coprecipitation cefc method: Topics by Science.gov

Sample records for coprecipitation cefc method

Synthesis of layered double hydroxides containing Mg2+, Zn2+, Ca2+ and Al3+ layer cations by co-precipitation methods-A review

NASA Astrophysics Data System (ADS)

Theiss, Frederick L.; Ayoko, Godwin A.; Frost, Ray L.

2016-10-01

Co-precipitation is a common method for the preparation of layered double hydroxides (LDHs) and related materials. This review article is aimed at providing newcomers to the field with some examples of the types of co-precipitation reactions that have been reported previously and to briefly investigate some of the properties of the products of these reactions. Due to the sheer volume of literature on the subject, the authors have had to limit this article to the synthesis of Mg/Al, Zn/Al and Ca/Al LDHs by co-precipitation and directly related methods. LDHs have been synthesised from various reagents including metal salts, oxides and hydroxides. Co-precipitation is also useful for the direct synthesis of LDHs with a wide range of interlayer anions and various bases have been successfully employed to prepare LDHs. Examples of other synthesis techniques including the urea method, hydrothermal synthesis and various mechanochemical methods that are undoubtedly related to co-precipitation have also been included in this review. The effect of post synthesis hydrothermal has also been summarised.
Encapsulation of albumin in self-assembled layer-by-layer microcapsules: comparison of co-precipitation and adsorption techniques.

PubMed

Labala, Suman; Mandapalli, Praveen Kumar; Bhatnagar, Shubhmita; Venuganti, Venkata Vamsi Krishna

2015-01-01

The objective of this study is to prepare and characterize polymeric self-assembled layer-by-layer microcapsules (LbL-MC) to deliver a model protein, bovine serum albumin (BSA). The aim is to compare the BSA encapsulation in LbL-MC using co-precipitation and adsorption methods. In co-precipitation method, BSA was co-precipitated with growing calcium carbonate particles to form a core template. Later, poly(styrene sulfonate) and poly(allylamine hydrochloride) were sequentially adsorbed onto the CaCO3 templates. In adsorption method, preformed LbL-MC were incubated with BSA and encapsulation efficiency is optimized for pH and salt concentration. Free and BSA-encapsulated LbL-MC were characterized using Zetasizer, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy and differential scanning calorimeter. Later, in vitro release studies were performed using dialysis membrane method at pH 4, 7.4 and 9. Results from Zetasizer and SEM showed free LbL-MC with an average size and zeta-potential of 2.0 ± 0.6 μm and 8.1 ± 1.9 mV, respectively. Zeta-potential of BSA-loaded LbL-MC was (-)7.4 ± 0.7 mV and (-)5.7 ± 1.0 mV for co-precipitation and adsorption methods, respectively. In adsorption method, BSA encapsulation in LbL-MC was found to be greater at pH 6.0 and 0.2 M NaCl. Co-precipitation method provided four-fold greater encapsulation efficiency (%) of BSA in LbL-MC compared with adsorption method. At pH 4, the BSA release from LbL-MC was extended up to 120 h. Polyacrylamide gel electrophoresis showed that BSA encapsulated in LBL-MC through co-precipitation is stable toward trypsin treatment. In conclusion, co-precipitation method provided greater encapsulation of BSA in LbL-MC. Furthermore, LbL-MC can be developed as carriers for pH-controlled protein delivery.
Highly transparent cerium doped gadolinium gallium aluminum garnet ceramic prepared with precursors fabricated by ultrasonic enhanced chemical co-precipitation.

PubMed

Zhang, Ji-Yun; Luo, Zhao-Hua; Jiang, Hao-Chuan; Jiang, Jun; Chen, Chun-Hua; Zhang, Jing-Xian; Gui, Zhen-Zhen; Xiao, Na

2017-11-01

Cerium doped gadolinium gallium aluminum garnet (GGAG:Ce) ceramic precursors have been synthesized with an ultrasonic chemical co-precipitation method (UCC) and for comparison with a traditional chemical co-precipitation method (TCC). The effect of ultra-sonication on the morphology of powders and the transmittance of GGAG:Ce ceramics are studied. The results indicate that the UCC method can effectively improve the homogenization and sinterability of GGAG:Ce powders, which contribute to obtain high transparent GGAG ceramic with the highest transmittance of 81%. Copyright © 2017 Elsevier B.V. All rights reserved.
An acetate precursor process for BSCCO (2223) thin films and coprecipitated powders

NASA Technical Reports Server (NTRS)

Haertling, Gene H.

1992-01-01

Since the discovery of high temperature superconducting oxides much attention has been paid to finding better and useful ways to take advantage of the special properties exhibited by these materials. One such process is the development of thin films for engineering applications. Another such process is the coprecipitation route to producing superconducting powders. An acetate precursor process for use in thin film fabrication and a chemical coprecipitation route to Bismuth based superconducting materials has been developed. Data obtained from the thin film process were inconclusive to date and require more study. The chemical coprecipitation method of producing bulk material is a viable method, and is preferred over the previously used solid state route. This method of powder production appears to be an excellent route to producing thin section tape cast material and screen printed devices, as it requires less calcines than the oxide route to produce quality powders.
Investigation of Nd xY 0.25-xZr 0.75O 1.88 inert matrix fuel materials made by a co-precipitation synthetic route

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hayes, John R.; Grosvenor, Andrew P.

Yttria-stabilized zirconia (YSZ) is a material that we are considering in our inert matrix fuel nuclear reactors, but a complete characterization of these materials is required for them to be licensed for use. A series of NdxY0.25–xZr0.75O1.88 materials have been synthesized using a co-precipitation method, and the thermal stability of these materials has been studied by annealing them at 1400 and 1500 °C. (Nd was used as surrogate for Am.) The long-range and local structures of the materials were characterized via powder X-ray diffraction, scanning electron microscopy, wavelength dispersive spectroscopy, and X-ray absorption spectroscopy at the Zr K- and Ymore » K-edges. These results were compared with the previous characterization of Nd-YSZ materials synthesized using a ceramic method. Moreover, the results indicated that the ordering in the local metal–oxygen polyhedral remains relatively unaffected by the synthetic method, but there was increased long-range disorder in the materials prepared by the co-precipitation method. Further, it was found that the materials produced by the co-precipitation method were unexpectedly unstable when annealed at high temperature. This study highlights the importance of determining the effect of synthetic method on material properties and demonstrates how the co-precipitation route could be used to produce inert matrix fuels.« less
Development of a calcium phosphate co-precipitate/poly(lactide-co-glycolide) DNA delivery system: release kinetics and cellular transfection studies.

PubMed

Kofron, Michelle D; Laurencin, Cato T

2004-06-01

One of the most common non-viral methods for the introduction of foreign deoxyribonucleic acid (DNA) into cultured cells is calcium phosphate co-precipitate transfection. This technique involves the encapsulation of DNA within a calcium phosphate co-precipitate, particulate addition to in vitro cell culture, endocytosis of the co-precipitate, and exogenous DNA expression by the transfected cell. In this study, we fabricated a novel non-viral gene transfer system by adsorbing DNA, encapsulated in calcium phosphate (DNA/Ca-P) co-precipitates, to biodegradable two- and three-dimensional poly(lactide-co-glycolide) matrices (2D-DNA/Ca-P/PLAGA, 3D-DNA/Ca-P/PLAGA). Co-precipitate release studies demonstrated an initial burst release over the first 48 h. By day 7, approximately 96% of the initially adsorbed DNA/Ca-P co-precipitate had been released. This was followed by low levels of co-precipitate release for 42 days. Polymerase chain reaction was used to demonstrate the ability of the released DNA containing co-precipitates to transfect SaOS-2 cells cultured in vitro on the 3D-DNA/Ca-P/PLAGA matrix and maintenance of the structural integrity of the exogenous DNA. In summary, a promising system for the incorporation and controlled delivery of exogenous genes encapsulated within a calcium phosphate co-precipitate from biodegradable polymeric matrices has been developed and may have applicability to the delivery of therapeutic genes and the transfection of other cell types.
Autothermal reforming of propane over Mg-Al hydrotalcite-like catalysts.

PubMed

Lim, You-Soon; Park, Nam-Cook; Shin, Jae-Soon; Kim, Jong-Ho; Moon, Dong-Ju; Kim, Young-Chul

2008-10-01

The performance of hydrotalcite-like catalysts in propane autothermal reforming for hydrogen production was studied in fixed-bed flow reactor. Hydrotalcite-like catalysts were synthesized by coprecipitation and modified co-precipitation by the impregnation method and those were promoted by the addition of noble metals. Reaction test results indicated that hydrotalcite-like catalysts of modified method were showed higher H2-yield than co-precipitation method because surface Ni particles of catalysts by modified method were more abundant. When added noble metals, the activity was enhanced because the size of nickel particles was decreased and degree of dispersion was increased. Also the carbon deposit is low after the reaction. When solvent of solution was changed, activity was increased. It is because degree of dispersion was increased.
Effect of modification methods on the surface properties and n-butane isomerization performance of La/Ni-promoted SO42-/ZrO2-Al2O3

NASA Astrophysics Data System (ADS)

Wang, Pengzhao; Zhang, Jiaoyu; Han, Chaoyi; Yang, Chaohe; Li, Chunyi

2016-08-01

The La and/or Ni was introduced into alumina-promoted sulfated zirconia by impregnation and co-precipitation to improve the catalytic property of n-butane isomerization. Catalysts characterization shows that the addition of La/Ni has a remarkable influence on the surface and textual properties depending on the modification method. The impregnation of La/Ni facilitates the transformation of a small amount of tetragonal zirconia into monoclinic phase, while the co-precipitation improves the stability of tetragonal ZrO2. H2-TPR indicates that the addition of La/Ni changes the interaction between SO42- and supports, which affects the acidity on the surface. Specifically, the Lewis acidity is significantly enhanced by either modification method. The co-precipitation reserves almost all of the Brønsted acid sites, while the impregnation causes a remarkable decrease of Brønsted acid sites. Reaction results demonstrate that the co-precipitation exhibits a significant advantage over impregnation that the higher conversion of n-butane and selectivity to isobutane are obtained on the catalyst prepared by co-precipitation. The increase of catalytic activity is ascribed to the accelerated activation rate of n-butane molecules by hydride subtraction on the Lewis acid sites at higher reaction temperature. Furthermore, the addition of La/Ni improves the selectivity to isobutane by inhibiting the bimolecular reaction.
Synthesis of [Zn-Al-CO 3] layered double hydroxides by a coprecipitation method under steady-state conditions

NASA Astrophysics Data System (ADS)

Chang, Z.; Evans, D. G.; Duan, X.; Vial, C.; Ghanbaja, J.; Prevot, V.; de Roy, M.; Forano, C.

2005-09-01

A continuous co-precipitation method under steady-state conditions has been investigated for the preparation of nanometer-size layered double hydroxide (LDH) particles using Zn 2Al(OH) 6(CO 3) 0.5·2H 2O as a prototype. The objective was to shorten the preparation time by working without an aging step, using a short and controlled residence time in order to maintain a constant supersaturation level in the reactor and constant particle properties in the exit stream over time. The effects of varying the operating conditions on the structural and textural properties of the LDHs have been studied, including total cation concentration, solvent, residence time, pH and intercalation anion. The products have been characterized using ICP, XRD, FTIR, BET, SEM and TEM. The LDHs prepared by the continuous coprecipitation method have a poorer crystallinity and lower crystallite sizes than those synthesized by the conventional batch method. The results have shown that increasing either cation concentration or the fraction of monoethylene glycol (MEG) in MEG/H 2O mixtures up to 80% (v/v) affect salt solubility and supersaturation, which gives rise to smaller crystallites, larger surface areas and more amorphous compounds. This increase is however limited by the precipitation of zinc and aluminum hydroxides occurring around a total cation concentration of 3.0×10 -1 M in pure water and 3.0×10 -2 M in H 2O/EtOH mixtures. Crystallite size increases with residence time, suggesting a precipitation process controlled by growth. Finally, the continuous coprecipitation method under steady-state conditions has been shown to be a promising alternative to the traditional coprecipitation technique in either pure water or mixed H 2O/MEG solvents.
Determination of Aluminum in Dialysis Concentrates by Atomic Absorption Spectrometry after Coprecipitation with Lanthanum Phosphate.

PubMed

Selvi, Emine Kılıçkaya; Şahin, Uğur; Şahan, Serkan

2017-01-01

This method was developed for the determination of trace amounts of aluminum(III) in dialysis concentrates using atomic absorption spectrometry after coprecipitation with lanthanum phosphate. The analytical parameters that influenced the quantitative coprecipitation of analyte including amount of lanthanum, amount of phosfate, pH and duration time were optimized. The % recoveries of the analyte ion were in the range of 95-105 % with limit of detection (3s) of 0.5 µg l -1 . Preconcentration factor was found as 1000 and Relative Standard Deviation (RSD) % value obtained from model solutions was 2.5% for 0.02 mg L -1 . The accuracy of the method was evaluated with standard reference material (CWW-TMD Waste Water). The method was also applied to most concentrated acidic and basic dialysis concentrates with satisfactory results.
Method for producing UO$sub 2$ loaded refractory metals

DOEpatents

Baker, R.D.; Hayter, S.W.; Lewis, H.D.

1973-12-11

A finely divided dispersion of UO/sub 2/ in tungsten or molybdenum is prepared by co-precipitating the metals from mixed aqueous solution with oxine. The co-precipitate thus formed is separated from the solution, dried, calcined, and finally reduced to UO/sub 2/ and refractory metal. (Official Gazette)
CO-PRECIPITATION IN QUANTITATIVE ANALYSIS. COMMUNICATION V. THE INFLUENCE EXERCISED BY COMPLEXION UPON THE PRECIPITATION OF ZIRCONIUM PHOSPHATE

DOE Office of Scientific and Technical Information (OSTI.GOV)

Babko, A.K.; Shtokalo, M.I.

The influence exercised by ethylenediamino-tetraacetic acid upon some processes of precipitation was investigated. A sharp mopdification of the form of precipitate as well as a decrease of coprecipitation was ium and titanium by means of the phosphate ;method are given. (TCO-W.D.M.)
Determination of cadmium in grains by isotope dilution ICP-MS and coprecipitation using sample constituents as carrier precipitants.

PubMed

Inagaki, Kazumi; Narukawa, Tomohiro; Yarita, Takashi; Takatsu, Akiko; Okamoto, Kensaku; Chiba, Koichi

2007-10-01

A coprecipitation method using sample constituents as carrier precipitants was developed that can remove molybdenum, which interferes with the determination of cadmium in grain samples via isotope dilution inductively coupled plasma mass spectrometry (ID-ICPMS). Samples were digested with HNO3, HF, and HClO4, and then purified 6 M sodium hydroxide solution was added to generate colloidal hydrolysis compounds, mainly magnesium hydroxide. Cadmium can be effectively separated from molybdenum because the cadmium forms hydroxides and adsorbs onto and/or is occluded in the colloid, while the molybdenum does not form hydroxides or adsorb onto the hydrolysis colloid. The colloid was separated by centrifugation and then dissolved with 0.2 M HNO3 solution to recover the cadmium. The recovery of Cd achieved using the coprecipitation was >97%, and the removal efficiency of Mo was approximately 99.9%. An extremely low procedural blank (below the detection limit of ICPMS) was achieved by purifying the 6 M sodium hydroxide solution via Mg coprecipitation using Mg(NO3)2 solution. The proposed method was applied to two certified reference materials (NIST SRM 1567a wheat flour and SRM 1568a rice flour) and CCQM-P64 soybean powder. Good analytical results with small uncertainties were obtained for all samples. This method is simple and reliable for the determination of Cd in grain samples by ID-ICPMS.
Preparation and Characterization of Ato Nanoparticles by Coprecipitation with Modified Drying Method

NASA Astrophysics Data System (ADS)

Liu, Shimin; Liang, Dongdong; Liu, Jindong; Jiang, Weiwei; Liu, Chaoqian; Ding, Wanyu; Wang, Hualin; Wang, Nan

Antimony-doped tin oxide (ATO) nanoparticles were prepared by coprecipitation by packing drying and traditional direct drying (for comparison) methods. The as-prepared ATO nanoparticles were characterized by TG, XRD, EDS, TEM, HRTEM, BET, bulk density and electrical resistivity measurements. Results indicated that the ATO nanoparticles obtained by coprecipitation with direct drying method featured hard-agglomerated morphology, high bulk density, low surface area and low electrical resistivity, probably due to the direct liquid evaporation during drying, the fast shrinkage of the precipitate, the poor removal efficiency of liquid molecules and the hard agglomerate formation after calcination. Very differently, the ATO product obtained by the packing and drying method featured free-agglomerated morphology, low bulk density, high surface area and high electrical resistivity ascribed probably to the formed vapor cyclone environment and liquid evaporation-resistance, avoiding fast liquid removal and improving the removal efficiency of liquid molecules. The intrinsic formation mechanism of ATO nanoparticles from different drying methods was illustrated based on the dehydration process of ATO precipitates. Additionally, the packing and drying time played key roles in determining the bulk density, morphology and electrical conductivity of ATO nanoparticles.
Anaerobic microbial remobilization of coprecipitated metals

DOEpatents

Francis, Arokiasamy J.; Dodge, Cleveland J.

1994-10-11

A process is provided for solubilizing coprecipitated metals. Metals in wastestreams are concentrated by treatment with an iron oxide coprecipitating agent. The coprecipitated metals are solubilized by contacting the coprecipitate with a bacterial culture of a Clostridium species ATCC 53464. The remobilized metals can then be recovered and recycled.
Anaerobic microbial remobilization of coprecipitated metals

DOEpatents

Francis, A.J.; Dodge, C.J.

1994-10-11

A process is provided for solubilizing coprecipitated metals. Metals in waste streams are concentrated by treatment with an iron oxide coprecipitating agent. The coprecipitated metals are solubilized by contacting the coprecipitate with a bacterial culture of a Clostridium species ATCC 53464. The remobilized metals can then be recovered and recycled. 4 figs.
Influence of catalyst synthesis method on selective catalytic reduction (SCR) of NO by NH 3 with V 2O 5-WO 3/TiO 2 catalysts

DOE PAGES

He, Yuanyuan; Ford, Michael E.; Zhu, Minghui; ...

2016-04-14

We compared the molecular structures, surface acidity and catalytic activity for NO/NH 3/O 2 SCR of V 2O 5-WO 3/TiO 2 catalysts for two different synthesis methods: co-precipitation of aqueous vanadium and tungsten oxide precursors with TiO(OH) 2 and by incipient wetness impregnation of the aqueous precursors on a reference crystalline TiO 2 support (P25; primarily anatase phase). Bulk analysis by XRD showed that co-precipitation results in small and/or poorly ordered TiO 2(anatase) particles and that VO x and WO x do not form solid solutions with the bulk titania lattice. Surface analysis of the co-precipitated catalyst by High Sensitivity-Lowmore » Energy Ion Scattering (HS-LEIS) confirms that the VO x and WO x are surface segregated for the co-precipitated catalysts. In situ Raman and IR spectroscopy revealed that the vanadium and tungsten oxide components are present as surface mono-oxo O = VO 3 and O = WO 4 sites on the TiO 2 supports. Co-precipitation was shown for the first time to also form new mono-oxo surface VO 4 and WO 4 sites that appear to be anchored at surface defects of the TiO 2 support. IR analysis of chemisorbed ammonia showed the presence of both surface NH 3 * on Lewis acid sites and surface NH 4 +* on Brønsted acid sites. TPSR spectroscopy demonstrated that the specific SCR kinetics was controlled by the redox surface VO 4 species and that the surface kinetics was independent of TiO 2 synthesis method or presence of surface WO 5 sites. SCR reaction studies revealed that the surface WO5 sites possess minimal activity below ~325 °C and their primary function is to increase the adsorption capacity of ammonia. A relationship between the SCR activity and surface acidity was not found. The SCR reaction is controlled by the surface VO 4 sites that initiate the reaction at ~200 °C. The co-precipitated catalysts were always more active than the corresponding impregnated catalysts. Finally, we ascribe the higher activity of the co-precipitated catalysts to the presence of the new surface WO x sites associated surface defects on the TiO 2 support that increase the ammonia adsorption capacity.« less
Mg-Al and Zn-Fe layered double hydroxides used for organic species storage and controlled release.

PubMed

Seftel, E M; Cool, P; Lutic, D

2013-12-01

Layered double hydroxides (LDH) containing (Mg and Al) or (Zn and Fe) were prepared by coprecipitation at constant pH, using NaOH and urea as precipitation agents. The most pure LDH phase in the Zn/Fe system was obtained with urea and in Mg/Al system when using NaOH. The incorporation of phenyl-alanine (Phe) anions in the interlayer of the LDH was performed by direct coprecipitation, ionic exchange and structure reconstruction of the mixed oxide obtained by the calcination of the coprecipitated product at 400°C. The reconstruction method and the direct coprecipitation in a medium containing Phe in the initial mixture were less successful in terms of high yields of organic-mineral composite than the ionic exchange method. A spectacular change in sample morphology and yield in exchanged solid was noticed for the Zn3Fe sample obtained by ionic exchange for 6h with Phe solution. A delivery test in PBS of pH=7.4 showed the release of the Phe in several steps up to 25 h indicating different host-guest interactions between the Phe and the LDH matrix. This behavior makes the preparation useful to obtain late delivery drugs, by the incorporation of the anion inside the LDH layer. © 2013.
Comparative physicochemical properties of hydrocortisone-PVP composites prepared using supercritical carbon dioxide by the GAS anti-solvent recrystallization process, by coprecipitation and by spray drying.

PubMed

Corrigan, Owen I; Crean, Abina M

2002-10-01

Hydrocortisone-PVP composites were successfully prepared using the supercritical fluid gas anti-solvent method (GAS). Analysis by differential scanning calorimetry DSC and powder X-ray diffraction (XRD) indicated that these systems were more crystalline than corresponding systems prepared by spray drying. These systems, prepared by the GAS method were more similar in physicochemical properties to coprecipitates prepared by conventional solvent evaporation. Compressed composites of hydrocortisone-PVP systems, prepared by the GAS method, had dissolution rates lower than those of corresponding systems prepared by the other processing methods but equivalent to those of corresponding physical mixtures.
Removal of р-nitrophenol from aqueous solution by magnetically modified activated carbon

NASA Astrophysics Data System (ADS)

Han, Shuai; Zhao, Feng; Sun, Jian; Wang, Bin; Wei, Rongyan; Yan, Shiqiang

2013-09-01

Activated carbon was modified with γ-Fe2O3 nanoparticles, using the chemical co-precipitation technique and the carboxylic acid vapor treatment technique. Two magnetic composites were characterized and compared by Fourier Transform Infrared spectroscopy, X-ray diffractometry, vibrating sample magnetometry and nitrogen adsorption-desorption. Then the two materials were used to remove p-nitrophenol in water. The equilibrium data revealed that the Langmuir isotherm was better in fitting the experiment result than the Freundlich isotherm, and the sorption capacity of the nanocomposite made by the chemical co-precipitation technique was higher than that of the other one. We suggest that the chemical co-precipitation technique is a more efficient and practical method to produce magnetically modified activated carbon.

In Vitro and In Vivo Evaluation of Casein as a Drug Carrier for Enzymatically Triggered Dissolution Enhancement from Solid Dispersions.

PubMed

Bani-Jaber, Ahmad; Alshawabkeh, Iyad; Abdullah, Samaa; Hamdan, Imad; Ardakani, Adel; Habash, Maha

2017-07-01

Due to its unique properties, such as biodegradability, biocompatibility, high amphiphilic property, and micelle formation, casein (CS) has been increasingly studied for drug delivery. We used CS as a drug carrier in solid dispersions (SDs) and evaluated the effect of its degradation by trypsin on drug dissolution from the dispersions. SDs of CS and mefenamic acid (MA) were prepared by physical mixing, kneading, and coprecipitation methods. In comparison to pure MA, the dispersions were evaluated for drug-protein interaction, loss of drug crystalinity, and drug morphology by differential scanning calorimetry, X-ray diffractometry, Fourier transform infrared spectroscopy, and scanning electron microscopy. Drug dissolution from the dispersions was evaluated in simulated intestinal fluid as enzyme free and trypsin-enriched media. Furthermore, in vivo drug absorption of MA from CS-MA coprecipitate was evaluated in rats, in comparison with a reference SD of polyethylene glycol and MA (PEG-MA SD). Relative to other CS preparations, CS-MA coprecipitate showed the highest loss of drug crystallinity, drug micronization, and CS-MA interaction. CS remarkably enhanced the dissolution rate and extent of MA from the physical and kneaded mixtures. However, the highest dissolution enhancement was obtained when MA was coprecipitated with CS. Trypsin that can hydrolyze CS during dissolution resulted in further enhancement of MA dissolution from the physical and kneaded mixtures. However, a corresponding retardation effect was obtained for the coprecipitate. In correlation with in vitro drug release, CS-MA coprecipitate also showed significantly higher MA bioavailability in rats than PEG-MA SD.
Copper(II)-rubeanic acid coprecipitation system for separation-preconcentration of trace metal ions in environmental samples for their flame atomic absorption spectrometric determinations.

PubMed

Soylak, Mustafa; Erdogan, Nilgun D

2006-09-21

A simple and facile preconcentration procedure based on the coprecipitation of trace heavy metal ions with copper(II)-rubeanic acid complex has been developed. The analytical parameters including pH, amounts of rubeanic acid, sample volume, etc. was investigated for the quantitative recoveries of Pb(II), Fe(III), Cd(II), Au(III), Pd(II) and Ni(II). No interferic effects were observed from the concomitant ions. The detection limits for analyte ions by 3 sigma were in the range of 0.14 microg/l for iron-3.4 microg/l for lead. The proposed coprecipitation method was successfully applied to water samples from Palas Lake-Kayseri, soil and sediment samples from Kayseri and Yozgat-Turkey.
[Determination of trace lead and iron in nickel chloride and manganese sulfate by flame atomic absorption spectrometry after coprecipitation with yttrium phosphate].

PubMed

Su, Yao-Dong; Zhu, Wen-Ying; Ma, Hong-Mei; Chen, Long-Wu

2006-09-01

Using yttrium phosphate as the coprecipitation collector for the separation and preconcentration of trace lead and iron in nickel chloride and manganese sulfate, flame atomic absorption spectrometric (FAAS) determination was described in the present paper. Coprecipitation parameters including the pH of the solution, and the amounts of YCl3 and H3 PO4 were discussed. It was found that lead and iron in nickel chloride could be coprecipitated quantitatively in the range of pH 3.0-4.0, and so could be lead in manganese sulfate. The detection limits (3sigma) of lead and iron in 20 mL solution were 1.63 x 10(-2) mg x L(-1) and 4.58 x 10(-2) mg x L(-1) respectively. In NiCl2 solution the standard addition recoveries for lead and iron were 100.91% and 99.73% respectively, and in MnSO4 solution the standard addition recoveries were 99.45% and 98.98% respectively. The method has eliminated the interference of matrix, and the result is satisfied.
Dissimilatory reduction and transformation of ferrihydrite-humic acid coprecipitates.

