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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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All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Determination of 2,4-Dinitrophenol (2,4-DNP) in Simulated Radioactive Waste by High Performance Liquid Chromatography

The River Protection Project (RPP) at Hanford, Washington is evaluating an alternative treatment method for low activity tank waste (LAW) disposition. Specifically, grout solidification/immobilization for LAW needs to demonstrate adequate treatment for Land Disposal Restricted (LDR) Organic chemicals. LDR organic chemical pretreatment, such as evaporations testing and oxidation decomposition, are under assessment to reduce the LDR organic chemicals concentration in the LDR waste. 2,4-dinitrophenol was spiked into LAW simulated waste and monitored in these studies using High Performance Liquid Chromatography (HPLC). The development and implementation of this HPLC method is discussed in this presentation.

Dekarske, John R. [Savannah River National Laborat↗
DOE OSTI2023

Comparing π‐complexation capabilities of ionic liquids containing silver(I) and copper(I) ions by headspace single drop microextraction in combination with high‐performance liquid chromatography

Selective π‐complexation capabilities of silver(I) and copper(I) ions can be effectively facilitated in ionic liquids. To understand the effects of environmental factors that influence the π‐complexation of these metal ions with analytes, techniques that employ small volumes of ionic liquid that can be readily analyzed are desired. In this study, headspace single drop microextraction coupled with HPLC is used to investigate a diverse set of environmental factors on the metal ion‐mediated complexation with aromatic compounds in ionic liquid media. Silver(I) and copper(I) bis[(trifluoromethyl)sulfonyl]imide salts were both studied by dissolving them in the 1‐decyl‐3‐methylimidazolium bis[(trifluoromethyl)sulfonyl]imide ionic liquid and employing the mixture as extraction media for aromatic compounds. Water and acetonitrile within the sample solution were observed to interfere with the complexation of silver(I) ions and aromatic compounds, while ethylene glycol and triethylene glycol did not. The temperature and extraction times were optimized to fully facilitate the π‐complexation capabilities of metal ions in ionic liquid media. Partition coefficients between the sample headspace and metal ion were determined using a three‐phase equilibria model. Although no discernable difference in analyte partitioning between the headspace and ionic liquid solvent was observed, analyte partition coefficients to silver(I) ion tended to be greater compared to copper(I) ion.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Silver-mediated separations: A comprehensive review on advancements of argentation chromatography, facilitated transport membranes, and solid-phase extraction techniques and their applications

The use of silver(I) ions in chemical separations, also known as argentation separations, is a powerful approach for the selective separation and analysis of many natural and synthetic organic compounds. In this review, a comprehensive discussion of the most common argentation separation techniques, including argentation-liquid chromatography (Ag-LC), argentation-gas chromatography (Ag-GC), argentation-facilitated transport membranes (Ag-FTMs), and argentation-solid phase extraction (Ag-SPE) is provided. For each of these techniques, notable advancements, optimized separations, and innovative applications are discussed. The review begins with an explanation of the fundamental chemistry underlying argentation separations, mainly the reversible π-complexation between silver(I) ions and carbon-carbon double bonds. Within Ag-LC, the use of silver(I) ions in thin-layer chromatography, high-performance liquid chromatography, as well as preparative LC are explored. This discussion focuses on how silver(I) ions are employed in the stationary and mobile phase to separate unsaturated compounds. For Ag-GC and Ag-FTMs, different silver compounds and supporting media are discussed, often with relation to olefin-paraffin separations. Ag-SPE has been widely employed for the selective extraction of unsaturated compounds from complex matrices in sample preparation. This comprehensive review of Ag-LC, Ag-GC, Ag-FTMs, and Ag-SPE techniques emphasizes the immense potential of argentation separations in separations science and serves as a valuable resource for researchers seeking to learn, optimize, and utilize argentation separations.

