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At least 361 records · Page 20
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Decomposition of liquid-liquid extraction organic phase structure into critical and pre-peak contributions

Solution nanostructure induced by amphiphile self-association plays an important role in various chemical and physical processes, including liquid-liquid extraction (LLE). Small angle scattering techniques are an essential means of probing this structure, but, due to non-uniqueness of scattering patterns, their interpretation is not trivial. Here, in this study, we decompose small angle x-ray scattering (SAXS) patterns for a range of binary LLE organic phases into two components: Ornstein-Zernike and pre-peak contributions resulting from, respectively, critical concentration fluctuations and packing of the amphiphilic extractant molecules in the nonpolar aliphatic diluent. While we previously applied Ornstein-Zernike scattering models to similar organic phases, including the pre-peak explicitly in the fit allows us to measure weak fluctuations at high extractant concentration and simultaneously obtain information on the position and intensity of the correlation peak related to amphiphile packing. Scattering patterns and partial structure factors calculated from molecular dynamics simulations support this interpretation. We demonstrate how this minimal scattering model describes nanostructuring for a large number of extractant types over their entire extractant/diluent composition ranges, suggesting simple and universal behavior. The straightforward assignment of these structural contributions facilitates the comparison of these features between different classes of extractant molecules and will enable further studies of organic phase aggregation. Applicability to more complex, process-relevant organic phases is illustrated with post-contact organic phases containing significant quantities of extracted lanthanide nitrate salt, which we find are readily described by this model.

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2017

Recovery of zinc and cadmium from spent batteries using Cyphos IL 102 via solvent extraction route and synthesis of Zn and Cd oxide nanoparticles

Highlights: • First time Cyphos IL102 explored for recovery of Zn/Cd from spent batteries. • Recovery of metals with high purity was achieved at room temperature. • Quantitative extraction was achieved in two stages for Zn and Cd. •Loaded organic phases were used to synthesize ZnO and CdO nanoparticles. •Simple strippants for stripping isotherm was used. - Abstract: The overall aim of this study is to separate and recover zinc and cadmium from spent batteries. For this purpose Cyphos IL 102 diluted in toluene was employed for the extraction and recovery of Zn and Cd from Zn-C and Ni-Cd batteries leach liquor. The influence of extractant concentration for the leach liquors of Zn-C (0.01–0.05 mol/L) and Ni-Cd (0.04–0.20 mol/L) batteries has been investigated. Composition of the leach liquor obtained from Zn-C/Ni-Cd spent batteries is Zn - 2.18 g/L, Mn - 4.59 g/L, Fe - 4.0 × 10{sup −3} g/L, Ni - 0.2 × 10{sup −3} g/L/Cd - 4.28 g/L, Ni - 0.896 × 10{sup −1} g/L, Fe - 0.148 g/L, Co - 3.77 × 10{sup −3} g/L, respectively. Two stage counter current extraction at A/O 1:1 and 3:2 with 0.04 mol/L and 0.2 mol/L Cyphos IL 102 for Zn and Cd, respectively provide more than 99.0% extraction of both the metal ions with almost negligible extraction of associated metal ions. A stripping efficiency of around 99.0% for Zn and Cd was obtained at O/A 1:1 using 1.0 mol/L HNO{sub 3} in two and three counter current stages, respectively. ZnO and CdO were also synthesized using the loaded organic phase and characterized using XRD, FE-SEM and EDX techniques. XRD peaks of ZnO and CdO correspond to zincite and monteponite, respectively. The average particle size was ∼27.0 nm and ∼37.0 nm for ZnO and CdO, respectively. The EDX analysis of ZnO and CdO shows almost 1:1 atomic percentage.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2011

Extraction Chromatographic Methods in the Sample Preparation Sequence for Thermal Ionization Mass Spectrometric Analysis of Plutonium Isotopes