PubMed

Shimizu, Masayuki; Zhou, Jihai; Schröder, Christian; Obst, Martin; Kappler, Andreas; Borch, Thomas

2013-01-01

Organic matter (OM) is present in most terrestrial environments and is often found coprecipitated with ferrihydrite (Fh). Sorption or coprecipitation of OM with Fe oxides has been proposed to be an important mechanism for long-term C preservation. However, little is known about the impact of coprecipitated OM on reductive dissolution and transformation of Fe(III) (oxyhydr)oxides. Thus, we study the effect of humic acid (HA) coprecipitation on Fh reduction and secondary mineral formation by the dissimilatory Fe(III)-reducing bacterium Shewanella putrefaciens strain CN32. Despite similar crystal structure for all coprecipitates investigated, resembling 2-line Fh, the presence of coprecipitated HA resulted in lower specific surface areas. In terms of reactivity, coprecipitated HA resulted in slower Fh bioreduction rates at low C/Fe ratios (i.e., C/Fe ≤ 0.8), while high C/Fe ratios (i.e., C/Fe ≥ 1.8) enhanced the extent of bioreduction compared to pure Fh. The coprecipitated HA also altered the secondary Fe mineralization pathway by inhibiting goethite formation, reducing the amount of magnetite formation, and increasing the formation of a green rust-like phase. This study indicates that coprecipitated OM may influence the rates, pathway, and mineralogy of biogeochemical Fe cycling and anaerobic Fe respiration within soils.
Rapid determination of actinides in seawater samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maxwell, Sherrod L.; Culligan, Brian K.; Hutchison, Jay B.

2014-03-09

A new rapid method for the determination of actinides in seawater samples has been developed at the Savannah River National Laboratory. The actinides can be measured by alpha spectrometry or inductively-coupled plasma mass spectrometry. The new method employs novel pre-concentration steps to collect the actinide isotopes quickly from 80 L or more of seawater. Actinides are co-precipitated using an iron hydroxide co-precipitation step enhanced with Ti +3 reductant, followed by lanthanum fluoride co-precipitation. Stacked TEVA Resin and TRU Resin cartridges are used to rapidly separate Pu, U, and Np isotopes from seawater samples. TEVA Resin and DGA Resin were usedmore » to separate and measure Pu, Am and Cm isotopes in seawater volumes up to 80 L. This robust method is ideal for emergency seawater samples following a radiological incident. It can also be used, however, for the routine analysis of seawater samples for oceanographic studies to enhance efficiency and productivity. In contrast, many current methods to determine actinides in seawater can take 1–2 weeks and provide chemical yields of ~30–60 %. This new sample preparation method can be performed in 4–8 h with tracer yields of ~85–95 %. By employing a rapid, robust sample preparation method with high chemical yields, less seawater is needed to achieve lower or comparable detection limits for actinide isotopes with less time and effort.« less
Molecular Structures of Al/Si and Fe/Si Coprecipitates and the Implication for Selenite Removal

PubMed Central

Chan, Ya-Ting; Kuan, Wen-Hui; Tzou, Yu-Min; Chen, Tsan-Yao; Liu, Yu-Ting; Wang, Ming-Kuang; Teah, Heng-Yi

2016-01-01

Aluminum and iron oxides have been often used in the coagulation processes during water purification due to their unique surface properties toward anions. In the presence of silica, the coprecipitation of Al/Si or Fe/Si might decrease the efficiency of wastewater purification and reuse. In this study, surface properties and molecular structures of Al/Si and Fe/Si coprecipitates were characterized using spectroscopic techniques. Also, the selenite removal efficiency of Al/Si and Fe/Si coprecipitates in relation to their surface and structural properties was investigated. While dissolved silicate increased with increasing pH from Fe/Si coprecipitates, less than 7% of silicate was discernible from Al/Si samples over the range from acidic to alkaline conditions. Our spectroscopic results showed that the associations between Al and Si were relatively stronger than that between Fe and Si in coprecipitates. In Al/Si coprecipitates, core-shell structures were developed with AlO6/AlO4 domains as the shells and Si frameworks polymerized from the SiO2 as the cores. However, Si framework remained relatively unchanged upon coprecipitation with Fe hydroxides in Fe/Si samples. The Si core with Al shell structure of Al/Si coprecipitates shielded the negative charges from SiO2 and thereby resulted in a higher adsorption capacity of selenite than Fe/Si coprecipitates. PMID:27095071
[Studies on hydroxyapatite applicatied in coprecipitate of total salvianolic acids phospholipid complex].

PubMed

Chen, Xiao-Yun; Zhang, Zhen-Hai; Liu, Dan; Sun, E; Jia, Xiao-Bin

2014-03-01

The purpose of this research was to prepare total salvianolic acids-phytosome-HA coprecipitate to improve drug dissolution and its micromeritic properties. Firstly, the coprecipitate was prepared by solvent method and in vitro dissolution of tripterine was performed with the salvianolic acid B and danshensu as criteria. At the same time, the micromeritic properties was characterizated, the structure of samples was characterized by TEM, DSC, XRD and FTIR. Results showed that when the ratio of drug to HA was 1:2, it had a better dissolution, the accumulative drug-release percent in vitro at 60 min was over 90%. At the same time, it has good liquidity and low moisture absorption. Its micromeritic properties have improved. It is proved that the drug still existed amorphously by microstructure analysis. The preparation process is simple and feasible, it has practical value.
One-pot Synthesis and Surface Modification of Fe3O4 Nanoparticles Using Polyvinyl Alcohol by Coprecipitation and Ultrasonication Methods

NASA Astrophysics Data System (ADS)

Nugraha, Aditya D.; Wulandari, Ika O.; Hutami Rahayu, L. B.; Riva'i, Imam; Santojo, D. J. Djoko H.; Sabarudin, Akhmad

2018-01-01

Among the various substances developed through nanoparticles, iron oxide (Fe3O4) nanoparticle is one of the substances that have been widely used in various fields such as industry, agriculture, biotechnology and biomedicine. The synthesis of Fe3O4 nanoparticle can be carried out by two methods, consist of chemical and mechanical synthesis methods. Coprecipitation is one of the most commonly used methods for chemical synthesis. Fe3O4 compounds are easily oxidized because they are amphoteric. To avoid the continuous oxidation process, chemical modification process should be carried out with the addition of a solution of polyvinyl alcohol (PVA). In this study, PVA-coated Fe3O4 nanoparticles were synthesized by in-situ coprecipitation and ultrasonication methods through direct mixing (one-pot synthesis) of the iron (II) chloride tetrahydrate (FeCl2.4H2O), iron (III) chloride hexahydrate (FeCl3.6H2O), and PVA under alkaline condition. The effects of addition amount of NH3solution (by adjusting its flow rate using automated syringe pump) and PVA concentration were gently studied. Interaction of PVA with Fe3O4 nanoparticle was identified by infrared spectroscopy whereas lattice parameters and crystallite sizes of the synthesized Fe3O4 nanoparticles and PVA-coated Fe3O4 nanoparticles were assessed by X-ray diffraction (XRD).
Kinetics and equilibrium adsorption study of selenium oxyanions onto Al/Si and Fe/Si coprecipitates.

PubMed

Chan, Y T; Liu, Y T; Tzou, Y M; Kuan, W H; Chang, R R; Wang, M K

2018-05-01

Inappropriate treatments for the effluents from semiconductor plants might cause the releases and wide distributions of selenium (Se) into the ecosystems. In this study, Al/Si and Fe/Si coprecipitates were selected as model adsorbents as they often formed during the wastewater coagulation process, and the removal efficiency of selenite (SeO 3 ) and selenate (SeO 4 ) onto the coprecipitates were systematically examined. The removal efficiency of SeO 3 and SeO 4 was highly related to surface properties of Al/Si and Fe/Si coprecipitates. The surface-attached Al shell of Al/Si coprecipitates shielded a portion of negative charges from the core SiO 2 , resulting in a higher point of zero charge than that of Fe/Si coprecipitates. Thus, adsorption of SeO 3 /SeO 4 was favorable on the Al/Si coprecipitates. Adsorptions of both SeO 3 and SeO 4 on Al/Si coprecipitates were exothermic reactions. On Fe/Si coprecipitates, while SeO 3 adsorption also showed the exothermic behavior, SeO 4 adsorption occurred as an endothermic reaction. The kinetic adsorption data of SeO 3 /SeO 4 on Al/Si and Fe/Si coprecipitates were described well by the pseudo-second-order kinetic model. SeO 4 and SeO 3 adsorption on Fe/Si or Al/Si were greatly inhibited by the strong PO 4 ligand, whereas the weak ligand such as SO 4 only significantly affected SeO 4 adsorption. The weakest complex between SeO 4 and Al was implied by the essentially SeO 4 desorption as SeO 4 /PO 4 molar ratios decreased from 0.5 to 0.2. These results were further confirmed by the less SeO 4 desorption (41%) from Fe/Si coprecipitates than that from Al/Si coprecipitates (78%) while PO 4 was added sequentially. Copyright © 2018 Elsevier Ltd. All rights reserved.
Effects of Dissolved Organic Matter Properties on Formation and Composition of Mineral-Organic Co-Precipitates at the Nanometer Scale

NASA Astrophysics Data System (ADS)

Possinger, A. R.; Zachman, M.; Lehmann, J.

2016-12-01

An important, yet largely overlooked case of soil organic carbon (SOC) stabilization through mineral-organic associations is the co-precipitation of dissolved organic matter (DOM) into mineral precipitates as they form. The contribution of co-precipitated DOM to the mineral-stabilized SOC pool is expected to be greatest in soil environments with frequent mineral dissolution and precipitation processes. Compared to surface adsorption, properties of mineral-organic co-precipitates are expected to differ at both the particle scale (e.g., total carbon (C) content and composition) and the molecular scale (e.g., impurities in mineral structure), with potential implications for stability and C turnover; additionally, these properties vary across C sources, amounts, and forms. Consequently, high-resolution visualization and characterization combined with bulk chemical measurements is needed to provide a more complete understanding of co-precipitate formation processes and properties, especially as a function of C co-precipitant characteristics. In this study, we evaluate the effect of model C compound and DOM chemical properties (e.g., iron-binding affinity) on the formation, structure, and chemical properties of ferrihydrite (Fh) (Fe3+3O2 •0.5H2O) co-precipitates. Salicylic acid (SA), sucrose and water-extractable DOM from coniferous or deciduous-dominated organic soils were either adsorbed to pre-formed Fh or co-precipitated with Fh. At a C/Fe ratio 10, the amount of co-precipitated C differed among all organic compounds, and for DOM, was more than 2X greater for co-precipitation than adsorption, suggesting a greater capacity for C retention. To probe the molecular-scale C spatial distribution of Fh-SA particles, we obtained Scanning Transmission Electron Microscopy with Electron Energy Loss Spectroscopy (STEM-EELS) maps at a nanometer-scale spatial pixel resolution. Additionally, we will present chemical characteristics of organic-Fh co-precipitates and adsorption complexes investigated in bulk using C Near-Edge X-ray Absorption Fine Structure (NEXAFS) and Fourier Transform Infrared (FT-IR) spectroscopy. Ultimately, these observations of model co-precipitation systems will be used to better interpret observations of putative co-precipitated OM in natural soils.
Ultrasound assisted co-precipitation of nanostructured CuO-ZnO-Al2O3 over HZSM-5: effect of precursor and irradiation power on nanocatalyst properties and catalytic performance for direct syngas to DME.

PubMed

Allahyari, Somaiyeh; Haghighi, Mohammad; Ebadi, Amanollah; Hosseinzadeh, Shahin

2014-03-01

Nanostructured CuO-ZnO-Al2O3/HZSM-5 was synthesized from nitrate and acetate precursors using ultrasound assisted co-precipitation method under different irradiation powers. The CuO-ZnO-Al2O3/HZSM-5 nanocatalysts were characterized using XRD, FESEM, BET, FTIR and EDX Dot-mapping analyses. The results indicated precursor type and irradiation power have significant influences on phase structure, morphology, surface area and functional groups. It was observed that the acetate formulated CuO-ZnO-Al2O3/HZSM-5 nanocatalyst have smaller CuO crystals with better dispersion and stronger interaction between components in comparison to nitrate based nanocatalysts. Ultrasound assisted co-precipitation synthesis method resulted in nanocatalyst with more uniform morphology compared to conventional method and increasing irradiation power yields smaller particles with better dispersion and higher surface area. Additionally the crystallinity of CuO is lower at high irradiation powers leading to stronger interaction between metal oxides. The nanocatalysts performance were tested at 200-300 °C, 10-40 bar and space velocity of 18,000-36,000 cm(3)/g h with the inlet gas composition of H2/CO = 2/1 in a stainless steel autoclave reactor. The acetate based nanocatalysts irradiated with higher levels of power exhibited better reactivity in terms of CO conversion and DME yield. While there is an optimal temperature for CO conversion and DME yield in direct synthesis of DME, CO conversion and DME yield both increase with the pressure increase. Furthermore ultrasound assisted co-precipitation method yields more stable CuO-ZnO-Al2O3/HZSM-5 nanocatalyst while conventional precipitated nanocatalyst lost their activity ca. 18% and 58% in terms of CO conversion and DME yield respectively in 24 h time on stream test.
Coprecipitation of gold(III) complex ions with manganese(II) hydroxide and their stoichiometric reduction to atomic gold (Au(0)): analysis by Mössbauer spectroscopy and XPS.

PubMed

Yamashita, Mamiko; Ohashi, Hironori; Kobayashi, Yasuhiro; Okaue, Yoshihiro; Kurisaki, Tsutomu; Wakita, Hisanobu; Yokoyama, Takushi

2008-03-01

To elucidate the formation process of precursor of gold-supported manganese dioxide (MnO2), the coprecipitation behavior of [AuCl4-n(OH)n](-) (n=0-4) (Au(III)) complex ions with manganese(II) hydroxide (Mn(OH)2 and the change in their chemical state were examined. The Au(III) complex ions were rapidly and effectively coprecipitated with Mn(OH)(2) at pH 9. According to the Mössbauer spectra for gold (Au) coprecipitated with Mn(OH)2, below an Au content of 60 wt% in the coprecipitates, all of the coprecipitated Au existed in the atomic state (Au(0)), while, above an Au content of 65 wt%, part of the gold existed in the Au(III) state, and the proportion increased with increasing coprecipitated Au content. Based on the results of X-ray photoelectron spectroscopy, Mn(II) in Mn(OH)2 converted to Mn(IV) in conjunction with coprecipitation of Au(III) complex ions. These results indicate that the rapid stoichiometric reduction of Au(III) to Au(0) is caused by electron transfer from Mn(II) in Mn(OH)2 to the Au(III) complex ion through an Mn-O-Au bond.
Preparation, characterization, nanostructures and bio functional analysis of sonicated protein co-precipitates from brewers' spent grain and soybean flour.

PubMed

Alu'datt, Muhammad H; Gammoh, Sana; Rababah, Taha; Almomani, Mohammed; Alhamad, Mohammad N; Ereifej, Khalil; Almajwal, Ali; Tahat, Asma; Hussein, Neveen M; Nasser, Sura Abou

2018-02-01

This investigation was performed to assess the effects of sonication on the structure of protein, extractability of phenolics, and biological properties of isolated proteins and protein co-precipitates prepared from brewers' spent grain and soybean flour. Scanning electron micrographs revealed that the sonicated protein isolates and co-precipitates had different microstructures with fewer aggregates and smaller particles down to the nanometer scale compared to non-sonicated samples. However, the levels of free and bound phenolics extracted from non-sonicated protein isolates and protein co-precipitates increased compared to sonicated samples. The bound phenolics extracted after acid hydrolysis of sonicated protein co-precipitates showed improved ACE inhibitory activity and diminished antioxidant potency compared to non-sonicated samples. However, the free phenolics extracted from sonicated protein co-precipitates showed decreased ACE inhibitory activity and increased antioxidant activities compared to non-sonicated samples. The free and bound phenolics extracted from sonicated protein co-precipitates showed increased alpha-amylase inhibitory activity compared to non-sonicated samples. Copyright © 2017 Elsevier Ltd. All rights reserved.
Formation of Silica-Lysozyme Composites Through Co-Precipitation and Adsorption

NASA Astrophysics Data System (ADS)

van den Heuvel, Daniela B.; Stawski, Tomasz M.; Tobler, Dominique J.; Wirth, Richard; Peacock, Caroline L.; Benning, Liane G.

2018-04-01

Interactions between silica and proteins are crucial for the formation of biosilica and the production of novel functional hybrid materials for a range of industrial applications. The proteins control both precipitation pathway and the properties of the resulting silica-organic composites. Here we present data on the formation of silica-lysozyme composites through two different synthesis approaches (co-precipitation vs. adsorption) and show that the chemical and structural properties of these composites, when analyzed using a combination of synchrotron-based scattering (total scattering and SAXS), spectroscopic, electron microscopy and potentiometric methods vary dramatically. We document that while lysozyme was not incorporated into nor did its presence alter the molecular structure of silica, it strongly enhanced the aggregation of silica particles due to electrostatic and potentially hydrophobic interactions, leading to the formation of composites with characteristics differing from pure silica. The differences increased with increasing lysozyme content for both synthesis approaches. Yet, the absolute changes differ substantially between the two sets of composites, as lysozyme did not just affect aggregation during co-precipitation but also particle growth and likely polymerization during co-precipitation. Our results improve the fundamental understanding of how organic macromolecules interact with dissolved and nanoparticulate silica and how these interactions control the formation pathway of silica-organic composites from sodium silicate solutions, a widely available and cheap starting material.
Lithium recycling and cathode material regeneration from acid leach liquor of spent lithium-ion battery via facile co-extraction and co-precipitation processes.

PubMed

Yang, Yue; Xu, Shengming; He, Yinghe

2017-06-01

A novel process for extracting transition metals, recovering lithium and regenerating cathode materials based on facile co-extraction and co-precipitation processes has been developed. 100% manganese, 99% cobalt and 85% nickel are co-extracted and separated from lithium by D2EHPA in kerosene. Then, Li is recovered from the raffinate as Li 2 CO 3 with the purity of 99.2% by precipitation method. Finally, organic load phase is stripped with 0.5M H 2 SO 4 , and the cathode material LiNi 1/3 Co 1/3 Mn 1/3 O 2 is directly regenerated from stripping liquor without separating metal individually by co-precipitation method. The regenerative cathode material LiNi 1/3 Co 1/3 Mn 1/3 O 2 is miro spherical morphology without any impurities, which can meet with LiNi 1/3 Co 1/3 Mn 1/3 O 2 production standard of China and exhibits good electrochemical performance. Moreover, a waste battery management model is introduced to guarantee the material supply for spent battery recycling. Copyright © 2017 Elsevier Ltd. All rights reserved.
Structural and optical studies of Mg doped nanoparticles of chromium oxide (Cr2O3) synthesized by co-precipitation method

NASA Astrophysics Data System (ADS)

Singh, Jarnail; Verma, Vikram; Kumar, Ravi

2018-04-01

We present here the synthesization, structural and optical studies of Mg doped nanoparticles of Chromium oxide (Cr2O3) prepared using co-precipitation method. These samples were characterized using powder X-ray diffraction (XRD), Field emission scanning electron microscopy (FESEM), Raman spectroscopy and UV-Vis spectroscopy techniques. We have demonstrated that there is negligible change in optical band gap with the Mg doping. The prepared Cr2O3 nanoparticles are spherical in shape, but they are transformed into platelets when doped with Mg. The XRD studies reveal that the Mg doping in Cr2O3 doesn't affect the structure of Chromium oxide (Cr2O3).
Removal of dissolved actinides from alkaline solutions by the method of appearing reagents

DOEpatents

Krot, Nikolai N.; Charushnikova, Iraida A.

1997-01-01

A method of reducing the concentration of neptunium and plutonium from alkaline radwastes containing plutonium and neptunium values along with other transuranic values produced during the course of plutonium production. The OH.sup.- concentration of the alkaline radwaste is adjusted to between about 0.1M and about 4M. [UO.sub.2 (O.sub.2).sub.3 ].sup.4- ion is added to the radwastes in the presence of catalytic amounts of Cu.sup.+2, Co.sup.+2 or Fe.sup.+2 with heating to a temperature in excess of about 60.degree. C. or 85.degree. C., depending on the catalyst, to coprecipitate plutonium and neptunium from the radwaste. Thereafter, the coprecipitate is separated from the alkaline radwaste.
Effect of Gallium and Indium Co-Substituting on Upconversion Properties of Er/Yb:Yttrium Aluminum Garnet Powders Prepared by the Co-Precipitation Method.

PubMed

Zhang, Wei; Liang, Yun-Ling; Hu, Zheng-Fa; Feng, Zu-Yong; Lun, Ma; Zhang, Xiu-ping; Sheng, Xia; Liu, Qian; Luo, Jie

2016-04-01

Gallium and Indium co-substituted Yb, Er:YAG was fabricated through the chemical co-precipitation method. The formation process and structure of the Ga3+ and In3+ substituted phosphor powders were characterized by the X-ray diffraction, thermo-gravimetry analyzer, infrared spectra, and X-ray photoelectron spectroscopy, and the effects of Ga3+ and In3+ concentration on the luminescence properties were investigated by spectrum. The results showed that the blue shift occurred after the substitution of Ga3+ and In3+ for Al3+ in matrix, and the intensity of emission spectrum was affected by the concentration of Ga3+ and In3+.
Co-precipitation of protein and polyester as a method to isolate high molecular weight DNA.

PubMed

Dixson, Jamie D

2005-02-01

DNA isolation is often the limiting step in genetic analysis using PCR and automated fragment analysis due to low quality or purity of DNA, the need to determine and adjust DNA concentrations after isolation etc. Several protocols have been developed which are either safe and provide good quality DNA or hazardous and provide excellent quality DNA. In this brief communication I describe a new and rapid method of DNA isolation which employs the co-precipitation of protein and polyester, in the presence of acetone, to remove contaminating proteins from a lysed-tissue sample, thus leaving high quality pure DNA. The advantages of this method are increased safety over the phenol:chloroform and the chaotrophic salt methods and increased purity over the salting-out method. Since the concentrations of DNA isolated using this method are relatively consistent regardless of the amount of starting tissue (within limits), adjustments of the DNA concentrations before use as templates in PCR's are not necessary.
The effect of synthetic method and annealing temperature on metal site preference in Al(1-x)Ga(x)FeO3.

PubMed

Walker, James D S; Grosvenor, Andrew P

2013-08-05

Magnetoelectric materials couple both magnetic and electronic properties, making them attractive for use in multifunctional devices. The magnetoelectric AFeO3 compounds (Pna2(1); A = Al, Ga) have received attention as the properties of the system depend on composition as well as the synthetic method used. Al(1-x)Ga(x)FeO3. (0 ≤ x ≤ 1) was synthesized by the sol-gel and coprecipitation methods and studied by X-ray absorption near-edge spectroscopy (XANES). Al L(2,3-), Ga K-, and Fe K-edge XANES spectra were collected to examine how the average metal coordination number (CN) changes with the synthetic method. Al and Fe were found to prefer octahedral sites, while Ga prefers the tetrahedral site. It was found that composition played a larger role in determining site occupancies than synthetic method. Samples made by the sol-gel or ceramic methods (reported previously; Walker, J. D. S.; Grosvenor, A. P. J. Solid State Chem. 2013, 197, 147-153) showed smaller spectral changes than samples made via the coprecipitation method. This is attributed to greater ion mobility in samples synthesized via coprecipitation as the reactants do not have a long-range polymeric or oxide network during synthesis like samples synthesized via the sol-gel or ceramic method. Increasing annealing temperature increases the average coordination number of Al, and to a lesser extent Ga, while the average coordination number of Fe decreases. This study indicates that greater disorder is observed when the Al(1-x)Ga(x)FeO3. compounds have high Al content, and when annealed at higher temperatures.

An analytical method for hydrogeochemical surveys: Inductively coupled plasma-atomic emission spectrometry after using enrichment coprecipitation with cobalt and ammonium pyrrolidine dithiocarbamate

USGS Publications Warehouse

Hopkins, D.M.

1991-01-01

Trace metals that are commonly associated with mineralization were concentrated and separated from natural water by coprecipitation with ammonium pyrollidine dithiocarbamate (APDC) and cobalt and determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). The method is useful in hydrogeochemical surveys because it permits preconcentration near the sample sites, and selected metals are preserved shortly after the samples are collected. The procedure is relatively simple: (1) a liter of water is filtered; (2) the pH is adjusted; (3) Co chloride and APDC are added to coprecipitate the trace metals; and (4) later, the precipitate is filtered, dissolved, and diluted to 10 ml for a 100-fold concentration enrichment of the separated metals. Sb(III), As(III), Cd, Cr, Cu, Fe, Pb, Mo, Ni, Ag, V, and Zn can then be determined simultaneously by ICP-AES. In an experiment designed to measure the coprecipitation efficiency, Sb(III), Cd and Ag were recovered at 70 to 75% of their original concentration. The remaining metals were recovered at 85 to 100% of their original concentrations, however. The range for the lower limits of determination for the metals after preconcentration is 0.1 to 3.0 ??g/l. The precision of the method was evaluated by replicate analyses of a Colorado creek water and two simulated water samples. The accuracy of the method was estimated using a water reference standard (SRM 1643a) certified by the U.S. National Bureau of Standards. In addition, the method was evaluated by analyzing groundwater samples collected near a porphyry copper deposit in Arizona and by analyzing meltwater from glacier-covered areas favorable for mineralization in south-central Alaska. The results for the ICP-AES analyses compared favorably with those obtained using the sequential technique of GFAAS on the acidified but unconcentrated water samples. ICP-AES analysis of trace-metal preconcentrates for hydrogeochemical surveys is more efficient than GFAAS because a large suite of metals is simultaneously determined with acceptable analytical accuracy and precision. The proposed analytical technique can provide direct evidence of mineralization and is useful in the exploration for unknown ore deposits. ?? 1991.
pH-responsive drug delivery system based on AIE luminogen functionalized layered zirconium phosphate nano-platelets

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Dongdong, E-mail: lidongdong@jlu.edu.cn; Zhang, Yuping; Zhou, Bingbing

2015-05-15

Aggregation-induced emission (AIE) luminogen, quaternary tetraphenylethene cation (TPEN), was successfully incorporated into layered α-zirconium phosphate (α-ZrP) by using co-precipitation method to form inorganic–organic hybrid materials. The obtained materials show the characteristic hexagonal platelet shape with the interlayer distance did not reveal significant difference compared with pure α-ZrP. In addition, the obtained hybrid materials emit strong blue emission centered at 476 nm in aqueous media due to the electrostatic interactions of TPEN with the anionic framework of α-ZrP, which largely restrict their intramolecular rotation. More importantly, the materials provide a pH dependent release of doxorubicin (DOX), suggesting that AIE luminogen functionalizedmore » α-ZrP may be used as an imaging guided and pH-responsive delivery system for targeting therapy. - Graphical abstract: AIE luminogen was successfully incorporated into layered α-zirconium phosphate by a co-precipitation method to form inorganic–organic hybrid materials, showing a pH dependent release of DOX. - Highlights: • AIE luminogen cation was incorporated into layered α-ZrP by co-precipitation method. • The obtained material emits strong blue emission upon UV irradiation. • The material exhibits pH dependent release of DOX. • The AIE functionalized α-ZrP has potential applications in imaging guided therapy.« less
Coprecipitation of Arsenate and Arsenite with Green Rust Minerals

EPA Science Inventory

The objectives of this experiment were to evaluate the extent and nature of arsenic co-precipitation with green rusts and to examine the influence of arsenic incorporation on the mineralogy of formed solid phases. Stoichiometric green rusts were obtained by coprecipitation of fe...
Synthesis, characterization and adsorption properties of magnetite/reduced graphene oxide nanocomposites.

PubMed

Qi, Tingting; Huang, Chenchen; Yan, Shan; Li, Xiu-Juan; Pan, Si-Yi

2015-11-01

Three kinds of magnetite/reduced graphene oxide (MRGO) nanocomposites were prepared by solvothermal, hydrothermal and co-precipitation methods. The as-prepared nanocomposites were characterized and compared by Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction and zeta potential. The results showed that MRGO made by different methods differed in surface functional groups, crystal structure, particle sizes, surface morphology and surface charge. Due to their unlike features, these nanocomposites displayed dissimilar performances when they were used to adsorb drugs, dyes and metal ions. The MRGO prepared by the co-precipitation method showed special adsorption ability to negative ions, but those synthesized by the solvothermal method obtained the best extraction ability and reusability to the others and showed a good prospective in magnetic solid-phase extraction. Therefore, it is highly recommended to use the right preparation method before application in order to attain the best extraction performance. Copyright © 2015 Elsevier B.V. All rights reserved.
Effect of synthesis methods on the Ca{sub 3}Co{sub 4}O{sub 9} thermoelectric ceramic performances

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sotelo, A.; Rasekh, Sh.; Torres, M.A.

