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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 73 records · Page 4
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Hanging drop sample preparation improves sensitivity of spatial proteomics

Spatial proteomics holds great promise for revealing tissue heterogeneity in both physiological and pathological conditions. However, one significant limitation of most spatial proteomics workflows is the requirement of large sample amounts that blurs cell-type-specific or microstructure-specific information. In this study, we developed an improved sample preparation approach for spatial proteomics and integrated it with our previously-established laser capture microdissection (LCM) and microfluidics sample processing platform. Specifically, we developed a hanging drop (HD) method to improve the sample recovery by positioning a nanowell chip upside-down during protein extraction and tryptic digestion steps. Compared with the commonly-used sitting-drop method, the HD method keeps the tissue pixel away from the container surface, and thus improves the accessibility of the extraction/digestion buffer to the tissue sample. The HD method can increase the MS signal by 7 fold, leading to a 66% increase in the number of identified proteins. An average of 721, 1489, and 2521 proteins can be quantitatively profiled from laser-dissected 10 μm-thick mouse liver tissue pixels with areas of 0.0025, 0.01, and 0.04 mm 2 , respectively. The improved system was further validated in the study of cell-type-specific proteomes of mouse uterine tissues.

47 OTHER INSTRUMENTATION↗
DOE OSTI2018

Production Procedure and Characterization of Zn-Doped Y-123 Superconducting Samples Prepared by Sol-Gel Method

The superconducting YBa{sub 2}Cu{sub 3−x}Zn{sub x}O{sub 7} (Y-123) bulk materials have been synthesized by using the sol-gel method. Samples are produced as undoped Y-123 and transition metal (Zn)-doped Y-123. Before the final heat treatment, the samples are calcined at 850 °C for 24 h. This process is repeated three times. Then, samples are sintered at 950 °C for 24 h in an air environment and at 500 °C for 5 h in an oxygen atmosphere. The synthesized products are characterized by XRD, R-T, and Vickers microhardness tester. The XRD investigation revealed that the prepared sample has an orthorhombic structure. According to XRD measurements, an orthorhombic structure has not changed with Zn doping. It was observed that undoped and Zn-doped samples have superconductivity properties by electrical measurements. T{sub c}{sup onset} is 89 K for undoped Y-123 sample, and the T{sub c}{sup onset} value decreases monotically with Zn addition. All samples show metallic behavior above T{sub c}{sup onset} temperature. As a result of Vickers microhardness measurements, it is observed that all samples have reverse indentation size effect (RISE) behavior.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2023

Sputter sample preparation for ion beam delivery of radium-223 at ATLAS

A radium-223 ion beam was delivered to an experiment from the electron cyclotron resonance ion source, ECR2, at the Argonne Tandem Linac Accelerator System (ATLAS). Here, the radium-223 material was in a nitrate salt form within a vial, prior to being converted to a usable sputter sample. The sputter sample was produced using a new sample preparation method, where the radium nitrate was dissolved into a solution and pipetted onto pressed aluminum powder. This sample was then allowed to dry, distributing the radium-223 material throughout the sputter sample. Ion source operation using the radium sputter sample is described with the operating parameters listed. The intensity and energy requirements for this ion beam were 1 × 10 6 particles/s and 1.07 GeV, respectively. Because the intensity is relatively low compared to most experiments at ATLAS, previously developed accelerator mass spectrometry methods were used Scott et al. to avoid the need for tuning of the low-intensity beam of interest. Handling of the radium material, as well as loading and unloading of the sputter sample from ECR2, required collaboration with Health Physics. Procedures were used and dry runs were carried out before, during, and after the experiment to ensure the safety of the workers. The processes used and lessons learned are described within.

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2019

Adaptive Sample Preparation and Target Fabrication for High-Throughput Materials Science