A sample preparation sequence for actinide isotopic analysis by TIMS is described that includes column-based extraction chromatography as the first separation step, followed by anion exchange column separations. The sequence is designed to include a wet ashing step after the extraction chromatography to prevent any leached extractant or oxalic acid eluent reagents from interfering with subsequent separations, source preparation, or TIMS ionization. TEVA-resin and DGA-resin materials, containing extractants that consist only of C, N, O, and H atoms, were investigated for isolation of plutonium. Radiotracer level studies confirmed expected high yields from column-based separation procedures. Femtogram-level studies were carried out with TIMS detection, using multiple isotopic spikes through the separation sequence. Pu recoveries were 87% and 86% for TEVA- and DGA-resins separations respectively. The Pu recoveries from 400 {mu}L anion-exchange column separations were 89% and 93% for trial sequences incorporating TEVA and DGA-resin. Thus, a prior extraction chromatography step in the sequence did not interfere with the subsequent anion exchange separation when a simple wet ash step was carried out in between these column separations. The average measurement efficiency, for Pu, encompassing the chemical separation recoveries and the TIMS ionization efficiency, was 2.73 {+-} 0.77% (2-sigma) for the DGA-resin trials and 2.67 {+-} 0.54% for the TEVA-resin trials, compared to 3.41% and 2.37% (average 2.89%) for two spikes in the experimental set. These compare with an average measurement efficiency of 2.78 {+-} 1.70%, n = 33 from process benchmark analyses using Pu spikes processed through a sequence of oxalate precipitation, wet ash, iron hydroxide precipitation, and anion exchange column separations. We conclude that extraction chromatography can be a viable separation procedure as part of a multistep sequence for TIMS sample preparation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Confocal Raman Microscopy for in Situ Detection of Solid-Phase Extraction of Pyrene into Single C 18 –Silica Particles

Solid-phase extraction (SPE) is a well known method for separating and pre concentrating analytes prior to ex-situ detection and quantification. Despite advances in miniaturization of solid-phase extraction, the technique has not evolved to meet the needs for detection in small scale microfluidic devices. While successful efforts have led to smaller scale extractors that allow preconcentration from small volumes, detection within correspondingly small volumes has remained out of reach because of analyte dilution during a post extraction transfer or “wash off” step prior to detection. In this work, successful extraction into sub-picoliter collection volumes is accomplished by using a single chromatographic particle as an extractor; wash off dilution is totally avoided by using confocal Raman microscopy for in-situ detection within the single-particle collection phase. Specifically, micromolar concentrations of pyrene in methanol water solution were equilibrated with an individual C 18 -functionalized silica particle, and Raman spectra were acquired from a small confocal sampling volume (~1 fL) within the particle interior. By comparing the Raman scattering intensity of the pyrene with that of the C 18 -chains in the stationary phase, it was possible to quantify the equilibrium coverage of pyrene relative to the C 18 chains. Spectroscopic isotherms were measured to determine the saturation surface coverage of pyrene relative to C 18 -chains and to study how the preconcentration equilibrium can be controlled by the source-phase solution composition. For extraction from aqueous solutions having the lowest methanol concentration (5% by volume), the preconcentration factor for pyrene into the particle was found to be 4.8 (±0.8) × 10 4 , which allowed detection of pyrene extracted from a 10 nM solution into a 0.52-pL particle volume.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Toward Lithium Recovery Using Modular (and Membraneless) Phase Separation and Extraction (MPSE) Technology with Ionic Liquid (IL) Solvents: Effect of Coatings

In this work, a single-channel slope-plate Modular and Membrane-less Phase Separation and Extraction (MPSE) device was fabricated using 3D printing. The slope-plate was designed with an insertable glass slide to enable surface modification with coatings. Self-assembled monolayers (SAMs) and perfluoropolyether (Zdol) coatings were applied to tailor surface wettability and enhance phase separation. Using a model biphasic system of water and hexadecane, both coatings significantly improved the separation efficiency compared to the uncoated device by promoting selective wetting. Building on these results, lithium extraction from a simulated saline solution was investigated using 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([EMIM][NTf₂]) as the ionic liquid (IL) extractant. The IL effectively extracted Li⁺ from the aqueous phase in bulk extraction, demonstrating its potential for lithium recovery. However, the low interfacial tension between the IL and aqueous phases posed challenges for phase separation. The application of SAM and Zdol coatings effectively mitigated this issue. Overall, integrating tailored surface chemistry with the slope-plate MPSE design shows great promise as an efficient and scalable platform for studying liquid–liquid separation and optimizing ionic liquid–based extraction processes for lithium recovery from saline sources.

