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All sourcesNASA NTRSDOE OSTI
NASA NTRS1985

Properties of silicon suspensions and slip-cast bodies

The effect of varying pH, sonication times, and solid loading of silicon powder suspensions on the properties of powder/water suspensions and on the resulting pore characteristics of slip-cast bodies was studied. Aqueous suspensions of ground an aged silicon powder (of 0.3 micron median Stokes diameter and containing 1.3 vol pct Fe2O3 powder) were prepared, with solids loading in the range of 30-56 vol pct, and were adjusted to varying pH values by addition of either HCl or NH4OH or NaOH. Suspension aliquots were sonicated for 0, 15, 30, or 60 min. Suspensions were characterized by zeta potentials, ionic strength, and viscosity. Pore characteristics of cast bodies were determined by mercury porosimetry. It was found that intermediate pH values (pH 7-9), long sonication (60 min), and high solid loadings (56 vol pct) produced samples with highest green densities and smallest median pore radius.

Sacks, M. D.↗
DOE OSTI2020

Study of an Unrefined Humate Solution as a Possible Attenuation-based Remedy for Uranium Contamination in Acidic Groundwater - 20351

The Savannah River Site (SRS), joined the environmental cleanup program in 1981 after the Cold War, and was designated as a hazardous waste management facility. About 1.8 billion gallons of acid wastes were disposed into the F/H Area Seepage Basin that included many radionuclides and dissolved metals, resulting in highly contaminated groundwater plumes with pH of 3 - 5.5. The acidity of the plumes contributes to the mobility of several constituents of concern (COC) such as H-3, U-238, I-129, and Sr-90 for the F-Area plume and H-3, Sr-90 and mercury for the H-Area plume. An active treatment (pump-and-treat and re-injection) system was constructed and put in place in 1997 to address the removal of metals and radionuclides from the contaminated groundwater. As remediation projects advanced, active treatments were transitioned to more passive or enhanced-passive approaches such as the subsurface barrier with base injection system, which has been controlling the mobility of contaminants. However, new and more efficient attenuation-based remedies are always sought. Several studies have proposed that humic substances can be used to remediate sites contaminated with heavy metals by creating a permeable reactive barrier. Humic substances (HS) are major components of soil organic matter. HS are polyfunctional organic macromolecules formed by the chemo-microbiological decomposition of biomass or dead organic matter. These substances are usually divided into three main fractions: humin (insoluble at all pH values), humic acid (soluble at pH greater than 3.5), and fulvic acid (soluble at all pH values). Humic substances are major components of the soil at SRS and, in addition, are also helpful in the removal process of uranium. This research focuses on uranium (VI), which is a key contaminant of concern in the F-Area groundwater plume. The interaction of uranium with sediment in the presence or absence of humic substances involves complex mechanisms that are not yet well understood. The interaction of U(VI) with humic substances can affect the adsorption of U on sediment, altering its mobility in the subsurface. The objective of this study is to study the mobility of uranium in the presence of humic acid and to determine if sediments amended by humic acid can enhance the sorption of heavy metals onto sediments. In this research, experiments were conducted using background (clean) F-Area aquifer sediments to understand and predict uranium mobility. A blended material, humate, containing both humic and fulvic acids and a chemically modified humate (KW15 modified humic or mod-HA) was studied as a possible amendment for uranium remediation in SRS groundwater. Batch experiments were conducted in triplicates using 20 ml of aqueous suspension in DI water containing SRS sediment and mod-HA and studied the effect of pH, kinetics of humate sorption onto SRS sediment and also studied the sorption of uranium onto mod-HA amended SRS sediment. Results indicate that mod-HA amended sediment increases uranium removal significantly. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2013

Adsorption of Cu(II) on Oxidized Multi-Walled Carbon Nanotubes in the Presence of Hydroxylated and Carboxylated Fullerenes

