Search NASA⌕ Search

SEARCH · Search NASA

Results for “HPLC”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 91 records · Page 5

Nitrogen-doped char as a catalyst for wet oxidation of phenol-contaminated water

Catalytic wet oxidation (CWO) of aqueous effluents rich in organic compounds is a very promising technology for the treatment of liquid wastes from biomass conversion processes. CWO reactions occur through the formation of free radical species, produced in the presence of an oxidant, which act on organic contaminates in the effluent. Although the reaction is well known, there exists a lack of affordable catalysts to conduct this process at the lower temperatures and pressures in novel bioenergy processes. Here, this study assessed the catalytic effect of nitrogen-doped chars as such an option. Phenol in aqueous solution was used as a model waste effluent. Treatment was conducted at moderate temperatures (190 to 260 °C), oxygen partial pressure of 1 MPa, and reaction times of 15, 30, and 45 min in stainless steel and glass-lined tube reactors. High pressure liquid chromatography (HPLC) analyses of the products quantified phenol and by-product concentrations used in the calculation of reaction activation energy. The char catalyst was studied by X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), and scanning electron microscopy (SEM) in order to gain insight into its structure and surface composition. The results indicate that nitrogen-doped char catalysts accelerate the oxidation of phenol by decreasing its reaction activation energy from 82.2 kJ/mol (non-catalyzed) to 40.4 kJ/mol (catalyzed). An analysis from first principles using density functional theory (DFT) was conducted to ascertain which N functional group has the most significant impact on free radical formation in the presence of oxygen. Among all the N functional groups studied, the dipyridinic functional groups showed the most promising characteristics to facilitate the formation of hydroxyl free radicals.

Advanced Oxidation Processes for Organic Pollutant↗

Preliminary investigation of 48 V-labeled VO(acac) 2 for cancer imaging: An initial proof-of-concept study

In this preliminary study, a procedure for synthesizing novel PET radiotracer vanadium-48-labeled-vanadyl acetylacetonate was developed, including radioisotope production via cyclotron, separation of 48 V, chelation as 48 VO(acac) 2 , and assessment through in vitro cellular studies. We employed the beam-stop setup in a cyclotron as the target holder to irradiate titanium foils in the reaction of nat Ti (p,n) 48 V. The radioisotope production rate was 4.84 ± 0.67 μCi/μA-h. Overall radiochemical yield was 12.86 ± 0.51% with gamma-ray spectroscopy showing no detectable contaminant peaks. HPLC of 48 VO(acac) 2 showed a retention time (1:48) corresponding closely to that (1:50) of commercial VO(acac) 2 , verifying the successful synthesis of 8VO(acac) 2 . In vitro cellular studies demonstrated radiotracer uptake and saturation around 0.48 nM. These studies pave the way for improving methodologies and in vivo experiments, including imaging studies, in future investigations.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

Autonomous continuous flow reactor synthesis for scalable atom-precision

With new instrumentation design, robotics, and in-operando hyphenated analytical tool automation, the intelligent discovery of synthesis pathways is becoming feasible. It can potentially bridge the gap for the scale-up of new materials. In this article, we review current progress and describe a new system that uses an autonomous continuous flow chemistry framework to translate high-quality lead molecules and materials to quantities that can meet scalability demands. At the core is a continuous flow synthesis platform that can design its viable synthesis pathway to a particular molecule or material and then autonomously carry it out. This is realized by integrating: (1) A workflow/architecture for multimode chemical/materials characterization in-line. The in-line characterization modes are NMR, ESR, IR, Raman, UV-Vis, GC-MS, and HPLC, along with ex-situ modes for X-Ray and neutron scattering; (2) Integration for feedback/analysis/data storage of the control variables; (3) A core software stack that includes deep learning and reinforcement learning alongside quantum chemistry and molecular dynamics; (4) On-demand compute architectures that parse calculations to compute resources needed which include light-weight edge, mid-level edge (NVIDA DGX-2), and high-performance computing. We demonstrate preliminary results on how this autonomous reactor system can enhance our ability to deliver deuterated materials, copolymers, and site-substituted molecules.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

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↗

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↗

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↗

Studying the effect of drug-to-excipient ratio on drug release profile for drug coated balloons

