Radiochemical neutron activation analysis of indium, cadmium, yttrium and the 14 rare earth elements in rocks
Radiochemical neutron activation analysis of In, Cd, Y and rare earth elements in rocks
Rey, P.↗
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Rare earth elements in river waters
To characterize the input to the oceans of rare earth elements (REE) in the dissolved and the suspended loads of rivers, the REE concentrations were measured in samples of Amazon, Indus, Mississippi, Murray-Darling, and Ohio rivers and in samples of smaller rivers that had more distinct drainage basin lithology and water chemistry. It was found that, in the suspended loads of small rivers, the REE pattern was dependent on drainage basin geology, whereas the suspended loads in major rivers had relatively uniform REE patterns and were heavy-REE depleted relative to the North American Shale composite (NASC). The dissolved loads in the five major rivers had marked relative heavy-REE enrichments, relative to the NASC and the suspended material, with the (La/Yb)N ratio of about 0.4 (as compared with the ratio of about 1.9 in suspended loads).
Goldstein, Steven J.↗
Rare Earth Element Measurements of Melilite and Fassaite in Allende Cai by Nanosims
The rare earth elements (REEs) are concentrated in CAIs by approx. 20 times the chondritic average [e.g., 1]. The REEs in CAIs are important to understand processes of CAI formation including the role of volatilization, condensation, and fractional crystallization [1,2]. REE measurements are a well established application of ion microprobes [e.g., 3]. However the spatial resolution of REE measurements by ion microprobe (approx.20 m) is not adequate to resolve heterogeneous distributions of REEs among/within minerals. We have developed methods for measuring REE with the NanoSIMS 50L at smaller spatial scales. Here we present our initial measurements of REEs in melilite and fassaite in an Allende Type-A CAI with the JSC NanoSIMS 50L. We found that the key parameters for accurate REE abundance measurements differ between the NanoSIMS and conventional SIMS, in particular the oxide-to-element ratios, the relative sensitivity factors, the energy distributions, and requisite energy offset. Our REE abundance measurements of the 100 ppm REE diopside glass standards yielded good reproducibility and accuracy, 0.5-2.5 % and 5-25 %, respectively. We determined abundances and spatial distributions of REEs in core and rim within single crystals of fassaite, and adjacent melilite with 5-10 m spatial resolution. The REE abundances in fassaite core and rim are 20-100 times CI abundance but show a large negative Eu anomaly, exhibiting a well-defined Group III pattern. This is consistent with previous work [4]. On the other hand, adjacent melilite shows modified Group II pattern with no strong depletions of Eu and Yb, and no Tm positive anomaly. REE abundances (2-10 x CI) were lower than that of fassaite. These patterns suggest that fassaite crystallized first followed by a crystallization of melilite from the residual melt. In future work, we will carry out a correlated study of O and Mg isotopes and REEs of the CAI in order to better understand the nature and timescales of its formation process and subsequent metamorphic history.
Ito, M.↗
Rare Earth Element Partitioning in Lunar Minerals: An Experimental Study
The partitioning behavior of rare earth elements (REE) between minerals and melts is widely used to interpret the petrogenesis and geologic context of terrestrial and extra-terrestrial samples. REE are important tools for modelling the evolution of the lunar interior. The ubiquitous negative Eu anomaly in lunar basalts is one of the main lines of evidence to support the lunar magma ocean (LMO) hypothesis, by which the plagioclase-rich lunar highlands were formed as a flotation crust during differentiation of a global-scale magma ocean. The separation of plagioclase from the mafic cumulates is thought to be the source of the Eu depletion, as Eu is very compatible in plagioclase. Lunar basalts and volcanic glasses are commonly depleted in light REEs (LREE), and more enriched in heavy REEs (HREE). However, there is very little experimental data available on REE partitioning between lunar minerals and melts. In order to interpret the source of these distinctive REE patterns, and to model lunar petrogenetic processes, REE partition coefficients (D) between lunar minerals and melts are needed at conditions relevant to lunar processes. New data on D(sub REE) for plagioclase, and pyroxenes are now available, but there is limited available data for olivine/melt D(sub REE), particularly at pressures higher than 1 bar, and in Fe-rich and reduced compositions - all conditions relevant to the lunar mantle. Based on terrestrial data, REE are highly incompatible in olivine (i.e. D much less than 1), however olivine is the predominant mineral in the lunar interior, so it is important to understand whether it is capable of storing even small amounts of REE, and how the REEs might be fractionatied, in order to understand the trace element budget of the lunar interior. This abstract presents results from high-pressure and temperature experiments investigating REE partitioning between olivine and melt in a composition relevant to lunar magmatism.