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

Metabolome patterns identify active dechlorination in bioaugmentation consortium SDC-9™

Ultra-high performance liquid chromatography–high-resolution mass spectrometry (UPHLC–HRMS) is used to discover and monitor single or sets of biomarkers informing about metabolic processes of interest. The technique can detect 1000’s of molecules (i.e., metabolites) in a single instrument run and provide a measurement of the global metabolome, which could be a fingerprint of activity. Despite the power of this approach, technical challenges have hindered the effective use of metabolomics to interrogate microbial communities implicated in the removal of priority contaminants. Herein, our efforts to circumvent these challenges and apply this emerging systems biology technique to microbiomes relevant for contaminant biodegradation will be discussed. Chlorinated ethenes impact many contaminated sites, and detoxification can be achieved by organohalide-respiring bacteria, a process currently assessed by quantitative gene-centric tools (e.g., quantitative PCR). This laboratory study monitored the metabolome of the SDC-9™ bioaugmentation consortium during cis-1,2-dichloroethene (cDCE) conversion to vinyl chloride (VC) and nontoxic ethene. Untargeted metabolomics using an UHPLC-Orbitrap mass spectrometer and performed on SDC-9™ cultures at different stages of the reductive dechlorination process detected ~10,000 spectral features per sample arising from water-soluble molecules with both known and unknown structures. Multivariate statistical techniques including partial least squares-discriminate analysis (PLSDA) identified patterns of measurable spectral features (peak patterns) that correlated with dechlorination (in)activity, and ANOVA analyses identified 18 potential biomarkers for this process. Statistical clustering of samples with these 18 features identified dechlorination activity more reliably than clustering of samples based only on chlorinated ethene concentration and Dhc 16S rRNA gene abundance data, highlighting the potential value of metabolomic workflows as an innovative site assessment and bioremediation monitoring tool.

environmental monitoring↗
DOE OSTI2025

Direct Synthesis of Polyester from Biomass Derived 1,6-hexanediol using a Copper-Ceria Catalyst

Biomass derived polyesters are gaining attention due to their increased mechanical and thermal properties, and also because of their biodegradability. These polyesters are typically synthesized from polycondensation reactions between diols with dicarboxylic acids using catalysts. Other methods such as alcoholysis and acidolysis of low molecular weight esters and alcoholysis of acyl chlorides are also well known. Direct conversion of diol to ester without using dicarboxylic acid is not well known, and to our knowledge has not been reported over a solid catalyst. In this study, we report a direct synthesis of polyester from 1,6-hexanediol using a copper-ceria catalyst without using a dicarboxylic acid monomer. The copper-ceria catalysts were synthesized by incipient wetness impregnation method and characterized using X-ray photoelectron spectroscopy (XPS), X-ray diffraction analysis (XRD), Brunauer-Emmett-Teller (BET), and infrared spectroscopy (IR). Our initial studies show that 1,6-hexanediol can be converted to corresponding polyester at higher temperatures under atmospheric pressures of CO2 or N2. The reaction products were analyzed using nuclear magnetic resonance spectroscopy (NMR), gel permeation chromatography (GPC), high performance liquid chromatography (HPLC), and IR spectroscopy.

Biomass derived diols↗
DOE OSTI2026

A Unified Analytical Method Greenness Score ( uAMGS ) Quantifies How Microscopic Imaging Is Greener Than Conventional Liquid Chromatography

Green chemistry is a set of principles for assessing, developing, and implementing methods that are safer, more efficient, and less detrimental to the environment. The analytical method greenness score (AMGS) is one of many metrics that attempt to evaluate traditional liquid chromatography (LC) based on the energy consumption of the instrument and the safety, health risks, and environmental impact of the solvents employed. Unfortunately, in practice, the AMGS is primarily focused on traditional separation methods in the pharmaceutical industry and is not amenable to cutting-edge separation science, including miniaturization. To broaden this scope, the unified Analytical Method Greenness Score (uAMGS) is presented here, which clarifies and expands on the underlying mathematics and incorporates both dimensional and uncertainty analysis, enabling its application to a broader range of analytical techniques. The uAMGS is used to compare the greenness of two distinct methods: single-molecule microscopy (SMM) and high-performance liquid chromatography (HPLC), which were used to collect equivalent data. uAMGS determines that SMM is significantly greener than HPLC due primarily to decreased solvent consumption. Overall, the uAMGS should allow chemists ranging from undergraduates to industrial PhDs to assess the greenness of a wide range of separations.

chemical separations↗
DOE OSTI2023

Fouling characterization and treatment of water reuse concentrate with membrane distillation: Do organics really matter

