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Beryllium (Be) isotope measurements provide insight into weapon design, yield, etc. Sample preparation nor measurement capability currently existed at LANL. Potential capability directly benefits nuclear forensics venture. PI Goehring has nearly 20 years of Be chemistry experience, including method implementation with difficult samples.
Human disease states are biomolecularly multifaceted and can span across phenotypic states, therefore it is important to understand diseases on all levels, across cell types, and within and across microanatomical tissue compartments. To obtain an accurate and representative view of the molecular landscape within human lungs, this fragile tissue must be inflated and embedded to maintain spatial fidelity of the location of molecules and minimize molecular degradation for molecular imaging experiments. Here, we evaluated agarose inflation and carboxymethyl cellulose embedding media and determined effective tissue preparation protocols for performing bulk and spatial mass spectrometry-based omics measurements. Mass spectrometry imaging methods were optimized to boost the number of annotatable molecules in agarose inflated lung samples. This optimized protocol permitted the observation of unique lipid distributions within several airway regions in the lung tissue block. Laser capture microdissection of these airway regions followed by high-resolution proteomic analysis allowed us to begin linking the lipidome with the proteome in a spatially resolved manner, where we observed proteins with high abundance specifically localized to the airway regions. We also compared our mass spectrometry results to lung tissue samples preserved using two other inflation/embedding media, but we identified several pitfalls with the sample preparation steps using this preservation method. Overall, we demonstrated the versatility of the inflation method, and we can start to reveal how the metabolome, lipidome, and proteome are connected spatially in human lungs and across disease states through a variety of different experiments.
As codified in NASA Policy Directive 7100.10F, the Astromaterials Acquisition and Curation Office at NASA Johnson Space Center (hereafter JSC Curation) is charged with curation of all extraterrestrial material under NASA control, including future NASA missions. JSC Curation curates all or part of nine astromaterial collections in seven clean room suites: (1) Apollo Samples (1969; ISO 6-7), (2) Luna Samples (from USSR; 1972; ISO 7), (3) Antarctic Meteorites (1976; ISO 7), (4) Cosmic Dust (1981; ISO 5), (5) Microparticle Impact Collection (formerly called Space Exposed Hardware; 1985; ISO 5), (6) Genesis Solar Wind Atoms (2004; ISO 4); (7) Stardust Comet Particles (2006; ISO 5), (8) Stardust Interstellar Particles (2006; ISO 5), (9) Hayabusa Asteroid Particles (from JAXA; 2010; ISO 5). In addition to the labs that house the samples, we have installed and maintained a wide variety of facilities and infrastructure required to support the clean-rooms: more than 10 different HEPA-filtered air-handling systems, ultrapure dry gaseous nitrogen systems, an ultrapure water system (UPW) and cleaning facilities to provide clean tools and equipment for the labs. We also have sample preparation facilities for making thin sections, microtome sections, and even focused ion-beam (FIB) sections to meet the research requirements of scientists. To ensure that we are keeping the samples as pristine as possible, we routinely monitor the cleanliness of our clean rooms and infrastructure systems. This monitoring includes: daily monitoring of the quality of our UPW, weekly airborne particle counts in the labs, monthly monitoring of the stable isotope composition of the gaseous N2 system, and annual measurements of inorganic or organic contamination in processing cabinets. We track within our databases the current and ever-changing characteristics of more than 250,000 individual samples across our various collections (including the 19,141 samples on loan to 433 Principal Investigators in 24 countries). The next sample return missions that NASA will participate in are Hayabusa2 and OSIRIS-REx (Origins Spectral Interpretation Resource Identification Security - Regolith Explorer). The designs for a new state-of-the-art suite of clean rooms to house these samples at JSC have been finalized. This includes separate ISO class 5 clean rooms to house each collection, a common ISO class 7 area for general use, an ISO class 7 microtome laboratory, and a separate thin section lab. Additionally, a new cleaning facility is being designed and procedures developed that will allow for enhanced cleaning of cabinets and tools in an inorganically, organically, and biologically clean manner. We are also designing a large multi-purpose Advanced Curation laboratory that will allow us to develop the techniques necessary to fully support the Hayabusa2 and OSIRIS-REx missions, as well as future possible sample return missions (e.g., Lunar Polar Volatiles, Mars, Comet Surface). A micro-CT (micro Computed Tomography) laboratory dedicated to the study of astromaterials has come online within JSC Curation, and we plan to add additional facilities that will enable non-destructive (or minimally-destructive) analyses of astromaterials in the near future (e.g., micro-XRF (micro X-Ray Fluorescence), confocal imaging Raman Spectroscopy). These facilities will be available to: (1) develop sample handling and storage techniques for future sample return missions, (2) be utilized by PET (Positron Emission Tomography) for future sample return missions, (3) for retroactive PET-style analyses of our existing collections, and (4) for periodic assessments of the existing sample collections.