McIntosh, E. C.↗
Rare Earth Elements from Coal and By-Products: Separation Technologies
Presented at the Rare Earth Element and Critical Materials Project Review Meeting
Lopano, Christina↗
Luminescence based fiber optic probe for the detection of rare earth elements
The disclosure relates to an apparatus, method and process for detecting rare earth elements. The system includes an LED powered by a first power source and a focusing lens in optical communication with the LED. A shortpass filter is in optical communication with the focusing lens; and a fiber bifurcated cable in optical communication with the shortpass filter. The system includes a probe tip in optical communication with the fiber bifurcated cable and a sample; a first aspheric lens in optical communication with the fiber bifurcated cable. A longpass filter is in optical communication with the first aspheric lens and a second aspheric lens in optical communication with the longpass filter. The system includes a spectrometer connected to a power source, where the spectrometer is in optical communication with the second aspheric lens.
Ahern, John C.↗
High Yield, Economical and Environmentally Benign Production of Rare Earth Elements from Coal Ash (Phase II Final Summary Report)
Fly ash stored in landfills and ponds across the United States is an attractive, abundant domestic resource for the cost-effective recovery of rare earth elements (REE) and other critical minerals (CM). Physical Sciences Inc. (PSI) and its team members, Winner Water Services (WWS) and University of Kentucky/Center for Applied Energy Research (UK/CAER) successfully executed a multiphase program that developed technologies and their implementation in a pilot plant. We demonstrated plant operations for cost-effective and environmentally-friendly production of rare earth element oxide (REO) concentrates, and the critical minerals scandium and aluminum (in the forms of salts or oxide products), from coal ash. We also constructed and demonstrated a research-scale (0.5 kg/day) micropilot facility to validate the key physical and chemical processing operations, predict yields, and troubleshoot process bottlenecks. The project team then designed, constructed and operated two decoupled pilot plants: (1) an operational pilot plant for physical separation processes with capacity of 0.4 metric tons per day (tpd), where we optimized processes to produce selected ash fractions as the feedstock for chemical processing and as valuable byproducts such as cenospheres, magnetic ash, and secondary fuel carbon, and (2) an operational pilot plant for chemical ash processing with a capacity of 0.5 tpd that developed optimized processes for the production of: (a) REO concentrates, (b) critical minerals (Sc, Al), and (c) beneficiated ash as a valuable byproduct suitable for cement applications. In Phase I, the project team (with Equinox Chemicals in place of WWS) developed and demonstrated the feasibility of the physical and chemical separation processes, developed the design of a pilot plant, and began the development of a preliminary techno-economic model. In the baseline (initial) Phase II program, the project team developed and demonstrated the above pilot scale plant, producing salable REE concentrates, including Y and Sc (REYSc), plus commercially viable byproducts, using environmentally safe and high-yield physical and chemical enrichment processes. The team successfully demonstrated chemical pilot design, construction, shakedown, and operations of the plant. We produced the Phase II deliverable REYSc concentrate ((50 g of >60 wt.% purity REYSc salts on elemental basis), generated the feed for the Phase II follow-on program, identified processing challenges for future optimizations, and refined the techno-economic model. In the Phase II follow-on program, the project team: (1) developed and demonstrated processes to increase the REE amount by 3X (content basis) and convert the Phase II REE salt mixture to an oxide mixture, (2) produced/delivered >38 g of REO mixture with >85 wt.% purity (elemental basis); (3) developed processes to recover critical minerals scandium and aluminum from intermediate streams; (4) produced/delivered > 1 g of scandium salt mixture with >85 wt. % purity (elemental basis); (5) produced/delivered > 100 g of aluminum oxide type material with >70% wt. purity (elemental basis); and (6) updated the techno-economic model from the baseline Phase II program to assess CAPEX and OPEX of a commercial operation. This program has developed extensive databases on process chemistry, unit operations, plant engineering, and techno-economics that will enable further scale-up toward commercial plant design. Specific future developments will be focused on achieving dramatic savings in energy, reagent usage, and operating costs. The combined results will contribute significantly for maturing the technologies of REE recovery from coal byproducts and promote the establishment of domestic REE and CM supply chains.
