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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 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Concomitant ion effects on isotope ratio measurements with liquid sampling – atmospheric pressure glow discharge ion source Orbitrap mass spectrometry

RATIONALE: The field of highly accurate and precise isotope ratio (IR) analysis has been dominated by inductively coupled plasma and thermal ionization mass spectrometers. While these instruments are considered the gold standard for IR analysis, the International Atomic Energy Agency desires a field deployable instrument capable of accurately and precisely measuring U isotope ratios. METHODS: The proposed system interfaces the liquid sampling – atmospheric pressure glow discharge (LS-APGD) ion source with a high resolution Exactive Orbitrap mass spectrometer. With this experimental setup certified U isotope standards and unknown samples were analyzed. The accuracy and precision of the system were then determined. RESULTS: The LS-APGD /Exactive instrument measures a certified reference material of natural U (235U/238U = 0.007258) as 0.007041 with a relative standard deviation of 0.158% meeting the International Target Values for Uncertainty for the destructive analysis of U. Additionally, when three unknowns measured and compared to the results from an ICP multi collector instrument, there is no statistical difference between the two instruments. CONCLUSIONS: The LS-APGD / Orbitrap system, while still in the preliminary stages of development, offers highly accurate and precise IR analysis that suggest a paradigm shift in the world of IR analysis. Furthermore, the portability of the LS-APGD as an elemental ion source combined with the low overhead and small size of the Orbitrap suggest that the instrumentation is capable of being field deployable. With liquid sampling glow discharge-Orbitrap MS, isotope ratio and precision performance improves with rejection of concomitant ion species.

atmospheric pressure sampling↗
DOE OSTI2019

Estimating Sample Heterogeneity and Expected Scatter Due to Cracking in Packed Powder Samples Using a Two-Phase Model

High-precision Hugoniot measurements of heterogeneous materials are a key tool in creating accurate equations of state, but such measurements are prone to larger uncertainties than their homogeneous counterparts. To efficiently reduce these uncertainties one must estimate the relative contributions of different error sources. Sample cracking is one likely source. Here we estimate its contribution through modeling, using computed tomography scans of powdered single crystal quartz samples to estimate typical packing variation within and between samples. Samples were prepared using the same materials and methods. Furthermore, cracks were prominent in the samples. We describe a simple model to estimate shock transit time variation for a single shot due to cracking, and estimate that up to 3% variation can be attributed to these structures. This suggests that decreasing variation requires addressing such packing heterogeneities during target fabrication rather than experimental diagnostics.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Accuracy of tip-sample interaction measurements using dynamic atomic force microscopy techniques: Dependence on oscillation amplitude, interaction strength, and tip-sample distance

Atomic force microscopy (AFM) is a versatile surface characterization method that can map a sample’s topography with high spatial resolution while simultaneously interrogating its surface chemistry through the site-specific high-resolution quantification of the forces acting between the sample and the probe tip. Thanks to considerable advances in AFM measurement technology, such local measurements of chemical properties have gained much popularity in recent years. To this end, dynamic AFM methodologies are implemented where either the oscillation frequency or the oscillation amplitude and phase of the vibrating cantilever are recorded as a function of tip-sample distance and subsequently converted to reflect tip-sample forces or interaction potentials. Such conversion has, however, been shown to produce non-negligible errors when applying the most commonly used mathematical conversion procedures if oscillation amplitudes are of the order of the decay length of the interaction. Extending on these earlier findings, the computational study presented in this paper reveals that the degree of divergence from actual values may also critically depend on both the overall strength of tip-sample interaction and the distance at which the interaction is obtained. These systematic errors can, however, be effectively eliminated by using oscillation amplitudes that are sufficiently larger than the decay length of the interaction potential.