As a corrosion barrier layer, open-air plasma-assisted organosilicon coating was applied on AZ91D Mg alloy. Organosilicon-coated AZ91D samples, prepared from two different plasma coating processes, were used for corrosion evaluation based on multistep electrochemical and H 2 collection measurements in 3.5 wt% sodium chloride (NaCl) solution. Some coated AZ91D samples were characterized with and without corrosion exposure in NaCl solution using electron microscopies and X-ray chemical analysis techniques. Further, the results indicate that the organosilicon coatings from open-air plasma processes are effective to delay the initiation of corrosion attack and also reduce the corrosion rate for AZ91D substrate. The corrosion attack was considered to develop after permeation of NaCl solution through the coating layer.
Mass spectrometry imaging (MSI) is a powerful analytical technique that enables label-free spatial localization and identification of molecules in complex samples.1-4 MSI applications range from forensics5 to clinical research6 and from understanding microbial communication7-8 to imaging biomolecules in tissues.1, 9-10 Recently, MSI protocols have been reviewed.11 Ambient ionization techniques enable direct analysis of complex samples under atmospheric pressure without special sample pretreatment.3, 12-16 In fact, in ambient ionization mass spectrometry, sample processing (e.g., extraction, dilution, preconcentration, or desorption) occurs during the analysis.17 This substantially speeds up analysis and eliminates any possible effects of sample preparation on the localization of molecules in the sample.3, 8, 12-14, 18-20 Venter and co-workers have classified ambient ionization techniques into three major categories based on the sample processing steps involved: 1) liquid extraction techniques, in which analyte molecules are removed from the sample and extracted into a solvent prior to ionization; 2) desorption techniques capable of generating free ions directly from substrates; and 3) desorption techniques that produce larger particles subsequently captured by an electrospray plume and ionized.17 This review focuses on localized analysis and ambient imaging of complex samples using a subset of ambient ionization methods broadly defined as “liquid extraction techniques” based on the classification introduced by Venter and co-workers.17 Specifically, we include techniques where analyte molecules are desorbed from solid or liquid samples using charged droplet bombardment, liquid extraction, physisorption, chemisorption, mechanical force, laser ablation, or laser capture microdissection. Analyte extraction is followed by soft ionization that generates ions corresponding to intact species. Some of the key advantages of liquid extraction techniques include the ease of operation, ability to analyze samples in their native environments, speed of analysis, and ability to tune the extraction solvent composition to a problem at hand. For example, solvent composition may be optimized for efficient extraction of different classes of analytes from the sample or for quantification or online derivatization through reactive analysis. In this review, we will: 1) introduce individual liquid extraction techniques capable of localized analysis and imaging, 2) describe approaches for quantitative MSI experiments free of matrix effects, 3) discuss advantages of reactive analysis for MSI experiments, and 4) highlight selected applications (published between 2012 and 2015) that focus on imaging and spatial profiling of molecules in complex biological and environmental samples.
