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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 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
DOE OSTI2013

Ultra-trace determination of Strontium-90 in environmental soil samples from Qatar by collision/reaction cell-inductively coupled plasma mass spectrometry (CRC-ICP-MS/MS)

Because of the very low level of {sup 90}Sr in the environmental soil samples and its determination by beta counting may take several weeks, we developed a procedure for ultra-trace determination of {sup 90}Sr using collision reaction cell-inductively coupled plasma tandem mass spectrometry (CRC-ICP-MS/MS, Agilent 8800). Soil samples were dried at 105 deg. C and then heated in a furnace at 550 deg. C to remove any organics present. 500 g of each soil samples were aliquoted into 2000 ml glass beakers. Each Soils samples were soaked in 2 ppm Sr solution carrier to allow determination of chemical yield. The solid to liquid ratio was 1:1. Finally the soil samples were dried at 105 deg. C. Five hundred milliliters concentrated nitric acid and 250 ml hydrochloric acid volumes were added on 500 g soil samples. The samples were digested on hot plate at 80 deg. C to prevent spraying with continuous manual mixing. The leachate solution was separated. The solids were rinsed with 500 ml deionized water, warmed on a hot plate and the leachate plus previous leachate were filtered and the total volume was reduced to 500 ml by evaporation. Final leachate volume was transferred to a centrifuge tubes. The centrifuge tubes were centrifuged at 3,500 rpm for 10 min. The leachate was transferred to a 1 L beaker and heated on a hot plate to evaporate the leachate to dryness. The reside was re-dissolved in 100 ml of 2% HNO{sub 3} and reduced by evaporation to 10 mL. The solution was measured directly by CRC-ICP-MS/MS by setting the first quadruple analyzer to m/z 90 and introducing oxygen gas into the reaction cell for elimination isobar interference from zirconium-90. The method was validated by measurements of standard reference materials and applied on environmental soil samples. The overall time requirement for the measurement of strontium-90 by CRC-ICP-MS/MS is 2 days, significantly shorter than any radioanalytical protocol currently available. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2017

Synthesis and structure of ruthenium complexes [Ph{sub 3}PCH{sub 2}C{sub 6}H{sub 4}F-4]{sub 2}[RuCl{sub 6}] and [Ph{sub 3}PCH{sub 2}C{sub 6}H{sub 4}F-4][trans-RuCl{sub 4}(dmso-S){sub 2}]

The reaction of (4-fluorobenzyl)triphenylphosphonium chloride with ruthenium(III) chloride hydrate in the presence of hydrochloric acid in dimethyl sulfoxide affords the complex [Ph{sub 3}PCH{sub 2}C{sub 6}H{sub 4}F-4]{sub 2}[RuCl{sub 6}]. In the absence of hydrochloric acid, the reaction gives the complex [Ph{sub 3}PCH{sub 2}C{sub 6}H{sub 4}F-4][trans-RuCl{sub 4}(dmso-S){sub 2}]. The structures of the complexes were studied by {sup 1}H, {sup 19}F, and {sup 31}P NMR spectroscopy and X-ray diffraction.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Separation of gold from irradiated actinide material utilizing a 2- thenoyltrifluoroacetone extraction resin

Post-detonation nuclear forensics capabilities depend on the ability to rapidly isolate radionuclides to improve measurement quality. In this work an extraction chromatography resin was developed utilizing the extractants thenoyltrifluoroacetone and 1-octanol supported on Eichrom prefilter resin. Here the resin was tested in nitric and hydrochloric acid matrices. In nitric acid matrices the resin is able to extract zirconium, while in hydrochloric acid matrices it is possible to extract iron and gallium. In all acid conditions tested gold is retained but can be removed from the column with a 10% thiourea rinse.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2021

Morphology engineering of iridium electrodes via modifying titanium substrates with controllable pillar structures for highly efficient oxygen evolution reaction

