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All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Imaging and spatially resolved mass spectrometry applications in nephrology

The application of spatially resolved mass spectrometry (MS) and MS imaging approaches for studying biomolecular processes in the kidney is rapidly growing. These powerful methods, which enable label-free and multiplexed detection of many molecular classes across omics domains (including metabolites, drugs, proteins and protein post-translational modifications), are beginning to reveal new molecular insights related to kidney health and disease. Further, the complexity of the kidney often necessitates multiple scales of analysis for interrogating biofluids, whole organs, functional tissue units, single cells and subcellular compartments. Various MS methods can generate omics data across these spatial domains and facilitate both basic science and pathological assessment of the kidney. Optimal processes related to sample preparation and handling for different MS applications are rapidly evolving. Emerging technology and methods, improvement of spatial resolution, broader molecular characterization, multimodal and multiomics approaches and the use of machine learning and artificial intelligence approaches promise to make these applications even more valuable in the field of nephology. Overall, spatially resolved MS and MS imaging methods have the potential to fill much of the omics gap in systems biology analysis of the kidney and provide functional outputs that cannot be obtained using genomics and transcriptomic methods.

60 APPLIED LIFE SCIENCES↗
NASA NTRS2015

Non-destructive Evaluation of Bonds Between Fiberglass Composite and Metal

To assess the integrity and reliability of an adhesive joint in an automotive composite component, several non-destructive evaluation (NDE) methodologies are correlated to lap shear bond strengths. A glass-fabric-reinforced composite structure was bonded to a metallic structure with a two-part epoxy adhesive. Samples were subsequently cut and tested in shear, and flaws were found in some areas. This study aims to develop a reliable and portable NDE system for service-level adhesive inspection in the automotive industry. The results of the experimental investigation using several NDE methods are presented and discussed. Fiberglass-to-metal bonding is the ideal configuration for NDE via thermography using excitation with induction heating, due to the conductive metal and non-conductive glass-fiber-reinforced composites. Excitation can be either by a research-grade induction heater of highly defined frequency and intensity, or by a service-level heater, such as would be used for sealing windshields in a body shop. The thermographs thus produced can be captured via a high-resolution infrared camera, with principal component analysis and 2D spatial Laplacian processing. Alternatively, the thermographs can be captured by low resolution thermochromic microencapsulated liquid crystal film imaging, which needs no post-processing and can be very inexpensive. These samples were also examined with phased-array ultrasound. The NDE methods are compared to the lap shear values and to each other for approximate cost, accuracy, and time and level of expertise needed.

Zhao, Selina↗
DOE OSTI2023

Blackout Diffusion: Generative Diffusion Models in Discrete-State Spaces

Typical generative diffusion models rely on a Gaussian diffusion process for training the backward transformations, which can then be used to generate samples from Gaussian noise. However, real world data often takes place in discrete-state spaces, including many scientific applications. Here, we develop a theoretical formulation for arbitrary discrete-state Markov processes in the forward diffusion process using exact (as opposed to variational) analysis. We relate the theory to the existing continuous-state Gaussian diffusion as well as other approaches to discrete diffusion, and identify the corresponding reverse-time stochastic process and score function in the continuous-time setting, and the reverse-time mapping in the discrete-time setting. As an example of this framework, we introduce “Blackout Diffusion”, which learns to produce samples from an empty image instead of from noise. Numerical experiments on the CIFAR-10, Binarized MNIST, and CelebA datasets confirm the feasibility of our approach. Generalizing from specific (Gaussian) forward processes to discrete-state processes without a variational approximation sheds light on how to interpret diffusion models, which we discuss.

Santos, Javier E.↗
DOE OSTI2018

Expression profile analysis of differentially expressed genes in ruptured intracranial aneurysms: In search of biomarkers