The adsorption of Cu(II) on oxidized multi-walled carbon nanotubes (oMWCNTs) as a function of contact time, pH, ionic strength, temperature, and hydroxylated fullerene (C 60 (OH) n ) and carboxylated fullerene (C 60 (C(COOH) 2 ) n ) were studied under ambient conditions using batch techniques. The results showed that the adsorption of Cu(II) had rapidly reached equilibrium and the kinetic process was well described by a pseudo-second-order rate model. Cu(II) adsorption on oMWCNTs was dependent on pH but independent of ionic strength. Compared with the Freundlich model, the Langmuir model was more suitable for analyzing the adsorption isotherms. The thermodynamic parameters calculated from temperature-dependent adsorption isotherms suggested that Cu(II) adsorption on oMWCNTs was spontaneous and endothermic. The effect of C 60 (OH) n on Cu(II) adsorption of oMWCNTs was not significant at low C 60 (OH) n concentration, whereas a negative effect was observed at higher concentration. The adsorption of Cu(II) on oMWCNTs was enhanced with increasing pH values at pH < 5, but decreased at pH ≥ 5. The presence of C 60 (C(COOH) 2 ) n inhibited the adsorption of Cu(II) onto oMWCNTs at pH 4–6. The double sorption site model was applied to simulate the adsorption isotherms of Cu(II) in the presence of C 60 (OH) n and fitted the experimental data well.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2020

Flowthrough Pretreatment of Softwood under Water-only and Alkali Conditions

Flowthrough pretreatment provides valuable insight in the fundamentals of deconstruction of plant biomass. In this study, the potential softwood degradation pathways under water-only and alkali conditions were determined by elucidating the deconstructed biomass-derived products at 0-270 °C for 2-10 min at a flow rate of 25 mL/min with water-only or alkaline at initial pH of 8, 9, 11, and 12, respectively. Results indicated that the initial pH value was a convenient indicator along with the severity parameter to control biomass degradation through the non-oxidative (pH<9) and oxidative (pH=9) pathways. Up to 100 % of hemi-sugars, 90 % of cellulose, and 70 % of lignin were derived from softwood under non-oxidative conditions at severity parameter LogR0 around 5.5, respectively. On the contrary, at pH 12, the oxidative degradation resulted in pretreated hydrolysate rich in monomeric and oligomeric phenolic products as well as glycolic acid, acetic acid, and formic acid from carbohydrates. The two dimensional 1H-13C heteronuclear single quantum coherence (HSQC) nuclear magnetic resonance (NMR) analysis revealed that non-oxidative degradation at initial pH values lower than 9 mainly cleaved ß-O-4, all of the ß-ß, and ß-5/a-O-4 linkages, whereas substantial aromatic ring structures with limited ß-O-4 structures remaining at pH 12 through oxidative degradation.