2015-01-15

Three different synthesis methods producing nanometric grain sizes, coprecipitation with ammonium carbonate, oxalic acid, and by attrition milling have been studied to produce Ca{sub 3}Co{sub 4}O{sub 9} ceramics and compared with the classical solid state route. These three processes have produced high reactive precursors and all the organic material and CaCO{sub 3}·have been decomposed in a single thermal treatment. Coprecipitation leads to pure Ca{sub 3}Co{sub 4}O{sub 9} phase, while attrition milling and classical solid state produce small amounts of Ca{sub 3}Co{sub 2}O{sub 6} secondary phase. Power factor values are similar for all three samples, being slightly lower for the onesmore » produced by attrition milling. These values are much higher than the obtained in samples prepared by the classical solid state method, used as reference. The maximum power factor values determined at 800 °C (∼0.43 mW/K{sup 2} m) are slightly higher than the best reported values obtained in textured ones which also show much higher density values. - Graphical abstract: Impressive raise of PF in Ca{sub 3}Co{sub 4}O{sub 9} thermoelectric materials obtained from nanometric grains. - Highlights: • Ca{sub 3}Co{sub 4}O{sub 9} has been produced by four different methods. • Precursors particle sizes influences on the final performances. • Coprecipitation methods produce single Ca{sub 3}Co{sub 4}O{sub 9} phase. • Power factor reaches values comparable to high density textured materials.« less
Modification of nanostructured calcium carbonate for efficient gene delivery.

PubMed

Zhao, Dong; Wang, Chao-Qun; Zhuo, Ren-Xi; Cheng, Si-Xue

2014-06-01

In this study, a facile method to modify nanostructured calcium carbonate (CaCO3) gene delivery systems by adding calcium phosphate (CaP) component was developed. CaCO3/CaP/DNA nanoparticles were prepared by the co-precipitation of Ca(2+) ions with plasmid DNA in the presence of carbonate and phosphate ions. For comparison, CaCO3/DNA nanoparticles and CaP/DNA co-precipitates were also prepared. The effects of carbonate ion/phosphate ion (CO3(2-)/PO4(3-)) ratio on the particle size and gene delivery efficiency were investigated. With an appropriate CO3(2-)/PO4(3-) ratio, the co-existence of carbonate and phosphate ions could control the size of co-precipitates effectively, and CaCO3/CaP/DNA nanoparticles with a decreased size and improved stability could be obtained. The in vitro gene transfections mediated by different nanoparticles in 293T cells and HeLa cells were carried out, using pGL3-Luc as a reporter plasmid. The gene transfection efficiency of CaCO3/CaP/DNA nanoparticles could be significantly improved as compared with CaCO3/DNA nanoparticles and CaP/DNA co-precipitates. The confocal microscopy study indicated that the cellular uptake and nuclear localization of CaCO3/CaP/DNA nanoparticles were significantly enhanced as compared with unmodified CaCO3/DNA nanoparticles. Copyright © 2014 Elsevier B.V. All rights reserved.
Synthesis of layered double hydroxide nanosheets by coprecipitation using a T-type microchannel reactor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pang, Xiujiang; Sun, Meiyu; Ma, Xiuming

The synthesis of Mg{sub 2}Al–NO{sub 3} layered double hydroxide (LDH) nanosheets by coprecipitation using a T-type microchannel reactor is reported. Aqueous LDH nanosheet dispersions were obtained. The LDH nanosheets were characterized by X-ray diffraction, transmission electron microscopy, atomic force microscopy and particle size analysis, and the transmittance and viscosity of LDH nanosheet dispersions were examined. The two-dimensional LDH nanosheets consisted of 1–2 brucite-like layers and were stable for ca. 16 h at room temperature. In addition, the co-assembly between LDH nanosheets and dodecyl sulfate (DS) anions was carried out, and a DS intercalated LDH nanohybrid was obtained. To the bestmore » of our knowledge, this is the first report of LDH nanosheets being directly prepared in bulk aqueous solution. This simple, cheap method can provide naked LDH nanosheets in high quantities, which can be used as building blocks for functional materials. - Graphical abstract: Layered double hydroxide (LDH) nanosheets were synthesized by coprecipitation using a T-type microchannel reactor, and could be used as basic building blocks for LDH-based functional materials. Display Omitted - Highlights: • LDH nanosheets were synthesized by coprecipitation using a T-type microchannel reactor. • Naked LDH nanosheets were dispersed in aqueous media. • LDH nanosheets can be used as building blocks for functional materials.« less
SEPARATION OF TECHNETIUM FROM AQUEOUS SOLUTIONS BY COPRECIPITATION WITH MAGNETITE

DOEpatents

Rimshaw, S.J.

1961-10-24

A method of separating technetium in the 4+ oxidation state from an aqueous basic solution containing products of uranium fission is described. The method consists of contacting the solution with finely divided magnetite and recovering a technetium-bearing precipitate. (AEC)
Synthesis and magnetic properties of bacterial cellulose—ferrite (MFe2O4, M = Mn, Co, Ni, Cu) nanocomposites prepared by co-precipitation method

NASA Astrophysics Data System (ADS)

Sriplai, Nipaporn; Mongkolthanaruk, Wiyada; Pinitsoontorn, Supree

2017-09-01

The magnetic nanocomposites based on bacterial cellulose (BC) matrix and ferrite (MFe2O4, M = Mn, Co, Ni and Cu) nanoparticles (NPs) were fabricated. The never-dried and freeze-dried BC nanofibrils were used as templates and a co-precipitation method was applied for NPs synthesis. The nanocomposites were either freeze-dried or annealed before subjected to characterization. The x-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy showed that only MnFe2O4 and CoFe2O4 NPs could be successfully incorporated in the BC nanostructures. The results also indicated that the BC template should be freeze-dried prior to the co-precipitation process. The magnetic measurement by a vibrating sample magnetometer (VSM) showed that the strongest ferromagnetic signal was found for BC-CoFe2O4 nanocomposites. The morphological investigation by a scanning electron microscope (SEM) showed the largest volume fraction of NPs in the BC-CoFe2O4 sample which was complimentary to the magnetic property measurement. Annealing resulted in the collapse of the opened nanostructure of the BC composites. Invited talk at 5th Thailand International Nanotechnology Conference (Nano Thailand-2016), 27-29 November 2016, Nakhon Ratchasima, Thailand.
Extraction and quantification of adenosine triphosphate in mammalian tissues and cells.

PubMed

Chida, Junji; Kido, Hiroshi

2014-01-01

Adenosine 5'-triphosphate (ATP) is the "energy currency" of organisms and plays central roles in bioenergetics, whereby its level is used to evaluate cell viability, proliferation, death, and energy transmission. In this chapter, we describe an improved and efficient method for extraction of ATP from tissues and cells using phenol-based reagents. The chaotropic extraction reagents reported so far co-precipitate ATP with insoluble proteins during extraction and with salts during neutralization. In comparison, the phenol-based reagents extract ATP well without the risks of co-precipitation. The extracted ATP can be quantified by the luciferase assay or high-performance liquid chromatography.
Supercritical antisolvent co-precipitation of rifampicin and ethyl cellulose.

PubMed

Djerafi, Rania; Swanepoel, Andri; Crampon, Christelle; Kalombo, Lonji; Labuschagne, Philip; Badens, Elisabeth; Masmoudi, Yasmine

2017-05-01

Rifampicin-loaded submicron-sized particles were prepared through supercritical anti-solvent process using ethyl cellulose as polymeric encapsulating excipient. Ethyl acetate and a mixture of ethyl acetate/dimethyl sulfoxide (70/30 and 85/15) were used as solvents for both drug and polymeric excipient. When ethyl acetate was used, rifampicin was crystallized separately without being embedded within the ethyl cellulose matrix while by using the ethyl acetate/dimethyl sulfoxide mixture, reduced crystallinity of the active ingredient was observed and a simultaneous precipitation of ethyl cellulose and drug was achieved. The effect of solvent/CO 2 molar ratio and polymer/drug mass ratio on the co-precipitates morphology and drug loading was investigated. Using the solvent mixture, co-precipitates with particle sizes ranging between 190 and 230nm were obtained with drug loading and drug precipitation yield from respectively 8.5 to 38.5 and 42.4 to 77.2% when decreasing the ethyl cellulose/rifampicin ratio. Results show that the solvent nature and the initial drug concentrations affect morphology and drug precipitation yield of the formulations. In vitro dissolution studies revealed that the release profile of rifampicin was sustained when co-precipitation was carried out with the solvent mixture. It was demonstrated that the drug to polymer ratio influenced amorphous content of the SAS co-precipitates. Differential scanning calorimetry thermograms and infrared spectra revealed that there is neither interaction between rifampicin and the polymer nor degradation of rifampicin during co-precipitation. In addition, stability stress tests on SAS co-precipitates were carried out at 75% relative humidity and room temperature in order to evaluate their physical stability. SAS co-precipitates were X-ray amorphous and remained stable after 6months of storage. The SAS co-precipitation process using a mixture of ethyl acetate/dimethyl sulfoxide demonstrates that this strategy can be successful for controlling rifampicin delivery. Copyright © 2017 Elsevier B.V. All rights reserved.
Fabrication of Far Red Emission Phosphors Y3Al5O12:Eu(YAG:Eu) by Co-precipitation Method

NASA Astrophysics Data System (ADS)

Thu, L. D.; Trung, D. Q.; Lam, T. D.; Anh, T. X.

2016-05-01

Phosphors YAG:Eu (with seven molar percent of Eu to YAG) was synthesized by the co-precipitation method using NH3 solution as a precipitating agent. X-ray diffraction (XRD) patterns show that the samples are single phase, and the crystallinity starts forming at a sintering temperature of 1000°C. The crystallinity increases with the increasing sintered temperature. XRD studies followed by Rietveld refinement confirmed the body center cubic structure of the host lattice. The crystalline YAG:Eu showed four emission bands of europium ion with the force dipole transition ascribed to 5D0-7F4 located at 710 nm as the most dominating group (far-red emission—FR). The ratio of FR/OR (far-red/orange—red) is about 1.24 in all samples.
Room temperature ferromagnetism and luminescent behavior of Ni doped ZnO nanoparticles prepared by coprecipitation method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Arora, Deepawali; Mahajan, Aman; Kaur, Parvinder

2016-05-23

The samples of Zn{sub 1-x}Ni{sub x}O (x= 0.00 and 0.05) were prepared using coprecipitation method and annealed at different temperatures. The effect of Ni ion substitution on the structural and optical properties has been studied using X-ray Diffraction, UV-Visible, Photoluminescence and Magnetic measurements. XRD measurements demonstrate that all the prepared samples are wurtzite polycrystalline single phase in nature, ruling out the presence of any secondary phase formation. Ultraviolet visible measurements showed a decrease in band gap with the increase in annealing temperature and doping concentration. The PL data shows the red shift in all the samples and luminescence quenching withmore » Ni doping. Compared to undoped ZnO, Ni doped ZnO showed room temperature ferromagnetism.« less
Synthetic coprecipitates of exopolysaccharides and ferrihydrite. Part II: Siderophore-promoted dissolution

NASA Astrophysics Data System (ADS)

Mikutta, Christian; Kretzschmar, Ruben

2008-02-01

Ferrihydrite (Fh) coprecipitated with exopolymers of plants and microbes may differ in its geochemical reactivity from its abiotic counterpart. We synthesized Fh in the presence and absence of acid polysaccharides (polygalacturonic acid (PGA), alginate, xanthan) and characterized the physical and structural properties of the precipitates formed [Mikutta C., Mikutta R., Bonneville S., Wagner F., Voegelin A., Christl I. and Kretzschmar R. (2008) Synthetic coprecipitates of exopolysaccharides and ferrihydrite. Part I: Characterization. Geochim. Cosmochim. Acta]. In this paper, we focus on the reactivity of PGA and alginate coprecipitates and pure Fh, and studied their interaction with the microbial siderophore desferrioxamine B (DFOB) in the presence and absence of low molecular weight organic (LMWO) acid anions (malate, citrate). Batch adsorption and dissolution experiments were performed in the dark at pH 7 in 10 mM NaClO 4 background electrolyte. In the dissolution experiments, different modes of ligand addition were applied (single, simultaneous, stepwise). With an estimated Langmuir sorption maximum of 15 mmol/mol Fe, a PGA coprecipitate with 11% C org sorbed about four times as much DFOB as pure Fh, and the amount of DFOB sorbed was ˜4-fold larger than estimated from the sum of DFOB sorption to pure Fh and PGA alone. The apparent initial dissolution rates, Rapp-initial, and pseudo-first order rate coefficients, k, of the coprecipitates exceeded those of pure Fh by up to two orders of magnitude. Citrate and malate exerted a strong synergistic effect on the DFOB-promoted dissolution of pure Fh, whereas synergistic effects of both anions were absent or negligible for the coprecipitates. Rapp-initial of the citrate and DFOB-promoted dissolution of PGA coprecipitates increased with increasing molar C/Fe ratio of the coprecipitates, independent of the charge of the LMWO ligand. Our results indicate that polyuronates stabilize Fh particles sterically and /or electrostatically, thus increasing the mineral surface area accessible to LMWO ligands. In contrast, pure Fh was coagulated at pH 7 (pH iep of Fh = 7.1), and hence only a small fraction of the Fh surface underwent dissolution. The increase in ligand-accessible surface area of Fh upon coprecipitation with acid polysaccharides seems to primarily control the kinetics of the ligand-promoted dissolution at neutral pH. In pH environments where the solubility of Fe(III) is very low, dissolution rates of Fe(III) (hydr)oxides in such coprecipitates may therefore exceed those of pure minerals by several orders of magnitude, despite a similar crystallinity of the minerals.
Preparation of La 0.75Sr 0.25Cr 0.5Mn 0.5O 3- δ fine powders by carbonate coprecipitation for solid oxide fuel cells

NASA Astrophysics Data System (ADS)

Ha, Sang Bu; Cho, Pyeong-Seok; Cho, Yoon Ho; Lee, Dokyol; Lee, Jong-Heun

A range of La 0.75Sr 0.25Cr 0.5Mn 0.5O 3- δ (LSCM) powders is prepared by the carbonate coprecipitation method for use as anodes in solid oxide fuel cells. The supersaturation ratio (R = [(NH 4) 2CO 3]/([La 3+] + [Sr 2+] + [Cr 3+] + [Mn 2+])) during the coprecipitation determines the relative compositions of La, Sr, Cr, and Mn. The composition of the precursor approaches the stoichiometric one at the supersaturation range of 4 ≤ R ≤ 12.5, whereas Sr and Mn components are deficient at R < 4 and excessive at R = 25. The fine and phase-pure LSCM powders are prepared by heat treatment at very low temperature (1000 °C) at R = 7.5 and 12.5. By contrast, the solid-state reaction requires a higher heat-treatment temperature (1400 °C). The catalytic activity of the LSCM electrodes is enhanced by using carbonate-derived powders to manipulate the electrode microstructures.
Sintering of BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta) with/without SrTiO3 Dopant

NASA Technical Reports Server (NTRS)

Dynys, F.; Sayir, A.; Heimann, P. J.

2004-01-01

The perovskite composition, BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta), displays excellent protonic conduction at high temperatures making it a desirable candidate for hydrogen separation membranes. This paper reports on the sintering behavior of BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta) powders doped with SrTiO3. Two methods were used to synthesize BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta) powders: (1) solid state reaction and (2) wet chemical co-precipitation. Co-precipitated powder crystallized into the perovskite phase at 1000 C for 4 hrs. Complete reaction and crystallization of the perovskite phase by solid state was achieved by calcining at 1200 C for 24 hrs. Solid state synthesis produced a coarser powder with an average particle size of 1.3 microns and surface area of 0.74 sq m/g. Co-precipitation produced a finer powder with a average particle size of 65 nm and surface area of 14.9 sq m/g. Powders were doped with 1, 2, 5, and 10 mole % SrTiO3. Samples were sintered at 1450 C, 1550 C and 1650 C. SrTiO3 enhances sintering, optimal dopant level is different for powders synthesized by solid state and co-precipitation. Both powders exhibit similar grain growth behavior. Dopant levels of 5 and 10 mole % SrTiO3 significantly enhances the grain size.
Aging of coprecipitated Cu in alumina: changes in structural location, chemical form, and solubility

NASA Astrophysics Data System (ADS)

Martínez, Carmen Enid; McBride, Murray B.

2000-05-01

The longterm fate of metals in mineral solid phases is not well established, as aging effects can alter metal forms and solubility. We use a model system (Cu coprecipitation with alumina) to examine copper solubility, chemical form, and structural location during longterm aging (up to 2 y), and as a function of Cu concentration, suspension pH, and rate of coprecipitate formation. Electron spin resonance (ESR) spectroscopy and extractability with EDTA were used to determine the chemical form and structural location of Cu in coprecipitates with alumina. Soluble Cu was measured by differential pulse anodic stripping voltammetry (dpasv) and alumina transformation monitored by XRD. Decreased Cu solubility resulted after prolonged aging of the coprecipitates formed at pH 6 and pH 7.5. Longterm aging (up to 2 y at 23°C) induced the transformation of an initially noncrystalline alumina to more ordered products including gibbsite. Results obtained by ESR and EDTA extraction indicate Cu movement towards the surface of the coprecipitate at increased aging time. Copper was initially evenly distributed within the alumina, but segregated at or near the alumina surface forming CuO and/or clusters after longterm reaction (2 y) with alumina.
Sample preparation for the determination of 241Am in sediments utilizing gamma-spectroscopy.

PubMed

Ristic, M; Degetto, S; Ast, T; Cantallupi, C

2002-01-01

This paper describes a procedure developed to separate americium-241 from the bulk of a sample by coprecipitation followed by high sensitivity gamma-counting of the concentrate in a well-type detector. It enables the measurement of 241Am at low concentrations, e.g. fallout levels in soils and sediments, or where large sample sizes are not available. The method is much faster and more reliable than those involving separation from other alpha-emitters, electroplating and alpha-spectrometry. A number of tracer experiments was performed in order to optimize the conditions for coprecipitation of 241Am from sediment leachates. The general outline of the determination of americium is also given.
Synthesis of highly nanoporous YBO3 architecture via a co-precipitation approach and tunable luminescent properties.

PubMed

Liu, Lili; Zhang, Xianwen; Chaudhuri, Jharna

2015-01-01

We present a simple co-precipitation method to prepare highly nanoporous YBO(3) architecture using NaBO(3) · 4H(2)O as a boric source and 600°C as the annealing temperature. The reaction was carried out under an aqueous condition without any organic solvent, surfactant, or catalysts. The prepared samples were characterized by powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The photoluminescence of doped-nanoporous YBO(3):Eu(3+) was further investigated. It is expected that highly nanoporous YBO(3) architecture can be an ideal candidate for applications in catalysis, adsorption, and optoelectronic devices. © Wiley Periodicals, Inc.
Magnetic properties of co-precipitated hexaferrite powders with Sm-Co substitutions optimized with the molten flux method

NASA Astrophysics Data System (ADS)

Serletis, C.; Litsardakis, G.; Pavlidou, E.; Efthimiadis, K. G.

2017-11-01

In this work, using the chemical coprecipitation method, Sr1-xSmxFe12-xCoxO19 (x = 0, 0.1, 0.2) hexaferrite powders were prepared. Major magnetization loops were recorded at room temperature in order to determine the correct calcination temperature for optimum hard magnetic properties. It is found that a small degree of substitution increases substantially the coercive field. Also, the use of the molten flux calcination method increases the remanent magnetization. SEM/EDXS and XRD measurements were performed at the calcined powders: the results show that a single hexaferrite phase is formed and that the substituted powders consist of an assembly of grains with a mean diameter of 40 nm. Measurements of minor magnetization loops and of the temperature and time dependence of the magnetization confirm that the powders consist of a non-oriented single domain magnetic particles assembly. The results indicate that Sm could be a viable replacement for La in the manufacturing of hexaferrites with a high-energy product.

The Effects of Secondary Oxides on Copper-Based Catalysts for Green Methanol Synthesis.

PubMed

Hayward, James S; Smith, Paul J; Kondrat, Simon A; Bowker, Michael; Hutchings, Graham J

2017-05-10

Catalysts for methanol synthesis from CO 2 and H 2 have been produced by two main methods: co-precipitation and supercritical anti-solvent (SAS) precipitation. These two methods are compared, along with the behaviour of copper supported on Zn, Mg, Mn, and Ce oxides. Although the SAS method produces initially active material with high Cu specific surface area, they appear to be unstable during reaction losing significant amounts of surface area and hence activity. The CuZn catalysts prepared by co-precipitation, however, showed much greater thermal and reactive stability than the other materials. There appeared to be the usual near-linear dependence of activity upon Cu specific area, though the initial performance relationship was different from that post-reaction, after some loss of surface area. The formation of the malachite precursor, as reported before, is important for good activity and stability, whereas if copper oxides are formed during the synthesis and ageing process, then a detrimental effect on these properties is seen.
Soil Organic Matter Stabilization via Mineral Interactions in Forest Soils with Varying Saturation Frequency

NASA Astrophysics Data System (ADS)

Possinger, A. R.; Inagaki, T.; Bailey, S. W.; Kogel-Knabner, I.; Lehmann, J.

2017-12-01

Soil carbon (C) interaction with minerals and metals through surface adsorption and co-precipitation processes is important for soil organic C (SOC) stabilization. Co-precipitation (i.e., the incorporation of C as an "impurity" in metal precipitates as they form) may increase the potential quantity of mineral-associated C per unit mineral surface compared to surface adsorption: a potentially important and as yet unaccounted for mechanism of C stabilization in soil. However, chemical, physical, and biological characterization of co-precipitated SOM as such in natural soils is limited, and the relative persistence of co-precipitated C is unknown, particularly under dynamic environmental conditions. To better understand the relationships between SOM stabilization via organometallic co-precipitation and environmental variables, this study compares mineral-SOM characteristics across a forest soil (Spodosol) hydrological gradient with expected differences in co-precipitation of SOM with iron (Fe) and aluminum (Al) due to variable saturation frequency. Soils were collected from a steep, well-drained forest soil transect with low, medium, and high frequency of water table intrusion into surface soils (Hubbard Brook Experimental Forest, Woodstock, NH). Lower saturation frequency soils generally had higher C content, C/Fe, C/Al, and other indicators of co-precipitation interactions resulting from SOM complexation, transport, and precipitation, an important process of Spodosol formation. Preliminary Fe X-ray Absorption Spectroscopic (XAS) characterization of SOM and metal chemistry in low frequency profiles suggest co-precipitation of SOM in the fine fraction (<20 µm). Short-term (10d) aerobic incubation of high and low saturation frequency soils showed greater SOC mineralization per unit soil C for low saturation frequency (i.e., higher co-precipitation) soils; however, increased mineralization may be attributed to non-mineral associated fractions of SOM. Further work to identify the component of SOM contributing to rapid mineralization using 13C-labeled substrates will link the observed chemical characteristics (13C-NMR, C K-edge XANES, and Fe XAS) of mineral-organic associations resulting from varying saturation frequency with mechanisms driving mineralization processes.
Synthetic coprecipitates of exopolysaccharides and ferrihydrite. Part I: Characterization

NASA Astrophysics Data System (ADS)

Mikutta, Christian; Mikutta, Robert; Bonneville, Steeve; Wagner, Friedrich; Voegelin, Andreas; Christl, Iso; Kretzschmar, Ruben

2008-02-01

Iron(III) (hydr)oxides formed at extracellular biosurfaces or in the presence of exopolymeric substances of microbes and plants may significantly differ in their structural and physical properties from their inorganic counterparts. We synthesized ferrihydrite (Fh) in solutions containing acid polysaccharides [polygalacturonic acid (PGA), alginate, xanthan] and compared its properties with that of an abiotic reference by means of X-ray diffraction, transmission electron microscopy, gas adsorption (N 2, CO 2), X-ray absorption spectroscopy, 57Fe Mössbauer spectroscopy, and electrophoretic mobility measurements. The coprecipitates formed contained up to 37 wt% polymer. Two-line Fh was the dominant mineral phase in all precipitates. The efficacy of polymers to precipitate Fh at neutral pH was higher for polymers with more carboxyl C (PGA ˜ alginate > xanthan). Pure Fh had a specific surface area of 300 m 2/g; coprecipitation of Fh with polymers reduced the detectable mineral surface area by up to 87%. Likewise, mineral micro- (<2 nm) and mesoporosity (2-10 nm) decreased by up to 85% with respect to pure Fh, indicative of a strong aggregation of Fh particles by polymers in freeze-dried state. C-1s STXM images showed the embedding of Fh particles in polymer matrices on the micrometer scale. Iron EXAFS spectroscopy revealed no significant changes in the local coordination of Fe(III) between pure Fh and Fh contained in PGA coprecipitates. 57Fe Mössbauer spectra of coprecipitates confirmed Fh as dominant mineral phase with a slightly reduced particle size and crystallinity of coprecipitate-Fh compared to pure Fh and/or a limited magnetic super-exchange between Fh particles in the coprecipitates due to magnetic dilution by the polysaccharides. The pH iep of pure Fh in 0.01 M NaClO 4 was 7.1. In contrast, coprecipitates of PGA and alginate had a pH iep < 2. Considering the differences in specific surface area, porosity, and net charge between the coprecipitates and pure Fh, composites of exopolysaccharides and Fe(III) (hydr)oxides are expected to differ in their geochemical reactivity from pure Fe(III) (hydr)oxides, even if the minerals have a similar crystallinity.
Photocatalytic properties of BiVO{sub 4} prepared by the co-precipitation method: Degradation of rhodamine B and possible reaction mechanisms under visible irradiation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Martinez-de la Cruz, A., E-mail: azael70@yahoo.com.mx; Perez, U.M. Garcia

2010-02-15

Bismuth vanadate (BiVO{sub 4}) was synthesized by the co-precipitation method at 200 {sup o}C. The photocatalytic activity of the oxide was tested for the photodegradation of rhodamine B under visible light irradiation. The analysis of the total organic carbon showed that the mineralization of rhodamine B over a BiVO{sub 4} photocatalyst ({approx}40% after 100 h of irradiation) is feasible. In the same way, a gas chromatography analysis coupled with mass spectroscopy revealed the existence of organic intermediates during the photodegradation process such as ethylbenzene, o-xylene, m-xylene, and phthalic anhydride. The modification of variables such as dispersion pH, amount of dissolvedmore » O{sub 2}, and irradiation source was studied in order to know the details about the photodegradation mechanism.« less
Magnetic and dielectric characterization of Co{sub 0.9}Ni{sub 0.1}Fe{sub 2}O{sub 4} prepared by hydroxide co-precipitation method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mane, S. M., E-mail: manesagar99@gmail.com; Vijaysingh Mohite Patil Mahavidyalaya Natepute, Solapur-413109; Tirmali, P. M., E-mail: pravintirmali@gmail.com

2016-04-13

Co{sub 1–x} Ni{sub x}Fe{sub 2}O{sub 4} (where x=0.1) were prepared by using the hydroxide co-precipitation method. An obtained precipitate was sintered at 1100°C by microwave sintering technique. The structural analysis confirms the single-phase cubic spinel structure with Fd-3m space group. The magnetic characterization was carried out at temperature 300K.Saturation magnetisation and coercivity is 77.22 and 908 Oe. Irreversibility is observed between the ZFC and FC curves at 100 Oe. The variation in the dielectric constant and loss tangent are studied at room temperature with increasing frequency. Continues decrease in the the dielectric constant with increasing frequency shows inverse dependence onmore » frequency. Morphological and elemental studies were done by using the scanning electron microscope with EDAX.« less
Room Temperature Gas Sensing Properties of Sn-Substituted Nickel Ferrite (NiFe2O4) Thin Film Sensors Prepared by Chemical Co-Precipitation Method

NASA Astrophysics Data System (ADS)

Manikandan, V.; Li, Xiaogan; Mane, R. S.; Chandrasekaran, J.