Nowadays, Ti is the well-chosen anode substrate material for proton exchange membrane electrolyzer cells (PEMECs) and modifications of the substrate surfaces are essential for the fabrication of highly efficient electrodes. Herein, we introduce the morphology engineering of Ir/Ti electrodes with different acid treatments of hydrochloric acid (HCl) and oxalic acid (OA), and the comparative benefits of these two acid treatment methods are studied from the aspects of their impacts on the morphology, interfacial contact resistance (ICR), and oxygen evolution reaction (OER) performances of resultant electrodes. Notably, compared to the flat surface from OA treatment, Ti substrates with the pillar structure could be successfully achieved via HCl etching. Further, the HCl and the oxalic acid (OA) treatments would reduce the interfacial contact resistance (ICR) to 15.2% and 5.5% of the pristine Ti substrate at 1.38 MPa, respectively. By iridium electrodeposition on Ti substrates, Ir/Ti electrodes with different catalyst loadings are fabricated. With similar low-loadings of about 0.05 mgIr cm –2 , an Ir/Ti electrode with HCl treated substrate exhibits a lower overpotential of ~283 mV at 10 mA cm –2 current density than 305 mV from OA treatment, due to the boosted reaction areas from HCl treatment.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2013

1 kW/1 kWh advanced vanadium redox flow battery utilizing mixed acid electrolytes

This paper explores demonstration of an advanced vanadium redox flow battery (VRFB) using a mixed acid (sulfuric and hydrochloric acid) supporting electrolyte in a kW scale. The prototype VRFB is capable of delivering more than 1.1 kW in the whole operation range (15~85% state of charge) at 80 mA/cm2 with high energy efficiency of 82% and energy content of 1.4 kWh. The system has been operated stably without any precipitation even at elevated electrolyte temperatures of > 45°C, while the control tests with the conventional sulfuric acid electrolyte suffered from precipitation after 80 cycles. The mixed acid system enabled operation at elevated temperature (> 40°C), providing unique advantages over the conventional pure sulfate system; 1) high stack energy efficiency due to better kinetics and low electrolyte resistance, 2) low viscosity, resulting in reduced pumping loss, 3) elimination of additional heat exchanger, 4) high system efficiency and 5) simple system design and operation.

advanced vanadium redox flow battery↗
DOE OSTI2023

6 Li-loaded liquid scintillators produced by direct dissolution of compounds in diisopropylnaphthalene (DIPN)

Here, this paper describes preparation of 6 Li-loaded liquid scintillators by methods involving direct dissolution of 6Li salts in the commercial diisopropylnaphthalene (DIPN) solvent, without the formation of water-in-oil emulsions. Methods include incorporation of 6 Li that, unlike previously reported formulations, does not require additions of water or a strong acid such as hydrochloric acid (HCl). Results of the conducted experiments show that dissolution of aromatic and aliphatic 6 Li salts in DIPN can be easily achieved at 0.1%–0.3% by weight of atomic 6 Li, using small additions of waterless surfactants, or mild carboxylic acids. An alternative way suggests incorporation of 6 Li as a part of a surfactant molecule that can be dissolved in DIPN without any solubilizing additions. Proposed methods enable preparation of efficient 6 Li-loaded liquid scintillators that, at a large scale of 50 cm, exhibit good pulse shape discrimination (PSD) properties combined with up to 107% of light output and up to 115% of the attenuation length measured relative to standard undoped EJ-309 liquid scintillator.

36 MATERIALS SCIENCE↗
NASA NTRS1987

Magnetic particles

Metal oxide containing polymers and particularly styrene, acrylic or protein polymers containing fine, magnetic iron oxide particles are formed by combining a NO.sub.2 -substituted polymer with an acid such as hydrochloric acid in the presence of metal, particularly iron particles. The iron is oxidized to fine, black Fe.sub.3 O.sub.4 particles which deposit selectively on the polymer particles. Nitrated polymers are formed by reacting functionally substituted, nitrated organic compounds such as trinitrobenzene sulfonate or dinitrofluoro benzene with a functionally coreactive polymer such as an amine modified acrylic polymer or a protein. Other transition metals such as cobalt can also be incorporated into polymers using this method.