Zhang, Libing↗
DOE OSTI2019

Development of New Antifoam for High Level Waste Processing in DWPF

During processing in the Defense Waste Processing Facility (DWPF), the evaporation of sludge leads to large amounts of foaming. This foaming can cause a foam-over, which contaminates other parts of the facility, most importantly the condensate. Currently, the antifoam being used is not sufficient at more extreme pH values and relatively high concentrations are required to minimize foaming. This means that a foam-over is more likely in parts of the process where the pH moves away from the neutral point and antifoam is needed in large quantities to prevent such occurrences. Adding this antifoam can also double processing time. The current antifoam also degrades into flammable byproducts, which creates a hazard in the processing. There are two main ideas proposed in order to solve the problems with the current antifoam: A new antifoam; A mechanical solution (sprays, agitator, etc). The focus of this summer was to develop a new antifoam that works across a broader range of pH values, can be added in lower concentrations, and does not degrade into flammable byproducts. This solution was pursued by obtaining different superspreaders and antifoams from companies across the country in order to perform a series of tests on them; these tests include superspreader testing, Foamscan testing, boiling testing, and Sludge Receipt and Adjustment Tank (SRAT) and Slurry Mix Evaporator (SME) process testing. To begin testing, four different superspreaders were tested on their ability to spread. The four superspreaders include: Y-17112, Y-17309, Antifoam 747 (the old antifoam), and Silwet L77 (the main component in Antifoam 747). These superspreaders were tested across a range of pH values and concentrations from 100 ppm to 5000 ppm. After completion of the tests, the results indicated that Y-17112 spread across a wider pH range than the others, even at lower concentrations. This is ideal for developing a new antifoam, as the pH throughout processing in DWPF varies and the lower the necessary concentration, the less antifoam that must be added per cycle. In order to test whether or not the superspreaders work as an antifoam, they have to be tested on real foam. In order to test this, a foamy simulant similar to the foaminess of the sludge in DWPF needed to be developed. This required testing many different sludges and designing our own simulant with different concentrations of insoluble solids. Eventually, a simulant similar enough to what is seen in DWPF was identified. Each superspreader will be tested on the simulant at different pH values and at different concentrations. The simulant will be allowed to foam and small amounts of the superspreader will be added while the Foamscan software tracks the height of the foam column; this allows us to know if the superspreader decreased the foam or not. Next, boiling testing in the Foamscan will be completed. This is testing identical to the Foamscan testing at room temperature, only at boiling conditions similar to DWPF. After boiling testing, the superspreader that is deemed most successful will be tested in a real, scaled-down SRAT/SME cycle. This will ensure it works with all the real chemicals that are added in DWPF and that it will remain successful in all the conditions that it may face. After the SRAT/SME testing, a decision will be made on whether or not the superspreader is successful and it may or may not be chosen as the new antifoam for DWPF.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2018

Impact of pH and urea content on size and luminescence of upconverting Y2O3:Yb, Er nanophosphors

Highlights: • The granula size, morphology and upconversion luminescence of Y{sub 2}O{sub 3}:Yb{sup 3+}, Er{sup 3+} nanophosphors was tuned via altering the pH values and urea contents. • Steady state and transient spectroscopy along with FTIR analysis are performed to clarify the insight photophysical mechanism. • Nonradiative transition probability modulation due to the OH{sup −} group variation could be responsible for improved R/G intensity ratio. - Abstract: The pH value and urea concentration of precursor dramatically impact on the particle size, morphology and upconversion luminescence of Y{sub 2}O{sub 3}:Yb{sup 3+} , Er{sup 3+} nanophosphors. The lower pH leads to the smaller granula size of the final product, for instance, the crystalline size reduces from ∼30 nm to ∼16 nm as pH value varies from 9.3 to 6.7. The intensity of green (2H11/2, 4S3/2 → 4I15/2) and red emission (4F9/2 → 4I15/2) can be effectively and readily tuned by adjusting the pH value and urea content of precursor solution. The sample derived at pH of 6.7 and urea content of 384 mg/mL exhibits the highest red to green ratio, as a result of more surface defects and hydroxyl residues. Besides, the upconversion lifetime investigation further proved that the quenching and nonradiative relaxation from 2H11/2 and 4S3/2 to 4F9/2 caused by the surface defects could be responsible for the relative enhancement of the red emission.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2011

Influence of the precipitation pH on the compositions and properties of Bi-based oxyiodide photocatalysts

