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At least 109 records · Page 6

Quantitative Analysis of Drugs with Highly Different Concentrations of Pharmaceutical Components Using Spectral Subtraction Techniques

Two simple spectrophotometric methods were developed for determination of empagliflozin and metformin by manipulating their ratio spectra with application on a recently approved pharmaceutical combination, Synjardy® tablets. A spiking technique was used to increase the concentration of empagliflozin after extraction from the tablets to allow its simultaneous determination with metformin. Validation parameters according to ICH guidelines were acceptable over the concentration range of 2–12 μg/mL for both drugs using constant multiplication and spectrum subtraction methods. The optimized methods are suitable for QC labs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Quantitative analysis of Raman spectral parameters for carbon fibers: practical considerations and connection to mechanical properties

Although the literature on the Raman spectra of carbon fibers is vast, no consistent, robust predictive relationship between mechanical properties of carbon fibers and spectral parameters exists. This shortcoming is due to the use of numerous fitting functions to evaluate Raman spectra of carbon fibers and the inconsistencies in establishing the best fitting models in a statistically robust fashion. To address this gap, we present a comprehensive work on the Raman spectra of carbon fibers that combines a vast library of experimental data with a robust numerical analysis and a statistical evaluation of a wide range of suggested fitting models. This manuscript begins with a brief review of the commonly applied fitting models. Then, the Raman spectra of 32 commercially available polyacrylonitrile-based carbon fibers collected at excitation wavelengths 532, 633, and 785 nm are presented and the best fit for all fibers is evaluated based on several statistical criteria in conjunction with numerical calculations and physical arguments. The results suggest that high-performance fibers must be fit with at least five peaks, whereas high-tensile modulus fibers are best fit with at least six distinct peaks. Finally, we employ simultaneous fitting of the Raman spectra of specific fibers and wavelengths and demonstrate that strong correlations exist between mechanical properties and the D1 peak position and shape across the range of evaluated mechanical properties. Finally, we suggest straightforward improvements in fitting analysis procedures that can be implemented to increase coherency in the understanding of the underlying carbon fiber microstructure intuited from Raman spectroscopy.

36 MATERIALS SCIENCE↗

Effects of digestion, chemical separation, and deposition on Po-210 quantitative analysis

Polonium-210 is a radioactive isotope often used to study sedimentation processes, food chains, aerosol behavior, and atmospheric circulations related to environmental sciences. Materials for the analysis of Po-210 range from tobacco leaves or cotton fibers, to soils and sediments. The purpose of this work was to determine polonium losses from a variety of sample types (soil, cotton fiber, and air filter) due to digestion technique, chemical separation, and deposition method for alpha energy analysis. Results demonstrated that yields from a perchloric acid wet-ash were similar to that from a microwave digestion. Both were greater than the dry-ash procedure. The polonium yield from the perchloric acid wet ash was 87 ± 5%, the microwave digestion had a yield of 100 ± 7%, and the dry ash had a yield of 38 ± 5%. The chemical separation of polonium by an anion exchange resin was used only on the soil samples due to the complex nature of this sample. The yield of Po-209 tracer after chemical separation and deposition for alpha analysis was 83 ± 7% for the soil samples. Spontaneous deposition yields for the cotton and air filters were 87 ± 4% and 92 ± 6%, respectively. Based on the overall process yields for each sample type the amount of Po-210 was quantified using alpha energy analysis. The soil contained 0.18 ± 0.08 Bq/g, the cotton swipe contained 0.7 mBq/g, and the air filter contained 0.04 ± 0.02 mBq/g. High and robust yields of polonium are possible using a suitable digestion, separation, and deposition method.

Seiner, Brienne N.↗

Quantitative Analysis of Micro-structural Changes in a Bituminous Coal After Exposure to Supercritical CO{sub 2} and Water

High-volatile bituminous coal samples were reacted in deionized water with supercritical CO{sub 2} (ScCO{sub 2}–water) under simulated in situ pressure and temperature conditions (8 MPa and 40 °C) in unconfined stress state for 14 days, in order to characterize potential CO{sub 2}–water–coal reactions. Micro-structural changes were identified pre- and post-experiment using X-ray powder diffraction (XRD) analysis for powdered coal (mineralogical changes), optical microscopy and scanning electron microscopy (SEM) for polished thin sections (surface feature changes) and micro-CT scanning for a small core (porosity and permeability changes). XRD analysis revealed that carbonic acid leaches out mineral matters in coal, including carbonates (calcite) and silicate minerals (albite, illite and kaolinite). Optical microscopy, SEM and CT images confirmed that the interaction of coal with ScCO{sub 2}–water causes an abundance of micro-cracks to open or propagate in unconfined coal samples. Most micro-cracks preferably propagated along maceral–mineral and maceral–maceral interfaces, which demonstrates that the micro-cracking was caused by differential swelling of different coal lithotypes. Wormhole formation was observed in coal caused by mineral dissolution and hydrocarbon mobilization, which significantly increases coal porosity compared with swelling-induced cracking. 3-D pore network models extracted from CT images show that ScCO{sub 2}–water treatment enlarges the pore and throat size, increases the numbers of pores and throats and improves pore network connectivity. Overall, CO{sub 2}–water–coal interactions under unconfined conditions enhance coal porosity, connectivity and permeability, which can be attributed to the combined effect of micro-cracking, mineral dissolution and hydrocarbon mobilization.