Highlights: • Bioinformatics can identify potential biomarkers of ruptured intracranial aneurysm. • BASP1, CD74, CEBPB, ECHDC2, GZMK, HLA-DRB3, KLHL3, SLC2A3 & SOCS3 affect IA rupture. • DEGs are involved in antigen processing and presentation and immune response. • Vascular brain injury affects gene expression in IA tissue. Intracranial aneurysms (IAs) result from the bulging of arterial walls secondary to several factors such as flow, vessel morphology, and genetics. Subarachnoid hemorrhage occurs when such walls rupture, leading to high disability and mortality. Despite numerous investigations pertaining to the relationship between geometric characteristics and IA rupture, only a few have obtained consistent results. This study aimed to further identify the potential genes associated with the pathogenesis of IAs, which may provide novel molecular biomarkers. We downloaded and reanalyzed six datasets, which were divided into four groups. IA walls and blood samples were screened for differentially expressed genes (DEGs); then, functional and pathway enrichment analyses were conducted. In total, 158 common DEGs were identified from Groups 1–3 and 396 genes (187 upregulated and 209 downregulated genes) were differentially expressed in Group 4. The functional analysis revealed that the DEGs were mainly associated with the major histocompatibility complex class II protein complex and antigen processing and presentation. Finally, we identified nine key genes, both in aneurysm tissue samples and blood samples, of which three were mostly associated with the progression and rupture of IAs. Bioinformatics was used to analyze the datasets of the ruptured IAs and identify potential biomarkers, which may provide information for the early detection and treatment of IAs.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2014

Impact of collection container material and holding times on sample integrity for mercury and methylmercury in water

Mercury (Hg) and methylmercury (MeHg) concentrations in streamwater can vary on short timescales (hourly or less) during storm flow and on a diel cycle; the frequency and timing of sampling required to accurately characterize these dynamics may be difficult to accomplish manually. Automated sampling can assist in sample collection; however use has been limited for Hg and MeHg analysis due to stability concerns of trace concentrations during extended storage times. We examined the viability of using automated samplers with disposable low-density polyethylene (LDPE) sample bags to collect industrially contaminated streamwater for unfiltered and filtered Hg and MeHg analysis. Specifically we investigated the effect of holding times ranging from hours to days on streamwater collected during baseflow and storm flow. Unfiltered and filtered Hg and MeHg concentrations decreased with increases in time prior to sample processing; holding times of 24 hours or less resulted in concentration changes (mean 11 7% different) similar to variability in duplicates collected manually during analogous field conditions (mean 7 10% different). Comparisons of samples collected with manual and automated techniques throughout a year for a wide range of stream conditions were also found to be similar to differences observed between duplicate grab samples. These results demonstrate automated sampling into LDPE bags with holding times of 24 hours or less can be effectively used to collect streamwater for Hg and MeHg analysis, and encourage the testing of these materials and methods for implementation in other aqueous systems where high-frequency sampling is warranted.

holding time↗
DOE OSTI2016

Author Contribution to the Pu Handbook II: Chapter 37 LLNL Integrated Sample Preparation Glovebox (TEM) Section

The development of our Integrated Actinide Sample Preparation Laboratory (IASPL) commenced in 1998 driven by the need to perform transmission electron microscopy studies on naturally aged plutonium and its alloys looking for the microstructural effects of the radiological decay process (1). Remodeling and construction of a laboratory within the Chemistry and Materials Science Directorate facilities at LLNL was required to turn a standard radiological laboratory into a Radiological Materials Area (RMA) and Radiological Buffer Area (RBA) containing type I, II and III workplaces. Two inert atmosphere dry-train glove boxes with antechambers and entry/exit fumehoods (Figure 1), having a baseline atmosphere of 1 ppm oxygen and 1 ppm water vapor, a utility fumehood and a portable, and a third double-walled enclosure have been installed and commissioned. These capabilities, along with highly trained technical staff, facilitate the safe operation of sample preparation processes and instrumentation, and sample handling while minimizing oxidation or corrosion of the plutonium. In addition, we are currently developing the capability to safely transfer small metallographically prepared samples to a mini-SEM for microstructural imaging and chemical analysis. The gloveboxes continue to be the most crucial element of the laboratory allowing nearly oxide-free sample preparation for a wide variety of LLNL-based characterization experiments, which includes transmission electron microscopy, electron energy loss spectroscopy, optical microscopy, electrical resistivity, ion implantation, X-ray diffraction and absorption, magnetometry, metrological surface measurements, high-pressure diamond anvil cell equation-of-state, phonon dispersion measurements, X-ray absorption and emission spectroscopy, and differential scanning calorimetry. The sample preparation and materials processing capabilities in the IASPL have also facilitated experimentation at world-class facilities such as the Advanced Photon Source at Argonne National Laboratory, the European Synchrotron Radiation Facility in Grenoble, France, the Stanford Synchrotron Radiation Facility, the National Synchrotron Light Source at Brookhaven National Laboratory, the Advanced Light Source at Lawrence Berkeley National Laboratory, and the Triumph Accelerator in Canada.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2022

