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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 163 records · Page 9
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Comparison and validation of the QuEChERSER mega-method for determination of per- and polyfluoroalkyl substances in foods by liquid chromatography with high-resolution and triple quadrupole mass spectrometry

Instances of food contamination with per- and polyfluoroalkyl substances (PFAS) continue to occur globally, but sample preparation and analytical methods are quite limited and often monitor for a small percentage of known PFAS. This study aimed to evaluate, validate, and compare performance of two instruments with the recently developed “quick, easy, cheap, effective, rugged, safe, efficient, and robust” (QuEChERSER) sample preparation mega-method – a method developed to monitor chemicals over a broad range of physicochemical properties. Initial evaluation of the QuEChERSER mega-method for determination of PFAS in food demonstrated recoveries, matrix interferences, and co-extractive removal comparable to (or better than) US Food and Drug Administration (FDA) and USDA Food Safety and Inspection Service (FSIS) methods. Subsequent validation of QuEChERSER in beef, catfish, chicken, pork, liquid eggs, and powdered eggs on a high-resolution mass spectrometer achieved acceptable recoveries (70–120%) and precision (RSDs ≤20%) for all 33 target analytes at the 1 and 5 ng g –1 levels and 67–88% of analytes at the 0.1 ng g –1 level, depending on the matrix. Additional validation was performed by tandem mass spectrometry on a triple quadrupole instrument. This approach provided no non-detects and better recoveries at the 0.1 ng g –1 level than the HRMS method but exhibited more variability at 1 and 5 ng g –1 spiking levels. Analysis of NIST SRMs 1946 and 1947 gave accuracies of 70–117%. Furthermore, these results demonstrate the capability of combining PFAS analysis with a mega-method previously validated for 350 analytes, while collecting non-target data for future retrospective analysis of emerging alternatives with a high-resolution mass spectrometry method.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Identification and Quantification of Photosynthetic Pigments in Algae (Laboratory Analytical Procedure (LAP))

The Laboratory Analytical Procedure (LAP) outlined here describes a method to quantitatively extract phytopigments from microalgae biomass, as well as to identify and quantify individual pigments based on separation and detection with a High-Performance Liquid Chromatography (HPLC) system coupled to a Diode Array Detector (DAD). Pigments were extracted with greater than 95 % extraction efficiency. Chromatographic conditions allowed for isomeric resolution between pigments and identification based on UV/Vis spectra and comparison to analytical standards.

09 BIOMASS FUELS↗
DOE OSTI2021

Analysis and Testing of Parsons NGS Solvent Formulation

Three drums containing solvent used during the Next Generation Solvent Test (NGST) conducted by Parsons in 2014-2015 were received at SRNL. After homogenization, samples from each drum were removed, and a composite sample prepared. This composite was analyzed to determine current SRNL characterization method efficacy, and to determine if the 1,3-dicyclohexyl-2- (isotridecyl) guanidine (DCiTG) suppressor could be selectively removed. The results of this work indicate that the titration analytical method currently employed at SRNL is effective at quantitating the DCiTG. The nuclear magnetic resonance (NMR) method at SRNL can detect the DCiTG, as well its amine and urea decomposition products. However, further development work will be required to allow the 1 H NMR method to quantitate these species. A series of three washing tests were performed on composite samples of the solvent. The results show that up to 67% of the DCiTG was removed from the solvent by simple washing, at multiple ratios of solvent: aqueous phase. This may indicate that a simple pathway exists to wash out the DCiTG and reclaim the solvent (~150 gallons) for future use at the Salt Waste Processing Facility (SWPF).

