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All sources NASA NTRS DOE OSTI

DOE OSTI2015

Rapid Analysis of Microalgal Triacylglycerols with Direct-Infusion Mass Spectrometry

Cultivation of microalgae has the potential to provide lipid-derived feedstocks for conversion to liquid transportation fuels. Lipid extracts from microalgae are significantly more complex than those of traditional seed oils, and their composition changes significantly throughout the microalgal growth period. With three acyl side chains per molecule, triglycerides (TAGs) are an important fuel precursor, and the distribution of acyl chain composition for TAGs has a significant impact on fuel properties and processing. Therefore, determination of the distribution of microalgal TAG production is needed to assess the value of algal extracts designed for fuel production and to optimize strain, cultivation, and harvesting practices. Methods utilized for TAG speciation commonly involve complicated and time-consuming chromatographic techniques. Here we present a method for TAG speciation and quantification based on direct-infusion mass spectrometry, which provides rapid characterization of TAG profiles without chromatographic separation. Specifically, we utilize Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) to provide a reference library of TAGs for the microalgae Nannochloropsis sp. that provides the basis for high-throughput TAG quantitation by time-of-flight mass spectrometry (TOF MS). In conclusion, we demonstrate the application of this novel approach for lipid characterization with respect to TAG compound distribution, which informs both immediate and future strain and process optimization strategies.

09 BIOMASS FUELS↗

DOE OSTI2022

Comparative Analysis of Direct and Indirect Cooling of Wide-Bandgap Power Modules and Performance Enhancement of Jet Impingement-Based Direct Substrate Cooling

With the development of high-power and high-torque machines, requirements for high-power density electronics are increasing. Thermal management of such systems requires high heat extraction. Conventional air cooling based heat sinks and cold plate based liquid cooling have their own benefits for various applications but has limitations for high power density applications. The current study explores a jet impingement based direct substrate cooling system that was implemented for a SiC based direct bonded Cu substrate for various power losses. Numerical comparison between jet impingement cooling and conventional horizontal/indirect cooling (pin fin heat sink and genetic algorithm-optimized heat sink) showed that the area weighted average of the heat transfer coefficient (HTC) is high for both horizontal cooling designs, and the local HTC is higher for jet impingement. Design iterations were undertaken to resolve the bottleneck of this cooling system. Increasing the number of nozzles helped to cover more area at the direct bonded Cu bottom plate, which drops the chip temperature considerably. With a constant flow rate, increasing the number of nozzles would decrease local jet velocity, which reduces the heat extraction by jet impingement. This issue can be addressed by reducing the diameter of nozzle but doing so results in a high pressure drop where the design constraint is 2 psi. A flared nozzle design is proposed, which has a higher spreading angle of the jet that increases the flow coverage and reduces the pressure drop of the coolant loop.

Barua, Himel↗

DOE OSTI2020

Multivariate Linear Models for In Situ Monitoring of Low-Activity Nuclear Waste Using Infrared and Raman Spectroscopy - 20218

This paper presents the use of in situ monitoring tools for molecular analysis of non-radioactive species found in the supernatant liquid and dissolvable salt cake of nuclear waste at Hanford. We have selected two in situ spectroscopic techniques that do not require any sample preparation or consumables: infrared (in the form of attenuated total reflectance Fourier transform infrared or ATR-FTIR) and Raman spectroscopy. This work aims to evaluate their performance for liquid waste simulants representative of the Hanford DFLAW (Direct Feed Low-Activity Waste) feed. In addition, we have evaluated the performance of four multivariate linear models that extract concentrations from spectral measurements for a data set that was designed to include key molecular species found in liquid low-activity waste. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2023

Fault Detection in the Solvent Extraction Process with Non-traditional Sensors

Solvent extraction is used to separate metals or other complexes into two different immiscible liquids and is an essential component of the PUREX Process. Improvements to the solvent extraction process can directly contribute to an organization’s ability to ensure the purity and recovery of special nuclear materials from spent nuclear fuel. Such improvements can benefit nuclear reprocessing efforts, increase fuel reutilization, and limit the concentration of actinides in nuclear waste repositories.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗

DOE OSTI2016

Electrolysis of a molten semiconductor

Metals cannot be extracted by electrolysis of transition-metal sulfides because as liquids they are semiconductors, which exhibit high levels of electronic conduction and metal dissolution. Herein by introduction of a distinct secondary electrolyte, we reveal a high-throughput electro-desulfurization process that directly converts semiconducting molten stibnite (Sb 2 S 3 ) into pure (99.9%) liquid antimony and sulfur vapour. At the bottom of the cell liquid antimony pools beneath cathodically polarized molten stibnite. At the top of the cell sulfur issues from a carbon anode immersed in an immiscible secondary molten salt electrolyte disposed above molten stibnite, thereby blocking electronic shorting across the cell. In conclusion, as opposed to conventional extraction practices, direct sulfide electrolysis completely avoids generation of problematic fugitive emissions (CO 2 , CO and SO 2 ), significantly reduces energy consumption, increases productivity in a single-step process (lower capital and operating costs) and is broadly applicable to a host of electronically conductive transition-metal chalcogenides.

36 MATERIALS SCIENCE↗

NASA NTRS2010

Automated Desalting Apparatus

Because salt and metals can mask the signature of a variety of organic molecules (like amino acids) in any given sample, an automated system to purify complex field samples has been created for the analytical techniques of electrospray ionization/ mass spectroscopy (ESI/MS), capillary electrophoresis (CE), and biological assays where unique identification requires at least some processing of complex samples. This development allows for automated sample preparation in the laboratory and analysis of complex samples in the field with multiple types of analytical instruments. Rather than using tedious, exacting protocols for desalting samples by hand, this innovation, called the Automated Sample Processing System (ASPS), takes analytes that have been extracted through high-temperature solvent extraction and introduces them into the desalting column. After 20 minutes, the eluent is produced. This clear liquid can then be directly analyzed by the techniques listed above. The current apparatus including the computer and power supplies is sturdy, has an approximate mass of 10 kg, and a volume of about 20 20 20 cm, and is undergoing further miniaturization. This system currently targets amino acids. For these molecules, a slurry of 1 g cation exchange resin in deionized water is packed into a column of the apparatus. Initial generation of the resin is done by flowing sequentially 2.3 bed volumes of 2N NaOH and 2N HCl (1 mL each) to rinse the resin, followed by .5 mL of deionized water. This makes the pH of the resin near neutral, and eliminates cross sample contamination. Afterward, 2.3 mL of extracted sample is then loaded into the column onto the top of the resin bed. Because the column is packed tightly, the sample can be applied without disturbing the resin bed. This is a vital step needed to ensure that the analytes adhere to the resin. After the sample is drained, oxalic acid (1 mL, pH 1.6-1.8, adjusted with NH4OH) is pumped into the column. Oxalic acid works as a chelating reagent to bring out metal ions, such as calcium and iron, which would otherwise interfere with amino acid analysis. After oxalic acid, 1 mL 0.01 N HCl and 1 mL deionized water is used to sequentially rinse the resin. Finally, the amino acids attached to the resin, and the analytes are eluted using 2.5 M NH4OH (1 mL), and the NH4OH eluent is collected in a vial for analysis.