Resonant Ultrasonic Spectroscopy: A Modal-Analysis Approach for Additive Manufacturing

Resonant ultrasonic spectroscopy is a methodology capable of measuring a change in modal resonant frequencies of material structures. It encompasses an inversion technique based on the eigen-frequencies of a simple regular sample geometry to estimate the elastic tensor of a solid. Obtaining an accurate and complete set of resonant frequencies is a critical first step in the RUS process. In this paper a variety of techniques to extract and validate material resonances from complicated RUS measurement spectra are developed. Various processing methodologies employing modal analysis techniques are applied to estimate the underlying resonances that lead to the extraction of the elastic coefficients characterizing the specimen under test. A case study of a simple isotropic material (304 SS) is investigated to analyze the algorithms and evaluate their performance

Coal, lignite, and peat↗
DOE OSTI2016

SU-D-204-06: Integration of Machine Learning and Bioinformatics Methods to Analyze Genome-Wide Association Study Data for Rectal Bleeding and Erectile Dysfunction Following Radiotherapy in Prostate Cancer

Purpose: We investigated whether integration of machine learning and bioinformatics techniques on genome-wide association study (GWAS) data can improve the performance of predictive models in predicting the risk of developing radiation-induced late rectal bleeding and erectile dysfunction in prostate cancer patients. Methods: We analyzed a GWAS dataset generated from 385 prostate cancer patients treated with radiotherapy. Using genotype information from these patients, we designed a machine learning-based predictive model of late radiation-induced toxicities: rectal bleeding and erectile dysfunction. The model building process was performed using 2/3 of samples (training) and the predictive model was tested with 1/3 of samples (validation). To identify important single nucleotide polymorphisms (SNPs), we computed the SNP importance score, resulting from our random forest regression model. We performed gene ontology (GO) enrichment analysis for nearby genes of the important SNPs. Results: After univariate analysis on the training dataset, we filtered out many SNPs with p>0.001, resulting in 749 and 367 SNPs that were used in the model building process for rectal bleeding and erectile dysfunction, respectively. On the validation dataset, our random forest regression model achieved the area under the curve (AUC)=0.70 and 0.62 for rectal bleeding and erectile dysfunction, respectively. We performed GO enrichment analysis for the top 25%, 50%, 75%, and 100% SNPs out of the select SNPs in the univariate analysis. When we used the top 50% SNPs, more plausible biological processes were obtained for both toxicities. An additional test with the top 50% SNPs improved predictive power with AUC=0.71 and 0.65 for rectal bleeding and erectile dysfunction. A better performance was achieved with AUC=0.67 when age and androgen deprivation therapy were added to the model for erectile dysfunction. Conclusion: Our approach that combines machine learning and bioinformatics techniques enabled designing better models and identifying more plausible biological processes associated with the outcomes.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2015

Broadband down-conversion based near infrared quantum cutting in Eu{sup 2+}–Yb{sup 3+} co-doped SrAl{sub 2}O{sub 4} for crystalline silicon solar cells

Near infrared (NIR) quantum cutting involving the down conversion of an absorbed visible photon to emission of two NIR photons was achieved in SrAl{sub 2}O{sub 4}:0.01Eu{sup 2+}, xYb{sup 3+} (x=0, 1, 2, 5, 10, 20, 30 mol%) samples. The photoluminescence properties of samples in visible and NIR regions were measured to verify the energy transfer (ET) from Eu{sup 2+} to Yb{sup 3+}. The results demonstrated that Eu{sup 2+} was an efficient sensitizer for Yb{sup 3+} in the SrAl{sub 2}O{sub 4} host lattice. According to Gaussian fitting analysis and temperature-dependent luminescence experiments, the conclusion was drawn that the cooperative energy transfer (CET) process dominated the ET process and the influence of charge transfer state (CTS) of Yb{sup 3+} could be negligible. As a result, the high energy transfer efficiency (ETE) and quantum yield (QY) have been acquired, the maximum value approached 73.68% and 147.36%, respectively. Therefore, this down-conversion material has potential application in crystalline silicon solar cells to improve conversion efficiency. - Graphical abstract: Near infrared quantum cutting was achieved in Eu{sup 2+}–Yb{sup 3+} co-doped SrAl{sub 2}O{sub 4} samples. The cooperative energy transfer process dominated energy transfer process and high energy transfer efficiency was acquired. - Highlights: • The absorption spectrum of Eu{sup 2+} ion is strong in intensity and broad in bandwidth. • The spectra of Eu{sup 2+} in SrAl{sub 2}O{sub 4} lies in the strongest region of solar spectrum. • The cooperative energy transfer (CET) dominated the energy transfer process. • The domination of CET is confirmed by experimental analysis. • SrAl{sub 2}O{sub 4}:Eu{sup 2+},Yb{sup 3+} show high energy transfer efficiency and long lifetime.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