Drug-coated balloons (DCB) have emerged as the alternative procedure for restenosis because of their ability to treat a variety of occlusion types with a uniform dose of anti-proliferative drugs. DCB are balloons coated with antiproliferative drugs encapsulated in a polymer matrix. There are several types of coating matrices used to produce DCB. In this study, the relationship between coating composition and drug release under physiologically relevant conditions was examined to understand how differences in coating composition impacts the drug transfer from the balloon surface to the simulated body fluids. To conduct the experiments, the balloons were coated with different paclitaxel (drug)-to-iopromide (excipient) ratios (3:1, 3:2 and 1:2) using an in-house developed micro-pipetting method. Scanning electron microscopy (SEM) images showed that the 3:1 PTX:IOP ratio produced a more uniform, crystalline microstructure with a thinner coating throughout the balloon surface compared to the other drug-to-excipient ratios. The 1:2 PTX:IOP ratio showed the least crystalline microstructure among the three ratios evaluated in this study. Three different drug elution conditions were tested. The amount of drug released to the medium was quantified by high performance liquid chromatography (HPLC). Our soaking study and submerge & deploy study showed that ~20% of the drug transferred to the target site under physiological conditions. A track and deploy method was performed using a “mock” artery, to simulate an in vitro environment. Coated balloons were passed through the mock artery to mimic tracking turns the balloon within the arteries during the angioplasty procedures. Seven elution samples were collected at different stages of the procedure. Finally, drug release results suggest that the higher excipient ratio helps to deliver the lipophilic drug to the target site under simulated conditions but causes higher drug loss during the balloon transfer process.

60 APPLIED LIFE SCIENCES↗

Effect of overcharge on Li(Ni 0.5 Mn 0.3 Co 0.2 )O 2 /Graphite cells–effect of binder

Cells based on NMC/graphite, containing styrene-butadiene rubber/carboxymethylcellulose binder in the anodes and pVdF latex/carboxymethykellulose in the cathodes, were systematically overcharged to 100, 120, 140, 160, 180, 250% and 270% state-of-charge. The impact of the binder was characterized by elemental analysis, SEM, and HPLC. These results were compared to similar cells just using the poly (vinylidene difluoride) binder. Not only did the binder impact the rate of transition metal transport from the cathode to the anode, it also had a marked effect on the microstructure and composition of the materials on the anode surface.

25 ENERGY STORAGE↗

Insights into determining pore size properties of ultrafiltration membranes

The selectivity of porous membranes is often characterized using solute rejection tests, where membranes are challenged with dilute aqueous solutions of neutral solutes at operating conditions that minimize concentration polarization and fouling. In single solute tests, a membrane is challenged with one molecular weight (MW) solute at a time from low to high MW. Since single solute methods are time-intensive, mixed solute tests have become more common, where a mixture of several MW solutes challenges a membrane at once. However, the presence of large solutes in a mixture increases the rejection of smaller solutes. Furthermore, there are no universally accepted operating conditions or standard methods used by membrane manufacturers or researchers for the experiments, leading to difficulty in pore size and pore characteristic comparisons. In this paper, commercial ultrafiltration membranes were challenged with single and mixed solute polyethylene glycol (PEG) and dextran aqueous solutions. First, rejection values determined using total organic carbon (TOC) and high-performance liquid chromatography (HPLC) from single solute filtration experiments are compared. Differences in rejection curves obtained by the two techniques are attributed to solute polydispersity. Mixed solute filtration experiments with binary mixtures of solutes showcased co-solute interactions, which increase with both the size and weight percent of large solute in the mixture. Mixed solute filtration experiments at varying operating conditions (i.e., stir speed and flux) were conducted to determine operating conditions that mitigate co-solute interactions. Stir speed had a minimal effect on co-solute interactions. In contrast, low flux conditions can help minimize co-solute interactions, leading to pore size distributions that closely resemble results observed in single solute filtration using narrowly dispersed solutes. Additionally, at low flux conditions, the predicted membrane pore size distributions utilizing mixed solute experiments with PEG and dextran were similar.