Spencer, Maegan K.↗

DOE OSTI2012

Selective Extraction of Uranium from Liquid or Supercritical Carbon Dioxide

Current liquid-liquid extraction processes used in recycling irradiated nuclear fuel rely on (1) strong nitric acid to dissolve uranium oxide fuel, and (2) the use of aliphatic hydrocarbons as a diluent in formulating the solvent used to extract uranium. The nitric acid dissolution process is not selective. It dissolves virtually the entire fuel meat which complicates the uranium extraction process. In addition, a solvent washing process is used to remove TBP degradation products, which adds complexity to the recycling plant and increases the overall plant footprint and cost. A liquid or supercritical carbon dioxide (l/sc-CO 2 ) system was designed to mitigate these problems. Indeed, TBP nitric acid complexes are highly soluble in l/sc-CO 2 and are capable of extracting uranium directly from UO 2 , UO 3 and U 3 O 8 powders. This eliminates the need for total acid dissolution of the irradiated fuel. Furthermore, since CO 2 is easily recycled by evaporation at room temperature and pressure, it eliminates the complex solvent washing process. In this report, we demonstrate: (1) A reprocessing scheme starting with the selective extraction of uranium from solid uranium oxides into a TBP-HNO 3 loaded Sc-CO 2 phase, (2) Back extraction of uranium into an aqueous phase, and (3) Conversion of recovered purified uranium into uranium oxide. The purified uranium product from step 3 can be disposed of as low level waste, or mixed with enriched uranium for use in a reactor for another fuel cycle. After an introduction on the concept and properties of supercritical fluids, we first report the characterization of the different oxides used for this project. Our extraction system and our online monitoring capability using UV-Vis absorbance spectroscopy directly in sc-CO 2 is then presented. Next, the uranium extraction efficiencies and kinetics is demonstrated for different oxides and under different physical and chemical conditions: l/sc-CO 2 pressure and temperature, TBP/HNO 3 complex used, reductant or complexant used for selectivity, and ionic liquids used as supportive media. To complete the extraction and recovery cycle, we then demonstrate uranium back extraction from the TBP loaded sc-CO 2 phase into an aqueous phase and the characterization of the uranium complex formed at the end of this process. Another aspect of this project was to limit proliferation risks by either co-extracting uranium and plutonium, or by leaving plutonium behind by selectively extracting uranium. We report that the former is easily achieved, since plutonium is in the tetravalent or hexavalent oxidation state in the oxidizing environment created by the TBP-nitric acid complex, and is therefore co-extracted. The latter is more challenging, as a reductant or complexant to plutonium has to be used to selectively extract uranium. After undertaking experiments on different reducing or complexing systems (e.g., AcetoHydroxamic Acid (AHA), Fe(II), ascorbic acid), oxalic acid was chosen as it can complex tetravalent actinides (Pu, Np, Th) in the aqueous phase while allowing the extraction of hexavalent uranium in the sc-CO 2 phase. Finally, we show results using an alternative media to commonly used aqueous phases: ionic liquids. We show the dissolution of uranium in ionic liquids and its extraction using sc-CO 2 with and without the presence of AHA. The possible separation of trivalent actinides from uranium is also demonstrated in ionic liquids using neodymium as a surrogate and diglycolamides as the extractant.

carbone dioxide↗

DOE OSTI2020

Transport of coexisting Ni-Cu sulfide liquid and silicate melt in partially molten peridotite

Transport of coexisting sulfide and silicate melts in partially molten peridotite contributes to the redistribution of chalcophile elements within the upper mantle as well as the genesis of magmatic Ni-Cu sulfide deposits, but has not been investigated systematically. Using laboratory experiments, theoretical calculations, and X-ray synchrotron microtomography, this study documents the topology and considers controls on the extraction of two immiscible liquids during partial melting of mantle peridotite. Under hydrostatic conditions, the measured dihedral angle at silicate melt-mineral-mineral junctions is 13.7–21.3°. Silicate melt is distributed along grain edges forming incompletely interconnected melt channels that disconnected by some dead ends at melt fractions ~7–9 vol%. Application of theoretically predicted permeability (k ~10 -14 -10 -16 m 2 ) permits estimation of the extraction velocity of silicate melt of 0.7-11.1 μm/day within a single interconnected melt channel. In the absence of silicate melt, isolated sulfide droplets (3.77 vol%) show a sulfide-olivine-olivine dihedral angle of 91.5–101.3°. However, in the presence of silicate melt, sulfide droplets (average size ~2.53±2.14μm, 1σ) are partially surrounded by silicate melt and stranded in triple junctions or melt pockets due to the limitation of the smallest dimension (0.3μm) of melt channels. Thus, the extraction of sulfide liquid is highly restricted by these dead ends and the smallest dimension of melt channels during porous flow of silicate melt. In contrast, during large-strain shear deformation (strain ~1.6–2.5), initially stranded sulfide droplets were elongated and extracted with silicate melt into liquid-rich sheets with a length of several hundred microns, constantly oriented at 14.3±4.5°to the shear plane and antithetic to the shear direction. The angle is lower than that (18-30°) of those sheets containing sulfide liquid only, indicating that silicate melt dominates liquid-rich sheets. Driven by stress, silicate melt-dominated liquid-rich sheets open the appropriately oriented grain boundaries between silicate minerals, thus providing an efficient pathway for the extraction of sulfide liquid during deformation. When such sheet-like channels remain open, sulfide droplets (> millimeter-scale) can be potentially mobile through high strain domains of the upper mantle, contributing to the addition of chalcophile elements and the fertilization of the lithospheric mantle.

