SEARCH · Engineering Papers

Results for “sample preparation optimization”

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.

SourceResearch connectionFrom yearThrough year

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 55 records · Page 3

All sources NASA NTRS DOE OSTI

DOE OSTI2023

Improvements in iridium target chemistry

Abstract We developed and optimized the dissolution and separation chemistry of iridium (Ir) from irradiated Ir pellets and prepared Ir counting samples for analysis by a silicon drift detector. Previous Ir chemistry techniques used on the irradiated Ir pellets are tedious, lengthy, and require extra safety precautions and planning due to the use of perchloric acid in the dissolution step. The dissolution and separations method described in this paper are safer, eliminating the use of perchloric acid, more efficient, and can successfully replace the previous procedure.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

NASA NTRS1984

Process Research of Polycrystalline Silicon Material (PROPSM)

A passivation process (hydrogenation) that will improve the power generation of solar cells fabricated from presently produced, large grain, cast polycrystalline silicon (Semix), a potentially low cost material are developed. The first objective is to verify the operation of a DC plasma hydrogenation system and to investigate the effect of hydrogen on the electrical performance of a variety of polycrystalline silicon solar cells. The second objective is to parameterize and optimize a hydrogenation process for cast polycrystalline silicon, and will include a process sensitivity analysis. The sample preparation for the first phase is outlined. The hydrogenation system is described, and some early results that were obtained using the hydrogenation system without a plasma are summarized. Light beam induced current (LBIC) measurements of minicell samples, and their correlation to dark current voltage characteristics, are discussed.

Culik, J. S.↗

NASA NTRS2003

Use of Computed Tomography for Characterizing Materials Grown Terrestrially and in Microgravity

Computed Tomography (CT) has advanced considerably since being responsible for such dramatic advances in diagnostics within the medical field. It has become a major tool in non destructive evaluation (NDE), and is used in many fields as diverse as coal-mining to metal solidification to examination of rock cores. A review of industrial applications has been written by Dennis. It is only recently that the technique has been seriously used to determine composition through precise measurement of density. While such applications are restricted to cases when there is no ambiguity in the relationship of composition to density. Thus alloy solid solutions lend themselves to compositional analysis provided there is a large change in density with composition. The technique is most useful when rapid non-destructive evaluation is needed. Such cases will occur with samples returning from the International Space Station (ISS) when knowledge of the results could affect future strategies for processing of on-board samples. Experiments from those Principal Investigators (PI) that are most likely to benefit from early CT scanning are discussed. With a dearth of samples, the major emphasis in the first part of this project has been on preparing suitable standards, optimizing the CT technique for these applications, and using the CT system to determine density variations with temperature. An interesting application of CT has been in the examination of meteorites, which can be classified as space-grown materials and will certainly have solidified in a low gravity environment.

Gillies, Donald C.↗

NASA NTRS1975

Flight contaminant trace analyser. Phase 1: Chromatographic input system

The development of a chromatographic column capable of resolving compounds associated with spacecraft atmospheres is presented. Consideration is given to sampling techniques, column parameters and operation, and column interface with a mass spectrometer. A capillary column coated with a mixture of polyalkylene glycols is found to provide the best selectivity for resolving multicomponent mixtures found in spacecraft atmospheres. Temperature programming and isothermal operation of the column are evaluated and it is found that temperature programming has a shorter analysis time for a given carrier gas flow rate and overall superior resolution. It is observed that hydrogen provides a 15% savings in analysis time over helium. Following the optimization of column operational parameters, a mixed phase Ucon capillary is prepared for evaluation during the column test period in which the test sample is automatically analyzed. Analysis of the multicomponent test mixture is completed within 45 minutes provided temperature programming is used. All but two of the test compounds are well resolved.