DECOMMISSIONING AND ENVRIONMENTAL CLEANUP OF SMALL ARMS TRAINING FACILITY

USDOE performed a (CERCLA) non-time critical removal (NTCR) action at the Small Arms Training Area (SATA) Site Evaluation Area (SEA) located at the Savannah River Site (SRS), in Aiken, South Carolina. From 1951 to May 2010, the SATA was used as a small weapons practice and qualifying firing range. The SATA consisted of 870.1 ha (2,150 ac) of woodlands and open field, of which approximately 2.9 ha (7.3 ac) were used as a firing range. The SATA facility was comprised of three small arms ranges (one static and two interactive), storage buildings for supplies, a weapons cleaning building, and a control building. Additionally, a 113- m (370-ft) long earthen berm was used as a target backstop during live-fire exercises. The berm soils accumulated a large amount of spent lead bullets in the berm face during the facilities 59- years of operation. The accumulation of lead was such that soil concentrations exceeded the U.S. Environmental Protection Agency (USEPA) residential and industrial worker regional screening levels (RSLs). The RSL threshold values are based on standardized exposure scenarios that estimate contaminant concentrations in soil that the USEPA considers protective of humans over a lifetime. For the SATA facility, lead was present in soil at concentrations that exceed both the current residential (400 mg/kg) and industrial (800 mg/kg) RSLs. In addition, the concentration of lead in the soil exceeded the Toxicity Characteristic Leaching Procedure (TCLP) (40 Code of Federal Regulations [CFR] 261.24) regulatory limit. The TCLP analysis simulates landfill conditions and is designed to determine the mobility of contaminants in waste. In addition, a principal threat source material (PTSM) evaluation, human health risk assessment (HHRA), and contaminant migration (CM) analysis were conducted to evaluate soil contamination at the SATA SEA. This evaluation determined that there were no contaminants present that constitute PTSM and the CM analysis revealed that no constituents posed a migration risk to groundwater. The NTCR action involved removal of approximately 12,092 m3 (15,816 yd3) of spent bullets and lead-impacted soil and off-site disposal. The removal action included soils from the berm area, a fill area that received scraped soils from the berm, and soil from a drainage ditch located on the edge of the berm area. Also included in the removal action was a mixture of soil, concrete, and asphalt from the other three range areas. Under this action, 11,796 m3 (15,429 yd3) of hazardous waste and impacted soil were removed from the SATA and transported to a permitted hazardous waste disposal facility (Lone Mountain Facility in Oklahoma) and 296 m3 (387 yd3) of nonhazardous waste (primarily concrete debris) were removed and transported to a local solid waste landfill for disposal. During the excavation process, the extent was continuously assessed through the use of a hand-held, field-portable X-ray fluorescence unit with results verified using confirmation sampling with certified laboratory analysis. Following the completion of the excavation and confirmation sampling, final contouring, grading, and establishment of vegetative cover was performed to stabilize the affected areas. The NTCR action began on August 17, 2010, and mechanical completion was achieved on April 27, 2011. The selected removal action met the removal action objectives (RAOs), is protective of human health and the environment both in the short- and long-term, was successful in removing potential ecological risks, and is protective of surface water and groundwater. Furthermore, the selected NTCR action met residential cleanup goals and resulted in the release of the SEA from restricted use contributing to the overall footprint reduction at SRS.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2018

Rapid Microwave Preparation and Composition Tuning of the High-Performance Magnetocalorics (Mn,Fe) 2 (P,Si)