high P-T experiment↗

DOE OSTI2017

Porous Chitin Microbeads for More Sustainable Cosmetics

Not provided.

Chemistry↗

DOE OSTI2025

Discovering Ni/Cu Single-Atom Alloy as a Highly Active and Selective Catalyst for Direct Methane Conversion to Ethylene: A First-Principles Kinetic Study

Direct methane conversion to liquid fuels or value-added chemicals is a promising technology to utilize natural resources without resorting to further petroleum extraction. However, discovering efficient catalysts for this reaction is challenging due to either coke formation or unfavorable C-H bond activation. Herein, we design single-atom alloy (SAA) catalysts to simultaneously eliminate the above two bottlenecks based on mechanism-guided strategies: (1) the active single atom enables favorable C-H bond breaking and (2) the less reactive host metal facilitates C-C coupling and thus avoids strong binding of carbonaceous species. Employing electronic structure theory calculations, we screened the stability of multiple SAAs with 3d-5d transition metals atomically dispersed on a copper surface in terms of avoiding dopant aggregation and segregation. We then evaluated reactivities of the stable SAAs as catalysts for direct methane conversion to C2 products, including methane dehydrogenation and C-C coupling mechanisms. Combining selectivity analysis with kinetic modeling, we predicted that nickel dispersed on copper, i.e., Ni/Cu SAA, is a highly active and selective catalyst that can efficiently transform methane to ethylene. This work designs efficient SAA catalysts for direct methane activation and provides chemical insights into engineering compositions of SAAs to tune their catalytic performances.

Kothakonda, Manish↗

DOE OSTI2013

Systems and methods for laser assisted sample transfer to solution for chemical analysis

Systems and methods are described for laser ablation of an analyte from a specimen and capturing of the analyte in a dispensed solvent to form a testing solution. A solvent dispensing and extraction system can form a liquid microjunction with the specimen. The solvent dispensing and extraction system can include a surface sampling probe. The laser beam can be directed through the surface sampling probe. The surface sampling probe can also serve as an atomic force microscopy probe. The surface sampling probe can form a seal with the specimen. The testing solution including the analyte can then be analyzed using an analytical instrument or undergo further processing.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2014

Systems and methods for laser assisted sample transfer to solution for chemical analysis

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2015

Systems and methods for laser assisted sample transfer to solution for chemical analysis