Chang, Manchium↗
NASA NTRS2012

Comparison of Four Strong Acids on the Precipitation Potential of Gypsum in Brines During Distillation of Pretreated, Augmented Urine

In this study, three different mineral acids were substituted for sulfuric acid (H2SO4) in the urine stabilizer solution to eliminate the excess of sulfate ions in pretreated urine and assess the impact on maximum water recovery to avoid precipitation of minerals during distillation. The study evaluated replacing 98% sulfuric acid with 85% phosphoric acid (H3PO4), 37% hydrochloric acid (HCl), or 70% nitric acid (HNO3). The effect of lowering the oxidizer concentration in the pretreatment formulation also was studied. This paper summarizes the test results, defines candidate formulations for further study, and specifies the injection masses required to stabilize urine and minimize the risk of mineral precipitation during distillation. In the first test with a brine ersatz acidified with different acids, the solubility of calcium in gypsum saturated solutions was measured. The solubility of gypsum was doubled in the brines acidified with the alternative acids compared to sulfuric acid. In a second series of tests, the alternative acid pretreatment concentrations were effective at preventing precipitation of gypsum and other minerals up to 85% water recovery from 95th-percentile pretreated, augmented urine. Based on test results, phosphoric acid is recommended as the safest alternative to sulfuric acid. It also is recommended that the injected mass concentration of chromium trioxide solution be reduced by 75% to minimize liquid resupply mass by about 50%, reduce toxicity of brines, and reduce the concentration of organic acids in distillate. The new stabilizer solution formulations and required doses to stabilize urine and prevent precipitation of minerals up to 85% water recovery are given. The formulations in this study were tested on a limited number of artificially augmented urine batches collected from employees at the Johnson Space Center (JSC). This study successfully demonstrated that the desired physical and chemical stability of pretreated urine and brines can be achieved using alternate pretreatment formulations under laboratory conditions. Additional testing and hazard assessments will be required to determine the feasibility of utilizing the proposed urine pretreatment formulations on ISS.

Muirhead, Dean↗
DOE OSTI2016

K West Basin Sand Filter Backwash Sample Analysis

A sand filter is used to help maintain water clarity at the K West Basin where highly radioactive sludge is stored. Eventually that sand filter will require disposal. The radionuclide content of the solids trapped in the sand filter will affect the selection of the sand filter disposal pathway. The Pacific Northwest National Laboratory (PNNL) was contracted by the K Basin Operations & Plateau Remediation Project (operations contractor CH2M Hill) to analyze the radionuclide content of the solids collected from the backwash of the K West Basin sand filter. The radionuclide composition in the sand filter backwash solids will be used by CH2M Hill to determine if the sand filter media and retained sludge solids will be designated as transuranic waste for disposal purposes or can be processed through less expensive means. On October 19, 2015, K Basin Operations & Plateau Remediation Project staff backwashed the sand filter into the North Load-Out Pit (NLOP) and immediately collected sample slurry from a sampling tube positioned 24 in. above the NLOP floor. The 764 g sand filter backwash slurry sample, KW-105 SFBW-001, was submitted to PNNL for analysis on October 20, 2015. Solids from the slurry sample were consolidated into two samples (i.e., a primary and a duplicate sample) by centrifuging and measured for mass (0.82 g combined – wet centrifuged solids basis) and volume (0.80 mL combined). The solids were a dark brown/orange color, consistent with iron oxide/hydroxide. The solids were dried; the combined dry solids mass was 0.1113 g, corresponding to 0.0146 weight percent (wt%) solids in the original submitted sample slurry. The solids were acid-digested using nitric and hydrochloric acids. Insoluble solids developed upon dilution with 0.5 M HNO 3 , corresponding to an average 6.5 wt% of the initial dry solids content. The acid digestate and insoluble solids were analyzed separately by gamma spectrometry. Nominally, 7.7% of the 60 Co was present in the insoluble solids; less than 1% of other gamma-emitters (i.e., 137 Cs, 154/155 Eu, and 241 Am) were present in the insoluble solids. Aliquots of the acid digestate were analyzed directly using gamma energy analysis (GEA) and after separations for 238 Pu, 239+240 Pu, 237 Np, and 241 Am radioisotopes using alpha energy analysis (AEA). The 90 Sr was measured by liquid scintillation counting (LSC) on the Sr-separated fraction. The plutonium isotopic distribution of the acid digestate was analyzed following Pu separations by thermal ionization mass spectrometry (TIMS). A table summarizes the results for the primary and duplicate samples. The 239+240 Pu concentration (µCi/g dry) relative to 90 Sr and to 137 Cs concentrations (µCi/g dry) was examined. The K West Basin sludge has a 239+240 Pu/ 90 Sr ranging from 0.1 to 1.2 and the 239+240 Pu/ 137 Cs ratio ranging from 0.10 to 0.47. In contrast, the sand filter backwash solids 239+240 Pu/ 90 Sr ratio was 10.6 and the 239+240 Pu/ 137 Cs ratio was 2.0. The ratio differences indicate a relative enhancement of the Pu concentration in the sand filter solids relative to the 137 Cs and 90 Sr sludge concentrations currently in the K West Basin. A dose-to-curie radioisotope evaluation of the sand filter waste form may need to consider this dissimilarity.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2014