2018-04-01

Tin (Sn) substituted nickel ferrite (NiFe2O4) thin film sensors were prepared by a simple chemical co-precipitation method, which initially characterized their structure and surface morphology with the help of x-ray diffraction and scanning electron microscopy. Surface morphology of the sensing films reveals particles stick together with nearer particles and this formation leads to a large specific area as a large specific area is very useful for easy adsorption of gas molecules. Transmission electron microscopy and selected area electron diffraction pattern images confirm particle size and nanocrystallnity as due to formation of circular rings. Fourier transform infrared analysis has supported the presence of functional groups. The 3.69 eV optical band gap of the film was found which enabled better gas sensing. Gas sensors demonstrate better response and recovery characteristics, and the maximum response was 68.43%.
Influence of gamma-irradiation on the non-isothermal decomposition of calcium-gadolinium oxalate

NASA Astrophysics Data System (ADS)

Moharana, S. C.; Praharaj, J.; Bhatta, D.

Thermal decomposition of co-precipitated unirradiated and irradiated Ca-Gd oxalate has been studied by adopting differential thermal analysis (DTA) and thermogravimetric (TG) techniques. The reaction occurs through two stages corresponding to the decomposition of gadolinium oxalate (Gd-Ox) followed by that of calcium oxalate (Ca-Ox). The kinetic parameters for both the stages are calculated by using solid state reaction models and Coats-Redfern's equation. The co-precipitation as well as irradiation alter the DTA peak temperatures and the kinetic parameters of Ca-Ox. The decomposition of Gd-Ox follows the two dimensional Contracting area (R-2) mechanism, while that of Ca-Ox follows the Avrami-Erofeev (A(2)) mechanism (n =2), which are also exhibited by the co-precipitated and irradiated samples. Co-precipitation decreases the energy of activation and the pre-exponential factor of the individual components but the reverse phenomenon takes place upon irradiation of the co-precipitate. The mechanisms underlying the phenomena are explored.
Enhanced removal of arsenic from a highly laden industrial effluent using a combined coprecipitation/nano-adsorption process.

PubMed

Jiang, Yingnan; Hua, Ming; Wu, Bian; Ma, Hongrui; Pan, Bingcai; Zhang, Quanxing

2014-05-01

Effective arsenic removal from highly laden industrial wastewater is an important but challenging task. Here, a combined coprecipitation/nano-adsorption process, with ferric chloride and calcium chloride as coprecipitation agents and polymer-based nanocomposite as selective adsorbent, has been validated for arsenic removal from tungsten-smelting wastewater. On the basis of operating optimization, a binary FeCl3 (520 mg/L)-CaCl2 (300 mg/L) coprecipitation agent could remove more than 93% arsenic from the wastewater. The resulting precipitate has proved environmental safety based on leaching toxicity test. Fixed-bed column packed with zirconium or ferric-oxide-loaded nanocomposite was employed for further elimination of arsenic in coprecipitated effluent, resulting in a significant decrease of arsenic (from 0.96 to less than 0.5 mg/L). The working capacity of zirconium-loaded nanocomposite was 220 bed volumes per run, much higher than that of ferric-loaded nanocomposite (40 bed volumes per run). The exhausted zirconium-loaded nanocomposite could be efficiently in situ regenerated with a binary NaOH-NaCl solution for reuse without any significant capacity loss. The results validated the combinational coprecipitation/nano-adsorption process to be a potential alternative for effective arsenic removal from highly laden industrial effluent.
Fe-based Fischer Tropsch Synthesis of biomass-derived syngas: Effect of synthesis method

Treesearch

Khiet Mai; Thomas Elder; Les Groom; James J. Spivey

2015-01-01

Two 100Fe/4Cu/4K/6Zn catalysts were prepared using two different methods: coprecipitation or impregnation methods. The effect of the preparation methods on the catalyst structure, catalytic properties, and the conversion of biomass-derived syngas via FischerâTropsch synthesis was investigated. Syngas was derived from gasifying Southern pine woodchips and had the...
Pulsed laser deposition of functionalized Mg-Al layered double hydroxide thin films

NASA Astrophysics Data System (ADS)

Vlad, A.; Birjega, R.; Tirca, I.; Matei, A.; Mardare, C. C.; Hassel, A. W.; Nedelcea, A.; Dinescu, M.; Zavoianu, R.

2018-02-01

In this paper, magnesium-aluminium layered double hydroxide (LDH) has been functionalized with sodium dodecyl sulfate (DS) and deposited as thin film by pulsed laser deposition (PLD). Mg, Al-LDH powders were prepared by co-precipitation and used as reference material. Intercalation of DS as an anionic surfactant into the LDHs host layers has been prepared in two ways: co-precipitation (P) and reconstruction (R). DS intercalation occurred in LDH powder via both preparation methods. The films deposited via PLD, in particular at 532 and 1064 nm, preserve the organic intercalated layered structure of the targets prepared from these powders. The results reveal the ability of proposed deposition technique to produce functional composite organo-modified LDHs thin films.
Tunable Properties of Exfoliated Polyvinylalcohol Nanocomposites by In Situ Coprecipitation of Layered Double Hydroxides

NASA Astrophysics Data System (ADS)

Liu, Jiajia; Yuen, Richard K. K.; Hu, Yuan

2017-10-01

Poly(vinyl alcohol) (PVA) nanocomposites were prepared by a “one step” method based on the coprecipitation of layered double hydroxide (LDH) nanosheets in the polymer aqueous solution. The morphology, fire resistance properties, mechanical and optical properties of the PVA/LDH nanocomposites were studied. The LDH nanosheets were homogeneously dispersed in the PVA matrix as indicated by X-ray diffraction (XRD) pattern and transmission electron microscopy (TEM) characterization. Meanwhile, the peak of heat release rate (pHRR) and total heat release (THR) were decreased by 58% and 28%, respectively. Storage modulus at 30 °C was increased, and the transmittance of more than 90% at the visible region was obtained upon addition of 5 wt% LDH.
Structural and optical properties of co-precipitated copper doped zinc oxide

NASA Astrophysics Data System (ADS)

Pandey, Devendra K.; Modi, Anchit; Pandey, Padmini; Gaur, N. K.

2018-05-01

We have synthesized pure and copper doped zinc oxide Zn1-xO:Cux (x = 0, 0.03) powder by wet chemical co-precipitation method followed by sintering of the co-precipitated amorphous phase powder at 450°C for 4 hours. The experiment is performed to recognize the effect of nominal doping of transition metal over the structural, morphological and optical properties. The structural parameters are observed by using Rietveld refinement of X-ray diffraction data which clearly represents that Cu ion is perfectly incorporated at the Zn site with minimal distortions within the lattice. The crystallite size is estimated by Debye-Scherrer and Hall-Williamson formulation. The particle morphology and size is determined with scanning electron microscopic (SEM) technique. The band gap and optical measurements are carried out with UV-visible absorption and photoluminescence (PL) spectroscopic technique, respectively. Enhanced PL spectral response is observed for ZnO:Cu along with non-radiative transitions from conduction band to valence band. The energy levels near the conduction band that are commonly involved in the optoelectronic transitions in the UV-region are traced by using absorption and luminescence spectral graphs.
Site-specific incorporation of uranyl carbonate species at the calcite surface

NASA Astrophysics Data System (ADS)

Reeder, Richard J.; Elzinga, Evert J.; Tait, C. Drew; Rector, K. D.; Donohoe, Robert J.; Morris, David E.

2004-12-01

Spatially resolved luminescence spectra from U(VI) co-precipitated at the (101¯4) growth surface of synthetic calcite single crystals confirm heterogeneous incorporation corresponding to the distribution of structurally non-equivalent steps composing the vicinal surfaces of spiral growth hillocks. Spectral structure from U(VI) luminescence at the "-" vicinal regions and featureless, weak luminescence at the "+" vicinal regions are consistent with previously reported observations of enrichment at the former sites during calcite growth. Luminescence spectra differ between the non-equivalent regions of the crystal, with the spectral features from the "-" vicinal region corresponding to those observed in bulk calcite samples. Subtle spectral shifts are observed from U(VI) co-precipitated with microcrystalline calcite synthesized by a different method, and all of the U(VI)-calcite sample spectra differ significantly from that of U(VI) co-precipitated with aragonite. The step-selective incorporation of U(VI) can be explained by a proposed model in which the allowed orientation for adsorption of the dominant calcium uranyl triscarbonate species is controlled by the atomic arrangement at step edges. Differences in the tilt angles of carbonate groups between non-equivalent growth steps favor adsorption of the calcium uranyl triscarbonate species at "-" steps, as observed in experiments.
Properties and reactivity of Fe-organic matter associations formed by coprecipitation versus adsorption: Clues from arsenate batch adsorption

NASA Astrophysics Data System (ADS)

Mikutta, Robert; Lorenz, Dennis; Guggenberger, Georg; Haumaier, Ludwig; Freund, Anja

2014-11-01

Ferric oxyhydroxides play an important role in controlling the bioavailability of oxyanions such as arsenate and phosphate in soil. Despite this, little is known about the properties and reactivity of Fe(III)-organic matter phases derived from adsorption (reaction of organic matter (OM) to post-synthesis Fe oxide) versus coprecipitation (formation of Fe oxides in presence of OM). Coprecipitates and adsorption complexes were synthesized at pH 4 using two natural organic matter (NOM) types extracted from forest floor layers (Oi and Oa horizon) of a Haplic Podzol. Iron(III) coprecipitates were formed at initial molar metal-to-carbon (M/C) ratios of 1.0 and 0.1 and an aluminum (Al)-to-Fe(III) ratio of 0.2. Sample properties were studied by X-ray diffraction, X-ray photoelectron spectroscopy (XPS), N2 gas adsorption, dynamic light scattering, and electrophoretic mobility measurements. Arsenic [As(V)] adsorption to Fe-OM phases was studied in batch experiments (168 h, pH 4, 100 μM As). The organic carbon (OC) contents of the coprecipitates (82-339 mg g-1) were higher than those of adsorption complexes (31 and 36 mg g-1), leading to pronounced variations in specific surface area (9-300 m2 g-1), average pore radii (1-9 nm), and total pore volumes (11-374 mm3 g-1) but being independent of the NOM type or the presence of Al. The occlusion of Fe solids by OM (XPS surface concentrations: 60-82 atom% C) caused comparable pHPZC (1.5-2) of adsorption complexes and coprecipitates. The synthesis conditions resulted in different Fe-OM association modes: Fe oxide particles in 'M/C 0.1' coprecipitates covered to a larger extent the outermost aggregate surfaces, for some 'M/C 1.0' coprecipitates OM effectively enveloped the Fe oxides, while OM in the adsorption complexes primarily covered the outer aggregate surfaces. Despite of their larger OC contents, adsorption of As(V) was fastest to coprecipitates formed at low Fe availability (M/C 0.1) and facilitated by desorption of weakly bonded OC and disaggregation. In contrast, 'M/C 1.0' coprecipitates showed a comparable rate of As uptake as the adsorption complexes. While small mesopores (2-10 nm) promoted the fast As uptake particularly to 'M/C 0.1' coprecipitates, the presence of micropores (<2 nm) appeared to impair As desorption. This study shows that the environmental reactivity of poorly crystalline Fe(III) oxides in terrestrial and aquatic systems can largely vary depending on the formation conditions. Carbon-rich Fe phases precipitated at low M/C ratios may play a more important role in oxyanion immobilization and Fe and C cycling than phases formed at higher M/C ratios or respective adsorption complexes.
Structure and composition of Fe-OM co-precipitates that form in soil-derived solutions

NASA Astrophysics Data System (ADS)

Fritzsche, Andreas; Schröder, Christian; Wieczorek, Arkadiusz K.; Händel, Matthias; Ritschel, Thomas; Totsche, Kai U.

2015-11-01

Iron oxides represent a substantial fraction of secondary minerals and particularly affect the reactive properties of natural systems in which they formed, e.g. in soils and sediments. Yet, it is still obscure how transient conditions in the solution will affect the properties of in situ precipitated Fe oxides. Transient compositions, i.e. compositions that change with time, arise due to predominant non-equilibrium states in natural systems, e.g. between liquid and solid phases in soils. In this study, we characterize Fe-OM co-precipitates that formed in pH-neutral exfiltrates from anoxic topsoils under transient conditions. We applied soil column outflow experiments, in which Fe2+ was discharged with the effluent from anoxic soil and subsequently oxidized in the effluent due to contact with air. Our study features three novel aspects being unconsidered so far: (i) the transient composition of soil-derived solutions, (ii) that pedogenic Fe oxides instead of Fe salts serve as major source for Fe2+ in soil solution and (iii) the presence of exclusively soil-derived organic and inorganic compounds during precipitation. The experiments were carried out with two topsoil materials that differed in composition, texture and land use. Derived from Mössbauer spectroscopy, broad distributions in quadrupole splittings (0-2 mm s-1) and magnetic hyperfine fields (35-53 T) indicated the presence of low-crystalline ferrihydrite and even lower crystalline Fe phases in all Fe-OM co-precipitates. There was no unequivocal evidence for other Fe oxides, i.e. lepidocrocite and (nano)goethite. The Fe-OM co-precipitates contained inorganic (P, sulfate, silicate, Al, As) and organic compounds (proteins, polysaccharides), which were concurrently discharged from the soils. Their content in the Fe-OM co-precipitates was controlled by their respective concentration in the soil-derived solution. On a molar basis, OC and Fe were the main components in the Fe-OM co-precipitates (OC/Fe ratio = 0.5-2). The elemental composition of the Fe-OM co-precipitates was in accordance with the sequential precipitation of Fe(III)phosphates/arsenates prior to the formation of ferrihydrite. This explains decreasing Si contents in the Fe-OM co-precipitates with increasing availability of P. With respect to constant mean quadrupole splittings and slightly decreasing mean magnetic hyperfine fields, increasing contents of OC, P and Al in the Fe-OM co-precipitates did not further increase the structural disorder of the Fe polyhedra, while the crystallite interactions slightly decreased. Scanning electron microscopy and dynamic light scattering revealed the coincidental presence of variably sized aggregates and a considerable amount of Fe-OM co-precipitates, which remained dispersed in solution for months. Thus, variably composed Fe-OM co-precipitates with highly diverse aggregate sizes and comparably constant poor crystallinity can be expected after the oxidation of Fe2+ in transient, soil-derived solutions.
Size-regulated group separation of CoFe2O4 nanoparticles using centrifuge and their magnetic resonance contrast properties

NASA Astrophysics Data System (ADS)

Kang, Jongeun; Lee, Hyunseung; Kim, Young-Nam; Yeom, Areum; Jeong, Heejeong; Lim, Yong Taik; Hong, Kwan Soo

2013-09-01

Magnetic nanoparticle (MNP)-based magnetic resonance imaging (MRI) contrast agents (CAs) have been the subject of extensive research over recent decades. The particle size of MNPs varies widely and is known to influence their physicochemical and pharmacokinetic properties. There are two commonly used methods for synthesizing MNPs, organometallic and aqueous solution coprecipitation. The former has the advantage of being able to control the particle size more effectively; however, the resulting particles require a hydrophilic coating in order to be rendered water soluble. The MNPs produced using the latter method are intrinsically water soluble, but they have a relatively wide particle size distribution. Size-controlled water-soluble MNPs have great potential as MRI CAs and in cell sorting and labeling applications. In the present study, we synthesized CoFe2O4 MNPs using an aqueous solution coprecipitation method. The MNPs were subsequently separated into four groups depending on size, by the use of centrifugation at different speeds. The crystal shapes and size distributions of the particles in the four groups were measured and confirmed by transmission electron microscopy and dynamic light scattering. Using X-ray diffraction analysis, the MNPs were found to have an inverse spinel structure. Four MNP groups with well-selected semi-Gaussian-like diameter distributions were obtained, with measured T2 relaxivities ( r 2) at 4.7 T and room temperature in the range of 60 to 300 mM-1s-1, depending on the particle size. This size regulation method has great promise for applications that require homogeneous-sized MNPs made by an aqueous solution coprecipitation method. Any group of the CoFe2O4 MNPs could be used as initial base cores of MRI T2 CAs, with almost unique T2 relaxivity owing to size regulation. The methodology reported here opens up many possibilities for biosensing applications and disease diagnosis.
Lithium-Rich Nanoscale Li 1.2 Mn 0.54 Ni 0.13 Co 0.13 O 2 Cathode Material Prepared by Co-Precipitation Combined Freeze Drying (CP-FD) for Lithium-Ion Batteries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bai, Ying; Li, Yu; Wu, Chuan

Nanoscale Li-rich Li1.2Mn0.54Ni0.13Co0.13O2 material is synthesized by a co-precipitation combined freeze drying (CP-FD) method, and compared with a conventional co-precipitation method combined vacuum drying (CP-VD). With the combination of X-ray diffraction (XRD) and scanning electron microscopy (SEM), it is found that the sample from CP-FD method consists of a pure phase with good crystallinity and small, homogenous particles (100-300 nm) with uniform particle size distribution. Inductively coupled plasma spectroscopy (ICP) shows that the sample has a stoichiometric ratio of n((Li)): n((Mn)): n((Ni)): n((Co))=9: 4: 1: 1; and its Brunauer-Emmett-Teller (BET) specific surface area is 5.749 m(2)g(-1). This sample achieves excellentmore » electrochemical properties: its initial discharge capacities are 298.9 mAhg(-1) at 0.1C (20 mAg(-1)), 246.1 mAhg(-1) at 0.5C, 215.8 mAhg(-1) at 1C, and 154.2 mAhg(-1) at 5C (5C charge and 5C discharge), as well as good cycling performance. In addition, the Li+ chemical diffusion coefficient of Li1.2Mn0.54Ni0.13Co0.13O2 material prepared by the CP-FD method is 4.59 x 10(-11) cm(2) s(-1), which is higher than that of the Li1.2Mn0.54Ni0.13Co0.13O2 material prepared by CP-VD. This phenomenon illustrates the potential for Li1.2Mn0.54Ni0.13Co0.13O2 with good rate performance synthesized by CP-FD method.« less
One-step synthesis and characterizations of cerium oxide nanoparticles in an ambient temperature via Co-precipitation method

NASA Astrophysics Data System (ADS)

Pujar, Malatesh S.; Hunagund, Shirajahammad M.; Desai, Vani R.; Patil, Shivaprasadgouda; Sidarai, Ashok H.

2018-04-01

We report the simple Co-precipitation method for the synthesis of Cerium oxide (CeO2) nanoparticles (NPs) in an ambient temperature. We have taken the Cerium (III) nitrate hexahydrate (Ce(NO3)3.6H2O) and Sodium hydroxide (NaOH) as the precursors. The obtained NPs were analyzed using the UV-Vis spectrophotometer, Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The obtained results signify that UV-Vis spectrum exhibited a well-defined absorption peak at 274 nm and the estimated energy gap (Eg) is 4.05 eV. The FT-IR analysis provides the supporting evidence for the presence of bonding of O-H, nitrates, alcohols and O-Ce-O vibrations. The XRD result reveals that the synthesized CeO2 NPs was crystallite with cubic phase structure and the estimated average crystallite size of CeO2 NPs using Scherer's and W-H method was significantly different due to their assumptions. Further, it is purposed to study their photocatalytic biological activities.
Variation of Strontium (Sr) in the Ferroelectric Material Barium Strontium Titanate (Ba1-xSrxTiO3) by Co precipitation Method

NASA Astrophysics Data System (ADS)

Subarwanti, Y.; Safitri, R. D.; Supriyanto, A.; Iriani, Y.; Jamaludin, A.

2017-02-01

Barium Strontium Titanate (BST) have been made with variation strontium (Sr) 10%, 30% and 50% by co-precipitation method. This study aims to determine influence addition Sr against the crystal structure, crystallite size, lattice parameter, grain size and dielectric constant. Samples have been made by co-precipitation method and then the samples were sintered by furnace at 1100°C with holding time 4 hours. Characterization of BST use X-Ray Diffraction instrument, Scanning Electron Microscopy and Resistance Capacitance Inductance (RCL meter). Based on result obtained, the larger Sr content cause the diffraction angle shift to the right (the greater) and crystallinity increasing. But, the value of dielectric constant, crystallite size and grain size decreasing with additional Sr content. Measurement of dielectric constant (K) performed in the frequency range 1 kHz to 100 kHz and the highest value at Sr content 0.1 i.e. 258.35. The addition of Sr content 30% and 50% change the crystal structure from tetragonal to cubic which has paraelectric phase.
PREPARATION OF FLOWER-LIKE Co3O4/Fe3O4 MAGNETIC MICROSPHERES FOR PHOTODEGRADATION OF RhB UNDER UV LIGHT

NASA Astrophysics Data System (ADS)

Zhang, Baoliang; Zhang, Hepeng; Zhou, Lunwei; Ali, Nisar; Geng, Wangchang; Zhang, Qiuyu

2013-07-01

Flower-like Co3O4/Fe3O4 magnetic microspheres were prepared by coprecipitation of Fe2+ and Fe3+ in presence of flower-like Co3O4 microspheres as template. The preparation process included three steps: preparation of flower-like Co3O4 microspheres by hydrothermal method; immersion of Fe2+ and Fe3+ ions; coprecipitation in the presence of OH-. Rhodamine B (RhB) was chosen as model pollutants to investigate the photodegradation capacities of Co3O4/Fe3O4 magnetic microspheres. The results showed that the microspheres exhibited excellent degradation property and can be recycled to use again. After four times use the degradation efficiency was still above 90%.

An innovative carbonate coprecipitation process for the removal of zinc and manganese from mining impacted waters

USGS Publications Warehouse

Sibrell, P.L.; Chambers, M.A.; Deaguero, A.L.; Wildeman, T.R.; Reisman, D.J.

2007-01-01

Although mine drainage is usually thought of as acidic, there are many cases where the water is of neutral pH, but still contains metal species that can be harmful to human or aquatic animal health, such as manganese (Mn) and zinc (Zn). Typical treatment of mine drainage waters involves pH adjustment, but this often results in excessive sludge formation and removal of nontoxic species such as magnesium and calcium. Theoretical consideration of the stability of metal carbonate species suggests that the target metals could be removed from solution by coprecipitation with calcium carbonate. The U.S. Geological Survey has developed a limestone-based process for remediation of acid mine drainage that increases calcium carbonate saturation. This treatment could then be coupled with carbonate coprecipitation as an innovative method for removal of toxic metals from circumneutral mine drainage waters. The new process was termed the carbonate coprecipitation (CCP) process. The CCP process was tested at the laboratory scale using a synthetic mine water containing 50 mg/L each of Mn and Zn. Best results showed over 95% removal of both Mn and Zn in less than 2 h of contact in a limestone channel. The process was then tested on a sample of water from the Palmerton zinc superfund site, near Palmerton, Pennsylvania, containing over 300 mg/L Zn and 60 mg/L Mn. Treatment of this water resulted in removal of over 95% of the Zn and 40% of the Mn in the limestone channel configuration. Because of the potential economic advantages of the CCP process, further research is recommended for refinement of the process for the Palmerton water and for application to other mining impacted waters as well. ?? Mary Ann Liebert, Inc.
Continuous flow hydrogenation of nitroarenes, azides and alkenes using maghemite-Pd nanocomposites

EPA Science Inventory

Maghemite-supported ultra-fine Pd (1-2 nm) nanoparticles, prepared by a simple co-precipitation method, find application in the catalytic continuous flow hydrogenation of nitroarenes, azides, and alkenes wherein they play an important role in reduction of various functional group...
Synthesis of YAG nanopowder by the co-precipitation method: Influence of pH and study of the reaction mechanisms

NASA Astrophysics Data System (ADS)

Marlot, Caroline; Barraud, Elodie; Le Gallet, Sophie; Eichhorn, Marc; Bernard, Frédéric

2012-07-01

YAG nanopowders with an average grain size of 30 nm have been successfully synthesized by the co-precipitation method using nitrates with precipitant of ammonium hydrogen carbonate. The influence of precipitation conditions such as pH, aging time and calcination temperature on the formation of secondary phases has been studied. The accurate control of pH value at every stage of precipitation process is crucial to avoid the presence of YAM (Yttrium Aluminium Monoclinic, Y4Al2O9) and yttrium oxide (Y2O3) after calcination. The reaction mechanisms have been investigated using different techniques such as infrared spectroscopy, x-ray diffraction and thermal analyses. The YAG phase is formed around 1050 °C passing through an intermediate phase called YAP (Yttrium Aluminium Perovskite, YAlO3). Local chemical heterogeneities are responsible for the deviation of the Y:Al ratio and the formation of YAP during heat treatment.
Preparation of LuAG Powders with Single Phase and Good Dispersion for Transparent Ceramics Using Co-Precipitation Method

PubMed Central

Pan, Liangjie; Jiang, Benxue; Fan, Jintai; Yang, Qiuhong; Zhou, Chunlin; Zhang, Pande; Mao, Xiaojian; Zhang, Long

2015-01-01

The synthesis of pure and well dispersed lutetium aluminum garnet (LuAG) powder is crucial and important for the preparation of LuAG transparent ceramics. In this paper, high purity and well dispersed LuAG powders have been synthesized via co-precipitation method with lutetium nitrate and aluminum nitrate as raw materials. Ammonium hydrogen carbonate (AHC) was used as the precipitant. The influence of aging time, pH value, and dripping speed on the prepared LuAG powders were investigated. It showed that long aging duration (>15 h) with high terminal pH value (>7.80) resulted in segregation of rhombus Lu precipitate and Al precipitate. By decreasing the initial pH value or accelerating the dripping speed, rhombus Lu precipitate was eliminated and pure LuAG nano powders were synthesized. High quality LuAG transparent ceramics with transmission >75% at 1064 nm were fabricated using these well dispersed nano LuAG powders. PMID:28793510
Preparation and characterization of polyol assisted ultrafine Cu-Ni-Mg-Ca mixed ferrite via co-precipitation method

NASA Astrophysics Data System (ADS)

Boobalan, T.; Pavithradevi, S.; Suriyanarayanan, N.; Manivel Raja, M.; Ranjith Kumar, E.

2017-04-01

Nanocrystalline spinel ferrite of composition Cu0.2Ni0.2Mg0.2Ca0.4Fe2O4 is synthesized by wet hydroxyl co-precipitation method in ethylene glycol as chelating agent and sodium hydroxide as precipitator at pH 8. Ethylene glycol is utilized as the medium which serves as the dissolvable and in addition a complexing specialist. The synthesized particles are annealed at various temperatures. Thermogravimetric investigation affirms that at 280 °C ethylene glycol is dissipated totally and stable phase arrangement happens over 680 °C. FTIR spectra of as synthesized and annealed at 1050 °C recorded between 400 cm-1 and 4000 cm-1. Structural characterizations of all the samples are carried out by X-ray diffraction (XRD) technique. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) affirm that the particles are spherical and cubic shape with the crystallite size of 12 nm to 32 nm. Magnetic measurements are performed utilizing vibrating sample magnetometer at room temperature.
Preparation of LuAG Powders with Single Phase and Good Dispersion for Transparent Ceramics Using Co-Precipitation Method.