47 OTHER INSTRUMENTATION↗

NASA NTRS2001

Performance Testing of a Lightweight, High Efficiency 95 K Cryocooler

Performance data are presented for a flight-like, lightweight, high efficiency pulse tube cryogenic cooler. The cooler has a mass of less than 4.0 kg, and an efficiency of 12 W/W, which is 18% of Carnot at 95 K, nearly double the efficiency of previous cooler designs, The mass of the cooler has been reduced by approximately a factor of three. The design point cooling power is 10 watts at 95 K at a heat rejection temperature of 300 K. The no-load temperature is 45 K. The compressor is built by Hymatic Engineering, UK, and is of a horizontally opposed piston design using flexure bearings. The vertical pulse tube is built by TRW with the heat exchanger or cold block located approximately mid-way along the tube. The final assembly and integration is also performed by TRW. The inertance tube and dead volume are contained within one of the compressor end caps. The cooler was developed by TRW under a joint NASA-DOD program, and has a goal of 10 yr operating lifetime. Potential NASA applications will focus on using coolers of this type in Zero boil off (ZBO) cryogen storage topologies for next generation launch vehicles. Zero boil off systems will feature significant reductions in tank size and Initial Mass to Low Earth Orbit (IMLEO), thereby significantly reducing the cost of access to space, and enabling future missions. The coolers can be used directly in liquid oxygen (LOx) or liquid methane ZBO systems, as shield coolers in liquid hydrogen tanks, or as first stage coolers in two-stage liquid hydrogen (LH2) ZBO cooler systems. Finally, the coolers could find applications in exploration missions where either propellants or breathable oxygen are extracted from the planetary atmosphere using a Sabatier or similar process. The gases could then be liquefied for storage either directly in return vehicle propellant tanks or on the planetary surface. Data presented were taken with the cooler operating in a vacuum of 10 (exp -5) torr, at controlled rejection temperatures from 300 K down to 275 K using a cold water heat exchanger bolted to the cooler. Heat loads were varied between 0.5 W and 15 W by supplying current to a 50 omega resistor mounted on a copper cold plate which was bolted to the cooler cold block. Silicon diodes mounted on both the cold plate and the heat exchanger provided accurate temperature measurement to within plus or minus 0.25 K and plus or minus 0.5 K respectively, up to 100 K with plus or minus 1% accuracy above 100 K. Input power to the compressor was limited to 180 W, corresponding to a maximum stroke of 80%.

Salerno, Lou↗

DOE OSTI2012

Evaluation of Flow-Injection Tandem Mass Spectrometry for Rapid and High-Throughput Quantitative Determination of B-Vitamins in Nutritional Supplements

The use of flow-injection electrospray ionization tandem mass spectrometry for rapid and high-throughput mass spectral analysis of selected B-vitamins, viz. B1, B2, B3, B5, and B6, in nutritional formulations was demonstrated. A simple and rapid (~5 min) in-tube sample preparation was performed by adding extraction solvent to a powdered sample aliquot followed by agitation, centrifugation, and filtration to recover an extract for analysis. Automated flow injection introduced 1 L of the extracts directly into the mass spectrometer ion source without chromatographic separation. Sample-to-sample analysis time was 60 s representing significant improvement over conventional liquid chromatography approaches which typically require 25-45 min, and often require more significant sample preparation procedures. Quantitative capabilities of the flow-injection analysis were tested using the method of standard additions and NIST standard reference material (SRM 3280) multivitamin/multielement tablets. The quantity determined for each B-vitamin in SRM 3280 was within the statistical range provided for the respective certified values. The same sample preparation and analysis approach was also applied to two different commercial vitamin supplement tablets and proved to be successful in the quantification of the selected B-vitamins as evidenced by an agreement with the labels values and the results obtained using isotope dilution liquid chromatography/mass spectrometry.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2017

Combined Falling Drop/Open Port Sampling Interface System for Automated Flow Injection Mass Spectrometry

The aim of this work was to demonstrate and to evaluate the analytical performance of a combined falling drop/open port sampling interface (OPSI) system as a simple noncontact, no-carryover, automated system for flow injection analysis with mass spectrometry. The falling sample drops were introduced into the OPSI using a widely available autosampler platform utilizing low cost disposable pipet tips and conventional disposable microtiter well plates. The volume of the drops that fell onto the OPSI was in the 7–15 μL range with an injected sample volume of several hundred nanoliters. Sample drop height, positioning of the internal capillary on the sampling end of the probe, and carrier solvent flow rate were optimized for maximum signal. Sample throughput, signal reproducibility, matrix effects, and quantitative analysis capability of the system were established using the drug molecule propranolol and its isotope labeled internal standard in water, unprocessed river water and two commercially available buffer matrices. A sample-to-sample throughput of ~45 s with a ~4.5 s base-to-base flow injection peak profile was obtained in these experiments. In addition, quantitation with minimally processed rat plasma samples was demonstrated with three different statin drugs (atorvastatin, rosuvastatin, and fluvastatin). Direct characterization capability of unprocessed samples was demonstrated by the analysis of neat vegetable oils. Employing the autosampler system for spatially resolved liquid extraction surface sampling exemplified by the analysis of propranolol and its hydroxypropranolol glucuronide phase II metabolites from a rat thin tissue section was also illustrated.