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

Comprehensive Chemical Fingerprinting by Multidimensional GC and Supervised Machine Learning

This project leveraged advances in machine learning based data analysis techniques and untargeted analytical methods for organic analysis to progress nuclear nonproliferation technologies beyond current capabilities. The developed approaches can be used to detect and identify complex chemical fingerprints of facilities of interest. These techniques have been developed for fields such as metabolomics and genomics but have not been applied to nuclear nonproliferation applications. Adaptation of these techniques for volatile organic compound analysis has far reaching application within the scientific community including environmental chemistry, atmospheric physics, and climate sciences.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗
DOE OSTI2025

Characterization of Tank 9H Annulus Sample in Support of Residual Material Inventory Determinations

The Savannah River National Laboratory (SRNL) was requested by Savannah River Mission Completion (SRMC) to provide sample preparation and characterization of the Tank 9H annulus sample in support of Residual Material Inventory Determinations. One Tank 9H sample in three vials [HTF-9-25-13, HTF-9-25-14 and HTF-9-25-15], with each vial containing approximately 200 mL of the Tank 9H annulus salt solution, were delivered to the SRNL Shielded Cells for sample preparation and characterizations in February 2025. The density of the “as-received” solution contained in each of the three Tank 9H annulus sample vials were determined followed by a solid-liquid separation on each one using 0.45-micron Nalgene® nylon filter membranes. The resulting filtrates were combined to form the Tank 9H annulus sample with a total volume of about 600 mL. The combined wet solid fractions, about a total of 4.8 grams of salt material, remaining on the filter membranes were air-dried in the Shielded Cells for 72 hours. The total weight of the air-dried solids was 2.1 grams. These air-dried solids were washed with deionized water (DI water) at a phase ratio of 60 mL DI water/gram of solids to recover insoluble solids, if any. No visible or measurable quantity of insoluble solids were recovered after DI water washing of the air-dried solids because the air-dried solids completely dissolved in the DI water. The solid fraction-wash water was not combined with the 600 mL of the filtrate solution, and the resulting solution was not screened or analyzed for radionuclides. Aliquot sample volumes of the undiluted Tank 9H annulus sample were sent to the SRNL analytical services groups for radionuclides, elementals, anions and total mercury analysis by various methods including radiochemical separations/counting methods, inductively coupled plasma-atomic emission spectroscopy (ICP-AES), and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS) and special preparations. All sample analyses were performed in triplicate. This report presents the analytical characterization results for the Tank 9H annulus sample. The results are also reported where analytical methods yielded additional analytes, other than those requested by SRMC. In the characterization of the Tank 9H annulus sample, the detection limits for all the analytes, as specified in the Technical Task Request (TTR) and Task Technical and Quality Assurance Plan (TTQAP), were met.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
NASA NTRS2001

Analysis of Volatile Organic Compounds in a Controlled Environment: Ethylene Gas Measurement Studies on Radish

Volatile organic compound(VOC), ethylene gas, was characterized and quantified by GC/FID. 20-50 ppb levels were detected during the growth stages of radish. SPME could be a good analytical tool for the purpose. Low temperature trapping method using dry ice/diethyl ether and liquid nitrogen bath was recommended for the sampling process for GC/PID and GC/MS analysis.

Kong, Suk Bin↗
NASA NTRS2004

Microscale Concentration Measurements Using Laser Light Scattering Methods

The development of lab-on-a-chip devices for microscale biochemical assays has led to the need for microscale concentration measurements of specific analyses. While fluorescence methods are the current choice, this method requires developing fluorophore-tagged conjugates for each analyte of interest. In addition, fluorescent imaging is also a volume-based method, and can be limiting as smaller detection regions are required.

Niederhaus, Charles↗
NASA NTRS2011

MEPAG Recommendations for a 2018 Mars Sample Return Caching Lander - Sample Types, Number, and Sizes