Graphical abstract: A series of Bi-based oxyiodide photocatalysts with different compositions were synthesized via a precipitation-filtration process followed by hydrothermal treatment. The effects of the precipitation pH values on the compositions and photocatalytic activities of the bismuth oxyiodides were investigated. Research highlights: {yields} BiOI, Bi{sub 4}O{sub 5}I{sub 2}, Bi{sub 7}O{sub 9}I{sub 3} and Bi{sub 5}O{sub 7}I were obtained via a precipitation-filtration process followed by hydrothermal treatment. {yields} The compositions of the bismuth oxyiodides could be controlled by adjusting the precipitation pH values. {yields} All the bismuth oxyiodides exhibit photocatalytic activity on decomposing methyl orange. -- Abstract: A series of Bi-based oxyiodide photocatalysts with different compositions were synthesized via a precipitation-filtration process followed by hydrothermal treatment. The compositions of the bismuth oxyiodides could be controlled by adjusting the precipitation pH values. The effects of the precipitation pH values on the compositions and photocatalytic activities of the bismuth oxyiodides were investigated and the relationship between structure and photocatalytic property is discussed. All the as-prepared powders exhibit photocatalytic activity on decomposing methyl orange under visible light irradiation. The activity increases with increasing content of iodine in the bismuth oxyiodides.

36 MATERIALS SCIENCE↗
NASA NTRS1994

Computation of iodine species concentrations in water

During an evaluation of the use of iodine as a water disinfectant and the development of methods for measuring various iodine species in water onboard Space Freedom, it became necessary to compute the concentration of the various species based on equilibrium principles alone. Of particular concern was the case when various amounts of iodine, iodide, strong acid, and strong base are added to water. Such solutions can be used to evaluate the performance of various monitoring methods being considered. The authors of this paper present an overview of aqueous iodine chemistry, a set of nonlinear equations which can be used to model the above case, and a computer program for solving this system of equations using the Newton-Raphson method. The program was validated by comparing results over a range of concentrations and pH values with those previously presented by Gottardi for a given pH. Use of this program indicated that there are multiple roots to many cases and selecting an appropriate initial guess is important. Comparison of program results with laboratory results for the case when only iodine is added to water indicates the program gives high pH values for the iodine concentrations normally used for water disinfection. Extending the model to include the effects of iodate formation results in the computer pH values being closer to those observed, but the model with iodate does not agree well for the case in which base is added in addition to iodine to raise the pH. Potential explanations include failure to obtain equilibrium conditions in the lab, inaccuracies in published values for the equilibrium constants, and inadequate model of iodine chemistry and/or the lack of adequate analytical methods for measuring the various iodine species in water.

Schultz, John R.↗
DOE OSTI2011

Small-Angle Neutron Scattering Reveals pH-Dependent Conformational Changes in Trichoderma reesei Cellobiohydrolase I: Implications for Enzymatic Activity

Cellobiohydrolase I (Cel7A) of the fungus Trichoderma reesei (now classified as an anamorph of Hypocrea jecorina) hydrolyzes crystalline cellulose to soluble sugars, making it of key interest for producing fermentable sugars from biomass for biofuel production. The activity of the enzyme is pH-dependent, with its highest activity occurring at pH 4 5. To probe the response of the solution structure of Cel7A to changes in pH, we measured small angle neutron scattering of it in a series of solutions having pH values of 7.0, 6.0, 5.3, and 4.2. As the pH decreases from 7.0 to 5.3, the enzyme structure remains well defined, possessing a spatial differentiation between the cellulose binding domain and the catalytic core that only changes subtly. At pH 4.2, the solution conformation of the enzyme changes to a structure that is intermediate between a properly folded enzyme and a denatured, unfolded state, yet the secondary structure of the enzyme is essentially unaltered. The results indicate that at the pH of optimal activity, the catalytic core of the enzyme adopts a structure in which the compact packing typical of a fully folded polypeptide chain is disrupted and suggest that the increased range of structures afforded by this disordered state plays an important role in the increased activity of Cel7A through conformational selection.

