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At least 145 records · Page 8

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DOE OSTI2022

Iron-modified biochar-based bilayer permeable reactive barrier for Cr(VI) removal

In this study, iron (Fe)-modified biochar (FeBC) has been developed to remove hexavalent chromium (Cr(VI)) from groundwater and is suitable for use in permeable reactive barriers (PRBs). However, Cr(VI) removal behavior and chemical processes in FeBC-based PRBs are not fully understood, and the potential for Fe release has not been addressed. In this study, three FeBC-based PRBs were assessed in column experiments for 563 days with respect to their ability to remove Cr(VI). Bilayer column filled with FeBC+limestone and BC+limestone in two separate layers (FeBC_Ca_BC) showed the best performance in terms of Cr(VI) removal with a low treatment cost. The corrosion of FeBC was mainly related to pH and Cr(VI) concentration rather than flow rate. Leached Fe was attenuated by BC and limestone and reutilized in FeBC_Ca_BC. Cr(VI) was reduced to Cr(III) and then adsorbed or precipitated on the biochars. Cr and Fe formed inner-sphere complexes and then transformed from double corner sharing to edge sharing. During the reaction, Cr penetrated from the surface to the interior of the biochars and became a more stable species. This study provides evidence of the effectiveness of a new combination of biochars for Cr(VI) removal and insights into the reaction mechanisms.

42 ENGINEERING↗

DOE OSTI2021

Selective recovery of rare earth elements with ligand-functionalized polymers in fixed-bed adsorption columns

Rare earth elements (REE) are a group of valuable metals with growing demand and broad applications. Mineral ores, the traditional sources of REE, require significant capital investment and their refinement has been a source of environmental contamination. Industrial fluids and natural REE-bearing liquids are potential alternative sources for these metals. This work investigated the performance and REE selectivity of polymer resin beads functionalized with N,N-bis(phosponomethyl)glycine (BPG) for extraction of REE from saline solutions in fixed-bed adsorption columns. Competitive batch adsorption experiments were conducted with various metals (Nd, Gd, Ho, Al, Fe, Co, Ni, Ba, Pb, Th, and U) and the BPG-functionalized resins were up to 137 times more selective for REE than aminated resins. In column experiments, the BPG-functionalized resins preferentially adsorbed heavier metals and REE were strongly retained in the functionalized column, taking 270 times longer than the amine column to reach 10% breakthrough and 128 times longer to reach 50% breakthrough. REE bound to the BPG-functionalized resins were recovered with a dilute HNO3 solution, yielding REE concentrations up to 236 times higher than the influent feedstock. This work provides new insight into the operational performance of novel functionalized adsorbents for recovery of REE from saline fluids.

42 ENGINEERING↗

DOE OSTI2022

Raw tensiometer soil matric potential data, from Oct 2017-Jun 2020 in Manaus, Brazil

This data package contains raw output from two Campbell Scientific CR1000 data loggers each connected to three UMS T4e tensiometer sensors in Manaus, Brazil. Tensiometers at each data logger location were installed to depths of 10 cm, 20 cm and 50 cm below the ground surface for the purpose of measuring soil matric potential at each depth. “Station 3” tensiometers were installed at approximately 2°36'31.68"S, 60°12'34.70"W. “Station 4” tensiometers were installed at approximately 2°36'32.46"S, 60°12'34.92"W. The files “tensio3.edit.202109.csv” and “tensio4.edit.202109.csv” contain raw data (with invalid data removed). A text editor will be required to view the raw files in .csv (comma-separated values) format. Data processing was limited to: 1) Editing column headers for clarity; 2) Applying a correction that converts voltage read by the data loggers to pressure units (kPa); 3) removing all data greater than 50 kPa and less than -115 kPa; 4) Adding columns entitled “Caution.10cm”, “Caution.20cm” and “Caution.50cm” that contains values of either “NA” or “Caution”, the latter of which is applied when data exceeds the manufacturer reported data validity range of less than -85 kPa to suggest use of these data with caution; 5) Adding columns entitled “Invalid.10cm”, “Invalid.20cm”, and “Invalid.50cm” that contains values of either “NA” or “Invalid”, the latter of which is applied when data accuracy is deemed compromised due to the introduction of air bubbles into the instrument. Data marked “Invalid” may still indicate general trends of wet/high matric potential and dry/low matric potential, but values are inaccurate and dry/low matric potential values are likely not low enough. Wet/high matric potential values are likely to be more accurate than dry/low matric potential values; 6) Data format changed from .dat to .csv. This research was performed as a part of the NGEE Tropics project, which aims to advance model predictions of tropical forest carbon cycle responses to a changing climate over the 21st Century.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2022