Membrane distillation (MD) for the treatment of concentrated brines has been limited in part by membrane fouling, resulting in subsequent flux decline and membrane wetting. This study provides new insight into the identification of fouling and scaling mechanisms and pretreatment strategies for mitigating flux decline with MD treatment of water reuse reverse osmosis concentrate (ROC). Bench-scale direct contact MD experiments were performed with untreated and pretreated ROC. Biological activated carbon (BAC), chemical water softening, or fluidized bed crystallization reactor coupled with ion exchange (FBCR-IX) were selected as pretreatment strategies to isolate the effects of organic fouling and calcium scaling. Organic and inorganic compounds were analyzed by high-performance liquid chromatography (HPLC) and inductively coupled plasma mass spectrometry (ICP-MS). Calcium ions were found to be the major contributor to flux decline despite the high organic content in the ROC. Minimal organic fouling is likely because the organic matter in the ROC is hydrophilic, limiting hydrophobic-hydrophobic interactions between the organics and the membrane. Furthermore, the water flux declined by 63 % after removing organic compounds by BAC pretreatment, with 60 % of the calcium mass precipitating from the solution. Whereas, the water flux remained constant after removing multivalent ions with fluidized bed crystallization. Cleaning the membrane by acid washing and temperature reversal recovered 73 % and 12 % of the water flux, respectively. The analyses outlined in this study can assist in selecting appropriate fouling and scaling mitigation strategies for water reuse ROC and a wide range of feed solutions used in MD applications.

42 ENGINEERING↗
DOE OSTI2023

Evaluation of 134 Ce/ 134 La as a PET Imaging Theranostic Pair for 225 Ac α-Radiotherapeutics

225 Ac-targeted α-radiotherapy is a promising approach to treating malignancies, including prostate cancer. However, α-emitting isotopes are difficult to image because of low administered activities and a low fraction of suitable γ-emissions. The in vivo generator 134 Ce/ 134 La has been proposed as a potential PET imaging surrogate for the therapeutic nuclides 225 Ac and 227 Th. In this report, we detail efficient radiolabeling methods using the 225 Ac-chelators DOTA and MACROPA. These methods were applied to radiolabeling of prostate cancer imaging agents, including PSMA-617 and MACROPA-PEG 4 -YS5, for evaluation of their in vivo pharmacokinetic characteristics and comparison to the corresponding 225 Ac analogs. Methods: Radiolabeling was performed by mixing DOTA/MACROPA chelates with 134 Ce/ 134 La in NH 4 OAc, pH 8.0, at room temperature, and radiochemical yields were monitored by radio–thin-layer chromatography. In vivo biodistributions of 134 Ce-DOTA/MACROPA.NH 2 complexes were assayed through dynamic small-animal PET/CT imaging and ex vivo biodistribution studies over 1 h in healthy C57BL/6 mice, compared with free 134 CeCl 3 . In vivo, preclinical imaging of 134 Ce-PSMA-617 and 134 Ce-MACROPA-PEG 4 -YS5 was performed on 22Rv1 tumor–bearing male nu/nu-mice. Ex vivo biodistribution was performed for 134 Ce/ 225 Ac-MACROPA-PEG 4 -YS5 conjugates. Results: 134 Ce-MACROPA.NH 2 demonstrated near-quantitative labeling with 1:1 ligand-to-metal ratios at room temperature, whereas a 10:1 ligand-to-metal ratio and elevated temperatures were required for DOTA. Rapid urinary excretion and low liver and bone uptake were seen for 134 Ce/ 225 Ac-DOTA/MACROPA. NH 2 conjugates in comparison to free 134 CeCl 3 confirmed high in vivo stability. An interesting observation during the radiolabeling of tumor-targeting vectors PSMA-617 and MACROPA-PEG 4 -YS5—that the daughter 134 La was expelled from the chelate after the decay of parent 134 Ce—was confirmed through radio–thin-layer chromatography and reverse-phase high-performance liquid chromatography. Both conjugates, 134 Ce-PSMA-617 and 134 Ce-MACROPA-PEG 4 -YS5, displayed tumor uptake in 22Rv1 tumor–bearing mice. The ex vivo biodistribution of 134 Ce-MACROPA.NH 2 , 134 Ce-DOTA and 134 Ce-MACROPA-PEG 4 -YS5 corroborated well with the respective 225 Ac-conjugates. Conclusion: These results demonstrate the PET imaging potential for 134 Ce/ 134 La-labeled small-molecule and antibody agents. The similar 225 Ac and 134 Ce/ 134 La-chemical and pharmacokinetic characteristics suggest that the 134 Ce/ 134 La pair may act as a PET imaging surrogate for 225 Ac-based radioligand therapies.