09 BIOMASS FUELS↗
DOE OSTI2013

Investigation of thermal treatment on selective separation of post consumer plastics prior to froth flotation

Highlights: • Both PET and PVC have nearly the same densities. • The best pH value will be 4 for optimizing pH values. • Malic acid gave the best results for selective separation of PET and PVC. - Abstract: Plastics have become the widely used materials because of their advantages, such as cheapness, endurance, lightness, and hygiene. However, they cause waste and soil pollution and they do not easily decompose. Many promising technologies are being investigated for separating mixed thermoplastics, but they are still uneconomical and unreliable. Depending on their surface characteristics, these plastics can be separated from each other by flotation method which is useful mineral processing technique with its low cost and simplicity. The main objective of this study is to investigate the flotation characteristics of PET and PVC and determine the effect of plasticizer reagents on efficient plastic separation. For that purpose, various parameters such as pH, plasticizer concentration, plasticizer type, conditioning temperature and thermal conditioning were investigated. As a result, PET particles were floated with 95.1% purity and 65.3% efficiency while PVC particles were obtained with 98.1% purity and 65.3% efficiency.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2013

Surface modifications and optical variations of (−1 1 1) lattice oriented CuO nanofilms for solar energy applications

Graphical abstract: - Highlights: • The films are grown using a low cost SILAR method. • The pH value is found to play a significant role in the property of the resulting films. • The fabrication of band pass filters between 450 nm and 1000 nm is envisaged. • Electrical conductivity and optical band gap values were found to be 68.1 × 10{sup −3} Ω{sup −1} cm{sup −1} and 1.08 eV. • Coating may aid the small band of frequencies could pave way for enhancing the efficiency. - Abstract: This paper reports on the preparation and characterization of Successive Ionic Layer by Adsorption and Reaction (SILAR) grown CuO thin films. The films were deposited onto glass substrates at various solution pH values. The thickness of the film is increased with increase of solution pH values. X-ray diffraction analysis revealed that the prepared films exhibited the monoclinic structure with (−1 1 1) predominant orientation. The optimized pH value is 11 ± 0.1. The microstructure, morphology, optical and electrical properties are studied and reported. The transmission spectra (T) at normal incidence revealed that the films exhibit indirect transitions and may be tailored for passing selected bands of frequencies in visible near IR range. The activation energy is estimated to be about 0.29 eV.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Sol-gel Synthesis and Characterization of Gels with Compositions Relevant to Hydrated Glass Alteration Layers

During the processes associated with glass corrosion, porous alteration gel layers typically form upon exposure to aqueous conditions for extended time periods. The impacts of the alteration gel layer on glass durability have not been agreed upon in the glass science community. In particular, the formation mechanisms of the alteration gel layers are still largely unknown and require further investigation. However, alteration gel layers often require months to years to develop and are often too thin to adequately characterize. Meanwhile, silicate sol-gels are relatively easy to synthesize in bulk with custom compositions relevant to alteration gel layers. If glass alteration gel layers and synthetic sol-gel silicate gels demonstrate physical and chemical properties that are sufficiently similar, synthetic silicate gels could be used as analogues for glass alteration gel layers in future studies. In this study, sol-gels were made with custom compositions at various pH values to evaluate the effect of pH on gel structure and morphology. Several other variables were examined as well, such as composition, drying, and aging. Sol-gels were created by sequential additions of organometallic precursors in a single container. Synthesis procedural steps are provided in further detail within the text. Sol-gels were analyzed with several techniques including Small Angle X-ray Scattering (SAXS), gas adsorption, and He pynchometry to determine the effects of the variables on physical properties. Results show that sol-gels prepared at pH 3 consistently contained fewer primary particles with diameters larger than 72 Å and fewer pores with diameters larger than 300 Å compared to sol-gels synthesized at pH 7 and 9. Composition was shown to have no discernable effect on primary particle and pore sizes at any pH.