The return to Earth of geological and atmospheric samples from the surface of Mars is among the highest priority objectives of planetary science. The MEPAG Mars Sample Return (MSR) End-to-End International Science Analysis Group (MEPAG E2E-iSAG) was chartered to propose scientific objectives and priorities for returned sample science, and to map out the implications of these priorities, including for the proposed joint ESA-NASA 2018 mission that would be tasked with the crucial job of collecting and caching the samples. The E2E-iSAG identified four overarching scientific aims that relate to understanding: (A) the potential for life and its pre-biotic context, (B) the geologic processes that have affected the martian surface, (C) planetary evolution of Mars and its atmosphere, (D) potential for future human exploration. The types of samples deemed most likely to achieve the science objectives are, in priority order: (1A). Subaqueous or hydrothermal sediments (1B). Hydrothermally altered rocks or low temperature fluid-altered rocks (equal priority) (2). Unaltered igneous rocks (3). Regolith, including airfall dust (4). Present-day atmosphere and samples of sedimentary-igneous rocks containing ancient trapped atmosphere Collection of geologically well-characterized sample suites would add considerable value to interpretations of all collected rocks. To achieve this, the total number of rock samples should be about 30-40. In order to evaluate the size of individual samples required to meet the science objectives, the E2E-iSAG reviewed the analytical methods that would likely be applied to the returned samples by preliminary examination teams, for planetary protection (i.e., life detection, biohazard assessment) and, after distribution, by individual investigators. It was concluded that sample size should be sufficient to perform all high-priority analyses in triplicate. In keeping with long-established curatorial practice of extraterrestrial material, at least 40% by mass of each sample should be preserved to support future scientific investigations. Samples of 15-16 grams are considered optimal. The total mass of returned rocks, soils, blanks and standards should be approximately 500 grams. Atmospheric gas samples should be the equivalent of 50 cubic cm at 20 times Mars ambient atmospheric pressure.

Allen, Carlton C.↗
DOE OSTI2020

Low Level Calibration of Liquid Scintillation Counting

Liquid Scintillation Counting (LSC) is an analytical laboratory method that quantifies the concentrations of alpha and beta emitting isotopes. The LSC method can be utilized for the detection of tritium, both environmentally and at nuclear facilities. Most LSC samples are aqueous-based and prepared as a radioactive sample dissolved or suspended in a high efficiency scintillation cocktail that converts radioactive energy into light pulses. When placed in counting vials, the liquid scintillation cocktail allows for optical coupling in which energy is released from the samples radioactive decay, and transferred to the scintillator. That energy is then absorbed to produce excited electrons that fall back to their ground-state and emit a pulse of light that is detected by the liquid scintillation analyzers photomultiplier tubes. Quench is a signal attenuation due to physical, chemical, or color interferences. To compensate for quench, quench standards of a known concentration are implemented at increasing increments of quench per vial to create a quench curve. Quench standards can be purchased pre-made or customized from the manufacturer, however, there are several issues that arise from purchasing the pre-made quench standards. The main issues with ordering pre-made quench standards is that they use higher count values, between 30,000 and 250,000 disintegrations per minute (dpm) of tritium per vial and only come in glass vials. Using higher counting standards in glass vials makes it hard to see lower concentrations in plastic vials. Additionally, when using higher energy standards the accuracy of the calibration readings tend to be lower. On the other hand, making a set of quench standards in-house allows for the customization of the dpm concentration to roughly 1,500-3,000 and preparation in plastic vials. This allows for lower activity readings that results in closer precision of the samples' true concentration. Technical Objectives: Create a quench curve and calibrate the LSA for tritium. Verify the calibration of the quench curve prior to cross sample runs. Check calibration against Quality Control (QC) reference value. Conclusion: a tritium quench curve calibration was performed using a scintillation cocktail with ultima gold (AB and AB/F), acetone (only with AB), and water (only with AB/F). By performing the tritium quench curve calibration, the counting efficiency was correlated to various levels of quench. Calibration checks with quality control standards were also performed to verify that the calibration was correct. The observed results provided acceptable values that matched the quality control standard reference values with an acceptable uncertainty. The next step will be fine tuning and cross comparison checks with legacy instrumentation.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2024