Electrical properties and parameters↗
DOE OSTI2026

Dark Energy Survey Year 6 results: Clustering redshifts and importance sampling of self-organized-maps 𝑛⁡(𝑧) realizations for 3 × 2 ⁢pt samples

This work is part of a series establishing the redshift framework for the 3 × 2 ⁢pt analysis of the Dark Energy Survey Year 6 (DES Y6). For DES Y6, photometric redshift distributions are estimated using self-organizing maps (SOMs), calibrated with spectroscopic and many-band photometric data. To overcome limitations from color-redshift degeneracies and incomplete spectroscopic coverage, we enhance this approach by incorporating clustering-based redshift constraints (clustering-z, or WZ) from angular cross-correlations with BOSS and eBOSS galaxies and eBOSS quasar samples. We define a WZ likelihood and apply importance sampling to a large ensemble of SOM-derived 𝑛⁡(𝑧) realizations, selecting those consistent with the clustering measurements to produce a posterior sample for each lens and source bin. The analysis uses angular scales corresponding to 1.5–5 Mpc to optimize signal-to-noise ratio while mitigating modeling uncertainties and marginalizes over redshift-dependent galaxy bias and other systematics informed by the N-body simulation CARDINAL . While a sparser spectroscopic reference sample limits WZ constraining power at 𝑧 >1.1, particularly for source bins, we demonstrate that combining SOM with WZ improves redshift accuracy and enhances the overall cosmological constraining power of DES Y6. As a result, we estimate an improvement in 𝑆 8 of approximately 10% for cosmic shear and 3 ×2⁢pt analysis, primarily due to the WZ calibration of the source samples.

Cosmological parameters↗
DOE OSTI2018

Sampling for Confidence: Guidance for Evaluating the Quality of Canister Sampling Plans

There is a need for an inspection frequency that demonstrates reasonable assurance that the confinement function of dual-purpose-canisters (DPCs) is maintained as these DPCs are returned to storage service following transportation. The DPCs contain spent fuel from shutdown reactor sites. The currently-proposed 100% DPC inspection frequency is overly conservative and unnecessary to demonstrate reasonable assurance that the confinement function of all DPCs is maintained for return to storage service. Testing all DPCs does not appropriately reflect the very low risk of leakage (i.e., low probability based on design and low consequences based on analysis). Currently, there are 1066 DPCs forecast to be loaded at reactor sites which either are shutdown or plan to cease operations by 2025. These DPCs may be transported by rail in sets of 3 to 5 DPCs per shipment. Assuming each rail consist originates at a single reactor site, an alternative proposal to test one canister/consist/site would result in 356 to 214 canisters, respectively, being tested given the population of 1,066 canisters This Savannah River National Laboratory (SRNL) report outlines statistically-based, random sampling plans that provide guidance on the number of samples of these canisters that are needed to establish bounds on the quality of the outcome of such sampling. The quality of each proposed sampling plan is expressed in the form of a statement that the number of undetected, unacceptable canisters in the population is less than some number, call it D, at a high level of confidence. In addition, evaluations using a similar approach for random sampling at the proposed levels of 214 and 356 canisters are provided.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2019

Sampling for Confidence: Guidance for Evaluating the Quality of Canister Sampling Plans

There is a need for an inspection frequency that demonstrates reasonable assurance that the confinement function of dual-purpose-canisters (DPCs) is maintained as these DPCs are returned to storage service following transportation. The DPCs contain spent fuel from shutdown reactor sites. The currently-proposed 100% DPC inspection frequency is overly conservative and unnecessary to demonstrate reasonable assurance that the confinement function of all DPCs is maintained for return to storage service. Testing all DPCs does not appropriately reflect the very low risk of leakage (i.e., low probability based on design and low consequences based on analysis). Currently, there are 1066 DPCs forecast to be loaded at reactor sites which either are shutdown or plan to cease operations by 2025. These DPCs may be transported by rail in sets of 3 to 5 DPCs per shipment. Assuming each rail consist originates at a single reactor site, an alternative proposal to test one canister/consist/site would result in 356 to 214 canisters, respectively, being tested given the population of 1,066 canisters This Savannah River National Laboratory (SRNL) report outlines statistically-based, random sampling plans that provide guidance on the number of samples of these canisters that are needed to establish bounds on the quality of the outcome of such sampling. The quality of each proposed sampling plan is expressed in the form of a statement that the number of undetected, unacceptable canisters in the population is less than some number, call it D, at a high level of confidence. In addition, evaluations using a similar approach for random sampling at the proposed levels of 214 and 356 canisters are provided. This is a technical report that does not take into account the contractual limitations under the Standard Contract for Disposal of Spent Nuclear Fuel and/or High-Level Radioactive Waste (Standard Contract) (10 CFR Part 961). Under the provisions of the Standard Contract, DOE does not consider spent nuclear fuel in multi-assembly canisters to be an acceptable waste form, absent a mutually agreed upon contract amendment. To the extent discussions or recommendations in this report conflict with the provisions of the Standard Contract, the Standard Contract provisions prevail.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2021