Reiser, Joelle TG↗
DOE OSTI2014

Preparation and characterization on nano-hybrid composite solid polymer electrolyte of PVdF-HFP /MG49-ZrO{sub 2} for battery application

Initial study on nano composite polymer electrolyte of PVdF-HFP/MG49-ZrO{sub 2} has been done. The zirconium was synthesis via in-situ sol-gel method in a dissolved polymer blends. The effects of different concentrations of zirconium and pH values have been investigated on nano composite polymer (NCP). Analysis impedance show that only at 6 wt. % of zirconium for all pH values show a semi-circle arc which have lowest value of bulk resistance. No ionic conductivity value is obtain due to the absent of ion charge carriers. Analysis of XRD revealed that crystallinity phase of the nano composite polymer was affect by different pH values. However, no significant changes have been observed in IR bands. This could well indicate that different pH medium did not affect the chemical bonding in the structure.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Study of an unrefined humate solution as a possible remediation method for groundwater contamination - 15698

Savannah River Site (SRS) was one of the major nuclear processing facilities in the U.S. where plutonium was produced during the Cold War. Approximately 1.8 billion gallons of low level acidic waste solution containing radionuclides and dissolved metals were discharged to a series of unlined seepage basins at the F/H Area. Uranium is a key contaminant of concern in the basin's groundwater. It is migrating into the groundwater creating an acidic plume with a pH between 3-5.5. Groundwater Actions: The pump-and-treat water treatment unit was designed and built in 1997 to remove metals and radionuclides. In 2004 a hybrid funnel-and-gate system was constructed to create a treatment zone in which the acidic nature of the contaminated sediments could be reversed. Huma-K is an organic fertilizer that comes from the alkaline extraction of leonardite (a low-rank coal). Huma-K has a high content of humic substances which consist of complex organic compounds formed by the decomposition of plant and animal tissue. The objective of this study is to determine if a low cost unrefined humate solution (Huma-K) can be used to facilitate uranium adsorption to control its mobility in acidic groundwater. This study can assist in evaluating whether Huma-K can be used as an in situ amendment for the remediation of groundwater contaminated with uranium. Sediments from FAW-1 70-90 ft were used in this experiment. Sediments were disaggregated and sieved to a particle size of . 2 mm. Concentrations in the range 10-500 ppm were tested. Once all the components were added, pH was adjusted to 4. Samples were vortex mixed and placed on a shaker table at 100 RPM for a period of 24 hours in order to reach the adsorption equilibrium. Once the adsorption equilibrate was reached, samples were centrifuged at 2700 RPM to separate the liquid and the solid phase. The liquid fraction was analyzed using a Thermo Scientific Genesys 10S UV-Vis spectrophotometer. The same experimental design was used as explained above. A known concentration of Huma-K was used to study the pH effect on the sorption process. pH values were measured at the beginning and at the end of the experiment. Spectra of Huma-K show a featureless character. Absorbance of light increases as the wavelength is decreased. Measurements were done at 254 nm due to the presence of aromatic rings. Apparently there are two sorption processes. The first one follows the same trend as the Langmuir isotherm up to 250 ppm. The second sorption process occurs after all the binding sites in the sediments have been occupied. Precipitation decreases as the pH is increased. Based on the sorption isotherm, humic substances apparently bind first to the binding sites of the sediments particles. Once all the binding sites have been occupied, other sorption processes may start to dominate. Sorption is affected by pH. Higher sorption is seen at low pH values. Increased precipitation at low pH values is probably due to the neutralization of surface charges of humic molecules making them agglomerate.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2019

Effect of Minerals on the Removal of Uranium (VI) in the Presence of Humic Acid and Colloidal Silica - 19406