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2024

Efficient Synthesis and HPLC-Based Characterization for Developing Vanadium-48-Labeled Vanadyl Acetylacetonate as a Novel Cancer Radiotracer for PET Imaging

Bis(acetylacetonato)oxidovanadium(IV) [(VO(acac) 2 ], generally known as vanadyl acetylacetonate, has been shown to be preferentially sequestered in malignant tissue. Vanadium-48 ( 48 V) generated with a compact medical cyclotron has been used to label VO(acac) 2 as a potential radiotracer in positron emission tomography (PET) imaging for the detection of cancer, but requires lengthy synthesis. Current literature protocols for the characterization of VO(acac) 2 require macroscale quantities of reactants and solvents to identify products by color and to enable crystallization that are not readily adaptable to the needs of radiotracer synthesis. We present an improved method to produce vanadium-48-labeled VO(acac) 2 , [ 48 V]VO(acac) 2 , and characterize it using high-performance liquid chromatography (HPLC) with radiation detection in combination with UV detection. The approach is suitable for radiotracer-level quantities of material. These methods are readily applicable for production of [ 48 V]VO(acac) 2 . Preliminary results of preclinical, small-animal PET studies are presented.

62 RADIOLOGY AND NUCLEAR MEDICINE↗
DOE OSTI2026

Insights into the Structure of Ultrasmall Fluorescent Core–Shell Silica Nanoparticles

Ultrasmall fluorescent core–shell nanoparticles (NPs) with a silica core and poly(ethylene glycol) ligand shell are the earliest example of hybrid NPs that have received U.S. investigational new drug FDA approval. They are among only a few inorganic NPs translated to safety, diagnostic, and therapeutic human clinical trials. Despite these achievements, little is known about the exact structure of their 3–4 nm sized silica cores. We report the surprising discovery of a well-defined pentagonal bipyramidal core structure preferentially formed in the aqueous synthesis built from seven primary silica NPs. A combination of reverse-phase high-performance liquid chromatography, cryogenic transmission electron microscopy, and coarse-grained simulations provides fundamental insights into this magic-size cluster formation and its unusual stability. Here, results rationalize the successful NP synthesis scale-up from 1 mL to 50 L, provide clues to the recent discovery of their self-therapeutic properties in oncology via ferroptosis, an iron-dependent cell death mechanism, and promise improved control of particle size distribution via chromatographic separations.

cluster chemistry↗
DOE OSTI2022

Analysis of persistent contaminants and personal care products by dispersive liquid-liquid microextraction using hydrophobic magnetic deep eutectic solvents

Here, in this work, hydrophobic magnetic deep eutectic solvents (HMDESs) were used in the development of a simple and rapid dispersive liquid-liquid microextraction (DLLME) approach coupled to high performance liquid chromatography with UV detection (HPLC-UV) for the determination of ten organic contaminants including five polycyclic aromatic hydrocarbons, four UV filters, and a pesticide from water at trace levels. The HMDESs were prepared by mixing a hydrogen bond acceptor, metal halide salt, and hydrogen bond donor in suitable molar ratios. Two HMDESs, 2 tetraoctylammonium bromide ([N 8888 + ][Br - ]): cobalt chloride (CoCl 2 ): 4 octanoic acid (OA) and 3 trioctylphosphine oxide (TOPO): neodymium chloride (NdCl 3 ): 3 OA, offered the highest analyte extraction efficiency overall and were chosen as suitable solvents for validation of the microextraction method. Under optimized extraction conditions, the method required 30 µL of HMDES as extraction solvent, acetone (87.5 µL) as disperser solvent, a NaCl concentration of 30% (w/v), and an extraction time of 120 s at 20°C. Enrichment factors of the analytes ranged from 44.6 for 3-(4-methylbenzylindene) camphor to 66.0 for 2-ethylhexyl-4-(dimethyl)aminobenzoate. The method provided low limits of detection (LODs) ranging from 0.5 to 4.5 µg L -1 , and acceptable precision, with RSD values lower than 9.6%. Furthermore, the validated method was successfully applied for tap and lake water analysis, resulting in relative recoveries of spiked samples ranging between 94.7 and 119.2%.