47 OTHER INSTRUMENTATION↗

DOE OSTI2020

In Situ Chemical Monitoring and Imaging of Contents within Microfluidic Devices Having a Porous Membrane Wall Using Liquid Microjunction Surface Sampling Probe Mass Spectrometry

The ability to observe dynamic chemical processes (e.g., signaling, transport, etc.) in vivo or in situ using nondestructive chemical imaging opens a new door to understanding the complex dynamics of developing biological systems. With the advent of “biology-on-a-chip” devices has come the ability to monitor dynamic chemical processes in a controlled environment, using these engineered habitats to capture key features of natural systems while allowing visual observation of system development. Having the capability to spatially and temporally map the chemical signals within these devices may yield new insights into the forces that drive biosystem development. Here, a porous membrane sealed microfluidic device was designed to allow normal microfluidic operation while enabling continuous, location specific sampling and chemical characterization by liquid microjunction surface sampling probe mass spectrometry (LMJ-SSP MS). LMJ-SSP was used to extract fluids with nL-to-μL/min flow rates directly from selected areas of the microfluidic device without negatively impacting the device function. These extracts were subsequently characterized using MS. This technique was used to acquire MS images of the entirety of several multi-input microfluidic devices having different degrees of fluid mixing. LMJ-SSP MS imaging visualized the spatial distribution of chemical components within the microfluidic channels and could visualize chemical reactions occurring in the device. These microfluidic devices with a porous membrane wall are wholly compatible with the construction of biology-on-a-chip devices. This ultimately would enable correlation of biosystem physical structure with an evolving chemical environment

47 OTHER INSTRUMENTATION↗

DOE OSTI2012

SCALED ELECTRON MODEL OF A DOGBONE MUON RLA WITH MULTI-PASS ARCS

The design of a dogbone RLA with linear-field multi-pass arcs was earlier developed for accelerating muons in a Neutrino Factory and a Muon Collider. It allows for efficient use of expensive RF while the multi-pass arc design based on linear combined-function magnets exhibits a number of advantages over separate-arc or pulsed-arc designs. Such an RLA may have applications going beyond muon acceleration. This paper describes a possible straightforward test of this concept by scaling a GeV scale muon design for electrons. Scaling muon momenta by the muon-to-electron mass ratio leads to a scheme, in which a 4.5 MeV electron beam is injected at the middle of a 3 MeV/pass linac with two double-pass return arcs and is accelerated to 18 MeV in 4.5 passes. All spatial dimensions including the orbit distortion are scaled by a factor of 7.5, which arises from scaling the 200 MHz muon RF to a readily available at CEBAF 1.5 GHz. The footprint of a complete RLA fits in an area of 25 by 7 m. The scheme utilizes only fixed magnetic fields including injection and extraction. The hardware requirements are not very demanding, making it straightforward to implement. In this report, we have shown first of all that measuring the energy spectrum of the fast neutrons in the liquid scintillators allows one to distinguish the two chemical forms of plutonium. In addition, combining this information with the Feynman 2-neutron and 3-neutron correlations allows one to extract the {alpha}-ratio without explicitly knowing the multiplication. Given the {alpha}-ratio one can then extract the multiplication as well as the {sup 239}Pu and {sup 240}Pu masses directly from the moment equations.

43 PARTICLE ACCELERATORS↗