties of the compound. We predict quasiparticle band gaps of 2.0(5) eV and 3.8(6) eV for the majority and minority spin channels, respectively, and an equilibrium volume of 92.8 Å 3 , which compares well to the experimental value of 94.4 Å 3 . A bulk modulus of 217 GPa is predicted for MnNiO 3 . As a result, we rationalize the difficulty for the formation of ordered ilmenite-type structure with specific sites for Ni and Mn to be potentially due to the formation of antisite defects that form during synthesis, which ultimately affects the physical properties of MnNiO 3 .

36 MATERIALS SCIENCE↗

Swept shock/boundary-layer interactions: Scaling laws, flowfield structure, and experimental methods

A general review is given of several decades of research on the scaling laws and flowfield structures of swept shock wave/turbulent boundary layer interactions. Attention is further restricted to the experimental study and physical understanding of the steady-state aspects of these flows. The interaction produced by a sharp, upright fin mounted on a flat plate is taken as an archetype. An overall framework of quasiconical symmetry describing such interactions is first developed. Boundary-layer separation, the interaction footprint, Mach number scaling, and Reynolds number scaling are then considered, followed by a discussion of the quasiconical similarity of interactions produced by geometrically-dissimilar shock generators. The detailed structure of these interaction flowfields is next reviewed, and is illustrated by both qualitative visualizations and quantitative flow images in the quasiconical framework. Finally, the experimental techniques used to investigate such flows are reviewed, with emphasis on modern non-intrusive optical flow diagnostics.

Settles, Gary S.↗

New theoretical and experimental methods for pressure broadened linewidths and their interpretation

A review of recent progress in the theory of collisional line broadening, particularly the impact of recent advances in collision dynamics calculations is presented. Some new approaches to the interpretation of experimentally measured linewidths and their impact on planetary atmosphere research are discussed. Experimental techniques which may have some advantage in providing pressure broadening data at very low temperatures are also mentioned.

Gelfand, J. J.↗

An Experimental Method to Measure Gaseous Diffusivity in Tight and Partially Saturated Porous Media via Continuously Monitored Mass Spectrometry

Detection of radioxenon and radioargon produced by underground nuclear explosions is one of the primary methods by which the Comprehensive Nuclear-Test–Ban Treaty (CTBT) monitors for nuclear activities. However, transport of these noble gases to the surface via barometric pumping is a complex process relying on advective and diffusive processes in a fractured porous medium to bring detectable levels to the surface. To better understand this process, experimental measurements of noble gas and chemical surrogate diffusivity in relevant lithologies are necessary. However, measurement of noble gas diffusivity in tight or partially saturated porous media is challenging due to the transparent nature of noble gases, the lengthy diffusion times, and difficulty maintaining consistent water saturation. Here, the quasi-steady-state Ney–Armistead method is modified to accommodate continuous gas sampling via effusive flow to a mass spectrometer. An analytical solution accounting for the cumulative sampling losses and induced advective flow is then derived. Experimental results appear in good agreement with the proposed theory, suggesting the presence of retained groundwater reduces the effective diffusivity of the gas tracers by 10–1000 times. Finally, by using a mass spectrometer, the method described herein is applicable to a broad range of gas species and porous media.

47 OTHER INSTRUMENTATION↗

A proposed experimental method for interpreting Doppler effect measurements and determining their precision

The principal problem in the measurement of the Doppler reactivity effect is separating it from the thermal reactivity effects of the expansion of the heated sample. It is shown in this proposal that the thermal effects of sample expansion can be experimentally determined by making additional measurements with porous samples having the same mass and/or volume as the primary sample. By combining these results with independent measurements of the linear temperature coefficient and the computed temperature dependence of the Doppler coefficient the magnitude of the Doppler coefficient may be extracted from the data. These addiational measurements are also useful to experimentally determine the precision of the reactivity oscillator technique used to measure the reactivity effects of the heated sample.

Klann, P. G.↗

Confined-Pyrolysis as an Experimental Method for Hydrothermal Organic Synthesis

A closed pyrolysis system has been developed as a tool for studying the reactions of organic compounds under extreme hydrothermal conditions. Small high pressure stainless steel vessels in which the ratio of sediment or sample to water has been adjusted to eliminate the headspace at peak experimental conditions confines the organic components to the bulk solid matrix and eliminates the partitioning of the organic compounds away from the inorganic components during the experiment. Confined pyrolysis experiments were performed to simulate thermally driven catagenetic changes in sedimentary organic matter using a solids to water ratio of 3.4 to 1. The extent of alteration was measured by monitoring the steroid and triterpenoid biomarkers and polycyclic aromatic hydrocarbon distributions. These pyrolysis experiments duplicated the hydrothermal transformations observed in nature. Molecular probe experiments using alkadienes, alkenes and alkanes in H2O and D2O elucidated the isomerization and hydrogenation reactions of aliphatic and the competing oxidative reactions occurring under hydrothermal conditions. This confined pyrolysis technique is being applied to test experiments on organic synthesis of relevance to chemical evolution for the origin of life.

Leif, Roald N.↗

Experimental methods to test photoionized plasma models in emission

The expanding foil photoionized plasma platform was developed on the Z-machine at Sandia National Laboratories to produce terrestrial photoionized plasmas at some of the same conditions as those observed in astrophysical black hole accretion disks. The specific scientific goals of the platform are motivated by long-standing astrophysical puzzles related to accreting black hole systems. Ultimately, the experimental goal is to inform the supersolar Fe abundance problem by testing photoionized plasma models in emission with at-parameter laboratory data. High quality high resolution emission data with absolute intensity calibration from a laboratory photoionized plasma have never been collected prior to the experiments described here, providing broader motivation. A robust test of the model predictions requires the successful production of a laboratory photoionized plasma along with measurements of the supporting model inputs including the radiation drive spectrum used to create the photoionized plasma, the electron density, and the temperature. The measured absolute spectral radiance in emission collected from the independently diagnosed plasma can be compared against model calculations performed using the measured inputs. In this paper, we focus on the experimental platform and the model inputs, specifically detailing the methodology used to measure the plasma conditions. The moderate electron temperature of ∼41 eV ± 15 eV and electron density of ∼1e19 ± 1.6e18 e−/cm3 and the ∼3e12 W/cm2 x-ray irradiance at the sample confirm that photoionization dominates the plasma ionization and spectra.

Cho, P. B. (ORCID:0000000291632905)↗

Experimental Methods for the Performance Test of Environment-Assisted Cracking (EAC) in Nuclear Industry and Examples through NSUF

Environmentally assisted cracking (EAC) is a critical failure mode in nuclear reactor environments, where materials are exposed to high temperatures, radiation, and corrosive media. Specific EAC studies in nuclear environments include stress corrosion cracking in primary water chemistry, irradiation-assisted stress corrosion cracking (IASCC) under neutron exposure, and hydrogen induced cracking (HIC) in reactor pressure vessels. The experimental methodologies of EAC include slow strain rate testing (SSRT), constant load, and cyclic loading techniques, conducted in autoclaves designed to simulate the reactor’s operational environments. This paper highlights several experimental case studies, especially on IASCC, conducted within the Nuclear Science User Facilities (NSUF).

36 - MATERIALS SCIENCE↗