Trace explosives sampling for security applications (TESSA) study: Evaluation of procedures and methodology for contact sampling efficiency

We report the detection of trace amounts of explosive materials is critical to the security at mass transit centers (e.g., airports and railway stations). In a typical screening process, a trap is used to probe a surface of interest to collect and transfer particulate residue to a detector for analysis. The collection of residues from the surface being probed is widely viewed as the limiting step in this process. A multi-institutional study was performed to establish a methodology for the evaluation of sampling media collection efficiencies. Dry deposited residues of 1,3,5-trinitroperhydro-1,3,5-triazine (RDX), C-4 (an RDX-based explosive), and pentaerythritol tetranitrate (PETN) were harvested from acrylonitrile butadiene styrene (ABS) plastic, ballistic nylon (NYL), and uncoated aluminum surfaces using muslin, Texwipe cotton, and stainless-steel mesh traps. Transfer and collection efficiencies of the sample media were calculated based on liquid chromatography-mass spectrometry analysis. Dry transfer efficiencies (DTE%) to all tested surfaces were greater than 75%, with transfer to ABS plastic being the lowest. Collection efficiency (CE%) varied significantly across the traps and the surfaces, yet some conclusions can be drawn; nylon had the lowest CE% for all cases (~10%), and the stainless steel mesh had the lowest CE% for the evaluated traps (~20%). Though the testing parameters have been standardized among the participants to establish a framework for an independent comparison of contact sampling media and surfaces, substantial variations in the DTE% and the CE% were observed, suggesting that other variables can affect contact sampling.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

Determination of Rare Earth Elements in Geological Samples Using Laser-Induced Breakdown Spectroscopy (LIBS) [Determination of Rare Earth Elements in Geological Samples by Laser-Induced Breakdown Spectroscopy (LIBS)]

Laser-induced breakdown spectroscopy (LIBS) was used to detect rare earth elements (REEs) in natural geological samples. Low and high intensity emission lines of Ce, La, Nd, Y, Pr, Sm, Eu, Gd, and Dy were identified in the spectra recorded from the samples to claim the presence of these REEs. Multivariate analysis was executed by developing partial least squares regression (PLS-R) models for the quantification of Ce, La, and Nd. Analysis of unknown samples indicated that the prediction results of these samples were found comparable to those obtained by inductively coupled plasma mass spectrometry analysis. In conclusion, data support that LIBS has potential to quantify REEs in geological minerals/ores.

58 GEOSCIENCES↗
DOE OSTI2020

Characterization of infrequent samples from the concentration, storage and transfer facility: leak detection box (LDB) drain cell sample LIMS# 20195

Savannah River Remediation Engineering (SRR-E) requested that the Savannah River National Laboratory (SRNL) analyze the Concentration, Storage, and Transfer Facility (CSTF) samples from the following Tank Farm areas: the sump encasement, catch tank, drain cell and waste tank annulus. In general, these CSTF samples will be analyzed on an infrequent basis and analyses will include detection for total beta/gamma, total alpha activities and pH measurements. This report presents characterization results for the Leak Detection Box Drain Cell (LDB-DC) sample. The results are measurements for total gamma, total alpha, total beta, pH, density, anions, elementals and total mercury for the LDB-DC sample.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2018

Quantitative Mapping of Nanoscale Chemical Dynamics in Sub-sampled Operando (S)TEM Images Using Spatio-Temporal Analytics

One of the main limitations in the use of operando scanning transmission electron microscopes to study dynamic chemical processes is the effect of the electron beam on the kinetics of the reaction being observed. Here we demonstrate that a flexible Gaussian mixture model can be used to extract quantitative information directly from sub-sampled images, i.e.~images where not all the pixels in the image are illuminated with the beam. The use of this method is demonstrated for the charge/discharge cycle of a Li-battery, where the deposition and dissolution of Li at the anode can be accurately quantified for sub-sampling levels down to 1%. Performing operando imaging using a small fraction of the pixels means that the observations can significantly reduce the effect of the beam, automatically increase the imaging speed and decrease the total data transfer rate required. Such new software capabilities offer the potential to significantly widen the application of operando hardware approaches to study nanoscale dynamics in materials.