Innovative Elution Processes for Recovering Uranium from Seawater

Utilizing amidoxime-based polymer sorbents for extraction of uranium from seawater has attracted considerable interest in recent years. Uranium collected in the sorbent is recovered typically by elution with an acid. One drawback of acid elution is deterioration of the sorbent which is a significant factor that limits the economic competitiveness of the amidoxime-based sorbent systems for sequestering uranium from seawater. Developing innovative elution processes to improve efficiency and to minimize loss of sorbent capacity become essential in order to make this technology economically feasible for large-scale industrial applications. This project has evaluated several elution processes including acid elution, carbonate elution, and supercritical fluid elution for recovering uranium from amidoxime-based polymer sorbents. The elution efficiency, durability and sorbent regeneration for repeated uranium adsorption- desorption cycles in simulated seawater have been studied. Spectroscopic techniques are used to evaluate chemical nature of the sorbent before and after elution. A sodium carbonate-hydrogen peroxide elution process for effective removal of uranium from amidoxime-based sorbent is developed. The cause of this sodium carbonate and hydrogen peroxide synergistic leaching of uranium from amidoxime-based sorbent is attributed to the formation of an extremely stable uranyl peroxo-carbonato complex. The efficiency of uranium elution by the carbonate-hydrogen peroxide method is comparable to that of the hydrochloric acid elution but damage to the sorbent material is much less for the former. The carbonate- hydrogen peroxide elution also does not need any elaborate step to regenerate the sorbent as those required for hydrochloric acid leaching. Several CO2-soluble ligands have been tested for extraction of uranium from the sorbent in supercritical fluid carbon dioxide. A mixture of hexafluoroacetylacetone and tri-n-butylphosphate shows the best result but uranium removal from the sorbent reaches only 80% after 10 hours of leaching. Some information regarding coordination of vanadium with amidoxime molecules and elution of vanadium from amidoxime- based sorbents is also given in the report.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2017

Lanthanide contraction effect on crystal structures of lanthanide coordination polymers with cyclohexanocucurbit[6]uril ligand