High-repetition-rate brilliant and coherent light sources are significantly increasing the rate at which scientific experiments can be performed. An investment in transformative technologies to make samples of condensed matter could enable a paradigm shift for that field or open new exciting frontiers in high-energy density science (HEDS). This will especially be true for dynamic materials in extremes research or HEDS, where the repetition rate for placing samples into extreme environments is increasing and the samples or targets are irreversibly destroyed in each experiment. Research teams that are able to implement solutions to all aspects of the experimental process and enable a paradigm of high-throughput science will have the greatest success and impact. There are two different directions for adaptive samples. One is research when the number of experiments can be greatly increased with increased volume, such as in high energy density science. The other is when flexibility and agility can aid Bayesian optimization computational methods and speed up the discovery process, as with materials science. Conducting a similar equation-of-state (EOS) experiment took three years on the OMEGA laser facility, compared to five days of shifts at the LCLS XFEL. New materials with improved properties have been found by guided optimization of experimental science. Adaptive sample preparation and target fabrication can create a tremendous return on scientific investment. High-throughput enabling precision science is also a desirable goal. To address these issues, we sought a diverse set of innovative participants who had ideas of how to achieve this paradigm shift. We invited 42 researchers from a variety of disciplines and fields to attend a workshop in College Station, Texas, May 14–16, 2019. Many of the participants had never been in the same room before, and most found it very exciting to hear about new and different research. The goal was twofold: to define the challenges, i.e., “what would we like to be able to do and why it is difficult to do so,” and to describe the progress, approaches and capabilities, as well as the vision, “what we could do if we had more support.”

36 MATERIALS SCIENCE↗
DOE OSTI2019

Effect of Cesium Substitution on the Superconducting Properties of Bi-2212 Samples Prepared Via Solid-State Reaction and Laser Floating Zone Technique

In this work, the effect of cesium substitution on the structural and superconducting properties of Bi{sub 2}Sr{sub 2}Ca{sub 1-x}Cs{sub x}Cu{sub 2}O{sub +y} (where x = 0.0, 0.025, 0.050, 0.075, 0.10, 0.125, and 0.15) samples prepared by the solid-state reaction route and by directional growth using the laser floating zone (LFZ) technique has been studied. X-ray diffraction has shown that both kinds of samples present the 2212 phase as the major one, with pseudo tetragonal structure, accompanied by minor amounts of (Sr,Ca)CuO{sub 2} and Bi{sub 2}(Sr,Ca){sub 4}O{sub 6 + d} secondary phases. SEM-EDX results indicate that Bi-2212 phase is the major one, with small amounts of secondary phases. Cs substitution diminishes the size and content of secondary phases. Magnetization measurements reflect different behavior for sintered and LFZ grown samples. Although the diamagnetic transition is very wide for the former samples, it is very sharp for the last ones. The critical onset temperatures, T{sub C}, are around 80 and 90 K, for sintered and LFZ grown samples, respectively. Moreover, M–H measurements indicate that LFZ grown samples exhibit larger areas than the sintered ones. The intragranular critical current, J{sub C}, calculated from the M–H loops and Bean’s formula, is maximum for x = 0.025Cs sintered and x = 0.05Cs LFZ grown samples. The maximum pinning forces, F{sub Pmax}, determined in these samples are higher than those obtained in undoped ones, reaching 9 × 10{sup 7} Oe*A/cm{sup 2} and 10 × 10{sup 8} Oe*A/cm{sup 2}, at 10 K, for sintered and LFZ grown samples, respectively.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Nanoparticle-assisted laser desorption/ionization mass spectrometry: Novel sample preparation methods and nanoparticle screening for plant metabolite imaging

The main goal of the presented research is development of nanoparticle based matrix-assisted laser desorption ionization-mass spectrometry (MALDI-MS). This dissertation includes the application of previously developed data acquisition methods, development of novel sample preparation methods, application and comparison of novel nanoparticle matrices, and comparison of two nanoparticle matrix application methods for MALDI-MS and MALDI-MS imaging.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Toward a Fieldable Atomic Mass Spectrometer for Safeguards Applications: Sample Preparation and Ionization

The International Atomic Energy Agency’s (IAEA’s) long-term research and development plan calls for the development of new methods to detect misuse at nuclear fuel cycle facilities such as reprocessing and enrichment plants. At enrichment plants, for example, the IAEA’s contemporary safeguards approaches are based on a combination of routine and random inspections that include collection of UF6 samples from in-process material and selected cylinders for subsequent analyses. These analyses include destructive analysis (DA) in a laboratory (typically by mass spectrometry [MS]) for isotopic characterization, and environmental sampling (ES) for subsequent laboratory elemental and isotopic analysis (also both typically by MS). One area of new method development includes moving this kind of isotope ratio analytical capability for DA and ES activities into the field. Some of the reasons for these developments include timeliness of results, avoidance of hazardous material shipments, and guidance for additional sample collecting. However, this capability does not already exist for several reasons, such as that most lab-based chemical and instrumental methods rely on laboratory infrastructure (highly trained staff, power, space, hazardous material handling, etc.) and require significant amounts of consumables (power, compressed gases, etc.). In addition, there are no currently available, fieldable instruments for atomic or isotope ratio analysis. To address these issues, Pacific Northwest National Laboratory (PNNL) and collaborator, Clemson University, are studying key areas that limit the fieldability of isotope ratio mass spectrometry for atomic ions: sample preparation and ionization, and reducing the physical size of a fieldable mass spectrometer. PNNL is seeking simple and robust techniques that could be effectively used by inspectors who may have no expertise in analytical MS. In this report, we present and describe the preliminary findings for three candidate techniques: matrix-assisted laser desorption/ionization (MALDI) MS, liquid sampling-atmospheric pressure glow discharge (LS-APGD), and laser ablation/ionization (LAI) MS at atmospheric pressure. Potential performance metrics for these techniques will be presented, including detectability, response, isotope ratio accuracy and precision, and ease of use.