Source record↗

NASA NTRS1984

Carbon-13 and proton nuclear magnetic resonance analysis of shale-derived refinery products and jet fuels and of experimental referee broadened-specification jet fuels

A proton and carbon-13 nuclear magnetic resonance (NMR) study was conducted of Ashland shale oil refinery products, experimental referee broadened-specification jet fuels, and of related isoprenoid model compounds. Supercritical fluid chromatography techniques using carbon dioxide were developed on a preparative scale, so that samples could be quantitatively separated into saturates and aromatic fractions for study by NMR. An optimized average parameter treatment was developed, and the NMR results were analyzed in terms of the resulting average parameters; formulation of model mixtures was demonstrated. Application of novel spectroscopic techniques to fuel samples was investigated.

Dalling, D. K.↗

NASA NTRS1991

Structural tailoring of advanced turboprops (STAT): User's manual

This user's manual describes the Structural Tailoring of Advanced Turboprops program. It contains instructions to prepare the input for optimization, blade geometry and analysis, geometry generation, and finite element program control. In addition, a sample input file is provided as well as a section describing special applications (i.e., non-standard input).

Brown, K. W.↗

NASA NTRS2014

Connecting Returned Apollo Soils and Remote Sensing: Application to the Diviner Lunar Radiometer

The Diviner Lunar Radiometer, onboard NASA's Lunar Reconnaissance Orbiter, has produced the first global, high resolution, thermal infrared observations of an airless body. The Moon, which is the most accessible member of this most abundant class of solar system objects, is also the only body for which we have extraterrestrial samples with known spatial context, returned Apollo samples. Here we present the results of a comprehensive study to reproduce an accurate simulated lunar environment, evaluate the most appropriate sample and measurement conditions, collect thermal infrared spectra of a representative suite of Apollo soils, and correlate them with Diviner observations of the lunar surface. It has been established previously that thermal infrared spectra measured in simulated lunar environment (SLE) are significantly altered from spectra measured under terrestrial or martian conditions. The data presented here were collected at the University of Oxford Simulated Lunar Environment Chamber (SLEC). In SLEC, we simulate the lunar environment by: (1) pumping the chamber to vacuum pressures (less than 10‐4 mbar) sufficient to simulate lunar heat transport processes within the sample, (2) cooling the chamber with liquid nitrogen to simulate radiation to the cold space environment, and (3) heating the samples with heaters and lamp to set‐up thermal gradients similar to those experienced in the upper hundreds of microns of the lunar surface. We then conducted a comprehensive suite of experiments using different sample preparation and heating conditions on Apollo soils 15071 (maria) and 67701 (highland) and compared the results to Diviner noontime data to select the optimal experimental conditions. This study includes thermal infrared SLE measurements of 10084 (A11 - LM), 12001 (A12 - LM), 14259 (A14 - LM), 15071 (A15 - S1), 15601 (A15 - S9a), 61141 (A16 - S1), 66031 (A16 - S6), 67701 (A16 - S11), and 70181 (A17 - LM). The Diviner dataset includes all six Apollo sites at approximately 200 m spatial resolution We find that analyses of Diviner observations of individual sampling stations and SLE measurements returned Apollo soils show good agreement, while comparisons to thermal infrared reflectance under ambient conditions do not agree well, which underscores the need for SLE measurements and validates the Diviner compositional measurement technique.

Greenhagen, B. T.↗

DOE OSTI2022

An optimized approach and inflation media for obtaining complimentary mass spectrometry-based omics data from human lung tissue

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.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2023

High-Throughput Characterization and Optimization of Polyamide Hydrolase Activity Using Open Port Sampling Interface Mass Spectrometry