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

Comparing the extraction performance of cyclodextrin-containing supramolecular deep eutectic solvents versus conventional deep eutectic solvents by headspace single drop microextraction

A headspace single drop microextraction (HS-SDME) method coupled with high performance liquid chromatography was developed to compare the extraction of eighteen aromatic organic pollutants from aqueous solutions using cyclodextrin-based supramolecular deep eutectic solvents (SUPRADESs) and alkylammonium halide-based conventional deep eutectic solvents (DESs). Different derivatives of beta-cyclodextrin (β-CD) were employed as hydrogen bond acceptors (HBA) in SUPRADESs and the extraction performance investigated. SUPRADES comprised of the 20 wt% native β-CD HBA provided the highest enrichment factors of analytes compared to SUPRADESs comprised of other derivatives of β-CD (random methylated β-cyclodextrin, heptakis(2,3,6-tri-O-methyl)-β-cyclodextrin, and 2-hydroxypropyl β-cyclodextrin). In addition, native β-CD and its derivatives were dissolved in the neat DESs and their effect on the extraction of analytes examined. Dissolution of 20 wt% native β-CD in the choline chloride ([Ch + ][Cl - ]):2Urea DES resulted in a significant increase in the extraction efficiencies of target analytes compared to the neat [Ch + ][Cl - ]:2Urea DES. Under optimum conditions, the extraction method required a solvent microdroplet of 6.5 μL, 1000 rpm stir rate, 30% (w/v) salt concentration, and a temperature of 40 °C. The tetrabutylammonium chloride: 2 lactic acid DES resulted in the highest enrichment factors while the [Ch + ][Cl - ]:2Urea DES had the lowest for most of the analytes among the evaluated solvents. The method provided limits of detection (LODs) down to 35 μg L -1 . Finally, the developed method was applied for the analysis of spiked tap and lake water, where relative recoveries ranging from 83.7% -119.7% and relative standard deviations lower than 19.2% were achieved.

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

Photolytic Degradation of Water‐Soluble Organic Carbon in Snowmelts: Changes in Molecular Characteristics, Brown Carbon Chromophores, and Radiative Effects

Abstract Water‐soluble organic carbon (WSOC) deposited in ambient snowpack play key roles in regional carbon cycle and surface energy budget, but the impacts of photo‐induced processes on its optical and chemical properties are poorly understood yet. In this study, melted samples of the seasonal snow collected from northern Xinjiang, northwestern China, were exposed to ultraviolet (UV) radiation to investigate the photolytic transformations of WSOC. Molecular characteristics and chemical composition of WSOC and its brown carbon (BrC) constituents were investigated using high‐performance liquid chromatography interfaced with a photodiode array detector and a high‐resolution mass spectrometer. Upon illumination, formation of nitrogen‐ and sulfur‐containing species with high molecular weight was observed in snow samples influenced by soil‐ and plant‐derived organics. In contrast, the representative sample collected from remote region showed the lowest molecular diversity and photolytic reactivity among all samples, in which no identified BrC chromophores decomposed upon illumination. Approximately 65% of chromophores in urban samples endured UV irradiation. However, most of BrC composed of phenolic/lignin‐derived compounds and flavonoids disappeared in the illuminated samples containing WSOC from soil‐ and plant‐related sources. Effects of the photochemical degradation of WSOC on the potential modulation of snow albedo were estimated. Apparent half‐lives of WSOC estimated as albedo reduction in 300–400 nm indicated 0.1–0.4 atmospheric equivalent days, which are shorter than typical photolysis half‐lives of ambient biomass smoke aerosol. This study provides new insights into the roles of WSOC in snow photochemistry and snow surface energy balance.