PubMed

Pan, Liangjie; Jiang, Benxue; Fan, Jintai; Yang, Qiuhong; Zhou, Chunlin; Zhang, Pande; Mao, Xiaojian; Zhang, Long

2015-08-19

The synthesis of pure and well dispersed lutetium aluminum garnet (LuAG) powder is crucial and important for the preparation of LuAG transparent ceramics. In this paper, high purity and well dispersed LuAG powders have been synthesized via co-precipitation method with lutetium nitrate and aluminum nitrate as raw materials. Ammonium hydrogen carbonate (AHC) was used as the precipitant. The influence of aging time, pH value, and dripping speed on the prepared LuAG powders were investigated. It showed that long aging duration (>15 h) with high terminal pH value (>7.80) resulted in segregation of rhombus Lu precipitate and Al precipitate. By decreasing the initial pH value or accelerating the dripping speed, rhombus Lu precipitate was eliminated and pure LuAG nano powders were synthesized. High quality LuAG transparent ceramics with transmission >75% at 1064 nm were fabricated using these well dispersed nano LuAG powders.
The effect of precipitants on Ni-Al2O3 catalysts prepared by a co-precipitation method for internal reforming in molten carbonate fuel cells

PubMed Central

Jung, You-Shick; Yoon, Wang-Lai; Seo, Yong-Seog; Rhee, Young-Woo

2012-01-01

Ni-Al2O3 catalysts are prepared via the co-precipitation method using various precipitants: urea, Na2CO3, NaOH, K2CO3, KOH and NH4OH. The effects of the precipitants on the physicochemical properties and catalytic activities of the Ni-Al2O3 catalysts are investigated. The Ni50-urea catalyst displays the largest specific surface area and the highest pore volume. This catalyst also exhibits the highest Ni dispersion and the largest Ni surface area. Ni50-urea catalyst prepared with urea as precipitant and Ni50-K2CO3 catalyst prepared with K2CO3 as precipitant exhibit high pore volumes and good catalytic activities for methane steam reforming. The Ni50-urea catalyst exhibits the best physicochemical properties and shows good catalytic activity and a strong resistance to electrolyte contamination. PMID:22962548
Strontium Co-precipitation During Biomineralization of Calcite in Porous Media Using Differing Treatment Strategies

NASA Astrophysics Data System (ADS)

Lauchnor, E. G.; Schultz, L.; Mitchell, A.; Cunningham, A. B.; Gerlach, R.

2013-12-01

The process of ureolytically-induced calcium carbonate mineralization has been shown in laboratory studies to be effective in co-precipitation of heavy metals and radionuclides. During this process, the microbially catalyzed hydrolysis of urea increases alkalinity and pH, thus promoting CaCO3 precipitation in the presence of dissolved calcium. One proposed application of biomineralization includes the remediation of radionuclides such as strontium, which can be co-precipitated in situ within calcite. Strontium is of concern at several US DOE sites where it is a radioactive product of uranium fission and groundwater contaminant. Our research focuses on promoting attached bacteria, or biofilms, in subsurface environments where they serve as immobilized catalysts in biomineralization and can aide in co-precipitation of some contaminants. In this work, flat plate reactors with 1 mm etched flow channels designed to mimic a porous medium environment were used. Reactors were inoculated with the model ureolytic bacterium Sporosarcina pasteurii and addition of urea, calcium and strontium containing fluid was performed to induce biomineralization. Continuous flow and stopped-flow injection strategies were investigated to evaluate differences in strontium co-precipitation efficiency. During stopped-flow experiments, injection of cementation fluid containing urea, Ca2+ and Sr2+ was alternated with growth nutrients for stimulation of microbial activity. Control parameters such as urea and calcium concentration and injection flow rate are currently being varied to optimize rate and efficiency of strontium co-precipitation. Ureolytically induced calcite precipitation and strontium incorporation in the calcite was verified by chemical and mineralogical analyses, including X-ray diffraction and ICP-MS. Strontium co-precipitation efficiency was similar under different injection strategies. Alternating calcium-containing fluid with growth nutrients allowed for continued viability of the ureolytic biofilms and also insured that bacterially-induced mineralization was still occurring after 60 days of operation. Batch rate experiments demonstrated the effective use of alternative sources of substrates for biomineralization, which are economical for use in field-scale remediation. Fertilizer has been shown to be an effective urea source and several economical carbon and nutrient sources such as molasses and whey are being evaluated for stimulating ureolytic microorganisms. This research demonstrates on a bench scale the use of different injection strategies to control precipitation of calcium carbonate, as well as the feasibility of strontium co-precipitation in porous media. The ongoing optimization of strontium co-precipitation will lead to additional work on potential remediation of other heavy metal groundwater contaminants.
Application of microscopy technology in thermo-catalytic methane decomposition to hydrogen

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mei, Irene Lock Sow, E-mail: irene.sowmei@gmail.com; Lock, S. S. M., E-mail: serenelock168@gmail.com; Abdullah, Bawadi, E-mail: bawadi-abdullah@petronas.com.my

2015-07-22

Hydrogen production from the direct thermo-catalytic decomposition of methane is a promising alternative for clean fuel production because it produces pure hydrogen without any CO{sub x} emissions. However, thermal decomposition of methane can hardly be of any practical and empirical interest in the industry unless highly efficient and effective catalysts, in terms of both specific activity and operational lifetime have been developed. In this work, bimetallic Ni-Pd on gamma alumina support have been developed for methane cracking process by using co-precipitation and incipient wetness impregnation method. The calcined catalysts were characterized to determine their morphologies and physico-chemical properties by usingmore » Brunauer-Emmett-Teller method, Field Emission Scanning Electron Microscopy, Energy-dispersive X-ray spectroscopy and Thermogravimetric Analysis. The results suggested that that the catalyst which is prepared by the co-precipitation method exhibits homogeneous morphology, higher surface area, have uniform nickel and palladium dispersion and higher thermal stability as compared to the catalyst which is prepared by wet impregnation method. This characteristics are significant to avoid deactivation of the catalysts due to sintering and carbon deposition during methane cracking process.« less
Determination of heavy metals by ICP-OES and F-AAS after preconcentration with 2,2'-bipyridyl and erythrosine.

PubMed

Feist, Barbara; Mikula, Barbara; Pytlakowska, Katarzyna; Puzio, Bozena; Buhl, Franciszek

2008-04-15

The applicability of 2,2'-bipyridyl and erythrosine co-precipitation method for the separation and preconcentration of some heavy metals, such as Cd, Co, Cu, Ni, Pb and Zn in actual samples for their determination by ICP-OES and F-AAS was studied. Experimental conditions influencing the recovery of the investigated metals, such as pH, molar ratio of 2,2'-bipyridyl to erythrosine, the effect of time on co-precipitation were optimized. The analytical characteristics of the method (e.g. limit of detection, sensitivity, linear range and preconcentration factor) were obtained. The limits of detection LOD (ng mL(-1)) of the ICP-OES (F-AAS) method were: Cd: 4.0 (7.75), Co: 3.1 (57.2), Cu: 18 (10.3), Ni 21.3 (32.8), Pb: 35.9 (29.2) and Zn: 10.2 (6.90). The recovery of all the elements tested was more than 93%. The influence of inorganic matrix was examined. The proposed method was applied to determination of Cd, Co, Cu, Ni, Pb and Zn in vegetables and certified reference material (NCS ZC85006 Tomato).
Triethylamine-assisted Mg(OH)2 coprecipitation/preconcentration for determination of trace metals and rare earth elements in seawater by inductively coupled plasma mass spectrometry (ICP-MS).

PubMed

Arslan, Zikri; Oymak, Tulay; White, Jeremy

2018-05-30

In this paper, we report an improved magnesium hydroxide, Mg(OH) 2 , coprecipitation method for the determination of 16 trace elements (Al, V, Cr, Mn, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Sb, Sn and Pb) and 18 rare earth elements (REEs), including Sc, Y, U and Th in seawater and estuarine water samples. The procedure involves coprecipitation of the trace elements and REEs on Mg(OH) 2 upon addition of a small volume of triethylamine (TEA) followed by analysis of the dissolved pellet solutions by inductively coupled plasma mass spectrometry (ICP-MS). Three-step sequential coprecipitation was carried out on 10 mL aliquots of seawater to eliminate the matrix ions and to preconcentrate the analytes of interest into a 1 mL final volume. Spike recoveries varied from 85% (Th) to 105% (Y). Calcium (Ca), sodium (Na) and potassium (K) matrices were virtually eliminated from the analysis solutions. Collision reaction interface (CRI) technology utilizing H 2 and He gases was employed to determine its effectiveness in removing the spectral interferences originating from the residual Mg matrix, TEA and plasma gases. H 2 was more effective than He in reducing spectral interferences from TEA and plasma gases. Limits of detection (LODs) ranged from 0.01 ng L -1 (Ho) to 72 ng L -1  (Al). The method was validated by using certified seawater (CASS-4) and estuarine water (SLEW-3) reference materials. Precision for five (n = 5) replicate measurements were between 1.2% (Pr) and 18% (Lu). Fe, Pb, Sn, and Zn impurities in TEA were significant in comparison to the levels in CASS-4 and SLEW-3, while relatively high background signals impacted determinations of low levels of Sc and Th. The effects of these hurdles on precision and accuracy were alleviated by measuring these elements in spiked CASS-4 and SLEW-3. Copyright © 2018 Elsevier B.V. All rights reserved.
Development of space-stable thermal control coatings for use on large space vehicles

NASA Technical Reports Server (NTRS)

Gilligan, J. E.; Harada, Y.

1976-01-01

The potential of zinc orthotitanate as a pigment for spacecraft thermal control was demonstrated. The properties and performance of pigments prepared by solid state, coprecipitation, and mixed oxalate methods were compared. Environmental tests and subsequent spectral analysis were given primary emphasis.
Analysis of trace metals in water by inductively coupled plasma emission spectrometry using sodium dibenzyldithiocarbamate for preconcentration

USGS Publications Warehouse

Smith, C.L.; Motooka, J.M.; Willson, W.R.

1984-01-01

Since concentrations of trace elements in most natural waters seldom exceed the ??g/L level, analysis of trace elements in natural waters by inductively coupled plasma emission spectrometry (ICP) requires a preconcentration procedure. The elements Ag, Bi, Cd, Co, Cu, Fe, Mo, Ni, Pb, Sn, V, W, and Zn were separated and concentrated from 500 mL of water by coprecipitating them with sodium dibenzyldithiocarbamate (NaDBDTC) using nickel or silver as a carrier. The precipitated trace elements were collected on a membrane filter, redissolved from the filter with hot nitric and hydrochloric acids, and analyzed using ICP. Recoveries for all the trace elements except tungsten exceeded 80%. Coprecipitation of trace elements with NaDBDTC eliminated the use of difficult-to-inject organic solvents, and NaDBDTC coprecipitated a wider array of trace elements than ammoniumpyrrolidinedithiocarbamate (APDC), another commonly used coprecipitate.
Controlled superficial assembly of DNA-amorphous calcium phosphate nanocomposite spheres for surface-mediated gene delivery.

PubMed

Oyane, Ayako; Araki, Hiroko; Nakamura, Maki; Shimizu, Yoshiki; Shubhra, Quazi T H; Ito, Atsuo; Tsurushima, Hideo

2016-05-01

Surface-mediated gene delivery systems have many potential applications in tissue engineering. We recently fabricated an assembly consisting of DNA-amorphous calcium phosphate (DNA-ACP) nanocomposite spheres on a polymer substrate via coprecipitation in a labile supersaturated calcium phosphate (CaP) solution and demonstrated the assembly's high gene delivery efficacy. In this study, we conducted a detailed investigation of the coprecipitation process in solution and revealed that the negatively charged DNA molecules were immobilized in the ACP spheres during the initial stage of coprecipitation and functioned as both sphere-dispersing and size-regulating agents. As a result, the DNA-ACP nanocomposites grew into size-regulated submicrospheres in solution and assembled onto the substrate via gravity sedimentation. The assembled nanocomposite spheres were chemically anchored to the substrate surface through an intermediate layer of CaP-based nanoparticles that was formed heterogeneously at the substrate surface. The coprecipitation conditions, i.e., coprecipitation time and Ca and P concentrations in solution, greatly affected the state of assembly of the nanocomposite spheres, thereby influencing the gene expression level of the cells cultured on the substrate. Increasing the number density and decreasing the size of the nanocomposite spheres did not always increase the assembly's gene delivery efficacy (per surface area of the substrate) due to adverse effects on cellular viability. As demonstrated herein, controlling the coprecipitation conditions is important for designing a cell-stimulating and biocompatible scaffold surface consisting of an assembly of DNA-ACP nanocomposite spheres. Copyright © 2016 Elsevier B.V. All rights reserved.
Development of spray-dried co-precipitate of amorphous celecoxib containing storage and compression stabilizers.

PubMed

Dhumal, Ravindra S; Shimpi, Shamkant L; Paradkar, Anant R

2007-09-01

The purpose of this study was to obtain an amorphous system with minimum unit operations that will prevent recrystallization of amorphous drugs since preparation, during processing (compression) and further storage. Amorphous celecoxib, solid dispersion (SD) of celecoxib with polyvinyl pyrrollidone (PVP) and co-precipitate with PVP and carrageenan (CAR) in different ratios were prepared by the spray drying technique and compressed into tablets. Saturation solubility and dissolution studies were performed to differentiate performance after processing. Differential scanning calorimetry and X-ray powder difraction revealed the amorphous form of celecoxib, whereas infrared spectroscopy revealed hydrogen bonding between celecoxib and PVP. The dissolution profile of the solid dispersion and co-precipitate improved compared to celecoxib and amorphous celecoxib. Amorphous celecoxib was not stable on storage whereas the solid dispersion and co-precipitate powders were stable for 3 months. Tablets of the solid dispersion of celecoxib with PVP and physical mixture with PVP and carrageenan showed better resistance to recrystallization than amorphous celecoxib during compression but recrystallized on storage. However, tablets of co-precipitate with PVP and carageenan showed no evidence of crystallinity during stability studies with comparable dissolution profiles. This extraordinary stability of spray-dried co-precipitate tablets may be attributed to the cushioning action provided by the viscoelastic polymer CAR and hydrogen bonding interaction between celecoxib and PVP. The present study demonstrates the synergistic effect of combining two types of stabilizers, PVP and CAR, on the stability of amorphous drug during compression and storage as compared to their effect when used alone.
Polymer Directed Self-Assembly of pH-Responsive Antioxidant Nanoparticles

PubMed Central

Tang, Christina; Amin, Devang; Messersmith, Phillip B.; Anthony, John E.; Prud’homme, Robert K.

2015-01-01

We have developed pH-responsive, multifunctional nanoparticles based on encapsulation of an antioxidant, tannic acid (TA), using Flash NanoPrecipitation, a polymer directed self-assembly method. Formation of insoluble coordination complexes of tannic acid and iron during mixing drives nanoparticle assembly. Tuning the core material to polymer ratio, the size of the nanoparticles can be readily tuned between 50 and 265 nm. The resulting nanoparticle is pH-responsive, i.e. stable at pH 7.4 and soluble under acidic conditions due to the nature of the coordination complex. Further, the coordination complex can be coprecipitated with other hydrophobic materials such as therapeutics or imaging agents. For example, coprecipitation with a hydrophobic fluorescent dye creates fluorescent nanoparticles. In vitro, the nanoparticles have low cytotoxicity show antioxidant activity. Therefore, these particles may facilitate intracellular delivery of antioxidants. PMID:25760226
Iron on mixed zirconia-titania substrate Fischer-Tropsch catalyst and method of making same

DOEpatents

Dyer, Paul N.; Nordquist, Andrew F.; Pierantozzi, Ronald

1986-01-01

A Fischer-Tropsch catalyst comprising iron co-deposited with or deposited on particles comprising a mixture of zirconia and titania, preferably formed by co-precipitation of compounds convertible to zirconia and titania, such as zirconium and titanium alkoxide. The invention also comprises the method of making this catalyst and an improved Fischer-Tropsch reaction process in which the catalyst is utilized.
Binding of Cd by ferrihydrite organo-mineral composites: Implications for Cd mobility and fate in natural and contaminated environments.

PubMed

Du, Huihui; Peacock, Caroline L; Chen, Wenli; Huang, Qiaoyun

2018-09-01

Adsorption and coprecipitation of organic matter with iron (hydr)oxides can alter iron (hydr)oxide surface properties and their reactivity towards nutrient elements and heavy metals. Organo-mineral composites were synthesized using humic acid (HA) and iron oxide, during coprecipitation with ferrihydrite (Fh) and adsorption to pre-formed Fh with two C loadings. The Fh-HA coprecipitated composites have a higher C content and smaller surface area compared to the equivalent adsorbed composites. NanoSIMS shows there is a high degree of spatial correlation between Fe and C for both composites, but C distribution is more uniform in the coprecipitated composites. The C 1s NEXAFS reveals a similar C composition between the Fh-HA coprecipitated and adsorbed composites. However composites at high carbon loading are more enriched in aromatic C, likely due to preferential binding of carboxyl functional groups on aromatic rings in the HA. The amount of Cd sorbed is independent of the composite type, either coprecipitated or adsorbed, but is a function of the C loading. Composites with low C loading show Cd sorption that is almost identical to pure Fh, while composites with high C loading show Cd sorption that is intermediate between pure Fh and pure HA, with sorption significantly enhanced over pure Fh at pH < 6.5. A bidentate edge-sharing binding was identified for Cd on pure Fh and Cd-carboxyl binding on pure HA. These findings have significant implications not only for the sequestration of Cd in contaminated environments but also the coupled biogeochemical cycling of Cd, Fe and C in the critical zone. Crown Copyright © 2018. Published by Elsevier Ltd. All rights reserved.
Influence of Coprecipitated Organic Matter on Fe2+(aq) -Catalyzed Transformation of Ferrihydrite: Implications for Carbon Dynamics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Chunmei; Kukkadapu, Ravi K.; Sparks, Donald L.

2015-08-10

The poorly crystalline Fe(III) hydroxide ferrihydrite is an important sink for organic matter (OM), nutrients and contaminants in soils and sediments. Aqueous Fe(II) is known to catalyze the transformation of ferrihydrite to more crystalline and thus less reactive phases. While coprecipitation of OM with ferrihydrite could be a common process in many environments due to changes in pH, redox potential or ionic strength, little is known about the impacts of coprecipitated OM on Fe(II)-catalyzed ferrihydrite transformation and its consequences for C dynamics. Accordingly, we explored the extent and pathways of Fe(II)-induced transformation of OM-ferrihydrite coprecipitates and subsequent C mobility. Mössbauermore » spectroscopic results indicated that the coprecipitated OM within ferrihydrite weakened the inter-particle magnetic interactions and decreased average particle size. The coprecipitated OM resulted in diminished Fe(II)-induced ferrihydrite transformation and thus preservation of ferrihydrite. The secondary mineral profiles upon Fe(II) reaction with ferrihydrite were a function of OM content and Fe(II) concentration. At low Fe(II) levels, OM completely inhibited goethite formation and stimulated lepidocrocite formation. At high Fe(II) levels, whereas goethite was formed in the presence of OM, OM reduced the amount of goethite and magnetite formation and increased the formation of lepidocrcocite. The solid-phase C content remained unchanged after reaction, while OM desorpability by H2PO4- was enhanced following reaction of OM-ferrihydrites with aqueous Fe(II). These findings provide insights into the reactivity of natural ferrihydrite containing OM in soils and sediments and the subsequent impact on mineral evolution and C dynamics.« less
Standards for electron probe microanalysis of silicates prepared by convenient method

NASA Technical Reports Server (NTRS)

Walter, L. S.

1966-01-01

Standard compositions suitable for electron probe microanalysis of various silicates are prepared by coprecipitation of specified salts with colloidal silica to form a gel which is decomposed into a powdered oxide mixture and compressed into thin pellets. These pellets of predetermined standard are compared with a silicate sample to determine its composition.

Facile Synthesis and Characterization of ZrO₂ Nanoparticles via Modified Co-Precipitation Method.

PubMed

Ramachandran, M; Subadevi, R; Liu, Wei-Ren; Sivakumar, M

2018-01-01

The crystalline Zirconium oxide (ZrO2) nano particles were synthesized using optimized content of Zirconium nitrate (Zr(NO3)2·3H2O) with varying KOH concentration (0.5, 1 and 1.5 M) by co-precipitation method. The thermal history of the precursor was carefully analyzed through Thermogravimetric (TG/DTA) measurement. The as prepared samples were characterized to ensure structural, functional, morphological, compositional, chemical composition and band gap by X-ray diffractometer (XRD), Fourier transform infrared spectroscopy (FTIR), Laser Raman, scanning electron microscopy (SEM), High resolution Transverse Electron Microscopy (HR-TEM), X-ray photo electron spectroscopy (XPS), EDX, Photo luminescence spectroscopy (PL). The monoclinic structure with space group P21/c has been confirmed from XRD (JCPDS 89-9066). The Zr-O stretching vibration and Zr-O2-Zr bending vibrations were confirmed through FTIR analysis. The well dispersed particles with spherical morphology were confirmed through SEM and TEM analysis. The oxidation states of Zr, O and C were confirmed through XPS analysis. The oxygen vacancies and band gap of the particles were investigated through PL analysis.
Microwave resonant and zero-field absorption study of doped magnetite prepared by a co-precipitation method.

PubMed

Aphesteguy, Juan Carlos; Jacobo, Silvia E; Lezama, Luis; Kurlyandskaya, Galina V; Schegoleva, Nina N

2014-06-19

Fe3O4 and ZnxFe3-xO4 pure and doped magnetite magnetic nanoparticles (NPs) were prepared in aqueous solution (Series A) or in a water-ethyl alcohol mixture (Series B) by the co-precipitation method. Only one ferromagnetic resonance line was observed in all cases under consideration indicating that the materials are magnetically uniform. The shortfall in the resonance fields from 3.27 kOe (for the frequency of 9.5 GHz) expected for spheres can be understood taking into account the dipolar forces, magnetoelasticity, or magnetocrystalline anisotropy. All samples show non-zero low field absorption. For Series A samples the grain size decreases with an increase of the Zn content. In this case zero field absorption does not correlate with the changes of the grain size. For Series B samples the grain size and zero field absorption behavior correlate with each other. The highest zero-field absorption corresponded to 0.2 zinc concentration in both A and B series. High zero-field absorption of Fe3O4 ferrite magnetic NPs can be interesting for biomedical applications.
Synthesis of zeolite/nickel ferrite/sodium alginate bionanocomposite via a co-precipitation technique for efficient removal of water-soluble methylene blue dye.

PubMed

Bayat, Mahsa; Javanbakht, Vahid; Esmaili, Javad

2018-05-05

In this study, we sought to synthesize magnetic nanocomposite of zeolite/nickel ferrite through co-precipitation method and modify its surface by sodium alginate to enhance its methylene blue adsorption capacity and to prevent its oxidation. Nanocomposite characteristics were investigated by SEM, VSM, XRD and FTIR analyses. The results indicate that nanocomposite synthesis and modification has been completely successful. Adsorption thermodynamics, kinetics, and isotherms were examined and parameters were optimized by Minitab software using experimental design method, response surface methodology and Box-Behnken design. The highest capacity of methylene blue adsorption from the aqueous solution obtained at optimal pH of 5, the initial dye concentration of 10 mg/L and an adsorbent amount of 0.03 g was about 54.05 mg/g. Analyzing kinetic data of adsorption experiments confirmed that adsorption process complies with the pseudo-second-order kinetic model. Assessing equilibrium isotherm data at different temperatures showed that these data are in good agreement with Langmuir isotherm model. Copyright © 2018 Elsevier B.V. All rights reserved.
Nano-sized ZnO powders prepared by co-precipitation method with various pH

DOE Office of Scientific and Technical Information (OSTI.GOV)

Purwaningsih, S. Y., E-mail: sriyanisaputri@gmail.com; Pratapa, S.; Triwikantoro,

2016-04-19

In this work, nano-sized ZnO powders have been synthesized by the co-precipitation method with Zn(CH3COOH)2.2H2O, HCl, and NH3.H2O as raw materials in various pH ranging from 8 to 10. The purity, microstructure, chemical group analysis, morphology of the prepared ZnO powders were studied by X-ray diffraction (XRD), Fourier transform infrared spectrometer (FTIR), energy dispersive X-ray spectrometry (EDX), and scanning electron microscope (SEM), respectively. Rietveld refinement of XRD data showed that ZnO crystallizes in the wurtzite structure with high purity. The obtained powders were nano-sized particles with the average crystallite size about 17.9 ± 2.1 nm synthesized with pH of 9.5, atmore » 85°C, and stirring time of 6 h. The SEM results have visualied the morphology of ZnO nanoparticles with spherical-like shape. The effect of processing conditions on morphology of ZnO was also discussed.« less
Structure, morphology, and cathode performance of Li 1- x[Ni 0.5Mn 1.5]O 4 prepared by coprecipitation with oxalic acid

NASA Astrophysics Data System (ADS)

Liu, Dongqiang; Han, Jiantao; Goodenough, John B.

The cathode materials Li 1- x[Ni 0.5Mn 1.5]O 4 prepared by coprecipitation from acetate solution by oxalic acid and annealing at 900 °C in air had the preferred disordered Ni and Mn on the 16d octahedral sites of a spinel F d 3 bar m structure. The coprecipitation method provides better crystallinity than the F d 3 bar m phase previously obtained by quenching from the melt. Polycrystalline octahedral-shaped particles with smooth surfaces contained trace amounts of a Li yNi 1- yO impurity that introduced some Mn(III) into the spinel phase. Half-cells cycled at 0.2 C rate between 3.5 and 4.8 V versus Li exhibited a flat voltage V ≈ 4.7 V with a small step at x ≈ 0.5 and a capacity at room temperature of 130 mAh g -1 that showed no fade after 50 cycles. A small capacity fade was initiated with a cut-off voltage ≥4.9 V; a significant capacity loss between 2 and 5 C cycling rates was reversible to 134 mAh g -1 on returning to 0.1 C after 50 cycles at 10 C between 3.5 and 5.0 V.
Radio frequency abnormal dielectric response of manganese chromite (MnCr{sub 2}O{sub 4}) nanoparticles synthesized by coprecipitation method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gul, Muhammad, E-mail: mgul@upesh.edu.pk

2016-04-15

Highlights: • Uniform MnCr{sub 2}O{sub 4} nanoparticles synthesized by surfactant-free coprecipitation route. • XRD analysis confirmed the single spinel phase formation in the material. • Dielectric loss was found abnormal over certain lower frequencies. • AC conductivity proved the involvement of small polarons in conduction process. - Abstract: Radio frequency dielectric behavior of nanocrystalline MnCr{sub 2}O{sub 4} synthesized via surfactant-free controlled coprecipitation route has been studied. Keeping in view the necessity of particle size uniformity and phase purity for genuine performance, experimental conditions were optimized accordingly. The scanning electron micrographs of the synthesized product revealed the formation of monodispersed particlemore » system. X-ray diffraction analysis confirmed monophasic spinel structure formation with 65 nm crystallite size. Two characteristic peaks observed between 700 cm{sup −1} and 400 cm{sup −1} in the FTIR spectrum also supported the spinel phase purity of compound. The dielectric constant was found normal, but loss tangent of the sample showed abnormal behavior with frequency. The observed dielectric behavior of the synthesized product has been explained on the basis of space-charge polarization according to Maxwell–Wagner’s model and mutual contribution of n-type &p-type charge carriers (Rezlescu model). The ac conductivity linearly increased with frequency highlighting the existence of polaron hopping.« less
Achieving High Luminescent Performance K2SiF6:Mn4+ Phosphor by Co-precipitation Process with Controlling the Reaction Temperature

NASA Astrophysics Data System (ADS)

Tran, Tat-Dat; Nguyen, Duy-Hung; Pham, Thanh-Huy; Nguyen, Duy-Cuong; Duong, Thanh-Tung

2018-05-01

K2SiF6:Mn4+ (KSF:Mn) phosphor was synthesized by the one-step co-precipitation process, at different temperatures. It was found that the reaction temperature played a key role in photoluminescence performance of the product. When the reaction temperature decreased from 0°C to - 20°C, the doping concentration, Mn/Si ratio, increased from 2% to 10%. However, further decrement of temperature (to - 30°C) reduced the Mn/Si ratio to 7%. The photo-luminescence (PL) intensity was maximized at the highest Mn/Si (10%), which corresponds to a reaction temperature of - 20°C. The KSF:Mn phosphor showed excellent luminescent properties at a wide range of temperatures (from room temperature to 470 K), especially after being dispersed in a polymer matrix. When combined with a commercial white light emitting diode (WLED), KSF:Mn significantly improved luminescent properties, such as color rendering index (CRI), correlated color temperature (CCT) and luminous efficiency. In particular, CRI increased from 67.3 to 87.4, while the CCT decreased from 7800 K to 3204 K. The luminous efficiency increased from 82.0 lm/W to 95.3 lm/W. The results indicated that the high quality KSF:Mn red phosphor could be achieved by a simple one-step co-precipitation method with a fine control of reaction temperature.
Sonochemical assisted synthesis MnO2/RGO nanohybrid as effective electrode material for supercapacitor.