Enzymatic biodegradation of polymers, such as polyamides (PA), has the potential to cost-effectively reduce plastic waste, but enhancements in degradation efficiency are needed. Engineering enzymes through directed evolution is one pathway toward identification of critical domains needed for improving activity. However, screening such enzymatic libraries (100s-to-1000s of samples) is time-consuming. Here we demonstrate the use of robotic autosampler (PAL) and immediate drop on demand technology (I.DOT) liquid handling systems coupled with open-port sampling interface-mass spectrometry (OPSI-MS) to screen for PA6 and PA66 hydrolysis by 6-aminohexanoate-oligomer endo-hydrolase (nylon hydrolase, NylC) in a high-throughput (8–20 s/sample) manner. The OPSI-MS technique required minimal sample preparation and was amenable to 96-well plate formats for automated processing. Enzymatic hydrolysis of PA characteristically produced soluble linear oligomer products that could be identified by OPSI-MS. Incubation temperatures and times were optimized for PA6 (65 °C, 24 h) and PA66 (75 °C, 24 h) over 108 experiments. In addition, the I.DOT/OPSI-MS quantified production of PA6 linear dimer (8.3 ± 1.6 μg/mL) and PA66 linear monomer (13.5 ± 1.5 μg/mL) by NylC with a lower limit of detection of 0.029 and 0.032 μg/mL, respectively. For PA6 and PA66, linear oligomer production corresponded to 0.096 ± 0.018% and 0.204 ± 0.028% conversion of dry pellet mass, respectively. The developed methodology is expected to be utilized to assess enzymatic hydrolysis of engineered enzyme libraries, comprising hundreds to thousands of individual samples.

47 OTHER INSTRUMENTATION↗

DOE OSTI2025

Real-Time Screening for Uranium Enrichment by Paper Spray Ionization Mass Spectrometry for Field Applications

A rapid isotope ratio screening technique for uranium enrichment is demonstrated by utilizing paper spray ionization (PSI) high-resolution mass spectrometry (HRMS). Measurements were conducted using an ambient ionization mass spectrometer coupled to a custom-made JEOL PSI attachment apparatus, with de minimus sample preparation requirements. The current method detection limit for individual isotopes (e.g., 235 U and 238 U) is approximately 50 pg, with subsequent optimization expected to further improve U isotopic sensitivity. The PSI analytical method described herein can support rapid analysis (both in-field and in-lab screening) of isotopes-of-interest, as demonstrated by empirical differentiation of depleted uranium (DU) and low enriched uranium (LEU) analytical aliquots. Furthermore, this analytical workflow holds promise for applications in nuclear forensics, international nuclear safeguards, and nonproliferation missions.

Anions↗

NASA NTRS2001

High Resolution Chemical Study of ALH84001

We have studied the chemistry of a sample of the SNC meteorite ALH84001 using an environmental scanning electron microscope (ESEM) with an energy dispersive chemical analytical detector and a focused ion beam secondary ion mass spectrometer (FIB-SIMS). Here we present the chemical data, both spectra and images, from two techniques that do not require sample preparation with a conductive coating, thus eliminating the possibility of preparation-induced textural artifacts. The FIB-SIMS instrument includes a column optimized for SEM with a quadrupole type mass spectrometer. Its spatial and spectral resolution are 20 nm and 0.4 AMU, respectively. The spatial resolution of the ESEM for chemical analysis is about 100 nm. Limits of detection for both instruments are mass dependent. Both the ESEM and the FIB-SIMS instrument revealed contrasting surficial features; crumbled, weathered appearance of the matrix in some regions as well as a rather ubiquitous presence of euhedral halite crystals, often associated with cracks or holes in the surface of the rock. Other halogen elements present in the vicinity of the NaCl crystals include K and Br. In this report, elemental inventories are shown as mass spectra and as X-ray maps.

Conrad, Pamela G.↗

NASA NTRSDate not supplied

Culture-Independent Fungal Profiling for the International Space Station using Nanopore Sequencing: Method Development