Stanfill, Bryan A.↗
DOE OSTI2018

Determining aromatic and aliphatic carboxylic acids in biomass-derived oil samples using 2,4-dinitrophenylhydrazine and liquid chromatography-electrospray injection-mass spectrometry/mass spectrometry

Converting biomass to a useful fuel commonly incorporates the pyrolysis of the biomass feed stock. The base liquid fraction usually contains high concentrations of ketones, aldehydes and carboxylic acids, of which each can cause detrimental issues related to the storage and upgrading process. Knowing the carbonyl species and the concentration of each will provide value information to the pyrolysis researchers, specifically as that community branches into more targeted end-products such as jet fuel or biogenic-derived oxygenate-containing fuel products. The analysis of aldehydes, ketones and small alkyl carboxylic acids using 2,4-dinitrophenylhydrazine (DNPH) derivation method has been well documented and the method is commonly used the analytical community. By using liquid chromatograph coupled to tandem mass spectrometry, biomass sample analysis can be complete with identification of most carbonyl species. The issue of identifying isobaric ketone and aldehyde compounds can be resolved by utilizing differences in retention time or characteristic fragment ions of ketones and aldehydes. One issue which could not resolved using published methods was identifying aromatic or large non-aromatic carboxylic acids from their corresponding hydroxyl aldehyde or ketone analogs. By modifying the current method for determining carbonyls in biomass samples, carboxylic and hydroxyl-carbonyl can be determined. A careful adjustment of the pH during the extraction procedure and extended heating time of the DNPH solution allowed for the successful derivation of aromatic carboxylic acids. Like other dinitrophenylhydrazones, carboxylic acid derivatives also produce a unique secondary ion pattern, which was useful to distinguish these species from the non-acid analogs.

bio-oil↗
DOE OSTI2020

An Open-Cell Environmental Transmission Electron Microscopy Technique for In Situ Characterization of Samples in Aqueous Liquid Solutions

The desire to image specimens in liquids has led to the development of open-cell and closed-cell techniques in transmission electron microscopy (TEM). The closed-cell approach is currently more common in TEM and has yielded new insights into a number of biological and materials processes in liquid environments. The open-cell approach, which requires an environmental TEM (ETEM), is technically challenging but may be advantageous in certain circumstances due to fewer restrictions on specimen and detector geometry. Here, we demonstrate a novel approach to open-cell liquid TEM, in which we use salt particles to facilitate the in situ formation of droplets of aqueous solution that envelope specimen particles coloaded with the salt. This is achieved by controlling sample temperature between 1 and 10°C and introducing water vapor to the ETEM chamber above the critical pressure for the formation of liquid water on the salt particles. Our use of in situ hydration enables specimens to be loaded into a microscope in a dry state using standard 3 mm TEM grids, allowing specimens to be prepared using trivial sample preparation techniques. Furthermore, our future aim will be to combine this technique with an in situ light source to study photocorrosion in aqueous environments.