3D printing↗
DOE OSTI2022

Temperature-Dependent Carrier Extraction and the Effects of Excitons on Emission and Photovoltaic Performance in Cs0.05FA0.79MA0.16Pb(I0.83Br0.17)3 Solar Cells

The photovoltaic parameters of triple cation perovskite [Cs0.05FA0.79MA0.16Pb(I0.83Br0.17)3] solar cells are investigated focusing on the electro-optical properties and differences in performance at low and high temperatures. The signature of a parasitic barrier to carrier extraction is observed at low temperatures, which results in a loss of performance at T < 200 K. Intensity-dependent measurements indicate extraction across this parasitic interface is limited by a combination of the exciton binding energy and thermionic emission. However, the photovoltaic performance of the device is recovered at low intensity - where the photocarrier generation rate threshold is lower than the thermionic extraction rate. Loss of solar cell performance is also observed to be strongly correlated to an increase in photoluminescence intensity, indicating inhibited carrier extraction results in strong radiative recombination and that these systems do not appear to be limited by significant thermally activated non-radiative processes. Evidence of limited carrier extraction due to excitonic effects is also observed with a strong anti-correlation in photoluminescence and carrier extraction observed at lower temperatures.

barrier↗
DOE OSTI2026

Efficient Low-Temperature Direct Lithium Extraction from Chloride Brines Enabled by High-Capacity Sorbent

The demand for lithium, a key component in rechargeable batteries for electric vehicles and renewable energy storage systems, has surged in recent years. Meeting this demand requires efficient extraction methods that are both environmentally friendly and economically viable. This study investigates the utilization of the high-capacity sorbent amorphous aluminum hydroxide for enabling efficient direct lithium extraction at low temperatures. Traditional extraction methods often involve acid-leaching and energy-intensive processes that are not only expensive but also environmentally taxing. In contrast, our approach leverages the exceptional sorption properties of amorphous aluminum hydroxide to facilitate lithium extraction directly from brine, achieving extraction efficiencies of 94.4% in case 1 and 96.2% in case 2 at low temperatures. Kinetic modeling using the Avrami–Erofe’ev framework reveals a nucleation-growth mechanism ( n = 0.71, k = 0.131 h –1 ), providing quantitative insights into the solid-state phase transformation process. This method significantly reduces energy consumption and minimizes the environmental footprint. Through systematic experimentation and optimization, we demonstrate the effectiveness and scalability of our approach, highlighting its potential to revolutionize lithium extraction processes. Our findings highlight the potential of high-capacity sorbents, particularly amorphous aluminum hydroxide toward sustainable lithium production, contributing to the advancement of clean-energy technologies.

anions↗
DOE OSTI2021

Technoeconomic Assessment of a Sequential Step-Leaching Process for Rare Earth Element Extraction from Acid Mine Drainage Precipitates

Herein, Coal waste products have been studied as a new source of Rare Earth Elements (REEs) and other Critical Minerals (CM) essential for the development of renewable energy technologies, but the economic viability of these source materials is not well understood. This paper examines the technoeconomic performance of a novel process for rare earth element extraction from acid mine drainage precipitates (AMDp) in the Appalachian Coal Basin. The three phase extraction process includes excavation and transportation of AMDp, multi-phase pH driven step-leaching of REEs at ambient conditions, and commercial solvent extraction to produce a saleable grade rare earth oxide material that can be reduced to a pure metal. We estimate the life-cycle cost of bench-scale extraction of REEs from two representative Appalachian AMDp feedstock chemistries at between 4000 – 6000 $/kg of mixed REE concentrate produced. Both the AMDp composition and process parameters affect the profitability of REE extraction, with the REE concentration and distribution of REE in the feedstock, extraction and precipitation reagent consumption rates, and the potential for reagent recycling as the key variables. Economically profitable valorization of REE from AMDp will require a combination of continued process innovation and sizable financial incentives to substantially influence domestic supply of REEs.