PubMed

Ghasemi, Shahram; Hosseini, Sayed Reza; Boore-Talari, Omid

2018-01-01

Manganese dioxide (MnO 2 ) needle-like nanostructures are successfully synthesized by a sonochemical method from an aqueous solution of potassium bromate and manganese sulfate. Also, hybride of MnO 2 nanoparticles wrapped with graphene oxide (GO) nanosheets are fabricated through an electrostatic coprecipitation procedure. With adjusting pH at 3.5, positive and negative charges are created on MnO 2 and on GO, respectively which can electrostatically attract to each other and coprecipitate. Then, MnO 2 /GO pasted on stainless steel mesh is electrochemically reduced by applying -1.1V to obtain MnO 2 /RGO nanohybrid. The structure and morphology of the MnO 2 and MnO 2 /RGO nanohybrid are examined by Raman spectroscopy, X-ray diffraction (XRD), atomic force microscopy (AFM), field emission-scanning electron microscopy (FE-SEM), energy dispersive spectroscopy (EDX), and thermal gravimetric analysis (TGA). The capacitive behaviors of MnO 2 and MnO 2 /RGO active materials on stainless steel meshes are investigated by cyclic voltammetry (CV), galvanostatic charge/discharge test and electrochemical impedance spectroscopy (EIS) by a three-electrode experimental setup in an aqueous solution of 0.5M sodium sulfate in the potential window of 0.0-1.0V. The electrochemical investigations reveal that MnO 2 /RGO exhibits high specific capacitance (C s ) of 375Fg -1 at current density of 1Ag -1 and good cycle stability (93% capacitance retention after 500 cycles at a scan rate of 200mVs -1 ). The obtained results give good prospect about the application of electrostatic coprecipitation method to prepare graphene/metal oxides nanohybrids as effective electrode materials for supercapacitors. Copyright © 2017 Elsevier B.V. All rights reserved.
Study on the mechanism of copper-ammonia complex decomposition in struvite formation process and enhanced ammonia and copper removal.

PubMed

Peng, Cong; Chai, Liyuan; Tang, Chongjian; Min, Xiaobo; Song, Yuxia; Duan, Chengshan; Yu, Cheng

2017-01-01

Heavy metals and ammonia are difficult to remove from wastewater, as they easily combine into refractory complexes. The struvite formation method (SFM) was applied for the complex decomposition and simultaneous removal of heavy metal and ammonia. The results indicated that ammonia deprivation by SFM was the key factor leading to the decomposition of the copper-ammonia complex ion. Ammonia was separated from solution as crystalline struvite, and the copper mainly co-precipitated as copper hydroxide together with struvite. Hydrogen bonding and electrostatic attraction were considered to be the main surface interactions between struvite and copper hydroxide. Hydrogen bonding was concluded to be the key factor leading to the co-precipitation. In addition, incorporation of copper ions into the struvite crystal also occurred during the treatment process. Copyright © 2016. Published by Elsevier B.V.
Synthesis of Zn1-xCdxO Nanoparticles by Co-Precipitation: Structural, Optical and Photodetection Analysis

NASA Astrophysics Data System (ADS)

Jacob, Anju Anna; Balakrishnan, L.; Meher, S. R.; Shambavi, K.; Alex, Z. C.

Zinc oxide (ZnO) is a wide bandgap semiconductor with excellent photoresponse in ultra-violet (UV) regime. Tuning the bandgap of ZnO by alloying with cadmium can shift its absorption cutoff wavelength from UV to visible (Vis) region. Our work aims at synthesis of Zn1-xCdxO nanoparticles by co-precipitation method for the fabrication of photodetector. The properties of nanoparticles were analyzed using X-ray diffractometer, UV-Vis spectrometer, scanning electron microscope and energy dispersive spectrometer. The incorporation of cadmium without altering the wurtzite structure resulted in the red shift in the absorption edge of ZnO. Further, the photoresponse characteristics of Zn1-xCdxO nanopowders were investigated by fabricating photodetectors. It has been found that with Cd alloying the photosensitivity was increased in the UVA-violet as well in the blue region.
Negative inotropic effect of carbachol and interaction between acetylcholine receptor-operated potassium channel (K.ACh channel) and GTP binding protein in mouse isolated atrium--a novel methodological trial.

PubMed

Okada, Muneyoshi; Noma, Chihiro; Yamawaki, Hideyuki; Hara, Yukio

2013-01-01

Interaction between acetylcholine receptor-operated potassium channel (K.ACh channel) and GTP binding protein was examined by an immunoprecipitation-Western blotting system in mouse isolated atrium. The carbachol-induced negative inotropic action in indomethacin-pretreated mouse atrium was significantly inhibited by a K.ACh channel blocker, tertiapin or atropine. Kir3.1 K.ACh channel (Kir3.1) was immunoprecipitated with a mouse anti-Kir3.1 antibody. Coprecipitating Gβ with Kir3.1, detected by Western blotting, was significantly augmented by carbachol. Atropine, but not tertiapin, significantly inhibited the carbachol-induced coprecipitating Gβ with Kir3.1. The data indicate that immunoprecipitation with Kir3.1 and Western blotting of Gβ system is a useful method for assessing interaction between K.ACh channel and GTP binding protein in mouse atrium.
RATES OF HYDROUS FERRIC OXIDE CRYSTALLIZATION AND THE INFLUENCE ON COPRECIPITATED ARSENATE

EPA Science Inventory

Arsenate coprecipitated with hydrous ferric oxide (HFO) was stabilized against dissolution during transformation of HFO to more crystalline iron (hydr)oxides. The rate of arsenate stabilization approximately coincided with the rate of HFO transformation at pH 6 and 40 ?C. Compa...
Energy Efficiency Finance Programs: Use Case Analysis to Define Data Needs and Guidelines

DOE Office of Scientific and Technical Information (OSTI.GOV)

Thompson, Peter; Larsen, Peter; Kramer, Chris

There are over 200 energy efficiency loan programs—across 49 U.S. states—administered by utilities, state/local government agencies, or private lenders.1 This distributed model has led to significant variation in program design and implementation practices including how data is collected and used. The challenge of consolidating and aggregating data across independently administered programs has been illustrated by a recent pilot of an open source database for energy efficiency financing program data. This project was led by the Environmental Defense Fund (EDF), the Investor Confidence Project, the Clean Energy Finance Center (CEFC), and the University of Chicago. This partnership discussed data collection practicesmore » with a number of existing energy efficiency loan programs and identified four programs that were suitable and willing to participate in the pilot database (Diamond 2014).2 The partnership collected information related to ~12,000 loans with an aggregate value of ~$100M across the four programs. Of the 95 data fields collected across the four programs, 30 fields were common between two or more programs and only seven data fields were common across all programs. The results of that pilot study illustrate the inconsistencies in current data definition and collection practices among energy efficiency finance programs and may contribute to certain barriers.« less
Towards deriving Ni-rich cathode and oxide-based anode materials from hydroxides by sharing a facile co-precipitation method.

PubMed

Qiu, Haifa; Du, Tengfei; Wu, Junfeng; Wang, Yonglong; Liu, Jian; Ye, Shihai; Liu, Sheng

2018-05-22

Although intensive studies have been conducted on layered transition metal oxide(TMO)-based cathode materials and metal oxide-based anode materials for Li-ion batteries, their precursors generally follow different or even complex synthesis routes. To share one route for preparing precursors of the cathode and anode materials, herein, we demonstrate a facile co-precipitation method to fabricate Ni-rich hydroxide precursors of Ni0.8Co0.1Mn0.1(OH)2. Ni-rich layered oxide of LiNi0.8Co0.1Mn0.1O2 is obtained by lithiation of the precursor in air. An NiO-based anode material is prepared by calcining the precursor or multi-walled carbon nanotubes (MWCNTs) incorporated precursors. The pre-addition of ammonia solution can simplify the co-precipitation procedures and the use of an air atmosphere can also make the heat treatment facile. LiNi0.8Co0.1Mn0.1O2 as the cathode material delivers a reversible capacity of 194 mA h g-1 at 40 mA g-1 and a notable cycling retention of 88.8% after 100 cycles at 200 mA g-1. This noticeable performance of the cathode arises from a decent particle morphology and high crystallinity of the layered oxides. As the anode material, the MWCNTs-incorporated oxides deliver a much higher reversible capacity of 811.1 mA h g-1 after 200 cycles compared to the pristine oxides without MWCNTs. The improvement on electrochemical performance can be attributed to synergistic effects from MWCNTs incorporation, including reinforced electronic conductivity, rich meso-pores and an alleviated volume effect. This facile and sharing method may offer an integrated and economical approach for commercial production of Ni-rich electrode materials for Li-ion batteries.
Selective Catalytic Reduction of NO by NH 3 with WO 3-TiO 2 Catalysts: Influence of Catalyst Synthesis Method

DOE PAGES

He, Yuanyuan; Ford, Michael E.; Zhu, Minghui; ...

2016-02-02

A series of supported WO 3/TiO 2 catalysts was prepared by a new synthesis procedure involving co-precipitation of an aqueous TiO(OH) 2 and (NH 4) 10W 12O 41*5H 2O slurry under controlled pH conditions. The morphological properties, molecular structures, surface acidity and surface chemistry of the supported WO 3/TiO 2 catalysts were determined with BET, in situ Raman, in situ IR and temperature-programmed surface reaction (TPSR) spectroscopy, respectively. Isotopic 18O- 16O exchange demonstrated that tungsten oxide was exclusively present as surface WO x species on the TiO 2 support with mono-oxo W=O coordination. In contrast to previous studies employing impregnationmore » synthesis that found only surface one mono-oxo O=WO 4 site on TiO 2, the co-precipitation procedure resulted in the formation of two distinct surface WO x species: mono-oxo O=WO 4 (~1010-1017 cm -1) on low defect density patches of TiO 2 and a second mono-oxo O=WO 4 (~983-986 cm -1) on high defect density patches of TiO 2. The concentration of the second WO x surface species increases as a function of solution pH. Both surface WOx sites, however, exhibited the same NO/NH 3 SCR reactivity. The co-precipitated WO 3-TiO 2 catalysts synthesized in alkaline solutions exhibited enhanced performance for the NO/NH 3 SCR reaction that is ascribed to the greater number of surface defects on the resulting TiO2 support. For the co-precipitated catalyst prepared at pH10, surface NH 4 + species on Br nsted acid sites were found to be more reactive than surface NH 3* species on Lewis acid sites for SCR of NO with NH 3.« less
Mobilization of arsenite by dissimilatory reduction of adsorbed arsenate

USGS Publications Warehouse

Zobrist, J.; Dowdle, P.R.; Davis, J.A.; Oremland, R.S.

2000-01-01

Sulfurospirillum barnesii is capable of anaerobic growth using ferric iron or arsenate as electron acceptors. Cell suspensions of S. barnesii were able to reduce arsenate to arsenite when the former oxyanion was dissolved in solution, or when it was adsorbed onto the surface of ferrihydrite, a common soil mineral, by a variety of mechanisms (e.g., coprecipitation, presorption). Reduction of Fe(III) in ferrihydrite to soluble Fe(II) also occurred, but dissolution of ferrihydrite was not required in order for adsorbed arsenate reduction to be achieved. This was illustrated by bacterial reduction of arsenate coprecipitated with aluminum hydroxide, a mineral that does not undergo reductive dissolution. The rate of arsenate reduction was influenced by the method in which arsenate became associated with the mineral phases and may have been strongly coupled with arsenate desorption rates. The extent of release of arsenite into solution was governed by adsorption of arsenite onto the ferrihydrite or alumina phases. The results of these experiments have interpretive significance to the mobilization of arsenic in large alluvial aquifers, such as those of the Ganges in India and Bangladesh, and in the hyporheic zones of contaminated streams.Sulfurospirillum barnesii is capable of anaerobic growth using ferric iron or arsenate as electron acceptors. Cell suspensions of S. barnesii were able to reduce arsenate to arsenite when the former oxyanion was dissolved in solution, or when it was adsorbed onto the surface of ferrihydrite a common soil mineral, by a variety of mechanisms (e.g., coprecipitation, presorption). Reduction of Fe(III) in ferrihydrite to soluble Fe(II) also occurred, but dissolution of ferrihydrite was not required in order for adsorbed arsenate reduction to be achieved. This was illustrated by bacterial reduction of arsenate coprecipitated with aluminum hydroxide, a mineral that does not undergo reductive dissolution. The rate of arsenate reduction was influenced by the method in which arsenate became associated with the mineral phases and may have been strongly coupled with arsenate desorption rates. The extent of release of arsenite into solution was governed by adsorption of arsenite onto the ferrihydrite or alumina phases. The results of these experiments have interpretive significance to the mobilization of arsenic in large alluvial aquifers, such as those of the Ganges in India and Bangladesh, and in the hyporheic zones of contaminated streams.
Preparation of ZnO nanoparticles showing upconversion luminescence through simple chemical method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Anjana, R.; Subha, P. P.; Markose, Kurias K.

2016-05-23

Upconversion luminescence is an interesting area while considering its applications in a vast variety of fields. Rare earth ions like erbium is the most studied and efficient candidate for achieving upconversion. Erbium and ytterbium co-doped ZnO nanoparticles were prepared through co-precipitation method. A strong red emission has been obtained while exciting with 980 nm laser. Dependence of luminescence emission colour on ytterbium concentration has been studied.
Dissolution of fludrocortisone from phospholipid coprecipitates.

PubMed

Vudathala, G K; Rogers, J A

1992-03-01

The physical properties and dissolution behavior of phospholipid coprecipitates of fludrocortisone acetate (FA) prepared from ethyl acetate, as well as the effect of added polymer, have been determined. The fraction dissolved after 90 min and the initial dissolution rate (IDR) of coprecipitates containing dimyristoyl phosphatidylcholine (DMPC) (4:1, w/w; FA:DMPC) were 77% and 3.5-fold greater than for FA at pH 2.0 and 37 degrees C. The mechanisms of dissolution were similar to those previously established for griseofulvin, but no aging occurred over 4 months at room temperature in a desiccator. The addition of 0.01 mol% of dextran (MW = 2 million) or 0.1 mol% of poly(lactic acid) reduced the fraction of FA dissolved in 90 min by 15% and reduced the IDR by 35%. The addition of poly(vinylpyrrolidone) (PVP) resulted in a minimum of dissolution efficiency at 1 mol% of PVP 10 (MW = 10,000) or PVP 24 (MW = 24,000) and at 0.1 mol% PVP 40 (MW = 40,000). Only PVP 24 influenced the melting point and heat of fusion of the coprecipitates (determined by differential thermal analysis). Coprecipitate dissolution was reasonably described by either second-order or Weibull distribution kinetic models. These results support the application of high drug-containing solid dispersions using phospholipids to increase the dissolution behavior of poorly water-soluble drug solvates and the possibility of modifying drug release by the incorporation of small amounts of polymers.
Chemical processes for the extreme enrichment of tellurium into marine ferromanganese oxides

NASA Astrophysics Data System (ADS)

Kashiwabara, Teruhiko; Oishi, Yasuko; Sakaguchi, Aya; Sugiyama, Toshiki; Usui, Akira; Takahashi, Yoshio

2014-04-01

Tellurium, an element of growing economic importance, is extremely enriched in marine ferromanganese oxides. We investigated the mechanism of this enrichment using a combination of spectroscopic analysis and adsorption/coprecipitation experiments. X-ray Absorption Near-Edge Structure (XANES) analysis showed that in adsorption/coprecipitation systems, Te(IV) was oxidized on δ-MnO2 and not oxidized on ferrihydrite. Extended X-ray Absorption Fine Structure (EXAFS) analysis showed that both Te(IV) and Te(VI) were adsorbed on the surface of δ-MnO2 and ferrihydrite via formation of inner-sphere complexes. In addition, Te(VI) can be structurally incorporated into the linkage of Fe octahedra through a coprecipitation process because of its molecular geometry that is similar to the Fe octahedron. The largest distribution coefficient obtained in the adsorption/coprecipitation experiments was for the Te(VI)/ferrihydrite coprecipitation system, and it was comparable to those calculated from the distribution between natural ferromanganese oxides and seawater. Our XAFS and micro-focused X-ray fluorescence (μ-XRF) mapping of natural ferromanganese oxides showed that Te was structurally incorporated as Te(VI) in Fe (oxyhydr)oxide phases. We conclude that the main process for the enrichment of Te in ferromanganese oxides is structural incorporation of Te(VI) into Fe (oxyhydr)oxide phases through coprecipitation. This mechanism can explain the unique degree of enrichment of Te compared with other oxyanions, which are mainly enriched via adsorption on the surface of the solid structures. In particular, the great contrast in the distributions of Te and Se is caused by their oxidized species: (i) the similar geometry of the Te(VI) molecule to Fe octahedron, and (ii) quite soluble nature of Se(VI). Coexisting Mn oxide phases may promote structural incorporation of Te(VI) by oxidation of Te(IV), although the surface oxidation itself may not work as the critical enrichment process as in the case of some cations. This enrichment mechanism also means that ferromanganese oxides mainly scavenge dominant Te(VI) species from seawater and do not affect its species distribution in seawater, as described in a previous model. The variation in Te abundances and the correlation of Te concentration with the growth rate of natural ferromanganese oxides are consistent with the coprecipitation mechanism.
Drug delivery system for an anticancer agent, chlorogenate-Zn/Al-layered double hydroxide nanohybrid synthesised using direct co-precipitation and ion exchange methods

DOE Office of Scientific and Technical Information (OSTI.GOV)

Barahuie, Farahnaz; Hussein, Mohd Zobir, E-mail: mzobir@putra.upm.edu.my; Arulselvan, Palanisamy

A nano-structured drug-inorganic clay hybrid involving an active anticancer compound, which is chlorogenic acid (CA) intercalated into Zn/Al-layered double hydroxide, has been assembled via ion-exchange and co-precipitation methods to form a nanohybrid CZAE (a chlorogenic acid-Zn/Al nanohybrid synthesised using an ion-exchange method) and CZAC (a chlorogenic acid-Zn/Al nanohybrid synthesised using a direct method), respectively. The X-ray diffraction (XRD) results confirmed that the CA-LDH had a hybrid structure in which the anionic chlorogenate is arranged between the interlayers as a horizontal monolayer at 90 and 20° angles from the x axis for CZAE and CZAC, respectively. Both nanohybrids have the propertiesmore » of mesoporous materials. The high loading percentage of chlorogenic acid (approximately 43.2% for CZAE and 45.3% for CZAC) with basal spacings of 11.7 and 12.6 Å for CZAE and CZAC, respectively, corroborates the successful intercalation of chlorogenic acid into the interlayer gallery of layered double hydroxides. Free chlorogenic acid and the synthesised nanocomposites (CZAE, CZAC) were assessed for their cytotoxicity against various cancer cells. The Fourier transform infrared data supported the formation of both nanohybrids, and a thermal analysis showed that the nanohybrids are more thermally stable than their counterparts. The chlorogenate shows a sustained release, and the release rate of chlorogenate from CZAE and CZAC nanohybrids at pH 7.4 is remarkably lower than that at pH 4.8 due to their different release mechanisms. The release rate of chlorogenate from both nanohybrids can be described as pseudo-second order. The present investigation revealed the potential of the nanohybrids to enhance the in vitro anti-tumour effect of chlorogenic acid in liver and lung cancer cells in vitro. - Highlights: • We intercalated chlorogenic into Zn/Al-layered double hydroxide by ion-exchange and coprecipitation methods. • The two methods gave nanocomposites with slightly different physico-chemical properties. • Chlorogenate-zinc aluminium layered double hydroxide nanohybrids have the potential to be used as a controlled release formulation. • The thermal stability of chlorogenic acid is markedly enhanced upon the intercalation process. • The inhibition of cancer cell growth is higher for nanohybrids than for free chlorogenic acid.« less

Controlling the size and magnetic properties of nano CoFe2O4 by microwave assisted co-precipitation method

NASA Astrophysics Data System (ADS)

Prabhakaran, T.; Mangalaraja, R. V.; Denardin, Juliano C.

2018-02-01

In this report, cobalt ferrite nanoparticles synthesized using microwave assisted co-precipitation method was reported. Efforts have been made to control the particles size, distribution, morphology and magnetic properties of cobalt ferrite nanoparticles by varying the concentration of NaOH solution and microwave irradiation time. It was observed that the rate of nucleation and crystal growth was influenced by the tuning parameters. In that way, the average crystallite size of single phase cobalt ferrite nanoparticles was controlled within 9-11 and 10-12 nm with an increase of base concentration and microwave irradiation time, respectively. A narrow size distribution of nearly spherical nanoparticles was achieved through the present procedure. A soft ferromagnetism at room temperature with the considerable saturation magnetization of 58.4 emu g-1 and coercivity of 262.7 Oe was obtained for the cobalt ferrites synthesized with 2.25 M of NaOH solution for 3 and 7 min of microwave irradiation time, respectively. The cobalt ferrite nanoparticles synthesized with a shorter reaction time of 3-7 min was found to be advantageous over other methods that involved conventional heating procedures and longer reaction time to achieve the better magnetic properties for the technological applications.
Preparation of Fe3O4/Bentonite Nanocomposite from Natural Iron Sand by Co-precipitation Method for Adsorbents Materials

NASA Astrophysics Data System (ADS)

Sebayang, Perdamean; Kurniawan, Candra; Aryanto, Didik; Arief Setiadi, Eko; Tamba, Konni; Djuhana; Sudiro, Toto

2018-03-01

An adsorption method is one of the effective ways to filter the heavy metals wastes in aqueous system. In this paper, the Fe3O4/bentonite nanocomposites were successfully prepared from natural iron sand by co-precipitation method. The chemical process was carried out by dissolving and hot stirring the milled iron sand and bentonite in acid solution and precipitating it by NH4OH. The sediment was then washed using distilled water to neutralize pH and dried at 100 °C for 5 hours to produce Fe3O4/bentonite powders. The samples were characterized by XRD, FTIR, BET, TEM, VSM and AAS. All samples were composed by Fe3O4 single phase with a spinnel structure and lattice parameter of 8.373 Å. The transmittance peak of FTIR curve proved that the Fe3O4 particles and bentonite had a molecular bonding. The addition of bentonite to Fe3O4 nanoparticles generally reduced the magnetic properties of Fe3O4/bentonite nanocomposites. The optimum condition of 30 wt% bentonite resulted 105.9 m2/g in surface area, 14 nm in an average particle size and 3.2 nm in pore size. It can be used as Cu and Pb adsorbent materials.
STRUCTURAL, SURFACE MORPHOLOGICAL AND MAGNETIC STUDIES OF Zn1-xFexS (x=0.00-0.10) DILUTED MAGNETIC SEMICONDUCTORS GROWN BY CO-PRECIPITATION METHOD

NASA Astrophysics Data System (ADS)

Hassan, M.; Ghazanfar, M.; Arooj, N.; Riaz, S.; Hussain, S. Sajjad; Naseem, S.

We have fabricated Zn1-xFexS (x=0.00, 0.02, 0.04, 0.06, 0.08 and 0.10) diluted magnetic semiconductors using co-precipitation method. X-ray diffraction patterns depict that Zn1-xFexS appears as a dominant phase with cubic zinc blende structure and nanoscale crystallite size. In addition, a secondary phase of rhombohedral ZnS also appears; however, no additional phase arises that primarily belongs to Fe dopant. Using Debye-Scherrer relation, the crystallite size is found to be in the range of 20-27nm, which is in good agreement with the crystallite size calculated using the Williamson-Hall (WH) plot method. The appearance of secondary phase provoked to study the residual strain using Stokes-Wilson equation, which is nearly consistent to that observed using WH plot method. The surface morphology, revealed using scanning electron microscopy, depicts non-uniform surface structure with a variety of grains and void dimensions. Hysteresis loops measured for Zn1-xFexS at room temperature (RT) illustrate a paramagnetic behavior at higher fields; however, small ferromagnetic behavior is evident due to the small openings of the measured hysteresis loops around the origin. The measured RT ferromagnetism reveals the potential spintronic device applications of the studied diluted magnetic semiconductors.
Effects of solution concentration and capping agents on the properties of potassium titanyl phosphate noparticles synthesized using a co-precipitation method

NASA Astrophysics Data System (ADS)

Gharibshahian, E.; Jafar Tafershi, M.; Fazli, M.

2018-05-01

In this study, KTiOPO4 (KTP) nanoparticles were synthesized using a co-precipitation method. The effects of the solution concentration (M) and capping agents, such as PVA, oxalic acid, glycine, triethanolamine, and L-alanine, on the structural, microstructural, and optical properties of the products were investigated using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, ultraviolet-visible spectroscopy, field emission scanning electron microscopy, and transmission electron microscopy. Decreasing the solution concentration decreased the crystallite size from 53.07 nm (for M = 2) to 39.42 nm (for M = 0.5). After applying different capping agents to the sample at the optimum concentration (M = 0.5), the crystallite size decreased again and grains as small as 10.61 nm were obtained. XRD and FTIR analyses indicated the formation of KTP nanoparticles with an orthorhombic structure in all of the samples. The optical band gap increased as the crystallite size decreased. Different morphological patterns such as spherical, needle shaped, polyhedron, and tablet forms were observed in the nanoparticles, which were correlated with the effects of the capping agents employed.
Nanocrystalline composites of transition metal molybdate (Ni1-xCoxMoO4; x = 0, 0.3, 0.5, 0.7, 1) synthesized by a co-precipitation method as humidity sensors and their photoluminescence properties

NASA Astrophysics Data System (ADS)

Jeseentharani, V.; Dayalan, A.; Nagaraja, K. S.