Extended X-ray Absorption Fine Structure (EXAFS) measurements have been carried out on Mn doped CaF{sub 2} phosphors with synchrotron radiation at the Mn K edge. Measurements have been carried out on samples prepared with different concentrations of Mn dopants. The data have been analyzed to find out the Mn-F bond lengths and % of Mn doped CaF{sub 2} phase in the samples. The change in thermoluminescence glow peak temperature in CaF{sub 2}:Mn phosphor with variation in Mn concentration has been correlated to the parameters obtained from EXAFS measurements.
This particular project was completed in collaboration with the metallurgical diagnostics facility. The objective of this research had four major components. First, we required training in the operation of the environmental scanning electron microscope (ESEM) for imaging of selected materials including biological specimens. The types of materials range from cyanobacteria and diatoms to cloth, metals, sand, composites and other materials. Second, to obtain training in surface elemental analysis technology using energy dispersive x-ray (EDX) analysis, and in the preparation of x-ray maps of these same materials. Third, to provide training for the staff of the metallurgical diagnostics and failure analysis team in the area of image processing and image analysis technology using NIH Image software. Finally, we were to assist in the sample preparation, observing, imaging, and elemental analysis for Mr. Richard Hoover, one of NASA MSFC's solar physicists and Marshall's principal scientist for the agency-wide virtual Astrobiology Institute. These materials have been collected from various places around the world including the Fox Tunnel in Alaska, Siberia, Antarctica, ice core samples from near Lake Vostoc, thermal vents in the ocean floor, hot springs and many others. We were successful in our efforts to obtain high quality, high resolution images of various materials including selected biological ones. Surface analyses (EDX) and x-ray maps were easily prepared with this technology. We also discovered and used some applications for NIH Image software in the metallurgical diagnostics facility.
Graphical abstract: - Highlights: • MNb{sub 2}O{sub 6} was prepared by a mild two-step hydrothermal method. • Their flower-like nanostructure morphology was studied by SEM and TEM. • High BET surface areas for MnNb{sub 2}O{sub 6} (∼50 m{sup 2}/g) and ZnNb{sub 2}O{sub 6} (∼100 m{sup 2}/g). • Band gap energies were estimated by UV–vis diffuse reflectance spectra. • Photocatalytic activities were evaluated under UV-light irradiation. - Abstract: Nano-scaled MNb{sub 2}O{sub 6} (M = Mn, Zn) was successfully synthesized via a two-step hydrothermal method. It is important to control the exact pH of the reaction solution in order to obtain pure products. The as-prepared samples both crystallize in the columbite structure. Interestingly, the products possess a flower-like morphology in a pseudo-six-fold symmetry, which is in fact arrayed by two-dimensional nanosheets. Their surface areas (51 m{sup 2}/g for MnNb{sub 2}O{sub 6} and 103 m{sup 2}/g for ZnNb{sub 2}O{sub 6}) are about 25–50 times of those prepared by solid state reaction. UV–vis diffuse reflectance spectra show the nano-scaled sample has a stronger absorption and a narrower band gap than its bulk form. The estimated band gap energies are 2.70 eV (MnNb{sub 2}O{sub 6}) and 3.77 eV (ZnNb{sub 2}O{sub 6}), respectively. The nano-scaled ZnNb{sub 2}O{sub 6} exhibits a double enhancement of photocatalytic activity in the decolorization of methylene blue than bulk ZnNb{sub 2}O{sub 6}.
Au/Cu bilayers with different Au:Cu concentrations (25:75, 50:50 and 75:25 at.%) were deposited on Si(100) substrates by thermal evaporation. The thicknesses of all Au/Cu bilayers were 150 nm. The alloys were prepared by thermal diffusion into a vacuum oven with argon atmosphere at 690 K during 1 h. X-ray diffraction analysis revealed different phases of AuCu and CuSi alloys in the samples after annealing process. CuSi alloys were mainly obtained for 25:75 at.% samples, meanwhile the AuCuII phase dominates for samples prepared with 50:50 at.%. Additionally, the Au:Cu alloys with 75:25 at.%, produce Au{sub 2}Cu{sub 3} and Au{sub 3}Cu phases. The formed alloys were characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM), transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS) to study the morphology and the elemental concentration of the formed alloys. - Highlights: • AuCu/Si alloy thin films were prepared by thermal diffusion. • Alloys prepared with 50 at.% of Au produce the AuCuII phase. • Alloys prepared with 75 at.% of Au produce Au{sub 3}Cu and Au{sub 2}Cu{sub 3} phases. • All alloys present diffusion of Si and Cu through the CuSi alloy formation.