01 COAL, LIGNITE, AND PEAT↗
Signatures of rare earth element distributions in fly ash derived from the combustion of Central Appalachian, Illinois, and Powder River basin coals
We report the distribution of Rare Earth elements (REE) in coal-derived fly ashes can have distinctive patterns when fly ashes are produced from different coals within or between basins, such as the Pennsylvanian Class F fly ashes from the Illinois and Central Appalachian basins. Both the Fire Clay coal and a blend of a number of eastern Kentucky coals show strong Gd peaks and an H-type distribution in the Upper Continental Crust-corrected plots. The Fire Clay coal-derived ash has a higher heavy REE concentration than the blended coal-derived ash. The Illinois Basin-derived fly as has an overall lower REE concentration than the latter ashes. Class C fly ash derived from Powder River Basin coals has, with the exception of an Eu peak, a flatter distribution of REE and an overall L-type or indistinct H- versus L-type distribution. The signatures of the REE in fly ashes may be useful in predicting their behavior in the extraction of the REE; simple extrapolations from the basic concentrations and the predicted extraction percentages for ashes from different basins are not necessarily indicative of the actual distribution of the extracted REE.
01 COAL, LIGNITE, AND PEAT↗
PILOT PLANT EVALUATIONS OF RARE EARTH ELEMENT RECOVERY AND CONCENTRATION FROM PRE-COMBUSTION BITUMINOUS COAL SOURCES
Rare earths and other critical elements are commonly associated with coal-based sources and sometimes at concentrations that may be attractive for recovery as a byproduct of coal production. The results obtained from laboratory research performed during the past five years have led to the design, construction and testing of a pilot plant that recovered rare earth elements from several bituminous coal-based materials including coarse refuse as well as solutions from a small heap leach and acid mine drainage. From this initial design, rare earth oxide (REO) concentrates having a purity greater than 90% have been produced using solvent extraction as the primary means of concentration. Following cost reduction and process intensification efforts, the circuit was revised to include feed calcination and several selective precipitation stages as a substitute for the original direct leach-solvent extraction circuit. Pilot test results revealed that the modified circuit was ideal for treating the relatively low-grade feedstocks and provided similar final REO purities at a significantly lower cost. This communication will present the flowsheets evaluated in the pilot plant along with technical and economic analyses for each circuit.
Coal↗
Coupled Hydrothermal Extraction and Ligand-Associated Swellable Glass Media Recovery of Rare Earth Elements from Coal Fly Ash (Final Report)
Wayne State University (WSU) researchers, in collaboration with the University of California-Los Angeles (UCLA) and Los Alamos National Laboratory (LANL), have successfully developed a new sorbent media used in a process that concentrated the rare earth content in a coal fly ash sample from southeast MI by >350×, resulting in >13 wt% REO powder. The project developed a new DTPA-associated media that was used to concentrate total REEs. This project demonstrated a coupled hydrothermal extraction and solid-liquid recovery process that produced REO powder from raw fly ash while nearly eliminating the use of organic solvents. The project successfully: 1) identified a commercially viable ash supply with >$2.5 M in REO value being deposited monthly, 2) hydrothermally extracted >77% of REEs in coal fly ash (20% more than acid alone), 3) developed a new sorbent media that was used to concentrate REEs, 4) and engineered a process that resulted in a >13 wt% REO powder. The media also demonstrates a selectivity for mid and heavy REEs over Ce and La and the potential for use in separating individual rare earth elements. An invention disclosure for the sorbent media has been filed with WSU and a patent application will be submitted in the near future. The project examined the potential to couple hydrothermal leaching of coal fly ash with the engineering of a custom ligand-associated media to provide an organic solvent-free method of extracting and recovering REEs. Fly ash feedstock was collected from Detroit area coal-fired power plants, characterized for REE content, and subjected to a bench-top batch hydrothermal leaching/dissolution process inside custom-build pressure reactors at Los Alamos National Laboratory (LANL). This process applied a dissolution technique previously developed to process spent nuclear fuel and other nuclear materials. The modified ash was acidified and the resulting leachate was enriched with REEs along with Ca, Al, and Si. Ligands known to be effective in lanthanide/actinide separation were evaluated based on a series of criteria such as selectivity and association to organosilica through hydrophobicity. Batch experiments were conducted to establish the best conditions (e.g., pH, eluent, etc.) and best ligand systems for the effective extraction of REEs from the alkaline feed solution obtained from the hydrothermal leaching process. Once the organosilica-ligand extraction media was developed for REE concentration, an acidic solution was used to back extract and concentrate the REEs into a heavily REE-laden strip solution. The REEs in the strip solution were precipitated with oxalate to produce rare earth oxides.