2018-04-01

In this study, nanocrystalline transition metal nickel-cobalt molybdate (Ni1-xCoxMoO4, NiCM; x = 0, 0.3, 0.5, 0.7, 1) composites were prepared using a simple co-precipitation method. The composites were characterized by thermogravimetric/differential thermal analysis, Fourier transform-infrared spectroscopy, X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The NiCM composites were studied to determine their possible use as humidity sensors, and photoluminescence (PL) measurements were obtained. The sensing study was performed in environments with different relative humidity levels (5-98%). The maximum sensitivity of 18624 ± 168 was observed with the Ni0.7Co0.3MoO4 composite where the humidity could be calculated according to the relationship: Sf = R5%/R98%, where R5% and R98% are the dc resistances at 5 and 98% RH, respectively. The photoluminescence measurements acquired at room temperature for the NiCMs included green and red emission peaks when excited at a wavelength (λex) of 520 nm.
Preparation and characterization of natural bentonite in to nanoparticles by co-precipitation method

NASA Astrophysics Data System (ADS)

Sirait, Makmur; Bukit, Nurdin; Siregar, Nurdin

2017-01-01

The nanoparticle based on natural bentonite from Pahae village had been prepared using co-precipitation method. Bentonite was dried in the oven at 100°C during a week. Bentonite is crushed using a mortal and milled by planetary ball mill to obtain the powder form. Further, the bentonite powder is activated with chemical reaction by dissolves the 50 g bentonite to 100 ml of HCl at 10 M. The magnetic stirrer was employed to mix the solution at 300 rpm and temperature 70°C. After that, the bentonite solution is washed using distilled water until the pH is neutral. The bentonite powder is calcined at temperature of 600°C for 1 hour with fix increment 150°C. Finally, the powder is given High Energy Milling (HEM) treatment for 30 minutes to obtain the particle size. The X-ray Difractometer (XRD) and Scanning Electron Microscope (SEM) were used to characterize. From the characterization results it is reported that the average of bentonite nanoparticle size is 35.26 nm and the chemical constituents of natural bentonite Pahae are Al, Si, Ca, Fe and Ti.
Hierarchical Mesoporous Lithium-Rich Li[Li0.2Ni0.2Mn0.6]O2 Cathode Material Synthesized via Ice Templating for Lithium-Ion Battery.

PubMed

Li, Yu; Wu, Chuan; Bai, Ying; Liu, Lu; Wang, Hui; Wu, Feng; Zhang, Na; Zou, Yufeng

2016-07-27

Tuning hierarchical micro/nanostructure of electrode materials is a sought-after means to reinforce their electrochemical performance in the energy storage field. Herein, we introduce a type of hierarchical mesoporous Li[Li0.2Ni0.2Mn0.6]O2 microsphere composed of nanoparticles synthesized via an ice templating combined coprecipitation strategy. It is a low-cost, eco-friendly, and easily operated method using ice as a template to control material with homogeneous morphology and rich porous channels. The as-prepared material exhibits remarkably enhanced electrochemical performances with higher capacity, more excellent cycling stability and more superior rate property, compared with the sample prepared by conventional coprecipitation method. It has satisfactory initial discharge capacities of 280.1 mAh g(-1) at 0.1 C, 207.1 mAh g(-1) at 2 C, and 152.4 mAh g(-1) at 5 C, as well as good cycle performance. The enhanced electrochemical performance can be ascribed to the stable hierarchical microsized structure and the improved lithium-ion diffusion kinetics from the highly porous structure.
Fabrication of barium titanate doped strontium using co-precipitation method

NASA Astrophysics Data System (ADS)

Iriani, Y.; Yasin, M. A.; Suryana, R.

2018-03-01

Fabrication of barium titanate (BaTiO3/BT) doped strontium (Sr) using co-precipitation method has been successfully conducted. The research aim is to get the best of mole variation of Sr doping to ferroelectric material properties. Doping Sr was varied at 1%, 2%, 3%, 4% and 5% in BaTiO3. Each sample was sintered at temperature of 1100°C with holding time for 6 h and temperature rate at 10°C/min. They were then characterized by XRD instrument to investigate the crystal structure, LCR meter to measure the dielectric constant, and Sawyer Tower circuit to reveal the hysteresis curve. The peaks of XRD shift towards larger angle when mole doping Sr increase. The crystallinity of all samples is above 90% and the crystallite size is in the range of 27 nm to 34 nm. Hysteresis curve from Sawyer Tower testing confirms that all samples are ferroelectric material. The RLC measurement results reveal that the less frequency leads to the higher dielectric constant while the highest dielectric constant belongs to the BT doped 3% of Sr. Therefore, it is the best variation obtained in this research.
Preparation of theophylline-hydroxypropylmethylcellulose matrices using supercritical antisolvent precipitation: a preliminary study.

PubMed

Moneghini, M; Perissutti, B; Kikic, I; Grassi, M; Cortesi, A; Princivalle, F

2006-01-01

Several controlled release systems of drugs have been elaborated using a supercritical fluid process. Indeed, recent techniques using a supercritical fluid as a solvent or as an antisolvent are considered to be useful alternatives to produce fine powders. In this preliminary study, the effect of Supercritical Anti Solvent process (SAS) on the release of theophylline from matrices manufactured with hydroxypropylmethylcellulose (HPMC) was investigated. Two grades of HPMC (HPMC E5 and K100) as carriers were considered in order to prepare a sustained delivery system for theophylline which was used as a model drug. The characterization of the drug before and after SAS treatment, and the coprecipitates with carriers, was performed by X-ray Diffraction (XRD) and Differential Scanning Calorimetry (DSC). The dissolution rate of theophylline, theophylline-coprecipitates, and matricial tablets prepared with coprecipitates were determined. The physical characterizations revealed a substantial correspondence of the drug solid state before and after supercritical fluid treatment while drug-polymer interactions in the SAS-coprecipitates were attested. The dissolution studies of the matrices prepared compressing the coprecipitated systems showed that the matrices based on HPMC K100 were able to promote a sustained release of the drug. Further, this advantageous dissolution performance was found to be substantially independent of the pH of the medium. The comparison with the matrices prepared with untreated substances demonstrated that matrices obtained with SAS technique can provide a slower theophylline release rate. A new mathematical model describing the in vitro dissolution kinetics was proposed and successfully tested on these systems.
Immobilization of Iodate and Iodide using Iron Oxides through Sorption and Co-precipitation at Hanford Site

NASA Astrophysics Data System (ADS)

Wang, G.; Qafoku, N. P.; Truex, M. J.; Strickland, C. E.; Freedman, V. L.

2017-12-01

Isotopes of iodine were generated during plutonium production at the U.S. Department of Energy (DOE) Hanford Site. The long half-life 129I generated during reactor operations has been released into the subsurface, resulting in several large plumes at the Hanford subsurface. We studied the interaction of iodate (IO3-) and iodide (I-) with Fe oxides. A series of batch experiments were conducted to investigate adsorption and co-precipitation of iodine species in the presence of a variety of Fe oxides, such as ferrihydrite, goethite, hematite and magnetite. In the sorption experiments, each Fe oxide was added to an artificial groundwater containing either iodate or iodide, and reacted at room temperature. The sorption batch experiments for each mineral were conducted at varied initial iodate or iodide concentrations under 3 different pH conditions (pH 5, 7, and 9). In the co-precipitation batch experiments, the initial Fe-mineral-forming solutions were prepared in artificial groundwater containing iodate or iodide. Our results indicate that both sorption and co-precipitation are viable mechanisms of the attenuation of the liquid phase iodine. Species Fe oxides could serve as hosts of iodate and iodide that are present at the Hanford subsurface.
Kinetic precipitation of solution-phase polyoxomolybdate followed by transmission electron microscopy: a window to solution-phase nanostructure.

PubMed

Zhu, Yan; Cammers-Goodwin, Arthur; Zhao, Bin; Dozier, Alan; Dickey, Elizabeth C

2004-05-17

This study aimed to elucidate the structural nature of the polydisperse, nanoscopic components in the solution and the solid states of partially reduced polyoxomolybdate derived from the [Mo132] keplerate, [(Mo)Mo5]12-[Mo2 acetate]30. Designer tripodal hexamine-tris-crown ethers and nanoscopic molybdate coprecipitated from aqueous solution. These microcrystalline solids distributed particle radii between 2-30 nm as assayed by transmission electron microscopy (TEM). The solid materials and their particle size distributions were snap shots of the solution phase. The mother liquor of the preparation of the [Mo132] keplerate after three days revealed large species (r=20-30 nm) in the coprecipitate, whereas [Mo132] keplerate redissolved in water revealed small species (3-7 nm) in the coprecipitate. Nanoparticles of coprecipitate were more stable than solids derived solely from partially reduced molybdate. The TEM features of all material analyzed lacked facets on the nanometer length scale; however, the structures diffracted electrons and appeared to be defect-free as evidenced by Moiré patterns in the TEM images. Moiré patterns and size-invariant optical densities of the features in the micrographs suggested that the molybdate nanoparticles were vesicular.
Alcohol vapor sensing by cadmium-doped zinc oxide thick films based chemical sensor

NASA Astrophysics Data System (ADS)

Zargar, R. A.; Arora, M.; Chackrabarti, S.; Ahmad, S.; Kumar, J.; Hafiz, A. K.

2016-04-01

Cadmium-doped zinc oxide nanoparticles were derived by simple chemical co-precipitation route using zinc acetate dihydrate and cadmium acetate dihydrate as precursor materials. The thick films were casted from chemical co-precipitation route prepared nanoparticles by economic facile screen printing method. The structural, morphological, optical and electrical properties of the film were characterized relevant to alcohol vapor sensing application by powder XRD, SEM, UV-VIS and DC conductivity techniques. The response and sensitivity of alcohol (ethanol) vapor sensor are obtained from the recovery curves at optimum working temperature range from 20∘C to 50∘C. The result shows that maximum sensitivity of the sensor is observed at 25∘C operating temperature. On varying alcohol vapor concentration, minor variation in resistance has been observed. The sensing mechanism of sensor has been described in terms of physical adsorption and chemical absorption of alcohol vapors on cadmium-doped zinc oxide film surface and inside film lattice network through weak hydrogen bonding, respectively.
Synthesis, Optical and Electrochemical Properties of Y2O3 Nanoparticles Prepared by Co-Precipitation Method.

PubMed

Saravanan, Thulasingam; Raj, Srinivasan Gokul; Chandar, Nagamuthu Raja Krishna; Jayavel, Ramasamy

2015-06-01

Y2O3 nanoparticles were synthesized by co-precipitation route using yttrium nitrate hexahydrate and ammonium hydroxide as precursors. The prepared sample was calcined at 500 degrees C and subjected to various characterization studies like thermal analysis (TG/DTA), X-ray diffraction (XRD), transmission electron microscope (TEM), UV-visible (UV-Vis) and photoluminescence (PL) spectroscopy. The XRD pattern showed the cubic fluorite structure of Y2O3 without any impurity peaks, revealing high purity of the prepared sample. TEM images revealed that the calcined Y2O3 nanoparticles consist of spherical-like morphology with an average particle size of 12 nm. The absorption spectrum of calcined samples shows blue-shift compared to the as-prepared sample, which was further confirmed by PL studies. The possible formation mechanism of Y2O3 nanoparticles has been discussed based on the experimental results. Electrochemical behavior of Y2O3 nanoparticles was studied by cyclic voltammetry to assess their suitability for supercapacitor applications.
TRANSURANIC ELEMENT, COMPOSITION THEREOF, AND METHODS FOR PRODUCING SEPARATING AND PURIFYING SAME

DOEpatents

Wahl, A.C.

1961-09-19

A process of separating plutonium from fission products contained in an aqueous solution is described. Plutonium, in the tri- or tetravalent state, and the fission products are coprecipitated on lanthanum fluoride, lanthanum oxalate, cerous fluoride, cerous phosphate, ceric iodate, zirconyl phosphate, thorium iodate, or thorium fluoride. The precipitate is dissolved in acid, and the plutonium is oxidized to the hexavalent state. The fission products are selectively precipitated on a carrier of the above group but different from that used for the coprecipitation. The plutonium in the solution, after removal of the fission product precipitate, is reduced to at least the tetravalent state and precipitated on lanthanum fluoride, lanthanum phosphate, lanthanum oxalate, lanthanum hydroxide, cerous fluoride, cerous phosphate, cerous oxalate, cerous hydroxide, ceric iodate, zirconyl phosphate, zirconyl iodate, zirconium hydroxide, thorium fluoride, thorium oxalate, thorium iodate, thorium peroxide, uranium iodate, uranium oxalate, or uranium peroxide, again using a different carrier than that used for the precipitation of the fission products.
Co-precipitation synthesis of nanostructured Cu3SbSe4 and its Sn-doped sample with high thermoelectric performance.

PubMed

Li, Di; Li, Rui; Qin, Xiao-Ying; Song, Chun-Jun; Xin, Hong-Xing; Wang, Ling; Zhang, Jian; Guo, Guang-lei; Zou, Tian-Hua; Liu, Yong-Fei; Zhu, Xiao-Guang

2014-01-28

Large-scale fabrication of nanostructured Cu3SbSe4 and its Sn-doped sample Cu3Sb0.98Sn0.02Se4 through a low-temperature co-precipitation route is reported. The effects of hot-pressing temperatures, time and Sn doping on the thermoelectric properties of Cu3SbSe4 are explored. The maximum figure of merit ZTmax obtained here reaches 0.62 for the un-doped Cu3SbSe4, which is three times as large as that of Cu3SbSe4 synthesized by the fusion method. Due to the ameliorated power factor by optimized carrier concentration and the reduced lattice thermal conductivity by enhanced phonon scattering at grain interfaces, Sn doping leads to an improvement of thermoelectric performance as compared to Cu3SbSe4. The maximum ZT for Cu3Sb0.98Sn0.02Se4 is 1.05 in this work, which is 50% larger than the largest value reported.
Co-Precipitation Synthesis of Gadolinium Aluminum Gallium Oxide (GAGG) via Different Precipitants

NASA Astrophysics Data System (ADS)

Sun, Yan; Yang, Shenghui; Zhang, Ye; Jiang, Jun; Jiang, Haochuan

2014-02-01

In order to obtain a uniform transparent ceramic scintillator, well-dispersed fine starting powders with high-purity, small grain size, spherical morphology and high sinter-ability are necessary. In this study, Ce3+ doped gadolinium aluminum gallium garnet Gd3Al3Ga2O12 (GAGG) powders were synthesized by the co-precipitation method. NH4OH, NH4HCO3 and the mixed solution of NH4OH and NH4HCO3 were used as precipitants, respectively. The precursor composition, phase formation process, microstructure, morphology, particle size distribution and luminescent properties of obtained GAGG powders were measured. The results show that powders prepared using the mixed precipitant exhibit the best microstructural morphology, good sinter-ability and highest luminescent intensity. Pure GAGG polycrystalline powders could be obtained at about 950°C for 1.5 h and the average size of the particles is about 50 nm. The photoluminescence spectrum shows a strong green-yellow emission near 540 nm.
Aluminum Coprecipitates with Fe (hydr)oxides: Does Isomorphous Substitution of Al3plus for Fe3plus in Goethite Occur

DOE Office of Scientific and Technical Information (OSTI.GOV)

E Bazilevskaya; D Archibald; M Aryanpour

2011-12-31

Iron (hydr)oxides are common in natural environments and typically contain large amounts of impurities, presumably the result of coprecipitation processes. Coprecipitation of Al with Fe (hydr)oxides occurs, for example, during alternating reduction-oxidation cycles that promote dissolution of Fe from Fe-containing phases and its re-precipitation as Fe-Al (hydr)oxides. We used chemical and spectroscopic analyses to study the formation and transformation of Al coprecipitates with Fe (hydr)oxides. In addition, periodic density functional theory (DFT) computations were performed to assess the structural and energetic effects of isolated or clustered Al atoms at 8 and 25 mol% Al substitution in the goethite structure. Coprecipitatesmore » were synthesized by raising the pH of dilute homogeneous solutions containing a range of Fe and Al concentrations (100% Fe to 100% Al) to 5. The formation of ferrihydrite in initial suspensions with {<=}20 mol% Al, and of ferrihydrite and gibbsite in initial suspensions with {>=}25 mol% Al was confirmed by infrared spectroscopic and synchrotron-based X-ray diffraction analyses. While base titrations showed a buffer region that corresponded to the hydrolysis of Fe in initial solutions with {<=}25 mol% Al, all of the Al present in these solutions was retained by the solid phases at pH 5, thus indicating Al coprecipitation with the primary Fe hydroxide precipitate. In contrast, two buffer regions were observed in solutions with 30 mol% Al (at pH {approx}2.25 for Fe{sup 3+} and at pH {approx}4 for Al{sup 3+}), suggesting the formation of Fe and Al (hydr)oxides as two separate phases. The Al content of initial coprecipitates influenced the extent of ferrihydrite transformation and of its transformation products as indicated by the presence of goethite, hematite and/or ferrihydrite in aged suspensions. DFT experiments showed that: (i) optimized unit cell parameters for Al-substituted goethites (8 and 25 Mol% Al) in clustered arrangement (i.e., the formation of diaspore-like clusters) were in good agreement with available experimental data whereas optimized unit cell parameters for isolated Al atoms were not, and (ii) Al-substituted goethites with Al in diaspore-like clusters resulted in more energetically favored structures. Combined experimental and DFT results are consistent with the coprecipitation of Al with Fe (hydr)oxides and with the formation of diaspore-like clusters, whereas DFT results suggest isomorphous Al for Fe substitution within goethite is unlike at 8 mol% Al substitution.« less
Y-TZP ceramic processing from coprecipitated powders: a comparative study with three commercial dental ceramics.

PubMed

Lazar, Dolores R R; Bottino, Marco C; Ozcan, Mutlu; Valandro, Luiz Felipe; Amaral, Regina; Ussui, Valter; Bressiani, Ana H A

2008-12-01

(1) To synthesize 3mol% yttria-stabilized zirconia (3Y-TZP) powders via coprecipitation route, (2) to obtain zirconia ceramic specimens, analyze surface characteristics, and mechanical properties, and (3) to compare the processed material with three reinforced dental ceramics. A coprecipitation route was used to synthesize a 3mol% yttria-stabilized zirconia ceramic processed by uniaxial compaction and pressureless sintering. Commercially available alumina or alumina/zirconia ceramics, namely Procera AllCeram (PA), In-Ceram Zirconia Block (CAZ) and In-Ceram Zirconia (IZ) were chosen for comparison. All specimens (6mmx5mmx5mm) were polished and ultrasonically cleaned. Qualitative phase analysis was performed by XRD and apparent densities were measured on the basis of Archimedes principle. Ceramics were also characterized using SEM, TEM and EDS. The hardness measurements were made employing Vickers hardness test. Fracture toughness (K(IC)) was calculated. Data were analyzed using one-way analysis of variance (ANOVA) and Tukey's test (alpha=0.05). ANOVA revealed that the Vickers hardness (p<0.0001) and fracture toughness (p<0.0001) were affected by the ceramic materials composition. It was confirmed that the PA ceramic was constituted of a rhombohedral alumina matrix, so-called alpha-alumina. Both CAZ and IZ ceramics presented tetragonal zirconia and alpha-alumina mixture of phases. The SEM/EDS analysis confirmed the presence of aluminum in PA ceramic. In the IZ and CAZ ceramics aluminum, zirconium and cerium in grains involved by a second phase containing aluminum, silicon and lanthanum were identified. PA showed significantly higher mean Vickers hardness values (H(V)) (18.4+/-0.5GPa) compared to vitreous CAZ (10.3+/-0.2GPa) and IZ (10.6+/-0.4GPa) ceramics. Experimental Y-TZP showed significantly lower results than that of the other monophased ceramic (PA) (p<0.05) but it showed significantly higher fracture toughness (6.0+/-0.2MPam(1/2)) values when compared to the other tested ceramics (p<0.05). The coprecipitation method used to synthesize zirconia powders and the adopted ceramic processing conditions led to ceramics with mechanical properties comparable to commercially available reinforced ceramic materials.
Surface chemistry of ferrihydrite: Part 2. Kinetics of arsenate adsorption and coprecipitation

USGS Publications Warehouse

Fuller, C.C.; Dadis, J.A.; Waychunas, G.A.

1993-01-01

The kinetics of As(V) adsorption by ferrihydrite was investigated in coprecipitation and postsynthesis adsorption experiments conducted in the pH range 7.5-9.0. In coprecipitation experiments, As(V) was present in solution during the hydrolysis and precipitation of iron. In adsorption experiments, a period of rapid (<5 min) As(V) uptake from solution was followed by continued uptake for at least eight days, as As(V) diffused to adsorption sites on ferrihydrite surfaces within aggregates of colloidal particles. The time dependence of As(V) adsorption is well described by a general model for diffusion into a sphere if a subset of surface sites located near the exterior of aggregates is assumed to attain adsorptive equilibrium rapidly. The kinetics of As(V) desorption after an increase in pH were also consistent with diffusion as a rate-limiting process. Aging of pure ferrihydrite prior to As(V) adsorption caused a decrease in adsorption sites on the precipitate owing to crystallite growth. In coprecipitation experiments, the initial As(V) uptake was significantly greater than in post-synthesis adsorption experiments, and the rate of uptake was not diffusion limited because As(V) was coordinated by surface sites before crystallite growth and coagulation processes could proceed. After the initial adsorption, As(V) was slowly released from coprecipitates for at least one month, as crystallite growth caused desorption of As(V). Adsorption densities as high as 0.7 mole As(V) per mole of Fe were measured in coprecipitates, in comparison to 0.25 mole As(V) per mole of Fe in post-synthesis adsorption experiments. Despite the high Concentration of As(V) in the precipitates, EXAFS spectroscopy (Waychunas et al., 1993) showed that neither ferric arsenate nor any other As-bearing surface precipitate or solid solution was formed. The high adsorption densities are possible because the ferrihydrite particles are extremely small, approaching the size of small dioctahedral chains at the highest As(V) adsorption density. The results suggest that the solid solution model proposed by Fox (1989, 1992) for control of arsenate and phosphate concentrations in natural waters may be invalid. ?? 1993.
NMR spectroscopic study of organic phosphate esters coprecipitated with calcite

NASA Astrophysics Data System (ADS)

Phillips, Brian L.; Zhang, Zelong; Kubista, Laura; Frisia, Silvia; Borsato, Andrea

2016-06-01

Organic phosphorus incorporated in calcite during laboratory precipitation experiments and in natural cave deposits was investigated by solid-state NMR spectroscopy. For calcite precipitated in the presence of organic phosphoesters of varying size and functionality, solid-state 31P{1H} CP/MAS NMR shows that the phosphoesters were incorporated intact into the solid. Systematic changes in the 31P NMR chemical shift of the phosphate group were observed between the solid phosphoester and that incorporated in the solid precipitate, yielding 31P NMR chemical shifts of the coprecipitates in the range of +1.8 to -2.2 ppm. These chemical shifts are distinct from that of similarly prepared calcite coprecipitated with inorganic phosphate, 3.5 ppm. Only minor changes were noted in the phosphoester 31P chemical shift anisotropy (CSA) which suggests no significant change in the local structure of the phosphate group, which is dominated by C-O-P bonding. Close spatial proximity of the organic phosphate group to calcite structural components was revealed by 31P/13C rotational echo double resonance (REDOR) experiments for coprecipitates prepared with 13C-labeled carbonate. All coprecipitates showed significant 31P dephasing effects upon 13C-irradiation, signaling atomic-scale proximity to carbonate carbon. The dephasing rate for smaller organophosphate molecules is similar to that observed for inorganic phosphate, whereas much slower dephasing was observed for larger molecules having long and/or bulky side-chains. This result suggests that small organic molecules can be tightly enclosed within the calcite structure, whereas significant structural disruption required to accommodate the larger organic molecules leads to longer phosphate-carbonate distances. Comparison of 31P NMR spectroscopic data from the synthetic coprecipitates with those from calcite moonmilk speleothems indicates that phosphorus occurs mainly as inorganic orthophosphate in the natural deposits, although small signals occur with characteristics consistent with phosphate monoesters. The results of this study indicate that trace- to minor concentrations of dissolved organic molecules can be effectively taken up during calcite precipitation and incorporated in the structure, leaving a resilient record of materials present during crystallization.

Small-angle neutron scattering investigations of Co-doped iron oxide nanoparticles. Preliminary results

NASA Astrophysics Data System (ADS)

Creanga, Dorina; Balasoiu, Maria; Soloviov, Dmitro; Balasoiu-Gaina, Alexandra-Maria; Puscasu, Emil; Lupu, Nicoleta; Stan, Cristina

2018-03-01

Preliminary small-angle neutron scattering investigations on aqueous suspensions of several cobalt doped ferrites (CoxFe3-xO4, x=0; 0.5; 1) nanoparticles prepared by chemical co-precipitation method, are reported. The measurements were accomplished at the YuMO instrument in function at the IBR-2 reactor. Results of intermediary data treatment are presented and discussed.
Synthesis and structural characterization of CZTS nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lydia, R.; Reddy, P. Sreedhara

2013-06-03

The CZTS nanoparticles were successfully synthesized by Chemical co-precipitation method with different pH values in the range of 6 to 8. The synthesized nanoparticles were characterized by X-ray diffraction, scanning electron microscopy and energy dispersive spectroscopy. XRD studies revealed that the CZTS nanoparticles exhibited Kesterite Structure with preferential orientation along the (112) direction. Sample at pH value of 7 reached the nearly stoichiometric ratio.
F-T process using an iron on mixed zirconia-titania supported catalyst

DOEpatents

Dyer, Paul N.; Nordquist, Andrew F.; Pierantozzi, Ronald

1987-01-01

A Fischer-Tropsch catalyst comprising iron co-deposited with or deposited on particles comprising a mixture of zirconia and titania, preferably formed by co-precipitation of compounds convertible to zirconia and titania, such as zirconium and titanium alkoxide. The invention also comprises the method of making this catalyst and an improved Fischer-Tropsch reaction process in which the catalyst is utilized.
Synthesis and Characterization of Cu- and Co-Doped Bi4V2O11 for Intermediate-Temperature Solid Oxide Fuel Cell Electrolytes by Carbonate Coprecipitation

NASA Astrophysics Data System (ADS)

Lee, Jin Goo; Yoon, Hyon Hee

2011-01-01

Bi2MexV1-xO5.5-3x/2 (Me = Cu; 0≤x≤0.2) powders were prepared by the ammonium carbonate coprecipitation method. The starting salts were bismuth nitrate, copper nitrate, cobalt nitrate, and vanadium sulphate. The thermal decomposition of Bi2MexV1-xO5.5-3x/2 precursors was completed at about 500 °C. The crystallite structure, surface morphology, and ionic conductivity of the prepared powders and pellets were examined using X-ray diffractometry, field emission scanning electron microscopy, and an impedance analyzer, respectively. The average particle sizes of the Bi2Cu0.1V0.9O5.35 and Bi2Co0.1V0.9O5.35 powders were 10-50 nm. The tetragonal structure (γ-phase) appeared at sintering temperatures higher than 700 °C and the peak intensity increased at higher sintering temperatures. The ionic conductivities of the Bi2Cu0.1V0.9O5.35 and Bi2Co0.1V0.9O5.35 pellets sintered at 800 °C showed the highest values of 6.8×10-2 S cm-1 at 700 °C and 9.1×10-2 S cm-1 at 700 °C, respectively. The optimum concentration of the Cu and Co dopants in Bi2MexV1-xO5.5-3x/2 was determined to be 0.1. The results of this study demonstrated that the ammonium carbonate coprecipitation process could be used as an economical method for the preparation of Bi2MexV1-xO5.5-3x/2 electrolytes for intermediate-temperature solid oxide fuel cells.
Arsenic mobilization and immobilization in paddy soils

NASA Astrophysics Data System (ADS)

Kappler, A.; Hohmann, C.; Zhu, Y. G.; Morin, G.