Barinaga, Charles J.↗
DOE OSTI2017

A Comparative Study of Sample Preparation for Staining and Immunodetection of Plant Cell Walls by Light Microscopy

Staining and immunodetection by light microscopy are methods widely used to investigate plant cell walls. The two techniques have been crucial to study the cell wall architecture in planta , its deconstruction by chemicals or cell wall-degrading enzymes. They have been instrumental in detecting the presence of cell types, in deciphering plant cell wall evolution and in characterizing plant mutants and transformants. The success of immunolabeling relies on how plant materials are embedded and sectioned. Agarose coating, wax and resin embedding are, respectively, associated with vibratome, microtome and ultramicrotome sectioning. Here, we have systematically carried out a comparative analysis of these three methods of sample preparation when they are applied for cell wall staining and cell wall immunomicroscopy. In order to help the plant community in understanding and selecting adequate methods of embedding and sectioning for cell wall immunodetection, we review in this article the advantages and limitations of these three methods. Moreover, we offer detailed protocols of embedding for studying plant materials through microscopy.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2016

Sample Preparation Techniques for Grain Boundary Characterization of Annealed TRISO-Coated Particles

Crystallographic information about chemical vapor deposition layers of silicon carbide (SiC) is essential to understanding layer performance, especially when the layers are in non planar geometries, such as spherical. We performed electron Back Scatter Diffraction (EBSD) analysis of spherical SiC layers using a different approach to sample focus ion beam milling technique to avoid the negative impacts of traditional sample polishing and to address the need of very small samples of irradiated materials for analysis. Mechanical and chemical grinding and polishing of sample surfaces can introduce lattice strains and result in unequal removal of SiC and surrounding layers of different material due to the hardness differences of these materials. The nature of layer interfaces is thought to play a key role in performance of the SiC; therefore, analysis of representative samples at these interfacial areas is crucial. In work reported here, a focused ion beam (FIB) was employed in a novel manner to prepare a more representative sample for EBSD analysis from TRISO layers free of effects introduced by mechanical and chemical preparation methods. In addition, the difficulty of handling neutron irradiated microscopic samples such as those analyzed in this work has been simplified with pre tilted mounting stages. Our study showed that although the average grain size of samples may be similar, the grain boundary characteristics may differ significantly. It was also found that low angle grain boundaries, comprises 25% in the FIB-prepared sample vs only 1-2% in the polished sample measured in the same particle. From this study it was determined that results of FIB prepared sample will provide more repeatable results, as the role of sample preparation is eliminated.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2018

Importance of sample preparation on reliable surface characterisation of nano-objects: ISO Standard 20579-4

The international ISO Standard 20579-4, dealing with the history and preparation of nano-objects for surface analysis, has been developed to help address some of the replication and reproducibility issues caused by the fundamental nature of nano-objects. Although all types of samples requiring surface analysis need thoughtful preparation, nano-objects, for which many properties are controlled by their surfaces, present additional challenges in order to avoid variations and artefacts due to the handling and preparation of materials prior to analysis. This international standard is part of a series of standards related to preparation of samples for surface chemical analysis. Parts 1 and 2 of ISO Standard series 20579 address general issues that apply to many samples. Part 4 specifically considers issues that arise due to the inherent nature of nano-objects. Because of sensitivity to their environment, the standard indicates the minimum information that needs to be reported about the handling and preparation of nano-objects prior to surface analysis. This information should become part of sample provenance information that helps assure the reliability and usefulness of data obtained from surface-analysis in the context of the synthesis, processing and analysis history of a batch of material. Application of this standard can help address reproducibility and traceability issues associated with synthesis, processing, and characterization of nano-objects in research and commercial applications.