01 COAL, LIGNITE, AND PEAT↗
Electrokinetic Rare Earth Element Purification
I, Kyle McCarthy, am traveling to Boston, MA for the Materials Research Society conference. At the conference, I will give an oral presentation on research findings from Energy and Homeland Security LDRD "A New, Green Approach to Rare Earth Element (REE) Purification Based on Electrokinetics." in talk titled "Electrokinetic Rare Earth Element Purification." I will also attend other live presentations and conduct professional networking. This fits within Sandia's energy security mission.
McCarthy, Kyle Patrick [Sandia National Laboratori↗
Electrokinetically Driven Rare Earth Element Separation by Coated Capillary Arrays
I, Kyle McCarthy, am traveling to Austin, TX for the TechConnect World Innovation conference. At the conference, I will give an poster presentation on research findings from Energy and Homeland Security LDRD "A New, Green Approach to Rare Earth Element (REE) Purification Based on Electrokinetics." titled "Electrokinetically Driven Rare Earth Element Separation..." I will also attend other live presentations and conduct professional networking. This fits within Sandia's energy security mission.
Merrill, Laura Christine [Sandia National Laborato↗
Design and Optimization of Processes for Recovering Rare Earth Elements from End-of-Life Hard Disk Drives
In this conference paper, we propose a superstructure-based approach to finding the optimal pathways for recovering rare earth elements in their commercialized rare earth oxide form from end-of-life HDDs. The proposed superstructure was modeled as a MILP optimization problem, selecting the net present value as the objective function. Whenever possible, costing data taken from the literature was used to inform this mode. However, due to the novelty of this research area data were often not available thus requiring the generation of flowsheets that were implemented in Aspen Plus. To establish the base case optimal result, projections for the number of EOL HDDs in the U.S. available for recycling and estimates of the projected rare earth oxide prices over the lifetime of the plant were used to inform the model. The model was then expanded to include the recycling of EOL HDDs generated prior to the beginning of plant production (period ranging from 2006 through 2024).
Laliwala, Chris↗
Separation of rare earth element radioisotopes by reverse-phase high-speed counter-current chromatography
Analytical scale purification of rare earth element (REE) radioisotopes is typically accomplished using cation-exchange resins (e.g. AG 50W-X8) and high-performance liquid chromatography (HPLC). Despite the variety of improvements made since the development of this separation process in the 1950s, nearest neighbor separations remain a challenge, as does the issue of irreversible sample adsorption. Herein, we report a study that evaluates the potential of high-speed counter-current chromatography (HSCCC) as an alternative method for purifying REE elements, with specific reference to separations of fission product REE of interest to nuclear forensics. Complementary HSCCC REE separation experiments, one spiked with radiotracer and REE fission product activity, allowed for in depth analysis of resulting fractions from both an elemental (inductively coupled plasma atomic emission spectroscopy, ICP-AES) and radiological (gamma-ray spectrometry, beta counting) purity perspective. The highly reproducible nature of separation profiles generated from HSCCC instruments was leveraged to simplify work-up of samples containing radioisotopes. Subsequent radioanalytical evaluation revealed minimal carryover of Eu into neighboring Sm and Tb fractions (as indicated by presence of 150Eu), and trace contamination of the Tb fraction with Y (as indicated by presence of 91Y). Subtle differences in stationary phase retention across the two columns were reflected in significant variations in decontamination factors of duplicate parallel separations. Furthermore, these differences paired with obtained distribution of radioisotopes provided valuable insights into future improvements. Collectively, this study represents a significant step forward in development of HSCCC technology for task specific REE radioisotope purification.