36 MATERIALS SCIENCE↗
DOE OSTI2024

An Explainable Classification Framework for Determining and Understanding the Suitability of Solvent Extraction for Bioproduct Recovery

Lignocellulosic biomass is an abundant feedstock for producing sustainable fuels and chemicals. However, a key challenge in most biomass utilization strategies is the recovery of products from a dilute, typically aqueous, phase. In this respect, liquid–liquid extraction, which relies on a solvent to transfer a product of interest from one liquid phase to another (solvent-rich) phase, is a technology that can reduce the energy requirements for product recovery. To reduce solvent consumption, liquid–liquid extraction needs to be combined with another separation method (e.g., distillation) to recycle the solvent. Despite the research on solvent extraction, there are limited system-wide methods that allow us to determine when extraction is well suited to carry out a specific separation. Accordingly, we present a classification framework to predict whether extraction, coupled with distillation, is feasible and more economical than distillation. Our framework is based on features such as feed composition, liquid–liquid equilibrium constants, relative volatilities, and solvent price, and leads to trained classifiers that show good prediction accuracy. We further study how specific features influence the suitability of extraction. Furthermore, to showcase the applicability of the framework, we use it to analyze the separation of acetic acid from water.

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

Cell Extracts from Bacteria and Yeast Retain Metabolic Activity after Extended Storage and Repeated Thawing

Cell-free synthetic biology enables rapid prototyping of biological parts and synthesis of proteins or metabolites in the absence of cell growth constraints. Cell-free systems are frequently made from crude cell extracts, where composition and activity can vary significantly based on source strain, preparation and processing, reagents, and other considerations. This variability can cause extracts to be treated as black boxes for which empirical observations guide practical laboratory practices, including a hesitance to use dated or previously thawed extracts. To better understand the robustness of cell extracts over time, we assessed the activity of cell-free metabolism during storage. As a model, we studied conversion of glucose to 2,3-butanediol. We found that cell extracts from Escherichia coli and Saccharomyces cerevisiae subjected to an 18-month storage period and repeated freeze-thaw cycles retain consistent metabolic activity. Here this work gives users of cell-free systems a better understanding of the impacts of storage on extract behavior.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2016

Efficient Charge Extraction and Slow Recombination in Organic-Inorganic Perovskites Capped with Semiconducting Single-Walled Carbon Nanotubes

Metal-halide based perovskite solar cells have rapidly emerged as a promising alternative to traditional inorganic and thin-film photovoltaics. Although charge transport layers are used on either side of perovskite absorber layers to extract photogenerated electrons and holes, the time scales for charge extraction and recombination are poorly understood. Ideal charge transport layers should facilitate large discrepancies between charge extraction and recombination rates. Here, we demonstrate that highly enriched semiconducting single-walled carbon nanotube (SWCNT) films enable rapid (sub-picosecond) hole extraction from a prototypical perovskite absorber layer and extremely slow back-transfer and recombination (hundreds of microseconds). The energetically narrow and distinct spectroscopic signatures for charges within these SWCNT thin films enables the unambiguous temporal tracking of each charge carrier with time-resolved spectroscopies covering many decades of time. The efficient hole extraction by the SWCNT layer also improves electron extraction by the compact titanium dioxide electron transport layer, which should reduce charge accumulation at each critical interface. Finally, we demonstrate that the use of thin interface layers of semiconducting single-walled carbon nanotubes between the perovskite absorber layer and a prototypical hole transport layer improves device efficiency and stability, and reduces hysteresis.