A series of compounds based on the macrocyclic ligand cyclohexanocucurbit[6]uril (Cy6Q[6]) with formulas (Ln(H{sub 2}O){sub 6}Cy6Q[6])·2(CdCl{sub 4})·H{sub 3}O·xH{sub 2}O [isomorphous with Ln=La (1), Ce (2), Pr (3) and Nd (4), x=11 (1), 11 (2), 10 (3) and 11 (4)], (Sm(H{sub 2}O){sub 5}Cy6Q[6])·2(CdCl{sub 4})·H{sub 3}O·10H{sub 2}O (5) and (Ln(H{sub 2}O){sub 5}(NO{sub 3})@Cy6Q[6])·2(CdCl{sub 4})·2H{sub 3}O·xH{sub 2}O [isomorphous with Ln=Gd (6), Tb (7) and Dy (8), x=8 (6), 6 (7) and 6 (8)], have been successfully synthesized by the self-assembly of Cy6Q[6] with the corresponding lanthanide nitrate under hydrochloric acid aqueous solution in the presence of CdCl{sub 2}. Single-crystal X-ray diffraction analyses revealed that compounds 1–8 all crystallize in monoclinic space group P2{sub 1}/c, and display 1D coordination polymer structures. The lanthanide contraction effect on the structures of 1–8 has also been investigated and discussed in detail. In contrast, the reaction of Cy6Q[6] with the Ho(NO){sub 3}, Tm(NO){sub 3}, Yb(NO){sub 3} under the same conditions resulted in the compounds 9–11 with formulas Cy6Q[6]·2(CdCl{sub 4})·2H{sub 3}O·xH{sub 2}O [isomorphous with x=10 (9), 10 (10), and 9 (11)], in which no lanthanide cations are observed. The structural difference of these compounds indicates that the Cy6Q[6] may be used in the separation of lanthanide cations. - Graphical abstract: The reaction of cyclohexanocucurbit[6]uril with lanthanide ions (La{sup 3+}, Ce{sup 3+}, Pr{sup 3+}, Nd{sup 3+}, Sm{sup 3+}, Gd{sup 3+}, Tb{sup 3+}, Dy{sup 3+}, Ho{sup 3+}, Tm{sup 3+} and Yb{sup 3+}) under hydrochloric acid in the presence of CdCl{sub 2} resulted in eleven compounds, which demonstrate interesting lanthanide contraction effect and provide a means of separating lanthanide ions. - Highlights: • Eleven compounds of the Ln{sup 3+} with the Cy6Q[6] were synthesized and described. • Compounds 1-8 demonstrate interesting lanthanide contraction effect. • In solid-state structures of compounds 9-11, no lanthanide ions were observed. • This study provides a means of separating lanthanides cations.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Short-length and high-density TiO{sub 2} nanorod arrays for the efficient charge separation interface in perovskite solar cells

The TiO{sub 2} nanorod arrays with the length of 70 nm, the diameter of 20 nm, and the areal density of 1000 µm{sup −2} were firstly prepared by the hydrothermal method using the aqueous grown solution of 38 mM titanium isopropoxide and 6 M hydrochloric acid at 170 °C for 60 min. Over-500 nm-thickness CH{sub 3}NH{sub 3}PbI{sub 3−x}Br{sub x} absorber layers were successfully obtained by sequential deposition routes using 1.7 M PbI{sub 2}·DMSO complex precursor solution and 0.465 M isopropanol solution of the methylammonium halide mixture with the molar ratio of CH{sub 3}NH{sub 3}I/CH{sub 3}NH{sub 3}Br=85/15. The perovskite solar cells based on the TiO{sub 2} nanorod array and 560 nm-thickness CH{sub 3}NH{sub 3}PbI{sub 3−x}Br{sub x} absorber layer exhibited the best photoelectric conversion efficiency (PCE) of 15.93%, while the corresponding planar perovskite solar cells without the TiO{sub 2} nanorod array and with 530 nm-thickness CH{sub 3}NH{sub 3}PbI{sub 3−x}Br{sub x} absorber layer gave the best PCE of 12.82% at the relative humidity of 50–54%. - Graphical abstract: The TiO{sub 2} nanorod arrays with the length of 70 nm, the diameter of 20 nm, and the areal density of 1000 µm{sup −2} were prepared by the hydrothermal method using the aqueous grown solution of 38 mM titanium isopropoxide and 6 M hydrochloric acid at 170 °C for 60 min. The optimal annealing temperature of TiO{sub 2} nanorod arrays was 450 °C. The perovskite solar cells based on the TiO{sub 2} nanorod array and 560 nm-thickness CH{sub 3}NH{sub 3}PbI{sub 3−x}Br{sub x} absorber layer exhibited the best photoelectric conversion efficiency (PCE) of 15.93% and the average PCE of 13.41±2.52%, while the corresponding planar perovskite solar cells without the TiO{sub 2} nanorod array and with 530 nm-thickness CH{sub 3}NH{sub 3}PbI{sub 3−x}Br{sub x} absorber layer gave the best PCE of 12.82% and the average PCE of 10.54±2.28% at the relative humidity of 50–54%. - Highlights: • Preparation of TiO{sub 2} nanorod array with length of 70 nm and density of 1000 µm{sup −2}. • Influence of annealing temperatures on the -OH content of TiO{sub 2} nanorod arrays. • Preparation of over-500 nm-thickness CH{sub 3}NH{sub 3}PbI{sub 3−x}Br{sub x} absorber layer. • Combination of short-length TiO{sub 2} nanorod array and high-thickness perovskite layer. • The best and average PCE with TiO{sub 2} array of 15.93% and 13.41±2.52% at 50–54% RH.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1989