47 OTHER INSTRUMENTATION↗
DOE OSTI2020

Validation of selection function, sample contamination and mass calibration in galaxy cluster samples

ABSTRACT We construct and validate the selection function of the MARD-Y3 galaxy cluster sample. This sample was selected through optical follow-up of the 2nd ROSAT faint source catalogue with Dark Energy Survey year 3 data. The selection function is modelled by combining an empirically constructed X-ray selection function with an incompleteness model for the optical follow-up. We validate the joint selection function by testing the consistency of the constraints on the X-ray flux–mass and richness–mass scaling relation parameters derived from different sources of mass information: (1) cross-calibration using South Pole Telescope Sunyaev-Zel'dovich (SPT-SZ) clusters, (2) calibration using number counts in X-ray, in optical and in both X-ray and optical while marginalizing over cosmological parameters, and (3) other published analyses. We find that the constraints on the scaling relation from the number counts and SPT-SZ cross-calibration agree, indicating that our modelling of the selection function is adequate. Furthermore, we apply a largely cosmology independent method to validate selection functions via the computation of the probability of finding each cluster in the SPT-SZ sample in the MARD-Y3 sample and vice versa. This test reveals no clear evidence for MARD-Y3 contamination, SPT-SZ incompleteness or outlier fraction. Finally, we discuss the prospects of the techniques presented here to limit systematic selection effects in future cluster cosmological studies.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2022

Dark Energy Survey Year 3 results: calibration of lens sample redshift distributions using clustering redshifts with BOSS/eBOSS

ABSTRACT We present clustering redshift measurements for Dark Energy Survey (DES) lens sample galaxies used in weak gravitational lensing and galaxy clustering studies. To perform these measurements, we cross-correlate with spectroscopic galaxies from the Baryon Acoustic Oscillation Survey (BOSS) and its extension, eBOSS. We validate our methodology in simulations, including a new technique to calibrate systematic errors that result from the galaxy clustering bias, and we find that our method is generally unbiased in calibrating the mean redshift. We apply our method to the data, and estimate the redshift distribution for 11 different photometrically selected bins. We find general agreement between clustering redshift and photometric redshift estimates, with differences on the inferred mean redshift found to be below |Δz| = 0.01 in most of the bins. We also test a method to calibrate a width parameter for redshift distributions, which we found necessary to use for some of our samples. Our typical uncertainties on the mean redshift ranged from 0.003 to 0.008, while our uncertainties on the width ranged from 4 to 9 per cent. We discuss how these results calibrate the photometric redshift distributions used in companion papers for DES Year 3 results.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2024

Design and instrumentation for permanent magnet samples exposed to a radiation environment

This work is part of a larger program to study the effects of radiation on permanent magnets in an accelerator environment. In order to be sure that the permanent magnet samples are accurately placed, measured, and catalogued we have developed a system of sample racks, holders and measuring apparatuses. We have combined these holders and measurement racks with electronics to allow a single computer to catalogue the position and intensity of the magnet measurements. We outline the design of the apparatus, the collection software, and the methodology we will use to collect the data.

Accelerator Physics↗
DOE OSTI2018

DOE/DOT Crude Oil Characterization Research Study, Task 2 Test Report on Evaluating Crude Oil Sampling and Analysis Methods, Revision 1 - Winter Sampling

The Crude Oil Characterization Research Study is designed to evaluate whether crude oils currently transported in North America, including those produced from “tight” formations, exhibit physical or chemical properties that are distinct from conventional crudes, and how these properties associate with combustion hazards that may be realized during transportation and handling. The current report presents results from Task 2, investigating which commercially available methods can accurately and reproducibly collect and analyze crude oils for vapor pressure and composition, including dissolved gases. This issue, Revision 1 – Winter Sampling, incorporates additional seasonal data and compositional analysis results that have become available since publication of a prior report, SAND2017-12482, released in December 2017. Both reports compare performance of commercially available methods to that of a well-established mobile laboratory system that currently serves as the baseline instrument system for the U.S. Strategic Petroleum Reserve Crude Oil Vapor Pressure Program. The experimental matrix evaluates the performance of selected methods for (i) capturing, transporting, and delivering hydrocarbon fluid samples from the field to the analysis laboratory, coupled with (ii) analyzing for properties related to composition and volatility of the oil, including vapor pressure, gas-oil ratio, and dissolved gases and light hydrocarbons. Several combinations of sample capture and analysis were observed to perform well in both summer and winter sampling environments, though conditions apply that need to be considered carefully for given applications. Methods that perform well from Task 2 will then be utilized in subsequent Task 3 (combustion studies) and Task 4 (compositional analyses of multiple crude types), to be addressed in subsequent reports.

02 PETROLEUM↗