36 MATERIALS SCIENCE↗

Trithiol ligand provides tumor-targeting 191 Pt-complexes with high molar activity and promising in vivo properties

The Auger electron-emitting radionuclide 191 Pt is a promising candidate for radiopharmaceutical therapy. Herein, we explored novel labeling methods for 191 Pt using thiol-containing ligands to improve the in vivo stability and targeting ability of 191 Pt-labeled complexes. We synthesized dithiol-containing N 2 S 2 and NS 2 ligands, and a trithiol ligand, and then compared their radiochemical reactivity with 191 Pt. [ 191 Pt]Pt-trithiol was synthesized and its biodistribution was evaluated in mice and compared with free 191 Pt. Finally, a 191 Pt-trithiol complex targeting prostate-specific membrane antigen (PSMA): [ 191 Pt]Pt-trithiol-PSMA was developed and evaluated in mice bearing tumor xenografts and compared with a 191 Pt-complex labeled via monothiol-containing Cys ([ 191 Pt]Pt-Cys-PSMA). A comparison of N 2 S 2 , NS 2 , and trithiol showed that the trithiol ligand is the best for producing 191 Pt-labeled compounds in high yield and as a single peak in preparative HPLC. Notably, the trithiol ligand made 191 Pt-labeled compounds and precursors separatable, achieving 191 Pt-labeled products with a high molar activity: 200–400 mCi/μmol (7.4–14.8 GBq/μmol) at EOS. Additionally, [ 191 Pt]Pt-trithiol and [ 191 Pt]Pt-trithiol-PSMA were stable in vivo with rapid clearance compared with free 191 Pt and [ 191 Pt]Pt-Cys-PSMA. [ 191 Pt]Pt-trithiol-PSMA resulted in a low uptake in most normal organs and a high uptake in the kidneys and prostate cancer with PSMA expression. Furthermore, this study demonstrated that a labeling method with trithiol for Pt radionuclides achieves 191 Pt-labeled products with high molar activity. 191 Pt-trithiol-PSMA showed promising in vivo stability and tumor-targeting specificity, which should facilitate the pharmaceutical development of Pt radionuclides for radiopharmaceutical therapy, especially Auger electron cancer therapy.

Auger emitters↗

Developing a new ethylene glycol/H 2 O pretreatment system to achieve efficient enzymatic hydrolysis of sugarcane bagasse cellulose and recover highly active lignin: Countercurrent extraction

Improving pretreatment efficiency is a critical premise in achieving efficient biomass conversion, and obtaining high-performance natural polymers is the guarantee of high-value conversion of biomass. Here, in this study, a new pilot-scale continuous countercurrent pretreatment reaction unit about ethylene glycol-alkali solution was designed for pretreating sugarcane bagasse in order to achieve efficient separation of the three major components of lignocellulose when expanding the scale of pretreatment, reduce lignin deposition on the fiber surface, and obtain highly active lignin and excellent enzymatic hydrolysis efficiency of cellulose. X-ray diffractometer (XRD), X-ray photoelectron spectrometer (XPS), brunauer-emmett-teller (BET) and scanning electron microscope (SEM) methods are used to analyze the structural properties of sugarcane bagasse before and after pretreatment, and high-performance liquid chromatography (HPLC) is used to analyze the monosaccharide components in the enzymatic solution. In addition, the structural properties of the recovered lignin are analyzed by gel permeation chromatography (GPC), 31 P NMR and 2D-HSQC-NMR methods. The results indicate that the system can gain a high cellulose recovery of 92.99% along with a lignin removal of 95.33%, and recovered lignin has low lignin carbohydrate complexes, low condensation, and rich in phenolic hydroxyl groups for 1.95 mmol/g. Meanwhile, the countercurrent pretreatment system can effectively reduce the deposition of lignin on the cellulose surface, which is evidently superior to the non-countercurrent pretreatment and facilitates the efficiency of enzymatic saccharification of substrate, achieving a high glucose yield of 99% as well as a total sugar yield of 91.11%. The method efficiently separates biomass in a green manner, and solid residues are easily hydrolyzed, showing potential for industrial-scale production.

09 BIOMASS FUELS↗

Human in vitro metabolism of an environmental mixture of polycyclic aromatic hydrocarbons (PAH) found at the Portland Harbor Superfund Site