Rapid preparation utilizing assisted microwave heating permits significantly shorter preparation times for magnetocaloric compounds in the (Mn,Fe) 2 (P,Si) family, specifically samples of (Mn,Fe) 2–δ P 0.5 Si 0.5 with starting compositions of δ = 0, 0.06, and 0.12. To fully understand the effects of processing and composition changes on structure and properties, these materials are characterized using synchrotron powder diffraction, neutron powder diffraction, electron microprobe analysis (EMPA), X-ray fluorescence (XRF), and magnetic measurements. The diffraction analysis reveals that increasing δ results in decreasing amounts of the common Heusler (Mn,Fe) 3 Si secondary phase. EMPA shows (Mn,Fe) 2 (P,Si) in all three samples to be Mn and P rich, whereas XRF demonstrates that the bulk material is Mn rich yet P deficient. Increasing δ brings the Mn/Fe and P/Si ratios closer to their starting values. Measurements of magnetic properties show an increase in saturation magnetization and ordering temperature with increasing δ, consistent with the increase in Fe and Si contents. Increasing δ also results in a decrease in thermal hysteresis and an increase in magnetic entropy change. We note the latter reach values close to what have been previously reported on samples that take much longer to prepare.

36 MATERIALS SCIENCE↗
NASA NTRSDate not supplied

The Nature of Space Weathering in Samples From Asteroid (162173) Ryugu Revealed By Coordinated Analysis

Space weathering, driven primarily by micrometeorite bombardment and solar wind ion irradiation, alters the morphology, microstructure, and chemistry of the surface regolith on airless bodies. The accumulation of microstructural and chemical space weathering features, including melt deposits, amorphous rims, and nanophase iron-bearing particles (npFe), are associated with alterations of the spectral properties of the regolith. In particular, space weathering changes the spectral slope and reflectance of surface materials, and causes the attenuation of characteristic absorption bands in the visible to near-infrared wave-lengths, as well as a shift towards longer wavelengths of the Christiansen feature (CF)in thermal infrared spectra. Previous studies of space weathering characteristics have focused on siliceous bodies like the Moon and S-type asteroid Itokawa. However, observations of asteroid Ryugu by the JAXA Hayabusa2 spacecraft and subsequent analyses of returned samples revealed carbonaceous and hydrated materials. These samples provided our first opportunity to constrain the effects of space weathering processes on primitive, C-type asteroids. Analyses of returned samples to understand the space weathering of carbonaceous materials are important for accurately interpreting remote sensing observations of carbonaceous asteroids. In addition, the analysis of Hayabusa2 samples from Ryugu paved the way for the analysis of samples from the asteroid Bennu, re-turned by the NASA OSIRIS-REx mission. As space weathering impacts the microstructure, chemistry, and spectral characteristics of asteroidal surfaces, here we report the results of a coordinated analytical study of the micro-and nano-scale signatures of space weathering in samples returned from Ryugu.

L E Melendez↗
DOE OSTI2013

Decommissioning and Environmental Cleanup of a Small Arms Training Facility - 13225