System and process for purification of astatine-211 from target materials

A new column-based purification system and approach are described for rapid separation and purification of the alpha-emitting therapeutic radioisotope 211At from dissolved cyclotron targets that provide highly reproducible product results with excellent 211At species distributions and high antibody labeling yields compared with prior art manual extraction results of the prior art that can be expected to enable enhanced production of purified 211At isotope products suitable for therapeutic medical applications such as treatment of cancer in human patients.

O'Hara, Matthew J.↗

DOE OSTI2023

System and process for purification of Astatine-211 from target materials

A new column-based purification system and approach are described for rapid separation and purification of the alpha-emitting therapeutic radioisotope 211 At from dissolved cyclotron targets that provide highly reproducible product results with excellent 211 At species distributions and high antibody labeling yields compared with prior art manual extraction results of the prior art that can be expected to enable enhanced production of purified 211 At isotope products suitable for therapeutic medical applications such as treatment of cancer in human patients.

O'Hara, Matthew J.↗

DOE OSTI2026

INL Intern Poster Session

Characterization of off-gas constituents from nuclear fuel reprocessing can be measured using a residual gas analyzer. Characterization of this off-gas is important in a closed fuel cycle, where gasses such as Nox, Kr, I, and C-14 need to be removed from reprocessing plants to meet regulatory requirements. Both Kr and Xe have low chemical reactivity, making capture and separation difficult. Solid sorbents can be used to capture these gases as an alternative to cryogenic distillation, which is energy intensive and hazardous. AgZ-PAN and HZ-PAN are two solid sorbents that have demonstrated selective capture of Xe and Kr. A residual gas analyzer can be used to obtain breakthrough curves that demonstrate how well this adsorption and separation occur. The breakthrough curve is dependent on packing density, column size, and flow rate. Data obtained from the RGA was verified with a gas chromatographer.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

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↗

DOE OSTI2023

Influence of ion-pairing reagents on the separation of intact glycoproteins using hydrophilic-interaction liquid chromatography - high-resolution mass spectrometry

Hydrophilic-interaction liquid chromatography (HILIC) of intact proteins offers high-resolution separations of glycoforms of glycoproteins differing in the number of (neutral) glycans. However, to obtain efficient separations it is essential that the positively charged sites of the proteins are shielded by acidic (negative) ion-pair reagents (IPRs), so as to enhance the contribution of the hydroxyl groups of the (neutral) sugars in the glycoprotein. Here, we studied the influence of various IPRs that differ in physico-chemical properties, such as hydrophobicity and acidity, on the capillary-scale HILIC separation of intact (glyco)proteins. We evaluated the use of fluoroacetic acid (MFA), difluoroacetic acid (DFA), trifluoroacetic acid (TFA), and heptafluorobutyric acid (HFBA) as diluents for sample preparation, as solvents for sample loading on a reversed-phase trap prior to the HILIC separation, and as mobile-phase components for HILIC and HILIC-MS. To reduce the contribution of ion-exchange interaction with the (silica-based) stationary phase, we used an acrylamide-based monolithic column. We studied the influence of the different IPRs on each step of the separation of a mixture of proteins of different size and hydrophilicity and on the separation of the five glycoforms of ribonuclease B. The content of IPR in the sample was shown not to affect the separation and the MS detection. However, a low content of TFA and DFA in the mobile phase is favourable, as it reduces adduct formation and leads to higher signal intensity. The optimized HILIC conditions successfully resolved nine major glycoforms groups of a ~40 kDa glycoprotein horseradish peroxidase (HRP), as an example of a complex glycoprotein.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2025