Polycyclic aromatic hydrocarbons (PAHs) are widespread environmental contaminants that pose health risks to humans. Toxicity testing approaches of PAHs have evolved from traditional rodent models to New Approach Methodologies (NAMs), such as high-throughput screening in zebrafish, enabling rapid evaluation of chemical hazards. However, translating toxicity findings from laboratory systems to humans remains difficult due to complexity and species-specific differences. Chemical dosimetry modeling offers a quantitative framework to bridge this gap, but its accuracy depends on robust knowledge of PAH metabolism. The objective of this study was to measure human metabolism rates of Supermix-10, the ten most abundant PAHs found at the Portland Harbor Superfund Site, to support development of human pharmacokinetic models. We incubated individual PAHs from Supermix-10 in pooled human liver microsomes and quantified parent PAH disappearance using high-performance liquid chromatography (HPLC) with UV and florescent detection. To assess the potential of mixture interactions, we also measured metabolism of all 10 compounds in an equimolar mixture and compared rates of parent disappearance to those observed for individual PAHs. All Supermix-10 PAHs demonstrated rapid parent compound disappearance in human hepatic microsomes. PAHs grouped into three metabolism patterns: high metabolism rates and capacity (2-methylnaphthalene, acenaphthylene, fluorene, naphthalene), high affinity metabolism that rapidly achieves low-level saturation (benzo[a]anthracene, chrysene), and moderate metabolism rates and capacity (fluoranthene, pyrene, retene, phenanthrene). Smaller PAHs exhibited faster metabolism, and higher metabolism rates correlated inversely with molecular weight. When incubated in an equimolar mixture, Supermix-10 demonstrated significantly slower metabolism (47–89 %) compared to metabolism of individual PAHs at the same concentration. These findings enhance our understanding of PAH metabolism in humans and demonstrate significant mixture interactions under the conditions tested. Furthermore, our findings offer insights into the metabolic behavior of Supermix-10 and provide critical metabolism rate data to support the development of physiological based pharmacokinetic (PBPK) models. Dosimetry models can translate PAH chemical dosimetry from high-throughput testing platforms, like zebrafish and cellular system assays, to human exposures enhancing the accuracy and reliability of PAH risk assessments.

2-methylnaphthalene↗

Batch Scale Production of 3D Printed Extraction Sorbents Using a Low-Cost Modification to a Desktop Printer

This study reports a simple modification to a commercial resin 3D printer that significantly reduces the amount of prepolymer material needed for the production of extraction sorbents. Here, the modified printing platform is demonstrated in the printing of two imidazolium-based ionic liquid (IL) monomers. Two geometries resembling a blade-type polymeric ionic liquid (PIL) sorbent used in thin-film microextraction and a fiber-type sorbent used in solid-phase microextraction (SPME) were printed. The SPME PIL sorbents were used to extract 10 organic contaminants, including plasticizers, antimicrobial agents, UV filters, and pesticides, from water followed by high-performance liquid chromatographic (HPLC) analysis. To compare the extraction performance of the SPME sorbents, seven fibers printed with the same prepolymer composition from the same printing batch as well as different batches were evaluated. The results revealed highly reproducible extraction efficiencies for all tested sorbents with no statistical difference in their extraction performance. Method validation showed acceptable linearity ($R$ 2 > 0.92) for all analytes with limits of detection and limits of quantification ranging from 0.13 to 45 μg L –1 and 0.43 to 150 μg L –1 , respectively.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Chemical Diversity of Oligomers in Biomass Fast Pyrolysis Oils, Part 2: Heavy Lignin-Derived Molecules and Highly Dehydrated Sugars from Dichloromethane-Insoluble Pyrolytic Lignin

Here, this paper, the second in a series, investigates the water-insoluble, dichloromethane (DCM)-insoluble residue of BTG pyrolysis oil, also known in the literature as high-molecular-weight pyrolytic lignin (HMW-PL). HMW-PL accounts for 9.2 wt % of the original bio-oil, which is known to increase upon aging and contribute to coke formation during bio-oil upgrading. Understanding its composition is crucial for managing pyrolysis oil during the processing. The HMW-PL was fractionated using a silica gel column with solvents of increasing polarity: ethyl acetate (EA), acetone (AC), isopropanol (ISO), and methanol (MeOH), yielding 49.2, 19.9, 8.2, and 8.1 wt %, respectively. Each subfraction was characterized by UV-fluorescence, FTIR, HSQC NMR, and (−)APCI-FT-Orbitrap MS. Analysis revealed that the EA subfraction primarily contained aromatic dimers (C 19 –C 20 ) and trimers (C 17 –C 13 ), while the MeOH subfraction was rich in oxygenated aliphatic monomers (C 8 –C 16 ) likely derived from sugar dehydration products. The resulting fractions were further separated via preparatory HPLC. Fifty-five candidate molecular structures were proposed based on the Orbitrap MS data, supported by UV-fluorescence, FTIR, and NMR results. This fractionation strategy defined four distinct subfractions, enabling the proposal of surrogate molecular structures and advancing the molecular-level understanding of the HMW-PL fraction in the pyrolysis bio-oil.