Physics-Based Machine Learning Methods for U-235 Forensics Signatures

Signatures of low-intensity U-235 sources have been recently studied by utilizing a variety of machine learning (ML) classifiers using features derived from gamma spectral measurements collected under structured campaigns. Several ML classifiers, such as ensemble of tress and classification trees, revealed misleadingly-optimistic training error due to over-fitting, and furthermore, their performance is not directly relatable to the physical properties due to their data-driven, opaque designs. We present a regression-based ML method that first estimates the inverse distance to the source and then utilizes a threshold to infer its presence, by representing the background as a source located at an infinite distance. For the inverse distance estimation, we study the ensemble of trees and Gaussian process regression methods, and a hyper parameter auto-tuning and selection method that employs five regression estimators. These methods avoid the over-fitting observed in several ML classifiers, while providing the classification error nearly comparable to them based on independent test data. Their error is directly related to estimates of the inverse physical distance to source, and the precision of error determines the seperability property that determines the false alarm and missed detection rates. The property of monotonic decrease of the source strength with increasing detector distance combined with Poisson distribution of measurements is utilized to analytically validate these methods by deriving the generalization equations of underlying regression methods.

Rao, Nageswara↗
DOE OSTI2024

Methane Leak Detection from Natural Gas Power Plants

The results of a literature review around leak detection at NG-fueled power plants are presented. The results show that leak detection methods between plants are highly variable and mostly qualitative. Flanged connections and valves are the most common leak points. Plant analytics show a correlation between vibration and %LEL. No other variables show a significant correlation.

Boeke, Seth↗
DOE OSTI2025

Detection limits for laser absorption spectroscopy of Li in laser ablation plumes

A high-sensitivity laser absorption spectroscopy (LAS) method is demonstrated for rapid and non-contact analysis of Li in solids. Glass samples with Li concentrations ranging from 1-500 ppm by mass are ablated in 5 Torr air, and time-resolved Li atomic absorption is measured using a tunable laser near 671 nm. Significant improvements in analytical performance over prior laser-induced breakdown techniques are demonstrated. Here, a single-shot limit of detection (LOD) of 180 ppb is shown for fixed wavelength operation, improving to 6 ppb with averaging over 1000 ablation shots (100 s acquisition time). Isotope-resolved Li absorption spectra are measured with a 17 ppb LOD in 40 s. Methods for optimizing LOD based on noise/averaging properties of LAS experiments in LA plumes are discussed.

(020.3260) Isotope shifts↗
DOE OSTI2021

Improving Detection of Disease Re-emergence Using a Web-Based Tool (RED Alert): Design and Case Analysis Study

Background: Currently, the identification of infectious disease re-emergence is performed without describing specific quantitative criteria that can be used to identify re-emergence events consistently. This practice may lead to ineffective mitigation. In addition, identification of factors contributing to local disease re-emergence and assessment of global disease re-emergence require access to data about disease incidence and a large number of factors at the local level for the entire world. This paper presents Re-emerging Disease Alert (RED Alert), a web-based tool designed to help public health officials detect and understand infectious disease re-emergence. Objective: Our objective is to bring together a variety of disease-related data and analytics needed to help public health analysts answer the following 3 primary questions for detecting and understanding disease re-emergence: Is there a potential disease re-emergence at the local (country) level? What are the potential contributing factors for this re-emergence? Is there a potential for global re-emergence? Methods: We collected and cleaned disease-related data (eg, case counts, vaccination rates, and indicators related to disease transmission) from several data sources including the World Health Organization (WHO), Pan American Health Organization (PAHO), World Bank, and Gideon. We combined these data with machine learning and visual analytics into a tool called RED Alert to detect re-emergence for the following 4 diseases: measles, cholera, dengue, and yellow fever. We evaluated the performance of the machine learning models for re-emergence detection and reviewed the output of the tool through a number of case studies. Results: Our supervised learning models were able to identify 82%-90% of the local re-emergence events, although with 18%-31% (except 46% for dengue) false positives. This is consistent with our goal of identifying all possible re-emergences while allowing some false positives. The review of the web-based tool through case studies showed that local re-emergence detection was possible and that the tool provided actionable information about potential factors contributing to the local disease re-emergence and trends in global disease re-emergence. Conclusions: To the best of our knowledge, this is the first tool that focuses specifically on disease re-emergence and addresses the important challenges mentioned above.