Study of metal corrosion using ac impedance techniques in the STS launch environment

AC impedance measurements were performed to investigate the corrosion resistance of 19 alloys under conditions similar to the STS launch environment. The alloys were: Zirconium 702, Hastelloy C-22, Inconel 625, Hastelloy C-276, Hastelloy C-4, Inconel 600, 7Mo + N, Ferralium 255, Inco Alloy G-3, 20Cb-3, SS 904L, Inconel 825, SS 304LN, SS 316L, SS 317L, ES 2205, SS 304L, Hastelloy B-2, and Monel 400. AC impedance data were gathered for each alloy after one hour immersion time in each of the following three electrolyte solutions: 3.55 percent NaCl, 3.55 percent NaCl-0.1N HCl, and 3.55 percent NaCl-1.0N HCl. The data were analyzed qualitatively using the Nyquist plot and quantitatively using the Bode plot. Polarization resistance, Rp, values were obtained using the Bode plot. Zirconium 702 was the most corrosion resistant alloy in the three electrolytes. The ordering of the other alloys according the their resistance to corrosion varied as the concentration of hydrochloric acid in the electrolyte increased. The corrosion resistance of Zirconium 702 and Ferralium 255 increased as the concentration of hydrochloric acid in the electrolyte increased. The corrosion resistance of the other 17 alloys decreased as the concentration of the hyrdochloric acid in the electrolyte increased.

Calle, Luz M.↗
DOE OSTI2015

Elution of uranium and transition metals from amidoxime-based polymer adsorbents for sequestering uranium from seawater

High-surface-area amidoxime and carboxylic acid grafted polymer adsorbents developed at Oak Ridge National Laboratory were tested for sequestering uranium in a flowing seawater flume system at the PNNL-Marine Sciences Laboratory. FTIR spectra indicate that a KOH conditioning process is necessary to remove the proton from the carboxylic acid and make the sorbent effective for sequestering uranium from seawater. The alkaline conditioning process also converts the amidoxime groups to carboxylate groups in the adsorbent. Both Na 2 CO 3 H 2 O 2 and hydrochloric acid elution methods can remove ~95% of the uranium sequestered by the adsorbent after 42 days of exposure in real seawater. The Na 2 CO 3 H 2 O 2 elution method is more selective for uranium than conventional acid elution. Iron and vanadium are the two major transition metals competing with uranium for adsorption to the amidoxime-based adsorbents in real seawater. Tiron (4,5-Dihydroxy-1,3-benzenedisulfonic acid disodium salt, 1 M) can remove iron from the adsorbent very effectively at pH around 7. The coordination between vanadium (V) and amidoxime is also discussed based on our 51V NMR data.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Development and Testing of Diglycolamide Functionalized Mesoporous Silica for Sorption of Trivalent Actinides and Lanthanides

Sequestration of trivalent actinides and lanthanides present in used nuclear fuel and legacy wastes is necessary for appropriate long-term stewardship of these metals, particularly to prevent their release into the environment. Organically modified mesoporous silica is an efficient material for recovery and potential subsequent separation of actinides and lanthanides because of its high surface area, tunable ligand selection, and chemically robust substrate. Here, we have synthesized the first novel hybrid material composed of SBA-15 type mesoporous silica functionalized with diglycolamide ligands (DGA-SBA). Because of the high surface area substrate, the DGA-SBA was found to have the highest Eu capacity reported so far in the literature of all DGA solid-phase extractants. The sorption behavior of europium and americium on DGA-SBA in nitric and hydrochloric acid media was tested in batch contact experiments. DGA-SBA was found to have high sorption of Am and Eu in pH 1, 1 M, and 3 M nitric and hydrochloric acid concentrations, which makes it promising for sequestration of these metals from used nuclear fuel or legacy waste. The kinetics of Eu sorption were found to be two times slower than that for Am in 1 M HNO 3 . Additionally, the short-term susceptibility of DGA-SBA to degradation in the presence of acid was probed using 29 Si and 13 C solid-state NMR spectroscopy. Finally, the material was found to be relatively stable under these conditions, with the ligand remaining intact after 24 h of contact with 1 M HNO 3 , an important consideration in use of the DGA-SBA as an extractant from acidic media.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