Implementation and evaluation of multi-dual mode counter-current chromatography in the CUP Modeler software

Counter-current chromatography (CCC) is a separation technique that utilizes immiscible solvent pairs as stationary and mobile phases, which imparts numerous benefits compared to solid-liquid chromatography including the ability to treat either the more-dense or less-dense solvent layer as the mobile phase. Multi-dual mode (MDM) is a CCC elution mode capable of improving the separation of closely eluting compounds by alternating upper- and lower-layer solvent flows in opposing directions within the same separation. While some effort has been made to model MDM, implementation of these models in experimental design has yet to be widely adopted. Accordingly, we further developed our previously published cell utilized partitioning (CUP) model to include MDM predictions with CCC and packaged the full suite of CUP modeling capabilities into a user-friendly, open-source tool called the CUP Modeler. The mathematical model for MDM CCC was derived and validated with experimental separation of ethyl guaiacol (EG) and ethyl phenol (EP), two compounds that co-elute in our previously demonstrated reductive catalytic fractionation (RCF) lignin monomer isolation method. The developed MDM model provided insights into the effect of multiple operating parameters - including stationary phase retention, flow rate, column efficiency, feed concentration ratio, selectivity factor, and solute distribution ratios - on the separation yields, productivity, and purities. Our model agreed with prevailing understanding of MDM but also revealed new insights including that the ideal distribution ratios for co-eluting solutes to be separated by MDM is between 1.1 and 1.5, with the lower value ideally close to 1.25. Overall, this work provides fundamental insights for MDM process design and enables broader adoption of general liquid-liquid chromatography with a new, open-source user-friendly interface.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Selective Biosorption of Valuable Rare Earth Elements Among Co-Occurring Lanthanides

To meet the increasing demand for rare earth elements (REEs) essential for low carbon-intensity energy technologies, new methods are needed for selective REE extraction from unconventional resources. Only a few REEs have significant economic value, but isolation of target rare earths from co-occurring lanthanides is challenging due to their similar chemical behavior. We present a novel approach to enhance separation of specific REEs from lanthanide mixtures. Escherichia coli cells engineered with lanthanide binding tags (LBTs) were immobilized in nonadsorbing, permeable polyethylene glycol diacrylate beads and packed into continuous flow, fixed-bed columns. Breakthrough of 15 rare earths in the +3 oxidation state resulted in notable differences in adsorption selectivity, with greatest separation between europium (Eu) and lanthanum (La) due to competitive displacement. REE adsorption onto fixed-bed columns was predicted by coupling a surface complexation model to a calibrated one-dimensional dual porosity transport model that accounts for interbead advective and intrabead diffusive transport. A tradeoff between high-abundance, low-affinity native carboxyl sites and low-abundance, high-affinity engineered LBT sites dictates process recovery efficiency and selectivity. Key chemical and operational parameters are identified to maximize selective extraction of high-value lanthanides, achieving a threefold enhancement of Eu recovery relative to La in a mixed REE solution.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Imaging and dosimetric characteristics of 67 Cu