Microbial monitoring of the International Space Station (ISS) environment is a crew health requirement that encompasses both bacterial and fungal identification. To achieve this currently, culture-based methods are used for sample collection, and these samples must be returned to the laboratory for analysis. The use of culture and the need for sample return to Earth results in a bias toward culturable organisms and causes a significant delay between sample collection and delivery of final data (weeks to months), respectively. Recently, advancements in molecular technology have aided a broad range of applications, including medical, industrial, and basic sciences. Additionally, increases in portability and ease-of-use of molecular platforms have provided point-of-use capabilities demonstrated by the miniPCR thermal cycler (miniPCR bio) and the MinION sequencer (Oxford Nanopore Technologies). Together, these devices have been applied to, and validated for, the identification of bacteria onboard the ISS. Building on this work, we have developed a spaceflight-compatible fungal workflow. Molecular-based fungal analysis is complicated by low biomass, difficult-to-lyse spores, debate regarding the region for taxonomic assignment, and the lack of bioinformatic pipelines and reference databases. To overcome these difficulties, primers yielding an ~ 2 Kb amplicon were validated against a wide range of ISS fungal isolates. The current spaceflight library preparation was substantially optimized, a bioinformatic pipeline was created, and refinements to the UNITE database were implemented. To compare this optimized method to the current culture-based standard, 30 sample sets (60 total swabs, two swabs held in tandem) were evaluated. Parallel fungal profiles were obtained between the two methods, with the culture-independent method revealing increased diversity. The addition of this method to the already established bacterial process fulfills the crew health identification requirement. Moreover, the implementation of this method onboard ISS will enhance our understanding of its unique fungal microbiome.

Hang N. Nguyen↗

DOE OSTI2025

Site-specific plan-view (S)TEM sample preparation from thin films using a dual-beam FIB-SEM

To fully evaluate the atomic structure, and associated properties of materials using transmission electron microscopy, examination of samples from three non-collinear orientations is needed. This is particularly challenging for thin films and nanoscale devices built on substrates due to limitations with plan-view sample preparation. In this work, a new method for preparation of high-quality, site-specific, plan-view TEM samples from thin-films grown on substrates, is presented and discussed. Here, it is based on using a dual-beam focused ion beam scanning electron microscope (FIB-SEM) system. To demonstrate the method, the samples were prepared from thin films of perovskite oxide BaSnO 3 grown on a SrTiO 3 substrate and metal oxide IrO 2 on a TiO 2 substrate, ranging from 20–80 nm in thicknesses using molecular beam epitaxy. While the method is optimized for the thin films, it can be extended to other site-specific plan-view samples and devices build on wafers. Aberration-corrected STEM was used to evaluate the quality of the samples and their applicability for atomic-resolution imaging and analysis.

BaSnO3↗

NASA NTRS2015

Extension of an Object-Oriented Optimization Tool: User's Reference Manual

The National Aeronautics and Space Administration Armstrong Flight Research Center has developed a cost-effective and flexible object-oriented optimization (O (sup 3)) tool that leverages existing tools and practices and allows easy integration and adoption of new state-of-the-art software. This object-oriented framework can integrate the analysis codes for multiple disciplines, as opposed to relying on one code to perform analysis for all disciplines. Optimization can thus take place within each discipline module, or in a loop between the O (sup 3) tool and the discipline modules, or both. Six different sample mathematical problems are presented to demonstrate the performance of the O (sup 3) tool. Instructions for preparing input data for the O (sup 3) tool are detailed in this user's manual.

Multidisciplinary design optimization↗

DOE OSTI2022

In Situ XAFS, XRD, and DFT Characterization of the Sulfur Adsorption Sites on Cu and Ce Exchanged Y Zeolites

Adsorptive desulfurization with Cu and Ce ion-exchanged Y zeolite (CuCeY) has proven to be an effective method for the removal of sulfur compounds from hydrocarbon fuels. In this study, Cu and Ce exchanged Y materials including CuY, CeY, and CuCeY were prepared and examined to investigate the mechanism behind the superior sulfur adsorption and selectivity of CuCeY. In situ conditions were used to study the materials as prepared for optimal desulfurization. X-ray diffraction (XRD) confirmed the absence of large well-ordered crystalline phases from metallic or oxide Cu and Ce after the reduction of the samples. The oxidation states and local environments of Cu and Ce were determined using X-ray adsorption fine structure (XAFS) analysis and correlated to theoretical findings obtained from density functional theory (DFT) calculations. XAFS data indicate the successful reduction of Cu species to Cu + and Cu o , and Ce to Ce 3+ . Analysis of XAFS spectra located Cu and Ce within the Y zeolite framework with Cu cations in the six-member ring sites and as small metallic Cu clusters. Ce cations were found to occupy both six-member ring and hexagonal prism sites. Furthermore, these results reveal the structure of CuCeY as prepared for desulfurization and provide insight into its superior sulfur adsorption performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1984