14 SOLAR ENERGY↗
DOE OSTI2019

Online supercritical fluid extraction mass spectrometry (SFE-LC-FTMS) for sensitive characterization of soil organic matter

We report a novel technical approach for subcritical fluid extraction (SFE) for organic matter characterization in complex matrices such as soil. The custom platform combines on-line SFE with micro-solid phase extraction, nano liquid chromatography (LC), electrospray ionization and Fourier transform mass spectrometry (SFE-LC-FTMS). We demonstrated the utility of SFE-LC-FTMS, including results from both Orbitrap and FTICR MS, for analysis of complex mixtures of organic compounds in a solid matrix by characterizing soil organic matter in peat, a high-carbon soil. For example, in a single experiment, >6000 molecular formulas can be assigned based upon FTICR MS data from 1–50 μL of soil samples (roughly 1–50 mg of soil, dependent on soil density), nearly twice that typically obtained from direct infusion liquid solvent extraction (LSE) from an order of magnitude larger volume of the same soil. The detected species consisted predominately of lipid-like, lignin-like and protein-like compounds, based on their O/C and H/C ratios, with predominantly CHO and CHONP molecular compositions. These results clearly demonstrate that SFE has the potential to effectively extract a variety of molecular species and could become an important member of a suite of extraction methods for studying SOM and other natural organic matter. This is especially true when comprehensive coverage, minimal sample volumes, and high sensitivity are required, or when the presence of organic solvent residue in residual soil is problematic. Lastly, the SFE based extraction protocol could potentially enable spatially resolved characterization of organic matter in soil with a resolution of ~1 mm3 to facilitate studies probing the spatial heterogeneity of soil.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2024

Volatile fatty acid extraction from fermentation broth using a hydrophobic ionic liquid and in situ enzymatic esterification

Efficient recovery of volatile fatty acids (VFAs) from fermentation broth is a challenge due to low VFA titers and thus limits the commercialization of VFA production using biological routes. Liquid–liquid extraction using hydrophobic ionic liquids (ILs) shows great promise for the extraction and esterification of hydrophilic VFAs. In this study, several ILs were evaluated to select a water-immiscible and efficient extraction solvent. The selected IL, trihexyltetradecyl phosphonium dibutylphosphate ([P 666,14 ][DBP]), gave a cumulative VFA extraction of around 842.8 mg per g IL. The predicted excess enthalpy (H E ) and logarithmic activity coefficients ln(γ) using the COSMO-RS model were validated with the experimentally obtained VFA recovery from fermentation broth. To understand the extraction mechanism of VFAs, quantum theory of atoms in molecules (QTAIM) and noncovalent interaction (NCI) were performed. The results suggest that long chain fatty acids exhibit strong van der Waals interaction with the DBP anion leading to higher VFA extraction. The enzymatic esterification of VFAs with ethanol in [P 666,14 ][DBP] was optimized using the Box–Behnken response surface design of experiment. Under the optimized conditions, up to 83.7% of hexanoic acid was converted to ethyl esters, while other shorter chain VFAs have lower conversion efficiency (38.3–63.2%).

09 BIOMASS FUELS↗
DOE OSTI2012

A new extraction system for the Linac4 H{sup -}ion source

As part of the CERN accelerator complex upgrade, a new linear accelerator for H{sup -} (Linac4) is under construction. The ion source design is based on the non-caesiated DESY RF-driven ion source, with the goal of producing an H{sup -} beam of 80 mA beam current, 45 keV beam energy, 0.4 ms pulse length, and 2 Hz repetition rate. The source has been successfully commissioned for an extraction voltage of 35 kV, corresponding to the one used at DESY. Increasing the extraction voltage to 45 kV has resulted in frequent high voltage breakdowns in the extraction region caused by evaporating material from the electron dump, triggering a new design of the extraction and electron dumping system. Results of the ion source commissioning at 35 kV are presented as well as simulations of a new pulsed extraction system for beam extraction at 45 kV.