07 ISOTOPE AND RADIATION SOURCES↗
Concentration and Recovery of Rare Earth Elements from Eastern US Coal Refuse
Recent studies funded by the US Department of energy have shown that coal and coal byproducts contain elevated contents of Rare Earth Elements (REEs), making them a potential resource for these critical materials. The approach employed in this research focused on the concentration and extraction of REEs from fine coal refuse derived from various preparation plants in the Appalachian coal basin of the United States. Initial efforts in this research focused on the identification and characterization of REEs in various fine coal refuse streams from nine distinct industrial preparation plants in Appalachia. The average REE content in these materials was determined to be approximately 200 ppm, but the REE content showed a strong correlation to the aluminum content, suggesting that the REEs are closely associated with the clay minerals present in the refuse. Given the relatively low REE concentrations, initial efforts sought to concentrate the REEs through decarbonization and dispersive liberation steps. In these tests, high-shear agitation in the presence of a polyelectrolyte, followed by sedimentation was able to isolate the REE-enriched fine clay particles from siliceous gangue minerals. Following the dispersive liberation step, all samples were found to have an REE content greater than 300 ppm, a benchmark used for many initial exploratory studies. In one case, the REE content was increased by more than 125%. Subsequent extraction tests initially utilized a direct ion-exchange leaching approach with ammonium sulfate as lixiviant. In all cases, the simple ion-exchange leaching process failed to recover significant quantities of rare earth elements, ultimately suggesting that the REEs in fine coal waste may be passivated or bound in a colloidal phase. To access this colloidal phase, several alternative approaches were evaluated, including leaching with alternative ion-exchange lixiviants, reductive leaching, gas-purged leaching, and others. The approach that showed the most promise was strong alkaline pretreatment, followed by ion-exchange leaching with ammonium sulfate at pH 4. A combination of strong alkali and high-temperatures treatment successfully liberated the REEs, converting them to a form amenable to ion-exchange leaching. The highest REE recovery achieved with this method was determined to be 39%. Lastly, bench-scale solvent extraction tests were used to further concentrate REEs in the leach solution and demonstrate that mixed rare earth concentrates can be successfully produced from fine coal refuse.
01 COAL, LIGNITE, AND PEAT↗
Recycling Rare Earth Elements from End-of-Life Electric and Hybrid Electric Vehicle Motors
In this paper, we propose a superstructure-based approach to finding the optimal pathways for recovering rare earth elements in their commercialized rare earth oxide form from end-of-life EV and HEV motors. The proposed superstructure was modeled as a MILP optimization problem, selecting the net present value as the objective function. Whenever possible, costing data taken from the literature was used to inform this mode. However, due to the novelty of this research area data were often not available thus requiring the generation of flowsheets that were implemented in Aspen Plus.
Laliwala, Chris↗
Phosphonate functionalized magnetic mesoporous silica for rare earth element recovery from citrate assisted solid waste extracts
The growing high demand of rare earth elements (REEs) has prompted extensive research on REE recovery from waste streams. This study reports the synthesis and evaluation of phosphonate-functionalized magnetic mesoporous silica (MMS-PP) for REE recovery from the acidic extracts of solid wastes. MMS-PP was synthesized using surfactant template and post-synthesis methods, and tested using simulated and real extraction solutions from citrate-assisted REE extracts from municipal solid waste incineration (MSWI) ash. The organic-inorganic hybrid MMS-PP was evaluated for La recovery from 50 mM simulated citrate extract, with the adsorption capacity of 13.5 mg/g compared to ∼2.5 mg/g for non-functionalized MMS. The MMS-PP material exhibited fast adsorption within 10 min, good La selectivity against competing Na + and Ca 2+ , moderate selectivity against Al 3+ and Fe 3+ , high recyclability over multiple adsorption-desorption cycles, and equivalent efficiency for La, Ce, Nd, and Y recovery. Furthermore, the MMS-PP material also demonstrated 70–95% REE recovery from real citrate extracts of MSWI ash, and the spent MMS-PP material can be regenerated and reused for multiple cycles. Functionalized mesoporous materials in combination with organic-ligand assisted extraction can potentially provide a green, effective, and tunable solid-liquid separation platform for REE recovery from complex solid waste streams.
REE recovery↗
Rare Earth Elements (REEs) Measurement in Coal and Rock Mineral Matrices
Although critical minerals including rare earth elements (REEs) can be analyzed in laboratory by some established and reliable laboratory based analytical techniques, their in-situ measurements in the field have always been challenging. For identification of REE-rich sites and REEs distribution measurement, portable field applicable technologies are paramount. As Laser-induced breakdown spectroscopy (LIBS) has enormous potential for field measurement, it has been explored for REEs measurements by many research groups. However, most of the studies are still dealing with simulated samples with traditional bench top experiments. In real world, REEs are available in various types of natural complex matrices in low content depending on the geographical locations. Considering this, LIBS has been evaluated for REE measurement in two different complex coal and rock mineral matrices representing some natural REE-rich sites. In addition, multiple samples collected from some natural sites in Wyoming, USA were experimented by using NETL’s bench top as well as miniaturized prototype setups for REE measurements.
Bhatt, Chet R.↗