In recent years the use of beta-emitting radiopharmaceuticals for cancer therapy has expanded rapidly following development of therapeutics for neuroendocrine tumors, prostate cancer, and other oncologic malignancies. One emerging beta-emitting radioisotope of interest for therapy is 67 Cu (t 1/2 : 2.6 d) due to its chemical equivalency with the widely-established positron-emitting isotope 64 Cu (t 1/2 : 12.7 h). Here we evaluate both the imaging and dosimetric characteristics of 67 Cu, as well as producing the first report of SPECT/CT imaging using 67 Cu. To this end, 67 Cu was produced by photon-induced reactions on isotopically-enriched 68 Zn at the Low-Energy Accelerator Facility (LEAF) of Argonne National Laboratory, followed by bulk separation of metallic 68 Zn by sublimation and radiochemical purification by column chromatography. Gamma spectrometry was performed by efficiency-calibrated high-purity germanium (HPGe) analysis to verify absolute activity calibration and establish radionuclidic purity. Absolute activity measurements corroborated manufacturer-recommended dose-calibrator settings and no radionuclidic impurities were observed. Using the Clinical Trials Network anthropomorphic chest phantom, SPECT/CT images were acquired. Medium Energy (ME) SPECT collimation was found to provide the best image quality from the primary 185 keV gamma emission of 67 Cu. Reconstructed images of 67 Cu were similar in quality to images acquired using 177 Lu. Recovery coefficients were calculated and compared against quantitative images of 99m Tc, 177 Lu, and 64 Cu within the same anthropomorphic chest phantom. Production and clinical imaging of 67 Cu appears feasible, and future studies investigating the therapeutic efficacy of 67 Cu-based radiopharmaceuticals are warranted.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

DOE OSTI2025

MINE: maximally informative next experiment—toward a new GWAS experimental design and methodology

Abstract The computational methodology of Genome Wide Association Studies (GWAS) currently has several limitations: (i) the number of observations (rows) on a quantitative trait tends to be smaller than the number of single nucleotide polymorphisms (SNPs) (columns) in the design matrix; (ii) each SNP is usually modeled separately, failing to acknowledge interaction between each other (ie epistasis); (iii) there is implicit linkage disequilibrium (LD) between neighboring SNPs due to their linkage. To overcome these issues, we developed a tool that uses ensemble methods to fit mixed linear models to GWAS data, and these ensemble methods include the development of a new experimental design approach in GWAS, which uses the resultant models and data to select the next informative experiment over time. This new adaptive and staged approach for GWAS experimental design was developed and tested in a 3 yr adaptive model-guided discovery experiment against a fixed classical design. In Sorghum bicolor a total of 79, 86, and 78 accessions were tested in years 1, 2, and 3, respectively out of 343 accessions available in the Bioenergy Association Panel (BAP) each identified for 232,303 SNPs, 1 every 2–3 kb in the genomes. We demonstrated the feasibility of MINE enacted with 8 people in the field per year over 3 yr vs in 1 large classical design enacted with 20 people in 1 yr. The MINE results for chromosomal regions identified controlling dry weight were confirmed against results from previous sorghum GWAS experiments and 1 large classical design for the BAP panel.

Genetics & Heredity↗

DOE OSTI2020

Chemical and bonding analysis of liquids using liquid cell electron microscopy

Liquid cell transmission electron microscopy (TEM) has become an essential tool for studying the structure and properties of both hard and soft condensed-matter samples, as well as liquids themselves. Liquid cell sample holders, often consisting of two thin window layers separating the liquid sample from the high vacuum of the microscope column, have been designed to control in situ conditions, including temperature, voltage/current, or flow through the window region. While high-resolution and time-resolved TEM imaging probes the structure, shape, and dynamics of liquid cell samples, information about the chemical composition and spatially resolved bonding is often difficult to obtain due to the liquid thickness, the window layers, the holder configuration, or beam-induced radiolysis. Here, we review different approaches to quantitative liquid cell electron microscopy, including recent developments to perform energy-dispersive x-ray and electron energy-loss spectroscopy experiments on samples in a liquid environment or the liquid itself. We also cover graphene liquid cells and other ultrathin window layer holders.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Development of Solid Isotope Harvesting Methods in Preparation for FRIB (Closeout Report)