A new concept for a Titan atmospheric probe

Since the Voyager 1 close-pass observations of Titan, scientific interest in the nature and composition of the atmosphere and surface of Titan has increased greatly. This enhanced interest has led to the study of mission options to the Saturnian system with a principal goal of depositing a probe into the atmosphere of Titan. Such a probe could carry instrumentation to perform in situ measurements of the structure and composition of the atmosphere and clouds and of the morphology and composition of the surface. Previous studies have examined the possibility of modifying, in a minimal way, the Galileo probe currently being prepared for an atmospheric sampling mission to Jupiter. The purpose of this paper is to report the results of a study of probe-system concepts optimized for the Titan mission. The scientific rationale for such a mission to Titan is discussed and instruments to accomplish the scientific goals are indicated. Probe systems compatible with those goals and instruments are described, and the associated development costs for each are discussed.

Swenson, B. L.↗

DOE OSTI2026

Optimization performance, fidelity, and cost: SIAM VQE

This dataset contains files storing results from classically-simulated quantum subroutines within a dynamical mean-field theory workflow, and jupyter notebooks processing the data in these files to generate plots. The files store: (1) Results from variational quantum eigensolver (VQE) simulations searching for optimal parameters allowing parametrized quantum circuits to prepare approximations to ground states of different Anderson impurity models (AIMs) (2) Results from simulations of a quantum Lanczos algorithm (QLA) estimating the Lanczos coefficients defining the continued-fraction representation of an (AIM) Green’s function Description: Any file named vqe_gs_results* stores approximations to the ground state and energy of a given AIM estimated using three different methods: (1) Numerical diagonalization (2) Ideal VQE simulation (3) VQE simulation with sampling noise For each VQE simulations metadata about the optimization (optimization results plus number of quantum circuits that would have been executed on real hardware) is also stored. Any file named qla_dos_results* estimations for the Lanczos coefficients defining the Green’s function of an AIM. The stored estimations are achieved using different methods: (1) Numerical Lanczos algorithm from initial states obtained from numerical diagonalization (2) Simulated quantum Lanczos algorithm from initial states prepared from parametrized quantum circuits yielded by corresponding ideal and noisy VQE subroutines. The dataset is used and described in M. Karabin et al., "Quantum solver for single-impurity Anderson models with particle-hole symmetry", Phys. Rev. Research 8, 033066 (2026). DOI: https://doi.org/10.1103/7ys3-tl4l

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2023

Sample Preparation Method for Low-Level Total 129 I Measurements by ICP-MS

Trace-level measurements of iodine’s isotopic ( 129 I and 127 I) and chemical species distributions are needed for an accurate understanding of radioiodine migration in the Hanford subsurface. Pacific Northwest National Laboratory (PNNL) previously developed a novel analytical method for iodine characterization that uses ion chromatography (IC) coupled to inductively coupled mass spectrometry (ICP-MS). While the method can measure speciated forms of 129 I at levels below the drinking water standard, an interference from molybdenum (Mo) prevents the assay from quantifying the $\underline{total}$ 129 I concentration in many Hanford sample matrices. In this work, solvent extraction was evaluated as a sample preparation method for eliminating the Mo interference. A series of 10 experiments was conducted in which solutions containing known amounts of iodate or iodide were treated by solvent extraction, and the extracted solutions were analyzed for total iodine concentrations by ICP MS. Several extraction parameters such as reagent concentrations and chemical reaction times were systematically adjusted in attempts to optimize the extraction process. While solvent extraction was shown to be effective at removing Mo, there was a consistent inability to recover more than approximately 75% of the total iodine in most experiments. This would reduce the ability to detect 129 I at levels near the drinking water standard. Additionally, the extraction efficiencies in several experiments were highly variable, suggesting that solvent extraction could add significant uncertainty to radioiodine measurements. We recommend evaluating ion exchange as an alternative sample preparation approach in fiscal year (FY) 2024.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