High-Molecular-Weight PL↗

Interinstitutional Study of the New EURO-GANEX Process Resistance by Gamma Irradiation Test Loops

As part of the homogeneous actinides recycling strategy, the EURO-GANEX process is one of the most promising options to achieve the goal of minor actinides recovery. However, EURO-GANEX also has various drawbacks that are being addressed. Improvements made to EURO-GANEX system have resulted in the emergence of the so-called New EURO-GANEX process, where the composition of the solvent has been modified by replacing TODGA and DMDOHEMA with cis-mTDDGA in the organic phase and SO3-Ph-BTP with PyTri-Diol in the aqueous phase in order to resolve important issues. The objective of this work is twofold: evaluate the gamma radiolysis resistance of the new EURO-GANEX process by dynamic irradiation conditions simulating the three main steps of the process and validate the design of CIEMAT Náyade, CEA Marcel and INL irradiation loop devices since each of them mimics different aspects of the real process. Náyade and the INL loops could irradiate together the organic and aqueous phases, whereas in the CEA loop, the irradiated solvent is recycled continuously inside a platform with several stages of mixer-settlers containing aqueous flows simulating the three main steps of the process. The extraction performances and changes in the composition of the solvent have been analysed during the irradiation experiment by different techniques: gamma spectrometry and ICP-MS/OES for cations or tracers extraction, and HPLC-MS to quantify the degradation and evaluate the degradation compounds. Additionally, in spite of some differences between the three-irradiation facilities, this inter-institutional study shows that they are three comparative tools, which provide results on the stability towards radiolysis of a liquid-liquid extraction system. Favourable extraction results for the different steps are obtained according to the static irradiation studies found in literature. However, the degradation of cis-mTDDGA is appreciable leading to degradation compounds, some of which form precipitates and produce important changes in viscosity, important aspects that must be addressed prior to the successful industrial application of the new EURO-GANEX process.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

A Third Generation Potentially Bifunctional Trithiol Chelate, Its nat,1XX Sb(III) Complex, and Selective Chelation of Radioantimony ( 119 Sb) from Its Sn Target

The therapeutic potential of the Meitner-Auger- and conversion-electron emitting radionuclide 119 Sb remains unexplored because of the difficulty of incorporating it into biologically targeted compounds. To address this challenge, we report the development of 119 Sb production from electroplated tin cyclotron targets and its complexation by a novel trithiol chelate. Here, the chelation reaction occurs in harsh solvent conditions even in the presence of large quantities of tin, which are necessary for production on small, low energy (16 MeV) cyclotrons. The 119 Sb-trithiol complex has high stability and can be purified by HPLC. The third generation trithiol chelate and the analogous stable nat Sb-trithiol compound were synthesized and characterized, including by single crystal X-ray diffraction analyses.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

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↗

Designing a Block Copolymer Membrane for Selective Transport of Lactic Acid from Aqueous Mixtures

We report the design and synthesis of a triblock copolymer-based membrane for enabling selective transport of lactic acid from aqueous solutions. This is relevant to the production of polylactic acid, one of the few biodegradable and biobased polymers with sufficient mechanical strength for practical applications. The end blocks are positively charged with negatively charged lactate counterions. The middle block is polybutadiene (PBD). Due to microphase separation, the charged blocks form channels for transporting lactic acid. The mechanical integrity of the membrane is controlled by cross-linking the PBD block. Transport of lactic acid and water across the membrane was studied by placing the membrane between two chambers, a feed chamber containing aqueous lactic acid solutions, and a receiving chamber containing pure water. The lactic acid concentration in the receiving chamber was monitored as a function of time using conductivity, HPLC, and NMR. The corresponding flux of water from the receiving chamber to the feed chamber was measured using an NMR-based approach. The lactic acid and water permeabilities through our membrane were (1.12 ± 0.05) × 10–8 and (8.58 ± 0.75) × 10–9 cm2 s–1. To our knowledge, there are no reports of lactic acid permeabilities through any membrane in the literature. The separation factor of our membrane, αLA/water, 1.305 ± 0.123, is comparable to that of membranes used for selective transport of ethanol, despite the fact that lactic acid is a much larger molecule than ethanol. Selective transport of lactic acid in our membrane is governed mainly by differences in solubility; lactic acid is 18 times more soluble in the membrane than water.

Jana, Rounak↗