60 APPLIED LIFE SCIENCES↗
NASA NTRS1990

Thermomechanical properties of polymeric materials and related stresses

The thermomechanical analysis (TMA) and dynamic mechanical analysis characterizations of a polymeric material yield useful data relating to the thermomechanical stresses of eight widely used polymeric materials. The materials encompass Lexan, Plexiglass, Epon, Conap, Uralane, Solithane, and Humiseal. A combined profile of the coefficient of thermal expansion (CTE) and the modulus change over a wide temperature range obtained by these analytical methods indicates the drastic effects of glass transition on both the CTE and the modulus of a polymer. TMA can also detect secondary transitions, and provides a convenient means for the study of a polymer's toughness.

Lee, Sheng Yen↗
NASA NTRS1977

A measurement system for the atmospheric trace gases CH4 and CO

A system for measuring ambient clean air levels of the atmospheric trace gases methane and carbon monoxide is described. The analytical method consists of a gas chromatographic technique that incorporates sample preconcentration with catalytic conversion of CO to CH4 and subsequent flame ionization detection of these gases. The system has sufficient sensitivity and repeatability to make the precise measurements required to establish concentration profiles for CO and CH4 in the planetary boundary layer. A discussion of the bottle sampling program being conducted to obtain the samples for the concentration profiles is also presented.

Condon, E. P.↗
NASA NTRS1994

Structural damage detection of space truss structures using best achievable eigenvectors

A method is presented by which measured modes and frequencies from a modal test can be used to determine the location and magnitude of damage in a space struss structure. The damage is located by computing the Euclidean distances between the measured mode shapes and the best achievable eigenvectors. The best achievable eigenvectors are the projection of the measured mode shapes onto the subspace defined by the refined analytical model of the structure and the measured frequencies. Loss of both stiffness and mass properties can be located and quantified. To examine the performance of the method when experimentally measured modes are employed, various damage detection studies using a laboratory eight-bay truss structure were conducted. The method performs well even though the measurement errors inevitably make the damage location more difficult.

Lim, Tae W.↗
DOE OSTI2024

CLimate Impact: Determining Etiology thRough pAthways (CLDERA)

Climate impacts have broad economic, health, political, and national security ramifications. Societally relevant impacts are typically farther downstream, are the product of multiple interacting processes, and can arise over small regions and timeframes because their sources are short-term and localized. Short-term forcings (as can be seen in volcanic eruptions, climatic tipping points (e.g., the collapse of rainforests or the disappearance of sea ice), or in increasingly plausible climate interventions) fundamentally possess low signal-to-noise and could benefit from accounting for the multiple conditional processes through which a downstream impact arises. Under the Grand Challenge LDRD CLDERA (CLimate impacts: Discovering Etiology thRough pAthways), we have developed tools to enable downstream impact attribution from geographically and temporally localized source forcings in the climate. CLDERA developed methods that can distinguish how a localized source drives the climate system to respond with particular impacts. The how is embodied in pathways – the spatio-temporally evolving chain of physical processes that connects a source to a series of increasingly distant impacts. Novel analytic methods in pursuit of downstream impact attribution were developed and demonstrated on simulations and observations of the 1991 eruption of Mt. Pinatubo in the Philippines. As described within this report we have • developed stratospheric expertise and aerosol modeling capabilities in E3SM, • created original methods to detect and model pathways from source-to-impact, and • advanced climate attribution through novel methods, cases, and approaches. Further, CLDERA developed a tiered verification process consisting of controlled datasets to prototype, verify, and refine the original method development. CLDERA increased Sandia’s footprint in the climate analytics community and developed new climate collaborations whilst also creating a cadre of climate analysts at Sandia. The products from CLDERA have been extensive with a total of 9 journal articles published, 12 articles submitted and under review, and an additional 8 articles in preparation. We have produced 1750 simulated years and developed 9 code-bases. This report details these accomplishments and serves as a summary of the work completed during the CLDERA Grand Challenge.

54 ENVIRONMENTAL SCIENCES↗