US DOE performed a (CERCLA) non-time critical removal (NTCR) action at the Small Arms Training Area (SATA) Site Evaluation Area (SEA) located at the Savannah River Site (SRS), in Aiken, South Carolina. From 1951 to May 2010, the SATA was used as a small weapons practice and qualifying firing range. The SATA consisted of 870.1 ha (2,150 ac) of woodlands and open field, of which approximately 2.9 ha (7.3 ac) were used as a firing range. The SATA facility was comprised of three small arms ranges (one static and two interactive), storage buildings for supplies, a weapons cleaning building, and a control building. Additionally, a 113- m (370-ft) long earthen berm was used as a target backstop during live-fire exercises. The berm soils accumulated a large amount of spent lead bullets in the berm face during the facilities 59- years of operation. The accumulation of lead was such that soil concentrations exceeded the U.S. Environmental Protection Agency (USEPA) residential and industrial worker regional screening levels (RSLs). The RSL threshold values are based on standardized exposure scenarios that estimate contaminant concentrations in soil that the USEPA considers protective of humans over a lifetime. For the SATA facility, lead was present in soil at concentrations that exceed both the current residential (400 mg/kg) and industrial (800 mg/kg) RSLs. In addition, the concentration of lead in the soil exceeded the Toxicity Characteristic Leaching Procedure (TCLP) (40 Code of Federal Regulations [CFR] 261.24) regulatory limit. The TCLP analysis simulates landfill conditions and is designed to determine the mobility of contaminants in waste. In addition, a principal threat source material (PTSM) evaluation, human health risk assessment (HHRA), and contaminant migration (CM) analysis were conducted to evaluate soil contamination at the SATA SEA. This evaluation determined that there were no contaminants present that constitute PTSM and the CM analysis revealed that no constituents posed a migration risk to groundwater. The NTCR action involved removal of approximately 12,092 m{sup 3} (15,816 yd{sup 3}) of spent bullets and lead-impacted soil and off-site disposal. The removal action included soils from the berm area, a fill area that received scraped soils from the berm, and soil from a drainage ditch located on the edge of the berm area. Also included in the removal action was a mixture of soil, concrete, and asphalt from the other three range areas. Under this action, 11,796 m{sup 3} (15,429 yd{sup 3}) of hazardous waste and impacted soil were removed from the SATA and transported to a permitted hazardous waste disposal facility (Lone Mountain Facility in Oklahoma) and 296 m{sup 3} (387 yd{sup 3}) of nonhazardous waste (primarily concrete debris) were removed and transported to a local solid waste landfill for disposal. During the excavation process, the extent was continuously assessed through the use of a hand-held, field-portable X-ray fluorescence unit with results verified using confirmation sampling with certified laboratory analysis. Following the completion of the excavation and confirmation sampling, final contouring, grading, and establishment of vegetative cover was performed to stabilize the affected areas. The NTCR action began on August 17, 2010, and mechanical completion was achieved on April 27, 2011. The selected removal action met the removal action objectives (RAOs), is protective of human health and the environment both in the short- and long-term, was successful in removing potential ecological risks, and is protective of surface water and groundwater. Furthermore, the selected NTCR action met residential cleanup goals and resulted in the release of the SEA from restricted use contributing to the overall footprint reduction at SRS. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
NASA NTRS1984

Chemical mechanisms and reaction rates for the initiation of hot corrosion of IN-738

Sodium-sulfate-induced hot corrosion of preoxidized IN-738 was studied at 975 C with special emphasis placed on the processes occurring during the long induction period. Thermogravimetric tests were run for predetermined periods of time, and then one set of specimens was washed with water. Chemical analysis of the wash solutions yielded information about water soluble metal salts and residual sulfate. A second set of samples was cross sectioned dry and polished in a nonaqueous medium. Element distributions within the oxide scale were obtained from electron microprobe X-ray micrographs. Evolution of SO was monitored throughout the thermogravimetric tests. Kinetic rate studies were performed for several pertinent processes; appropriate rate constants were obtained from the following chemical reactions: Cr2O3 + 2 Na2SO4(1) + 3/2 O2 yields 2 Na2CrO4(1) + 2 SO3(g)n TiO2 + Na2SO4(1) yields Na2O(TiO2)n + SO3(g)n TiO2 + Na2CrO4(1) yields Na2O(TiO2)n + CrO3(g).

Fryburg, G. C.↗
NASA NTRS1984

Chemical reactions involved in the initiation of hot corrosion of IN-738

Sodium-sulfate-induced hot corrosion of preoxidized IN-738 was studied at 975 C with special emphasis placed on the processes occurring during the long induction period. Thermogravimetric tests were run for predetermined periods of time, and then one set of specimens was washed with water. Chemical analysis of the wash solutions yielded information about water soluble metal salts and residual sulfate. A second set of samples was cross sectioned dry and polished in a nonaqueous medium. Element distributions within the oxide scale were obtained from electron microprobe X-ray micrographs. Evolution of SO was monitored throughout the thermogravimetric tests. Kinetic rate studies were performed for several pertinent processes; appropriate rate constants were obtained from the following chemical reactions; Cr203 + 2 Na2S04(1) + 3/2 02 yields 2 Na2Cr04(1) + 2 S03(g)n TiO2 + Na2S04(1) yields Na20(T102)n + 503(g)n T102 + Na2Cro4(1) yields Na2(T102)n + Cr03(g).