43 PARTICLE ACCELERATORS↗
DOE OSTI2012

Spatial distribution of the charged particles and potentials during beam extraction in a negative-ion source

We report on the characteristics of the electronegative plasma in a large-scale hydrogen negative ion (H{sup -}) source. The measurement has been made with a time-resolved Langmuir probe installed in the beam extraction region. The H{sup -} density is monitored with a cavity ring-down system to identify the electrons in the negative charges. The electron-saturation current decreases rapidly after starting to seed Cs, and ion-ion plasma is observed in the extraction region. The H{sup -} density steps down during the beam extraction and the electron density jumps up correspondingly. The time integral of the decreasing H{sup -} charge density agrees well with the electron charge collected with the probe. The agreement of the charges is interpreted to indicate that the H{sup -} density decreasing at the beam extraction is compensated by the electrons diffusing from the driver region. In the plasmas with very low electron density, the pre-sheath of the extraction field penetrates deeply inside the plasmas. That is because the shielding length in those plasmas is longer than that in the usual electron-ion plasmas, and furthermore the electrons are suppressed to diffuse to the extraction region due to the strong magnetic field.

43 PARTICLE ACCELERATORS↗
DOE OSTI2012

Wave frequency dependence of H{sup -} ion production and extraction in a transformer coupled plasma H{sup -} ion source at SNU

The effect of rf wave frequencies on the production of H{sup -} ion is investigated in a transformer coupled plasma H{sup -} ion source at Seoul National University. A Langmuir probe is installed to measure the plasma density and temperature, and these plasma parameters are correlated to the extracted H{sup -} beam currents at various frequencies. The Langmuir probe is also used to measure the density of H{sup -} ions at the ion source by generating photodetachment with an Nd:YAG laser. The extracted H{sup -} currents decrease to a minimum value until 13 MHz and then, increase as the driving frequency increases from 13 MHz while the relative H{sup -} population measured by photodetachment monotonically decreases as the driving rf frequency increases from 11 MHz to 15 MHz. A potential well formed at the extraction region at high frequencies of more than 13 MHz is considered responsible for the increased H{sup -} beam extraction even with a lower photodetachment signal. The variation in the driving rf frequency not only affects the density and temperature of the plasma but also modifies the plasma potential with the existence of a filtering magnetic field and consequently, influences the extracted H{sup -} current through the extraction as well as formation of H{sup -} ions.

43 PARTICLE ACCELERATORS↗
DOE OSTI2014

Computational study of ion beam extraction phenomena through multiple apertures

The process of ion extraction through multiple apertures is investigated using a two-dimensional particle-in-cell code. We consider apertures with a fixed diameter with a hydrogen plasma background, and the trajectories of electrons, H{sup +} and H{sub 2}{sup +} ions in the self-consistently calculated electric field are traced. The focus of this work is the fundamental physics of the ion extraction, and not particular to a specific device. The computed convergence and divergence of the extracted ion beam are analyzed. We find that the extracted ion flux reaching the extraction electrode is non-uniform, and the peak flux positions change according to operational parameters, and do not necessarily match the positions of the apertures in the y-direction. The profile of the ion flux reaching the electrode is mainly affected by the bias voltage and the distance between grid wall and extraction electrode.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2015

Electron-less negative ion extraction from ion-ion plasmas

This paper presents experimental results showing that continuous negative ion extraction, without co-extracted electrons, is possible from highly electronegative SF{sub 6} ion-ion plasma at low gas pressure (1 mTorr). The ratio between the negative ion and electron densities is more than 3000 in the vicinity of the two-grid extraction and acceleration system. The measurements are conducted by both magnetized and non-magnetized energy analyzers attached to the external grid. With these two analyzers, we show that the extracted negative ion flux is almost electron-free and has the same magnitude as the positive ion flux extracted and accelerated when the grids are biased oppositely. The results presented here can be used for validation of numerical and analytical models of ion extraction from ion-ion plasma.

74 ATOMIC AND MOLECULAR PHYSICS↗