Meteorology & Atmospheric Sciences↗
DOE OSTI2025

Molecular and structural characterization of a Bacillus cereus strain producing an anthrax-like capsule

Bacillus cereus is a ubiquitous Gram-positive, spore-forming, rod-shaped saprophytic bacterium, occasionally reported to cause food-borne illnesses. However, instances of B. cereus strains harboring anthrax toxin and capsule genes have elevated certain strains as formidable pathogens and biothreats. This study focuses on the genomic analysis and the structural characterization of capsular material produced by the virulent B. cereus PATH2418 strain, isolated from the wound of a traumatic open fracture patient. The genome was sequenced using Nanopore MinION sequencing, revealing a chromosome of 5,270,283 bp and three plasmids. One plasmid, pATH1, was found to encode an operon for the biosynthesis of a bacterial capsule. This operon had sequence homology to the Bacillus anthracis capBCADE operon, which encodes the poly-γ-D-glutamate (PDGA) capsule. The capsule production in B. cereus PATH2418 was influenced by temperature and CO 2 levels. Structural analysis of the capsular material using a combined approach of nuclear magnetic resonance (NMR) and high-performance liquid chromatography (HPLC) techniques confirmed the presence of a high-molecular-weight poly-γ-glutamate capsule, with an enantiomeric composition of approximately 67% D-glutamic acid and 33% L-glutamic acid, matching that of B. anthracis.

Bacillus cereus↗
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 OSTI2025

147 Nd Quantification Using HSCCC-Purified Samples

Quantifying the fission product 147 Nd in nuclear debris samples is an important component of post-detonation nuclear forensics. The most accurate quantifications are obtained when Nd is purified from all other fission products, actinides, activation products, and environmental matrix contained within the debris. In this study, a recently developed method for Nd purification was tested, purifying 147 Nd from solutions of mixed fission products using high-speed counter-current chromatography (HSCCC). Importantly, the new method allowed for faster elution of Nd from the column as compared with established high performance liquid chromatography (HPLC) methods, and resulted in accurate/precise 147 Nd quantification by gamma-ray spectrometry. While the up-front equipment costs associated with HSCCC may be higher, its operational costs are on par with those of HPLC (solvents, extractants, power). Gas-flow proportional beta decay counting revealed contamination from the nearest neighbor lanthanide 143 Pr (a gamma-silent radioisotope) in the HSCCC-purified samples, but the activity contribution from 147 Nd could still be quantified. Remarkably consistent elution profiles were observed for the HSCCC method, spanning rare earth element (REE) loadings of more than 10 orders of magnitude (tracer to mmol quantities). In conclusion, the reliability and speed of the new method suggest utility for the rapid separation and quantification of 147 Nd in unknown samples.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Ice Recrystallization Inhibition Activity of Soy Protein Hydrolysates

Identifying and developing ice recrystallization inhibitors from sustainable food proteins such as soy protein isolate (SPI) can lead to practical applications in both pharmaceutical and food industries. Here, the objective of this study was to investigate the ice recrystallization inhibition (IRI) activity of SPI hydrolysates, and this was achieved by using an IRI activity-guided fractionation approach and relating IRI activity to interfacial molecular activity measured by vibrational sum frequency generation (VSFG). In addition, the impact of molecular weight (MW) and enzyme specificity was analyzed using three different proteases (Alcalase, trypsin, and pancreatin) and varying hydrolysis times. Using preparative chromatography, hydrolysates from each enzyme treatment were fractionated into five different MW fractions (F1–F5), which were then characterized by high-performance liquid chromatography (HPLC). All SPI hydrolysates had IRI activity, resulting in a 57–29% ice crystal diameter reduction when compared to native SPI. The F1 fraction (of 4–14 kDa) was most effective among all tested hydrolysates, while the lower MW peptide fractions lacked activity. One sample (SPI-ALC 20-F1) had a 52% reduction of ice crystal size at a lower concentration of 2% compared to the typical 4% used. SFG showed a difference in H-bonding and hydrophobic interactions of the molecules on the water/air interface, which may be linked to IRI activity. This study demonstrates for the first time the ability of SPI hydrolysates to inhibit ice crystal growth and the potential application of SFG to study molecular interaction at the interface that may help illustrate the mechanism of action.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