Uranium is one of the key contaminants of concern in groundwater as a result of past nuclear processing activities at the Department of Energy (DOE) facilities such as the Savannah River Site (SRS) in Aiken, South Carolina. SRS was one of the major nuclear processing facilities during the Cold War where plutonium was produced. Beginning with the implementation of the environmental cleanup program in 1981, SRS has become a hazardous waste management facility responsible for the storage and remediation of contaminated soil and groundwater from radionuclides. Approximately 1.8 billion gallons of acidic waste containing radionuclides and dissolved heavy metals was disposed in the F/H Area seepage basins. This led to the unintentional creation of highly contaminated groundwater plumes, consisting of radionuclides with an acidic pH between 3 and 5.5. The acidity of the plumes contributed to the mobility of several constituents of concern (COC) such as tritium ({sup 3}H), uranium-238 ({sup 238}U), iodine-129 ({sup 129}I), and strontium-90 ({sup 90}Sr) for the F-Area plume and {sup 3}H, {sup 90}Sr and mercury for the H-Area plume. This investigation will focus on uranium in the oxidation state +6 (U(VI)), which is a key contaminant of concern in the groundwater plume of the FArea. Initially, the pump-treat-reinject system was implemented from 1997 to 2003 to remove contaminants from polluted groundwater. Downgrade groundwater within the system would be pumped to the water treatment facility and re-injected upgrade within the aquifer. The effectiveness and sustainability of this process diminished over time. Therefore, it was discontinued and replaced with a funnel-and-gate process in 2004. This new process injects sodium hydroxide directly into the gates of the F-Area groundwater to effectively raise pH levels. By raising the pH of the groundwater, a treatment zone is created by reversing the acidic nature of the contaminated sediments and producing a negative net charge on the surface of sediment particles. As a result, the adsorption of cationic contaminants is expected to be enhanced. So far, this process has resulted in a decrease of {sup 90}Sr and {sup 238}U concentrations, though the concentration of iodine has been unaffected by this treatment. The solution used for the injections contains a high carbonate alkalinity in order to overcome the surface acidic conditions and natural partitions in the groundwater system. To maintain the neutral pH in the treatment zone, systematic injections are required. The continuous use of high concentrations of a carbonate solution to raise pH could re-mobilize uranium previously adsorbed within the treatment zone, though this has not been observed in the monitoring data. Humic substances (HS) are major components of soil organic matter. HS are polyfunctional organic macromolecules formed by the chemo-microbiological decomposition of biomass or dead organic matter. These substances are usually divided into three main fractions: humin (insoluble at all pH values), humic acid (soluble at pH greater than 3.5), and fulvic acid (soluble at all pH values). Humic acid carries a large number of functional groups such as aromatic rings, carboxyl groups, phenols, aliphatic chains, etc. Humic acid is an important ion exchange and metal complexing ligand with a high complexation capacity. The ability of humic acid to chemically bind to metals influences in their migration behavior and fate in natural systems. Various studies have suggested that the retention of U(VI) via sorption in the presence of humic acid is a complex process. For instance, humic acid can form an organic coating at the surface of minerals, which can enhance the sequestration of metals. Ivanov et al. (2012) studied the sorption of U(VI) sorption onto bentonite in the presence and absence of humic acid. The study found that uranium sorption in the presence of humic acid was enhanced at low pH (below 3.8) while at moderate pH (3.8 and 6.5) uranium sorption was reduced compared to the absence of humic acid. At high pH (7 and 9), uranium sorption was reduced for both the presence and absence of humic acid. Also, Krepelova et al. (2007) not only found that U(VI) sorption onto kaolinite was influenced by pH, U(VI) concentration, the presence of inorganic carbon species, and humic acid but also that U(VI) preferred to be adsorbed onto kaolinite as a uranyl-humate complex. This investigation analyzed the mechanisms of the synergetic interactions of humic acid and colloidal silica on the removal of uranium in the presence of pure minerals such as quartz, kaolinite and goethite which are characteristic of the F/H area. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2015

Effects of different annealing atmospheres on the properties of cadmium sulfide thin films