Leaching of lanthanide and yttrium from a Central Appalachian coal and the ashes obtained at 550–950 °C

Here in this work, we investigated leaching of lanthanide and yttrium (REY) from a Central Appalachian coal and its ashes obtained at 550–950 °C with the main purpose of understanding the impact of ashing temperature on REY leachability in water, ammonium sulfate, and hydrochloric acid. It is found that the coal contains a negligible amount of water-soluble REY, less than 1% ion-exchangeable REY, and about 28% of HCl-soluble REY. Ashing leads to dramatic changes in REY leachability in both ammonium sulfate and hydrochloric acid solutions, which is believed to be related to transformation and redistribution of organically-associated REY in coal during the ashing process. Ashing temperature significantly affects REY leaching from coal ashes; higher ashing temperature results in lower REY leachability in both solutions. Clay minerals may play a significant role in changing the leachability of REY after ashing. In addition, the results also suggest that the organic matter in the coal is relatively enriched in heavy REY.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2018

Leaching Behavior of Rare Earth Elements in Fort Union Lignite Coals of North America

Rare earth elements are crucial materials in an incredible array of consumer goods, energy system components and military defense applications. However, the global production and entire value chain for rare earth elements is dominated by China, with the U.S. currently 100% import reliant for these critical materials. Traditional mineral ores including those previously mined in the U.S., however, have several challenges. Chief among these is that the content of the most critical and valuable of the rare earths are deficient, making mining uneconomical. Further, the supply of these most critical rare earths is nearly 100% produced in China from a single resource that is only projected to last another 10 to 20 years. The U.S. currently considers the rare earths market an issue of national security. It is imperative that alternative domestic sources of rare earths be identified and methods developed to produce them. Recently, coal and coal byproducts have been identified as one of these promising alternative resources. This paper details the results of a study on characterization of North Dakota lignite and lignite-related feedstocks as an assessment of their feasibility for rare earth element recovery. The abundance, distribution and modes of occurrence of the rare earth elements in the samples collected were determined in this initial study to inform the selection of appropriate extraction and concentration methods to recover the rare earth elements. Materials investigated include the lignite coals, clay-rich sediments associated with the coal seams, and materials associated with a lignite beneficiation system and power plant. The results show that high rare earth element levels exist both in lignite coals and associated sediments. The form of the rare earth elements in the clay materials is primarily as ultra-fine mineral grains. In the lignite coals, approximately 80-95% of the rare earths content is organically associated, primarily as coordination complexes.

Laudal, Daniel A.↗
DOE OSTI2015

Stability of the anodic growth porous tungsten oxide in different solutions

This article presents the study of the stability of the anodic growth porous tungsten oxide (WO{sub 3}) film in different solutions. As-anodized films are relatively stable in acidic electrolytes like sulphuric acid (H{sub 2}SO{sub 4}), hydrochloric acid (HCl) but not in oxalic acid. In higher pH solution, rate of dissolution of the WO{sub 3} film is higher. Annealing at 400 °C for 2 h transform the as-grown sample from amorphous phase to the crystalline phase and this significantly improve the stability of the film in high pH solution. Photocurrent measurements reveal that there is no significant difference of the electrolyte used (0.5 M H{sub 2}SO{sub 4}, 0.33 M H{sub 3}PO{sub 4}, 0.1 M sodium sulfate (Na{sub 2}SO{sub 4})) on the photocurrent. As-annealed films exhibit good stablility for the long photoelectrochemical (PEC) measurements (1700 s) in 0.5 M H{sub 2}SO{sub 4} and 0.1 M Na{sub 2}SO{sub 4}. There is no effect on the photocurrent for the variation of the concentration of the acidic solution (H{sub 2}SO{sub 4}). However, lower photocurrent was obtained as the concentration of Na{sub 2}SO{sub 4} was increased.

36 MATERIALS SCIENCE↗