This project developed the techniques necessary to isolate hydrolysable radiometals from irradiated accelerator components. It was a collaborative project headed by Dr. Jennifer Shusterman at Hunter College in coordination with Dr. Nick Scielzo at Lawrence Livermore National Laboratory and Dr. Gregory Severin at Michigan State University. To develop the methods for harvesting hydrolysable radiometals, both non-radioactive and radioactive experiments were conducted. Non-radioactive tests involved dissolving common accelerator materials (tungsten, copper, aluminum, and gold), adding trace amounts of Zr 4+ and Y 3+ , and then separating the added ions out again using a variety of column-based approaches. These methods were then tested on surrogate materials that were created by irradiating tungsten, copper, aluminum and gold foils with a low-purity 88 Zr beam at the National Superconducting Cyclotron Laboratory. The implanted 88 Zr (and co-implanted and daughter-product 88 Y) were recovered, validating the developed methods. MSU’s role in the project was to develop the chemistry for recovering Zr and Y from tungsten; build the target station for irradiating the foils; conduct the irradiations with the collaborators; to validate the tungsten methodology using the irradiated foils; and to disseminate the results.

07 ISOTOPE AND RADIATION SOURCES↗

DOE OSTI2020

Metal Oxide Sorbents for the Separation of Radium and Actinium

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

TALSPEAK-based separation of the trivalent actinides from rare earth elements using LN resin

The separation of 241 Am, 244 Cm and 249 Cf from rare earth elements using LN resin and lactate buffer solutions with diethylenetriaminepentaacetic acid is described with numerous columns studies. The elutions are based on TALSPEAK liquid–liquid extraction chemistry, and provide high yield (> 90%), rapid, simple separations of the trivalent actinides from the lanthanides, which is often challenging due to similarities in chemical behavior among the trivalent f-block elements. Further, all three actinides can be separated from rare earth elements, including from massless fission product samples and samples with small amounts (~ 1–5 mg) of stable lanthanides. Separations with no detectable overlap between the actinide and lanthanide elutions is possible with massless samples, and in samples with mass high separation factors can be achieved (Am/Eu: 171; Am/La: 10 6 ).

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2023

Microporous metal–organic frameworks for the purification of propylene

Separation of propylene from its analogous hydrocarbons such as propane is of great importance in the petrochemical industry to produce valuable chemical feedstocks with desired purity. However, the well-established method currently used for industrial propane/propylene separation is energy intensive. It involves repeated cycling in the cryogenic and high-pressure distillation process and requires multiple columns and high reflux ratios because of the very similar physical properties of the two species. Thus, it is identified as one of the most capital- and energy-intensive processes. Adsorptive separation based on porous adsorbents is regarded as an alternative energy-efficient technology to replace or supplement the traditional heat-driven cryogenic distillation processes. In this context, metal–organic frameworks (MOFs) have emerged as the most promising candidates for propane/propylene separation, taking into consideration their unique tunability with respect to pore geometry and pore functionality. In this highlight, we summarize the latest advancement in developing MOFs as physisorbents for the separation and purification of propylene from propane, with a focus on those that demonstrate selective molecular exclusion and propane-selective adsorption. We discuss the adsorption preferences related to the material design and separation mechanisms, and review the existing challenges. Lastly, we offer our perspectives on various strategies for the future design of MOFs that hold true potential for propylene purification under industrial settings.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Developing Inorganic Resins for Radium and Actinium Generators and Purifications

The inorganic, normal-phase sorbents alumina, titania, and zirconia were evaluated and screened for the separation of Ba, La, 228 Ra, 228 Ac, and 212 Pb in a dilute acid matrix. The results show that the sorbents are capable of fractionating the ions between pH 1–8. Acetate and total metal ion concentrations were experimentally evaluated as factors that could affect retention using La and Ba surrogates. Pseudo-second order rate constants were derived and the uptake of La was determined to be endothermic. A stationary zirconia column was used to isolate Ba from La and Ra from Ac/Pb; elution profiles of each separation are presented. The utility and implications of these sorbents are discussed with respects to large-scale production of 225 Ac from radium targets. This work was published in 2020 and in 2022.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