Graphical abstract: The effects of different annealing atmospheres (air and sulfur) on the structural, morphological and optical properties of CdS thin films were studied at three different pH values. - Highlights: • Compactness and smoothness of the films were enhanced after sulfur annealing. • Micro-strain values of some films were improved after sulfur annealing. • Dislocation density values of some films were improved after sulfur annealing. • Band gap values of the films were improved after sulfur annealing. - Abstract: Cadmium sulfide (CdS) thin films were prepared on glass substrates by using chemical bath deposition (CBD) technique. The effects of different annealing atmospheres (air and sulfur) on the structural, morphological and optical properties of CdS thin films were studied at three different pH values. Compactness and smoothness of the films (especially for pH 10.5 and 11) enhanced after sulfur annealing. pH value of the precursor solution remarkably affected the roughness, uniformity and particle sizes of the films. Based on the analysis of X-ray diffraction (XRD) patterns of the films, micro-strain and dislocation density values of the sulfur-annealed films (pH 10.5 and 11) were found to be lower than those of air-annealed films. Air-annealed films (pH 10.5, 11 and 11.5) exhibited higher transmittance than sulfur-annealed films in the wavelength region of 550–800 nm. Optical band gap values of the films were found between 2.31 eV and 2.36 eV.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Microwave-assisted synthesis and characterization of hierarchically structured calcium fluoride

Graphical abstract: CaF{sub 2} with different morphologies and hierarchical structure such as dendrites, spherical and cube was prepared under microwave-assisted condition by a simple solvothermal synthesis route using CaCl{sub 2} and [BMIM]BF{sub 4} as initial reagents, respectively. It was found that the species of precursor was of vital importance for the formation of CaF{sub 2} crystals. That is, precursors itself also acted as structure directing agent. The outstanding features of the approach to obtain hierarchical structure CaF{sub 2} were its simplicity, effectiveness and ease of assembly. On the basis of the experimental results, a possible growth mechanism of the CaF{sub 2} crystals was proposed. Display Omitted Highlights: ► CaF{sub 2} with hierarchical structure was synthesized under microwave-assisted conditions. ► Characteristic morphologies with cube, dendrite, hierarchical sphere, etc. were observed. ► Thin cubes assembled into a spherical structure. ► Ionic liquid of [BMIM]BF{sub 4} was fluorine source. ► Possible growth mechanisms of CaF{sub 2} crystals were discussed. -- Abstract: CaF{sub 2} with different morphologies and hierarchical structures was prepared under microwave-assisted condition by a simple hydrothermal route using CaCl{sub 2} and ionic liquid [BMIM]BF{sub 4} as initial reagents, respectively. It was found that both the precursor and pH values played an important role in the formation of CaF{sub 2} crystals with different morphologies. The results suggested that the CaF{sub 2} with cube and spherical structures was obtained at different pH values (4, 8, 11), while the CaF{sub 2} with dendrite shape was formed through an oriented self-assembly growth using (NH{sub 4}){sub 2}HPO{sub 4} as a structure directing agent. Scanning electron microscope observation showed that the as-prepared CaF{sub 2} was of three-dimensional eight-horn-shaped dendritic structure. The influence of the pH values for the reaction solution and precursors has been discussed in detail. On the basis of the experimental results, possible growth mechanisms of the CaF{sub 2} microcrystals were proposed.

36 MATERIALS SCIENCE↗
DOE OSTI2010

Template-free synthesis of ZnWO{sub 4} powders via hydrothermal process in a wide pH range

ZnWO{sub 4} powders with different morphologies were fabricated through a template-free hydrothermal method at 180 {sup o}C for 8 h in a wide pH range. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-visible and luminescence spectrophotometers were applied to study the effects of pH values on crystallinity, morphology, optical and luminescence properties. The XRD results showed that the WO{sub 3} + ZnWO{sub 4}, ZnWO{sub 4}, and ZnO phases could form after hydrothermal processing at 180 {sup o}C for 8 h with the pH values of 1, 3-11, and 13, respectively. The SEM and TEM observation revealed that the morphological transformation of ZnWO{sub 4} powders occurred with an increase in pH values as follows: star anise-, peony-, and desert rose-like microstructures and soya bean- and rod-like nanostructures. The highest luminescence intensity was found to be in sample consisting of star anise-like crystallites among all the samples due to the presence of larger particles with high crystallinity resulted from the favorable pH under the current hydrothermal conditions.

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