Halide solid electrolytes have emerged as promising candidates for solid-state batteries owing to their high oxidative stability and ionic conductivity. Among them, Li3InCl6 (LIC) has attracted significant attention. However, diffraction patterns of LIC synthesized via different methods exhibit distinct differences particularly at low-angle reflectionsindicative of underlying structural disorder. These variations are attributed to deviations from ideal crystallographic order, especially stacking faults, whose impact on structure and ion transport remains poorly understood. Here, we identify and quantify stacking faults in LIC samples prepared under different synthetic conditions. Using X-ray diffraction and time-of-flight neutron diffraction, we construct and refine stacking fault models that accurately reproduce the experimental diffraction features. LIC samples with higher degrees of stacking faults exhibit only negligible differences in ionic conductivities and activation energies. This indicates that stacking faults have a limited impact on altering the Li+ diffusion pathway along the c-axis, likely due to the high concentration of vacancies in the In layers, while Li+ diffusion remains nearly unchanged in the ab-plane. Our results account for the observed differences in diffraction patterns across samples and provide a quantitative assessment of faulting probabilities and stacking sequences. The insights gained from this study are expected to be broadly applicable to other layered halide solid electrolytes and contribute to a deeper understanding of the role of structural disorder in ion transport.
It is widely accepted that micro- and nanoscale inhomogeneities govern the performance of many thin-film solar cell absorbers. These inhomogeneities yield material properties (e.g., composition, structure, and charge collection) that are challenging to correlate across length scales and measurement modalities. The challenge is compounded if a correlation is sought during device operation or in conditions that mimic aging under particular stressors (e.g., heat and electrical bias). Correlative approaches, particularly those based on synchrotron x-ray sources, are powerful since they can access several material properties in different modes (e.g., fluorescence, diffraction, and absorption) with minimal sample preparation. Small-scale laboratory x-ray instruments have begun to offer multi-modality but are typically limited by low x-ray photon flux, low spatial resolution, or specific sample sizes. To overcome these limitations, a characterization stage was developed to enable multi-scale, multi-modal operando measurements of industrially relevant photovoltaic devices. The stage offers compatibility across synchrotron x-ray facilities, enabling correlation between nanoscale x-ray fluorescence microscopy, microscale x-ray diffraction microscopy, and x-ray beam induced current microscopy, among others. Furthermore, the stage can accommodate device sizes up to 25 × 25 mm 2 , offering access to multiple regions of interest and increasing the statistical significance of correlated properties. The stage materials can sustain humid and non-oxidizing atmospheres, and temperature ranges encountered by photovoltaic devices in operational environments (e.g., from 25 to 100 °C). As a case study, we discuss the functionality of the stage by studying Se-alloyed CdTe photovoltaic devices aged in the stage between 25 and 100 °C.
Molecular dynamics simulations were performed to study the effects of Si solute on the glass formation and crystallization of Pd liquid. Pure Pd sample prepared by quenching process with cooling rate of 10 13 K/s can be in an amorphous state but the structural analysis indicates there is nearly no glass-forming motif in the sample. However, doping a small amount Si (Si concentration ~ 4%) the sample can be vitrified at a cooling rate of 10 12 K/s. The glass-forming motifs such as Pd-centered Z13, Si-centered Z9-like and Mixed-ICO-Cube clusters with 5-fold local symmetry are found to be the dominant short-range orders in the glassy samples. With the increasing of the Si-doping concentration, these glass-forming motifs tend to aggregate and connect with each other forming a network structure. Our calculated results revealed that Si solutes in liquid Pd can significantly enhance the glass-forming ability.