Fryburg, G. C.↗
NASA NTRS2014

Nanophase Carbonates on Mars: Implications for Carbonate Formation and Habitability

Despite having an atmosphere composed primarily of CO2 and evidence for abundant water in the past, carbonate minerals have only been discovered in small amounts in martian dust [1], in outcrops of very limited extent [2, 3], in soils in the Northern Plains (the landing site of the 2007 Phoenix Mars Scout Mission) [4] and may have recently been detected in aeolian material and drilled and powdered sedimentary rock in Gale Crater (the Mars Science Laboratory [MSL] landing site) [5]. Thermal analysis of martian soils by instruments on Phoenix and MSL has demonstrated a release of CO2 at temperatures as low as 250-300 degC, much lower than the traditional decomposition temperatures of calcium or magnesium carbonates. Thermal decomposition temperature can depend on a number of factors such as instrument pressure and ramp rate, and sample particle size [6]. However, if the CO2 released at low temperatures is from carbonates, small particle size is the only effect that could have such a large impact on decomposition temperature, implying the presence of extremely fine-grained (i.e., "nanophase" or clay-sized) carbonates. We hypothesize that this lower temperature release is the signature of small particle-sized (clay-sized) carbonates formed by the weathering of primary minerals in dust or soils through interactions with atmospheric water and carbon dioxide and that this process may persist under current martian conditions. Preliminary work has shown that clay-sized carbonate grains can decompose at much lower temperatures than previously thought. The first work took carbonate, decomposed it to CaO, then flowed CO2 over these samples held at temperatures >100 degC to reform carbonates. Thermal analysis confirmed that carbonates were indeed formed and transmission electron microsopy was used to determine crystal sized were on the order of 10 nm. The next step used minerals such as diopside and wollastonite that were sealed in a glass tube with a CO2 and H2O source. After reacting these materials for a number of hours, thermal analysis demonstrated the formations of carbonates that decomposed at temperatures as low as 500 degC [7]. Further work is underway to carry out the weathering process under more Mars-like conditions (low pressure and low temperature) to determine if the carbonate decomposition temperature can be shifted to even lower temperatures, consistent with what has been detected by thermal analysis instruments on Mars.

Archer, P. Douglas, Jr.↗
DOE OSTI2013

Laser assisted crystallization of ferromagnetic amorphous ribbons: A multimodal characterization and thermal model study

This paper focuses on laser-based de-vitrification of amorphous soft magnetic Fe-Si-B ribbons and its consequent influence on the magnetic properties. Laser processing resulted in a finer scale of crystallites due to rapid heating and cooling during laser annealing compared to conventional furnace annealing process. A significant increase in saturation magnetization is observed for laser-annealed ribbons compared to both as-received and furnace annealed samples coupled with an increase in coercivity compared to the as received samples. The combined effect of thermal histories and stresses developed during laser annealing results in the formation of nano-crystalline phase along the laser track. The phase evolution is studied by micro-XRD and TEM analysis. Solute partitioning and compositional variation within the phases are obtained by Local Electrode Atom probe analysis. The evolution of microstructure is rationalized using a Finite Element based heat transfer multi-physics model.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2013

Redox cycle stability of mixed oxides used for hydrogen generation in the cyclic water gas shift process

Graphical abstract: - Highlights: • Fe{sub 2}O{sub 3} modified with CaO, SiO{sub 2} and Al{sub 2}O{sub 3} was studied in cyclic water gas shift reactor. • For the first time stability of such oxides were tested for 100 redox cycles. • Optimally added oxides significantly improved the activity and the stability of Fe{sub 2}O{sub 3}. • Increased stability was attributed to the impediment of neck formation. - Abstract: Repeated cycles of the reduction of Fe{sub 3}O{sub 4} with reductive gas, e.g. hydrogen and subsequent oxidation of the reduced iron material with water vapor can be harnessed as a process for the production of pure hydrogen. The redox behavior of iron oxide modified with various amounts of SiO{sub 2}, CaO and Al{sub 2}O{sub 3} was investigated in the present study. The total amount of the additional metal oxides was always below 15 wt%. The samples were prepared by co-precipitation using urea hydrolysis method. The influence of various metal oxides on the hydrogen production capacity and the material stability was studied in detail in terms of temperature-programmed reduction (TPR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and BET analysis. Furthermore, the activity and the stability of the samples were tested in repeated reduction with diluted H{sub 2} and re-oxidation cycles with H{sub 2}O. The results indicate that combination of several oxides as promoter increases the stability of the iron oxide material by mitigating the sintering process. The positive influence of the oxides in stabilizing the iron oxide material is attributed to the impediment of neck formation responsible for sintering.

36 MATERIALS SCIENCE↗