58 GEOSCIENCES↗

Qualitative and quantitative analysis of neutron irradiation effects in SiC/SiC composites using X-ray computed tomography

Silicon carbide fiber-reinforced silicon carbide matrix (SiC/SiC) composites are candidate materials for cladding of light water reactor (LWR) fuels. Loss of fission product gas retention due to the formation of microcrack networks is considered a potential failure mechanism for SiC/SiC-cladded fuels. In this work, a variety of SiC/SiC composite tubes were irradiated with and without an LWR-relevant radial heat flux in the High Flux Isotope Reactor, followed by detailed characterization with X-ray computed tomography (XCT). This first set of XCT data for neutron-irradiated samples confirmed that the internal stresses arising from a combination of temperature gradients and irradiation-induced swelling act as the primary driver for cracking. Consequently, while the observed cracking patterns varied depending on the tube architectures, the sharp edges of relatively large pores were found to be the common stress concentrator. These findings are useful to help improve the design and manufacturing of SiC/SiC fuel claddings for reduced failure probability.

42 ENGINEERING↗

Quantitative analysis of inclusion distributions in hot pressed silicon carbide

ABSTRACT Depth of penetration measurements in hot pressed SiC have exhibited significant variability that may be influenced by microstructural defects. To obtain a better understanding regarding the role of microstructural defects under highly dynamic conditions; fragments of hot pressed SiC plates subjected to impact tests were examined. Two types of inclusion defects were identified, carbonaceous and an aluminum-iron-oxide phase. A disproportionate number of large inclusions were found on the rubble, indicating that the inclusion defects were a part of the fragmentation process. Distribution functions were plotted to compare the inclusion populations. Fragments from the superior performing sample had an inclusion population consisting of more numerous but smaller inclusions. One possible explanation for this result is that the superior sample withstood a greater stress before failure, causing a greater number of smaller inclusions to participate in fragmentation than in the weaker sample.

36 MATERIALS SCIENCE↗

A Quantitative Analysis of the Relationship Between Radiation Therapy Use and Travel Time

Purpose: To model and quantify the relationship between radiation therapy (RT) use and travel time to RT services. Methods and Materials: Population-based registries and databases were used to identify both incident cancer patient and patients receiving RT within 1 year of diagnosis (RT1y) in British Columbia, Canada, between 1992 and 2011. The effects of age, gender, diagnosis year, income, prevailing wait time, and travel duration for RT on RT1y were assessed. Significant factors from univariate analyses were included in a multivariable logistic regression model. The shape of the travel time–RT1y curve was represented by generalized additive and segmented regression models. Analyses were conducted for breast, lung, and genitourinary cancer separately and for all cancer sites combined. Results: After adjustment for age, gender, diagnosis year, income, and prevailing wait times, increasing travel time to the closest RT facility had a negative impact RT1y. The shape of the travel time–RT1y curve varied with cancer type. For breast cancer, the odds of RT1y were constant for the first 2 driving hours and decreased at 17% per hour thereafter. For lung cancer, the odds of RT1y decreased by 16% after 20 minutes and then decreased at 6% per hour. Genitourinary cancer RT1y was relatively independent of travel time. For all cancer sites combined, the odds of RT1y were constant within the first 2 driving hours and decreased at 7% per hour thereafter. Conclusions: Travel time to receive RT has a different impact on RT1y for different tumor sites. The results provide evidence-based insights for the configuration of catchment areas for new and existing cancer centers providing RT.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

Most theoretical approaches used in nuclear astrophysics to model the nucleosynthesis of heavy elements incorporate the so-called statistical model in order to describe the excitation and decay properties of atomic nuclei. One of the basic assumptions of this model is the validity of the Brink–Axel hypothesis and the related concept of so-called photon strength functions to describe γ-ray transition probabilities. We present a novel experimental approach that allows for the first time to experimentally determine the photon strength function simultaneously in two independent ways by a unique combination of quasi-monochromatic photon beams and a newly implemented γ–γ coincidence setup. This technique does not assume a priori the validity of the Brink–Axel hypothesis and sets a benchmark in terms of the detection sensitivity for measuring decay properties of photo-excited states below the neutron separation energy. The data for the spherical off-shell nucleus 128 Te were obtained for γ-ray beam-energy settings between 3 MeV and 9 MeV in steps of 130 keV for the lower beam energies and in steps of up to 280 keV for the highest beam settings. We present a quantitative analysis on the consistency of the derived photon strength function with the Brink–Axel hypothesis. The data clearly demonstrate a discrepancy of up to a factor of two between the photon strength functions extracted from the photoabsorption and photon emission process, respectively. In addition, we observe that the photon strength functions are not independent of the excitation energy, as usually assumed. Thus, we conclude, that the Brink–Axel hypothesis is not strictly fulfilled in the excitation-energy region below the neutron separation threshold (S n = 8.78 MeV) for the studied case of 128 Te.

Not Available

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