The study of embedding matrix of radioactive waste is an important issue concerning the need to assure the radiological safety requirements for final disposal. The conditioning of the radioactive wastes by cementation process involves also a structural investigation by X-ray diffraction (XRD) of the samples prepared with cement and complexing agents at different concentration. This paper gives useful information about the influence of complexing agents related to damages produced in concrete microstructures. The experimental data obtained on samples kept in real repository environment for a period up to 15 years, offer structural information regarding the interaction between the different decontamination agents with the major components of the matrix. (authors)
Mass spectrometry (MS)-based proteomics has great potential for overcoming the limitations of antibody-based immunoassays for antibody-independent, comprehensive, and quantitative proteomic analysis of single cells. Indeed, recent advances in nanoscale sample preparation have enabled effective processing of single cells. In particular, the concept of using boosting/carrier channels in isobaric labeling to increase the sensitivity in MS detection has also been increasingly used for quantitative proteomic analysis of small-sized samples including single cells. However, the full potential of such boosting/carrier approaches has not been significantly explored, nor has the resulting quantitation quality been carefully evaluated. Herein, we have further evaluated and optimized our recent boosting to amplify signal with isobaric labeling (BASIL) approach, originally developed for quantifying phosphorylation in small number of cells, for highly effective analysis of proteins in single cells. This improved BASIL (iBASIL) approach enables reliable quantitative single-cell proteomics analysis with greater proteome coverage by carefully controlling the boosting-to-sample ratio (e.g. in general <100×) and optimizing MS automatic gain control (AGC) and ion injection time settings in MS/MS analysis (e.g. 5E5 and 300 ms, respectively, which is significantly higher than that used in typical bulk analysis). By coupling with a nanodroplet-based single cell preparation (nanoPOTS) platform, iBASIL enabled identification of ~2500 proteins and precise quantification of ~1500 proteins in the analysis of 104 FACS-isolated single cells, with the resulting protein profiles robustly clustering the cells from three different acute myeloid leukemia cell lines. This study highlights the importance of carefully evaluating and optimizing the boosting ratios and MS data acquisition conditions for achieving robust, comprehensive proteomic analysis of single cells.
Recently, 2D noble metal dichalcogenides have drawn considerable attention due to their thickness-tunable electronic and optical properties. However, the dynamical properties of photocarriers in these materials are less studied. In this report photocarrier dynamics in monolayer and bilayer PtSe 2 samples prepared by chemical vapor deposition are studied by transient absorption microscopy. Spatially and temporally resolved differential reflectance measurements yield room-temperature exciton lifetimes of 25 and 50 ps for monolayer and bilayer samples, respectively. The exciton diffusion coefficient in monolayer PtSe 2 is found to be as large as 48 cm 2 s -1 . This value is higher than exciton diffusion coefficients of most known monolayer semiconductors. The deduced exciton mobility is close to the theoretical limit of charge carrier mobility of monolayer PtSe 2 . The superior exciton transport property is unique to monolayers, as the exciton diffusion coefficient drops to 6.7 cm 2 s -1 in bilayers PtSe 2 . The novel exciton transport properties, along with its high air stability, make monolayer PtSe 2 an attractive material for ultrathin excitonic devices. These results provide insights on the exciton dynamic properties of 2D PtSe 2 and help develop fundamental understanding on the performance of various optoelectronic devices based on 2D PtSe 2 . .