nano-object characterization, surface analysis, sa↗
NASA NTRS1992

Glass sample preparation and performance investigations

This final report details the work performed under this delivery order from April 1991 through April 1992. The currently available capabilities for integrated optical performance modeling at MSFC for large and complex systems such as AXAF were investigated. The Integrated Structural Modeling (ISM) program developed by Boeing for the U.S. Air Force was obtained and installed on two DECstations 5000 at MSFC. The structural, thermal and optical analysis programs available in ISM were evaluated. As part of the optomechanical engineering activities, technical support was provided in the design of support structure, mirror assembly, filter wheel assembly and material selection for the Solar X-ray Imager (SXI) program. As part of the fabrication activities, a large number of zerodur glass samples were prepared in different sizes and shapes for acid etching, coating and polishing experiments to characterize the subsurface damage and stresses produced by the grinding and polishing operations. Various optical components for AXAF video microscope and the x-ray test facility were also fabricated. A number of glass fabrication and test instruments such as a scatter plate interferometer, a gravity feed saw and some phenolic cutting blades were fabricated, integrated and tested.

Johnson, R. Barry↗
DOE OSTI2016

U-10Mo Sample Preparation and Examination using Optical and Scanning Electron Microscopy

The purpose of this document is to provide guidelines to prepare specimens of uranium alloyed with 10 weight percent molybdenum (U-10Mo) for optical metallography and scanning electron microscopy. This document also provides instructions to set up an optical microscope and a scanning electron microscope to analyze U-10Mo specimens and to obtain the required information.

36 MATERIALS SCIENCE↗
DOE OSTI2016

U-10Mo Sample Preparation and Examination using Optical and Scanning Electron Microscopy

The purpose of this document is to provide guidelines to prepare specimens of uranium alloyed with 10 weight percent molybdenum (U-10Mo) for optical metallography and scanning electron microscopy. This document also provides instructions to set up an optical microscope and a scanning electron microscope to analyze U-10Mo specimens and to obtain the required information.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Sample Preparation Laboratory (SPL) Best Practices: CGD as the Primary Acceptance Method

The traditional paradigm applied to the construction of nuclear safety related systems, structures, and components (SSCs), like SPL, involves an owner/licensee hiring an EPC firm with an NQA 1 program to manage the engineering, procurement, and construction of the desired SSC. This traditional approach would have posed significant barriers to the successful completion of the SPL. As a smaller capital project, in the $\$$100–$\$$200 million range, there was concern that employing one of the larger EPC companies would escalate costs and extend the projected schedule beyond what would be feasible for the Department of Energy (DOE). The traditional acceptance method employed for nuclear facilities with credited safety functions requires the use of an EPC firm applying American Society of Mechanical Engineers (ASME) NQA 1 nuclear quality assurance (NQA) to accept safety SSCs. In lieu of this approach, INL elected to apply its own NQA 1 program to hire an EPC firm operating a commercial quality program. This method used commercial grade dedication (CGD) as outlined in NQA 1 which had not been applied at this scale. Use of the commercial supply chain was identified as a key factor to the successful completion of SPL. Favorable conditions enabling the use of CGD included: • INL serving as both the designer and the design authority • Design created by an NQA 1 qualified source • A mature CGD program • Availability of a CGD subject matter expert (SME) • A strong construction management program. This white paper elaborates on the methodology employed in the construction of the SPL, the successes achieved, and best practices implemented.

42 - ENGINEERING↗
NASA NTRS1979

Paleointensity determinations at elevated temperatures - Sample preparation technique

A technique has been developed for the encapsulation of rock samples in order to prevent the chemical alterations which commonly accompany paleointensity measurements at elevated temperatures. The technique involves vacuum pumping at about 100 C of the sample as placed in a silica tube. The tube containing the sample and a Ti 'getter' are sealed under vacuum. Measurements can be made at 200 and 300 C. Immediately after this, the sample is sealed-off from the getter. The sample is now ready for measurements at higher temperatures.

Taylor, L. A.↗
DOE OSTI2016

Fluidics platform and method for sample preparation

Provided herein are fluidics platforms and related methods for performing integrated sample collection and solid-phase extraction of a target component of the sample all in one tube. The fluidics platform comprises a pump, particles for solid-phase extraction and a particle-holding means. The method comprises contacting the sample with one or more reagents in a pump, coupling a particle-holding means to the pump and expelling the waste out of the pump while the particle-holding means retains the particles inside the pump. The fluidics platform and methods herein described allow solid-phase extraction without pipetting and centrifugation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