Frequency upconversion (UC) luminescence via cooperative energy transfer (CET) process between pairs of Yb{sup 3+} and Tb{sup 3+} ions was investigated in Tb{sup 3+}:Yb{sup 3+}:Y{sub 2}SiO{sub 5} crystalline ceramic powders prepared by combustion synthesis. Surface morphology and structure of the powders were investigated by scanning electronic microscopy and X-ray powder diffraction. Photoluminescence experiments were performed in Tb{sup 3+}-singly doped samples using ultraviolet light (λ=255 nm) and in Tb{sup 3+}:Yb{sup 3+} co-doped samples using a near-infrared (NIR) diode laser (λ=975 nm). Upon excitation with the NIR diode laser, UC luminescence with an intense emission band centered at ∼549 nm, corresponding to the 4f intraband {sup 5}D{sub 4}→{sup 7}F{sub 5} transition of Tb{sup 3+}, along with less intense emission bands at ∼490, ∼590 and ∼620 nm, corresponding to other {sup 5}D{sub 4}→{sup 7}F{sub J} transitions, was detected. The CET rate was estimated by analyzing the dynamics of UC luminescence with rate equations model of the electronic populations. -- Graphical Abstract: Left: Cooperative upconversion luminescence spectra of three powder samples prepared by combustion synthesis. Right: The SEM image of the powder showing that it consists of agglomerated flake-like shaped particles of various sizes. Full scale bar is 20 μm. Highlights: • Yttrium orthosilicate (Y{sub 2}SiO{sub 5}) powders were prepared by combustion synthesis. • Cooperative upconversion is observed for the first time in Tb{sup 3+}–Yb{sup 3+} doped Y{sub 2}SiO{sub 5}. • Energy transfer and back-transfer rates between Tb{sup 3+} and Yb{sup 3+} pairs were estimated.
Graphical abstract: Thermal plasma synthesized nanophase zirconia showing the blue shift in the band gap of monoclinic phase as found from the photoabsorption spectroscopy was found to be the dominant parameter for the enhancement in its photocatalytic activity. The existence of different defect states and their concentration in as synthesized samples also inferred from the photoabsorption measurements were also found to be responsible for the enhanced photocatalytic activity of the samples. Highlights: ► Phase controlled structural formation of nanophase ZrO{sub 2} by thermal plasma route. ► Enhanced photocatalytic degradation rate of methylene blue dye. ► The blue shift in the band gap of monoclinic phase of nanocrystalline ZrO{sub 2}. ► Existence of different defect states in the as synthesized nano phase ZrO{sub 2}. ► Several competing processes which controls the photocatalytic degradation rate. -- Abstract: The photocatalytic activity of pure ZrO{sub 2} samples, prepared by a thermal plasma route, and characterized by X-ray diffraction technique was tested for the degradation of methylene blue, which is known to be a hazardous dye. Although, all these samples synthesized at different operating pressures of the thermal plasma reactor showed the photocatalytic activity; the sample synthesized at 1.33 bar of operating pressure showed the highest photocatalytic activity. The blue shift in the band gap of monoclinic phase, as observed from the photo-absorption spectroscopy, may be attributed to the enhanced photocatalytic activity. The existence of different defect states and their concentration as, inferred from the photo-absorption measurements were also found to be responsible for the enhanced photocatalytic activity of the as synthesized samples.
Graphical abstract: Sodium europium fluorides NaEuF{sub 4} microcrystals have been prepared via a facile hydrothermal route. The possible growth mechanism and the luminescent properties of the as-prepared microcrystals have been discussed. - Highlights: • Sodium europium fluorides NaEuF{sub 4} microspheres were prepared by a facile hydrothermal route. • The as-prepared samples NaEuF{sub 4} and EuF{sub 3} exhibit respective red or orange-red emissions. • These finding may find potential applications in the fields of color display, UV laser and biomedicine. - Abstract: Sodium europium fluorides NaEuF{sub 4} microcrystals with uniform and well-dispersed shapes and dimensions have been prepared via a facile hydrothermal route using Na{sub 3}Cit as the chelating ligand and shape modifier. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected-area electron diffraction (SAED), energy-dispersive X-ray (EDX) and photoluminescence spectra (PL) were taken to characterize the samples. A series of controlled experiments reveal that the trisodium citrate (Na{sub 3}Cit) content, pH value of the initial solution, and reaction time have an indispensable role on the phase, size, and morphology of the as-prepared microcrystals. Based on the experimental results, the possible growth mechanism of the microcrystals prepared under different conditions was proposed. Moreover, we systematically investigated the luminescent properties of the as-prepared microcrystals with different morphologies obtained under different amounts of Na{sub 3}Cit, which have potential application in the fields of color display, UV laser and biomedicine.