2010-05-01

Arsenic is oftentimes of geogenic origin and in many cases bound to iron(III) minerals. Iron(III)-reducing bacteria can harvest energy by coupling the oxidation of organic or inorganic electron donors to the reduction of Fe(III). This process leads either to dissolution of Fe(III)-containing minerals and thus to a release of the arsenic into the environment or to secondary Fe-mineral formation and immobilisation of arsenic. Additionally, aerobic and anaerobic iron(II)-oxidizing bacteria have the potential to co-precipitate or sorb arsenic during iron(II) oxidation at neutral pH that is usually followed by iron(III) mineral precipitation. We are currently investigating arsenic immobilization by Fe(III)-reducing bacteria and arsenic co-precipitation and immobilization by anaerobic iron(II)-oxidizing bacteria in batch, microcosm and rice pot experiments. Co-precipitation batch experiments with pure cultures of nitrate-dependent Fe(II)-oxidizing bacteria are used to quantify the amount of arsenic that can be immobilized during microbial iron mineral precipitation, to identify the minerals formed and to analyze the arsenic binding environment in the precipitates. Microcosm and rice pot experiments are set-up with arsenic-contaminated rice paddy soil. The microorganisms (either the native microbial population or the soil amended with the nitrate-dependent iron(II)-oxidizing Acidovorax sp. strain BoFeN1) are stimulated either with iron(II), nitrate, or oxygen. Dissolved and solid-phase arsenic and iron are quantified. Iron and arsenic speciation and redox state in batch and microcosm experiments are determined by LC-ICP-MS and synchrotron-based methods (EXAFS, XANES).
ANNUAL REPORT FOR ENVIRONMENTAL MANAGEMENT SCIENCE PROGRAM PROJECT NUMBER 87016 CO-PRECIPITATION OF TRACE METALS IN GROUNDWATER AND VADOSE ZONE CALCITE: IN SITU CONTAINMENT AND STABILIZATION OF STRONTIUM-90 AND OTHER DIVALENT METALS AND RADIONUCLIDES AT ARID WESTERN DOE SITES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, Robert W.; Fujita, Yoshiko; Ferris, F. Grant

2003-06-15

Radionuclide and metal contaminants such as 90Sr are present beneath U.S. Department of Energy (DOE) lands in both the groundwater (e.g., 100-N area at Hanford, WA) and vadose zone (e.g., Idaho Nuclear Technology and Engineering Center at the Idaho National Engineering and Environmental Laboratory). In situ containment and stabilization of these contaminants is a cost-effective treatment strategy. However, implementing in situ containment and stabilization approaches requires definition of the mechanisms that control contaminant sequestration. We are investigating the in situ immobilization of radionuclides or contaminant metals (e.g., 90Sr) by their facilitated co-precipitation with calcium carbonate in groundwater and vadose zonemore » systems. Our facilitated approach, shown schematically in Figure 1, relies upon the hydrolysis of introduced urea to cause the acceleration of calcium carbonate precipitation (and trace metal co-precipitation) by increasing pH and alkalinity. Subsurface urea hydrolysis is catalyzed by the urease enzyme, which may be either introduced with the urea or produced in situ by ubiquitous subsurface urea hydrolyzing microorganisms. Because the precipitation process tends to be irreversible and many western aquifers are saturated with respect to calcite, the coprecipitated metals and radionuclides will be effectively removed from the aqueous phase over the long-term. Another advantage of the ureolysis approach is that the ammonium ions produced by the reaction can exchange with radionuclides sorbed to subsurface minerals, thereby enhancing the availability of the radionuclides for re-capture in a more stable solid phase (co-precipitation rather than adsorption).« less
Isolation of 236U and 239,240Pu from seawater samples and its determination by Accelerator Mass Spectrometry.

PubMed

López-Lora, Mercedes; Chamizo, Elena; Villa-Alfageme, María; Hurtado-Bermúdez, Santiago; Casacuberta, Núria; García-León, Manuel

2018-02-01

In this work we present and evaluate a radiochemical procedure optimised for the analysis of 236 U and 239,240 Pu in seawater samples by Accelerator Mass Spectrometry (AMS). The method is based on Fe(OH) 3 co-precipitation of actinides and uses TEVA® and UTEVA® extraction chromatography resins in a simplified way for the final U and Pu purification. In order to improve the performance of the method, the radiochemical yields are analysed in 1 to 10L seawater volumes using alpha spectrometry (AS) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Robust 80% plutonium recoveries are obtained; however, it is found that Fe(III) concentration in the precipitation solution and sample volume are the two critical and correlated parameters influencing the initial uranium extraction through Fe(OH) 3 co-precipitation. Therefore, we propose an expression that optimises the sample volume and Fe(III) amounts according to both the 236 U and 239,240 Pu concentrations in the samples and the performance parameters of the AMS facility. The method is validated for the current setup of the 1MV AMS system (CNA, Sevilla, Spain), where He gas is used as a stripper, by analysing a set of intercomparison seawater samples, together with the Laboratory of Ion Beam Physics (ETH, Zürich, Switzerland). Copyright © 2017 Elsevier B.V. All rights reserved.
High solar-light photocatalytic activity of using Cu3Se2/rGO nanocomposites synthesized by a green co-precipitation method

NASA Astrophysics Data System (ADS)

Nouri, Morteza; Saray, Abdolali Moghaddam; Azimi, H. R.; Yousefi, Ramin

2017-11-01

Current work presents a facile, cost-effective, and green method to synthesize copper selenide nanostructures and copper selenide/graphene nanocomposites. The products were synthesized by a co-precipitation method by glycine amino acid as a green surfactant and graphene oxide (GO) sheets as a graphene source. X-ray diffraction patterns (XRD) of the products indicated that the products were Cu2Se3 with tetragonal phase. Fourier transform infrared (FTIR) spectroscopy and the XRD patterns indicated that the GO sheets were changed into reduced GO (rGO) during the synthesis process. Scanning and transmission electron microscopy (SEM and TEM) images showed the nanoparticles (NPs) that were decorated on rGO sheets had the significantly smaller size in compared to the pristine NPs. UV-vis results revealed that, the absorption peak of the products were in the visible region with a band-gap value between 1.85 eV and 1.95 eV. Finally, the products were applied as photocatalytic materials to remove Methylene Blue (MB) dye under solar-light and visible-light irradiation conditions. It was observed; the rGO had a significant role in enhancing the photocatalytic performance of the products and Cu2Se3/rGO (15%) could degrade more than 91% and 73% of MB only during 1 h under solar-light and visible-light sources, respectively.
Determination of Trace Level Iodine in Biological and Botanical Reference Materials by Isotope Dilution Mass Spectrometry

PubMed Central

Gramlich, John W.; Murphy, Thomas J.

1989-01-01

A method has been developed for the determination of trace level iodine in biological and botanical materials. The method consists of spiking a sample with 129I, equilibration of the spike with the natural iodine, wet ashing under carefully controlled conditions, and separation of the iodine by co-precipitation with silver chloride. Measurement of the 129I/127I ratio is accomplished by negative thermal ionization mass spectrometry using LaB6 for ionization enhancement. The application of the method to the certification of trace iodine in two Standard Reference Materials is described. PMID:28053411
A rapid method for the sequential separation of polonium, plutonium, americium and uranium in drinking water.

PubMed

Lemons, B; Khaing, H; Ward, A; Thakur, P

2018-06-01

A new sequential separation method for the determination of polonium and actinides (Pu, Am and U) in drinking water samples has been developed that can be used for emergency response or routine water analyses. For the first time, the application of TEVA chromatography column in the sequential separation of polonium and plutonium has been studied. This method utilizes a rapid Fe +3 co-precipitation step to remove matrix interferences, followed by plutonium oxidation state adjustment to Pu 4+ and an incubation period of ~ 1 h at 50-60 °C to allow Po 2+ to oxidize to Po 4+ . The polonium and plutonium were then separated on a TEVA column, while separation of americium from uranium was performed on a TRU column. After separation, polonium was micro-precipitated with copper sulfide (CuS), while actinides were micro co-precipitated using neodymium fluoride (NdF 3 ) for counting by the alpha spectrometry. The method is simple, robust and can be performed quickly with excellent removal of interferences, high chemical recovery and very good alpha peak resolution. The efficiency and reliability of the procedures were tested by using spiked samples. The effect of several transition metals (Cu 2+ , Pb 2+ , Fe 3+ , Fe 2+ , and Ni 2+ ) on the performance of this method were also assessed to evaluate the potential matrix effects. Studies indicate that presence of up to 25 mg of these cations in the samples had no adverse effect on the recovery or the resolution of polonium alpha peaks. Copyright © 2018 Elsevier Ltd. All rights reserved.
Methods for making a supported iron-copper catalyst

DOEpatents

Dyer, Paul N.; Pierantozzi, Ronald

1986-01-01

A catalyst is described for the synthesis of hydrocarbons from CO+H.sub.2 utilizing a porous Al.sub.2 O.sub.3 support impregnated with iron and copper and optionally promoted with an alkali metal. The use of an Al.sub.2 O.sub.3 support results in the suppression of heavy waxes (C.sub.26 + hydrocarbons), particularly in slurry phase operation, when compared to unsupported or co-precipitated catalysts.
Synthesis and evaluation of α-Ag2WO4 as novel antifungal agent

NASA Astrophysics Data System (ADS)

Foggi, Camila C.; Fabbro, Maria T.; Santos, Luís P. S.; de Santana, Yuri V. B.; Vergani, Carlos E.; Machado, Ana L.; Cordoncillo, Eloisa; Andrés, Juan; Longo, Elson

2017-04-01

Because of the need for new antifungal materials with greater potency, microcrystals of α-Ag2WO4, a complex metal oxide, have been synthetized by a simple co-precipitation method, and their antifungal activity against Candida albicans has been investigated. A theoretical model based on clusters that are building blocks of α-Ag2WO4 has been proposed to explain the experimental results.
Dynamic Behavior and Optimization of Advanced Armor Ceramics: January-December 2011 Annual Report

DTIC Science & Technology

2015-03-01

however, under conventional methods of processing. To develop plasticity in ceramic like SiC, new fracture mechanisms and interesting behaviors need...and new fracture mechanisms . These improvements, in turn, could offer the potential for improved ballistic performance. Co-precipitation has been...experiments, the following deformed fragments were recovered for extensive SEM and TEM study.  A fracture mechanism map has been constructed in
Method for separating contaminants from solution employing an organic-stabilized metal-hydroxy gel

DOEpatents

Alexander, Donald H.

1996-01-01

Metals and organics are extracted from solution by co-precipitating them with a gel comprising aluminum hydroxide and a complexing agent such as EDTA. After the gel is processed to remove the metals and organics, it can be recycled for further use by dissolving it in a high-pH solution, leaving no secondary waste stream. A number of alternative complexing agents perform better than EDTA.
Uranium Redox Transformations after U(VI) Coprecipitation with Magnetite Nanoparticles.

PubMed

Pidchenko, Ivan; Kvashnina, Kristina O; Yokosawa, Tadahiro; Finck, Nicolas; Bahl, Sebastian; Schild, Dieter; Polly, Robert; Bohnert, Elke; Rossberg, André; Göttlicher, Jörg; Dardenne, Kathy; Rothe, Jörg; Schäfer, Thorsten; Geckeis, Horst; Vitova, Tonya

2017-02-21

Uranium redox states and speciation in magnetite nanoparticles coprecipitated with U(VI) for uranium loadings varying from 1000 to 10 000 ppm are investigated by X-ray absorption spectroscopy (XAS). It is demonstrated that the U M 4 high energy resolution X-ray absorption near edge structure (HR-XANES) method is capable to clearly characterize U(IV), U(V), and U(VI) existing simultaneously in the same sample. The contributions of the three different uranium redox states are quantified with the iterative transformation factor analysis (ITFA) method. U L 3 XAS and transmission electron microscopy (TEM) reveal that initially sorbed U(VI) species recrystallize to nonstoichiometric UO 2+x nanoparticles within 147 days when stored under anoxic conditions. These U(IV) species oxidize again when exposed to air. U M 4 HR-XANES data demonstrate strong contribution of U(V) at day 10 and that U(V) remains stable over 142 days under ambient conditions as shown for magnetite nanoparticles containing 1000 ppm U. U L 3 XAS indicates that this U(V) species is protected from oxidation likely incorporated into octahedral magnetite sites. XAS results are supported by density functional theory (DFT) calculations. Further characterization of the samples include powder X-ray diffraction (pXRD), scanning electron microscopy (SEM) and Fe 2p X-ray photoelectron spectroscopy (XPS).
Structure, molecular simulation, and release of aspirin from intercalated Zn-Al-layered double hydroxides.

PubMed

Meng, Zilin; Li, Xiaowei; Lv, Fengzhu; Zhang, Qian; Chu, Paul K; Zhang, Yihe

2015-11-01

Aspirin or acetylsalicylic acid (AA), a non-steroidal anti-inflammatory drug, is intercalated into Zn-Al-layered double hydroxides (ZnAl-LDHs) by co-precipitation and reconstruction methods. The composition, structure, and morphology of the intercalated products as well as their release behavior are determined experimentally and theoretically by Material Studio 5.5. Experimental results disclose the strong interaction between the LDHs sheets and AA in the intercalated ZnAl-LDHs produced by co-precipitation and slow release of AA from the intercalated ZnAl-LDHs in both phosphate buffered saline (PBS) and borate buffered saline (BBS) solutions. The percentage of AA released from the ZnAl-LDHs prepared by both methods in PBS (96.87% and 98.12%) are much more than those in BBS (68.59% and 81.22%) implying that both H4BO4(-) and H2PO4(-) can exchange with AA in the ZnAl-LDHs. After AA is released to PBS, ZnAl-LDHs break into small pieces. The experimental results are explained theoretically based on the calculation of the bonding energy between the anions and LDHs sheets as well as the AlO bond length change in the LDHs sheets. Copyright © 2015 Elsevier B.V. All rights reserved.
Synthesis of nano-sized ZnO particles by co-precipitation method with variation of heating time

DOE Office of Scientific and Technical Information (OSTI.GOV)

Purwaningsih, S. Y., E-mail: sriyanisaputri@gmail.com; Pratapa, S.; Triwikantoro

Zinc oxide powders have been synthesized by a co-precipitation method at low temperature (85 °C), using zinc acetate dihydrate, ammonia, hydrochloric acid solutions as the reactants. A number of process parameters such as reaction temperature, solution basicity or pH and heating time are the main factors affecting the morphology and physical properties of the ZnO nanostructures. In this work the effect of heating time on the morphology and particles size were studied. The as-synthesized ZnO powders were characterized using transmission electron microscopy (TEM) and X-ray diffraction (XRD) techniques. The samples were also analyzed using Fourier transform infrared (FTIR). Rietveld refinementmore » of XRD data confirms that ZnO crystallizes in the hexagonal wurtzite structure with high degree of purity and the (101) plane predominant. The XRD results show that the average crystallite sizes were about 66, 27 and 12 nm for 3, 4 and 5 h of heating times, respectively. The XRD analysis indicated that a fraction of nano-sized ZnO powders were in the form of aggregates, which was also verified by TEM image. The TEM photograph demonstrated that the nano-sized ZnO particles were a pseudo-spherical shape.« less
Superior magnetic properties of Ni ferrite nanoparticles synthesized by capping agent-free one-step coprecipitation route at different pH values

NASA Astrophysics Data System (ADS)

Iranmanesh, P.; Tabatabai Yazdi, Sh.; Mehran, M.; Saeednia, S.

2018-03-01

In this work, well-dispersed nanoparticles of NiFe2O4 with diameters less than 10 nm and good crystallinity and excellent magnetic properties were synthesized via a simple one-step capping agent-free coprecipitation route from metal chlorides. The ammonia was used as the precipitating agent and also the solution basicity controller. The effect of pH value during the coprecipitation process was investigated by details through microstructural, optical and magnetic characterizations of the synthesized particles using X-ray diffraction, transmission electron microscopy, Fourier transform infrared and UV-vis spectroscopy, and vibrating sample magnetometer. The results showed that the particle size, departure from the inverse spinel structure, the band gap value and the magnetization of Ni ferrite samples increase with pH value from 9 to 11 indicating the more pronounced surface effects in the smaller nanoparticles.
Physicochemical fabrication of antibacterial calcium phosphate submicrospheres with dispersed silver nanoparticles via coprecipitation and photoreduction under laser irradiation.

PubMed

Nakamura, Maki; Oyane, Ayako; Shimizu, Yoshiki; Miyata, Saori; Saeki, Ayumi; Miyaji, Hirofumi

2016-12-01

We achieved rapid, surfactant-free, and one-pot fabrication of antibacterial calcium phosphate (CaP) submicrospheres containing silver nanoparticles by combining physical laser and chemical coprecipitation processes. In this physicochemical process, weak pulsed laser irradiation (20min) was performed on a labile CaP reaction mixture supplemented with silver ions as a light-absorbing agent. The silver content in the submicrospheres was controlled for a wide range (Ag/P elemental ratio varied from 0.60 to 62.0) by tuning the initial concentration of silver ions (from 5 to 20mM) in the CaP reaction mixture. At the silver concentration of 5mM, we obtained unique nanocomposite particles: CaP submicrospheres (average diameter of approximately 500nm) containing metallic silver nanoparticles dispersed throughout, as a result of CaP and silver coprecipitation with simultaneous photoreduction of silver ions and spheroidization of the coprecipitates. These CaP submicrospheres containing silver nanoparticles (ca. 0.3mg silver per 1mg submicrospheres) exhibited antibacterial activity against major pathogenic oral bacteria, i.e., Streptococcus mutans, Aggregatibacter actinomycetemcomitans, and Porphyromonas gingivalis. Moreover, the CaP submicrospheres dissolved and neutralized the acidic environment generated by Streptococcus mutans, demonstrating their potential as acid-neutralizing and remineralizing agents. The present process and resulting antibacterial CaP-based submicrospheres are expected to be useful in dental healthcare and infection control. Nano- and microsized spheres of calcium phosphate (CaP) containing silver nanoparticles have great potential in dental applications. Conventional fabrication processes were time-consuming or weak regarding the size/shape control of the spheres. In this study, we achieved a simple (one-pot), rapid (20-min irradiation), and surfactant-free fabrication of CaP submicrospheres containing silver nanoparticles by pulsed laser irradiation to a mixture of calcium, phosphate, and silver ion solutions. The resulting CaP submicrospheres contained metallic silver nanoparticles dispersed throughout in a sequence of reactions: CaP and silver coprecipitation, laser-induced melting and spheroidization of the coprecipitates, and photoreduction of silver ions. These submicrospheres showed antibacterial activity against oral bacteria and acid-neutralizing property in the bacterial suspension, and hence are worth considering for dental applications. Copyright © 2016 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
Co-Precipitation Synthesis and Characterization of SrBi2Ta2O9 Ceramic

NASA Astrophysics Data System (ADS)

Afqir, Mohamed; Tachafine, Amina; Fasquelle, Didier; Elaatmani, Mohamed; Carru, Jean-Claude; Zegzouti, Abdelouahad; Daoud, Mohamed

2018-04-01

Strontium bismuth tantalate (SrBi2Ta2O9) was synthesized by a co-precipitation method. The sample was characterized by x-ray powder diffraction patterns (XRD), Fourier-transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The results of the dielectric properties are reported at room temperature. No secondary phases were found while heating the powder at 850°C and the pure SrBi2Ta2O9 phase was formed, as revealed by XRD. The characteristic bands for SrBi2Ta2O9 were observed by FTIR at approximately 619 cm-1 and 810 cm-1. SEM micrographs for the sample displayed thin plate-like grains. The grain size was less than 1 μm and the crystallite size of about 24 nm. Dielectric response at room temperature shows that the SrBi2Ta2O9 ceramic has low loss values, and the flattening of the dielectric constant at higher frequencies. The observed Curie temperature is comparable with those reported in the literature.

Molybdenum blue reaction and determination of phosphorus in waters containing arsenic, silicon, and germanium

USGS Publications Warehouse

Levine, H.; Rowe, J.J.; Grimaldi, F.S.

1955-01-01

Microgram amounts of phosphate are usually determined by the molybdenum blue reaction, but this reaction is not specific for phosphorus. The research established the range of conditions under which phosphate, arsenate, silicate, and germanate give the molybdenum blue reaction for differentiating these elements, and developed a method for the determination of phosphate in waters containing up to 10 p.p.m. of the oxides of germanium, arsenic(V), and silicon. With stannous chloride or 1-amino-2-naphthol-4-sulfonic acid as the reducing agent no conditions were found for distinguishing silicate from germanate and phosphate from arsenate. In the recommended procedure the phosphate is concentrated by coprecipitation on aluminum hydroxide, and coprecipitated arsenic, germanium, and silicon are volatilized by a mixture of hydrofluoric, hydrochloric, and hydrobromic acids prior to the determination of phosphate. The authors are able to report that the total phosphorus content of several samples of sea water from the Gulf of Mexico ranged from 0.018 to 0.059 mg. of phosphorus pentoxide per liter of water.
Determination of the platinum - Group elements (PGE) and gold (Au) in manganese nodule reference samples by nickel sulfide fire-assay and Te coprecipitation with ICP-MS

USGS Publications Warehouse

Balaram, V.; Mathur, R.; Banakar, V.K.; Hein, J.R.; Rao, C.R.M.; Gnaneswara, Rao T.; Dasaram, B.

2006-01-01

Platinum group elements (PGE) and Au data in polymetallic oceanic ferromanganese nodule reference samples and crust samples obtained by inductively coupled plasma mass spectrometry (ICP-MS), after separation and pre-concentration by nickel sulfide fire-assay and Te coprecipitation, are presented. By optimizing several critical parameters such as flux composition, matrix matching calibration, etc., best experimental conditions were established to develop a method suitable for routine analysis of manganese nodule samples for PGE and Au. Calibrations were performed using international PGE reference materials, WMG-1 and WMS-1. This improved procedure offers extremely low detection limits in the range of 0.004 to 0.016 ng/g. The results obtained in this study for the reference materials compare well with previously published data wherever available. New PGE data arc also provided on some international manganese nodule reference materials. The analytical methodology described here can be used for the routine analysis of manganese nodule and crust samples in marine geochemical studies.
Facile Synthesis of Calcium Borate Nanoparticles and the Annealing Effect on Their Structure and Size

PubMed Central

Erfani, Maryam; Saion, Elias; Soltani, Nayereh; Hashim, Mansor; Wan Abdullah, Wan Saffiey B.; Navasery, Manizheh

2012-01-01

Calcium borate nanoparticles have been synthesized by a thermal treatment method via facile co-precipitation. Differences of annealing temperature and annealing time and their effects on crystal structure, particle size, size distribution and thermal stability of nanoparticles were investigated. The formation of calcium borate compound was characterized by X-ray diffraction (XRD) and Fourier Transform Infrared spectroscopy (FTIR), Transmission electron microscopy (TEM), and Thermogravimetry (TGA). The XRD patterns revealed that the co-precipitated samples annealed at 700 °C for 3 h annealing time formed an amorphous structure and the transformation into a crystalline structure only occurred after 5 h annealing time. It was found that the samples annealed at 900 °C are mostly metaborate (CaB2O4) nanoparticles and tetraborate (CaB4O7) nanoparticles only observed at 970 °C, which was confirmed by FTIR. The TEM images indicated that with increasing the annealing time and temperature, the average particle size increases. TGA analysis confirmed the thermal stability of the annealed samples at higher temperatures. PMID:23203073
A novel multifunctional pharmaceutical excipient: modification of the permeability of starch by processing with magnesium silicate.

PubMed

Rashid, Iyad; Al-Remawi, Mayyas; Leharne, Stephen A; Chowdhry, Babur Z; Badwan, Adnan

2011-06-15

A directly compressible excipient has been developed by co-processing starch with magnesium silicate. The foregoing was achieved either by co-precipitation of magnesium silicate onto different types of starch or by dry granulation of maize starch with magnesium silicate. A variety of techniques (permeability, water retention/swelling, compression analysis, scanning electron microscopy, tensile strength and disintegration/dissolution studies) were used to characterize these systems. The permeability of the formulations produced using the two methods was evaluated experimentally using Darcy's permeability law. Magnesium silicate, as an anti-adhering agent, increases the permeability of both maize and partially pregelatinized starch, resulting in compacts of high mechanical strength, short disintegration time and low lubricant sensitivity. Such advantages are evident when the properties of the physical mixture of maize starch with magnesium silicate are compared with the co-precipitation and dry granulation techniques. Formulation with this novel excipient system, using paracetamol as a model drug, indicated its suitability as a single multifunctional excipient. Copyright © 2011 Elsevier B.V. All rights reserved.
Effect of Cu2+ substitution on the magnetic properties of co-precipitated Ni-Cu-Zn ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Ramakrishna, K. S.; Srinivas, Ch.; Tirupanyam, B. V.; Ramesh, P. N.; Meena, S. S.; Potukuchi, D. M.; Sastry, D. L.

2017-05-01

Spinel ferrite nanoparticles with chemical equation NixCu0.1Zn0.9-xFe2O4 (x = 0.5, 0.6, 0.7) have been synthsized using co-precipitation method followed by heat treatment at a temperature of 200 °C for 2h. The results of XRD, FE-SEM and VSM studies are reported. XRD patterns confirm the formation of cubic spinel phase of ferrite samples along with small amount of a secondary phase of α-Fe2O3 whose concentration decreases as Ni2+ concentration increases. The crystallite sizes (in the range of 7.5-13.9 nm) increase and the lattice parameter decreases with increase in Ni2+ ion concentration. These values are comparable to those of NiZn ferrite without Cu substitution. It has been observed that there is a considerable reduction in saturation magnetisation (Ms). This and differences in other magnetic parameters are attributed to considerable changes in cation distribution or core shell interactions of NiZn ferrite with 10 mole% Cu substitution in the place of Zn.
Cost and energy demand of producing nickel manganese cobalt cathode material for lithium ion batteries

DOE PAGES

Ahmed, Shabbir; Nelson, Paul A.; Gallagher, Kevin G.; ...

2017-01-05

The price of the cathode active materials in lithium ion batteries is a key cost driver and thus significantly impacts consumer adoption of devices that utilize large energy storage contents (e.g. electric vehicles). A process model has been developed and used to study the production process of a common lithium-ion cathode material, lithiated nickel manganese cobalt oxide, using the co-precipitation method. The process was simulated for a plant producing 6500 kg day –1. The results indicate that the process will consume approximately 4 kWh kg NMC –1 of energy, 15 L kg NMC –1 of process water, and cost $23more » to produce a kg of Li-NMC333. The calculations were extended to compare the production cost using two co-precipitation reactions (with Na 2CO 3 and NaOH), and similar cathode active materials such as lithium manganese oxide and lithium nickel cobalt aluminum oxide. Finally, a combination of cost saving opportunities show the possibility to reduce the cost of the cathode material by 19%.« less
[Determination of americium-241 in urine].

PubMed

Shvydko, N S; Mikhaĭlova, O A; Popov, D K

1988-01-01

A technique has been developed for the determination of americium 241 in urine by a radiochemical purification of the nuclide from uranium (upon co-precipitation of americium 241 with calcium and lanthanum), plutonium, thorium, and polonium 210 (upon co-precipitation of these radionuclides with zirconium iodate). alpha-Radioactivity was measured either in a thick layer of the americium 241 precipitate with a nonisotope carrier or in thin-layer preparations after electrolytic precipitation of americium 241 on a cathode.
Structure and properties of hybrid biopolymer particles fabricated by co-precipitation cross-linking dissolution procedure.

PubMed

Xiong, Yu; Georgieva, Radostina; Steffen, Axel; Smuda, Kathrin; Bäumler, Hans

2018-03-15

The Co-precipitation Crosslinking Dissolution technique (CCD-technique) allows a few-steps fabrication of particles composed of different biopolymers and bioactive agents under mild conditions. Morphology and properties of the fabricated biopolymer particles depend on the fabrication conditions, the nature of the biopolymers and additives, but also on the choice of the inorganic templates for co-precipitation. Here, we investigate the influence of an acidic biopolymer, hyaluronic acid (HA), on the formation of particles from bovine hemoglobin and bovine serum albumin applying co-precipitation with CaCO 3 and MnCO 3 . CaCO 3 templated biopolymer particles are almost spherical with particle size from 2 to 20 µm and protein entrapment efficiency from 13 to 77%. Presence of HA causes significant structural changes of the particles and decreasing protein entrapment efficiency. In contrast, MnCO 3 templated particles exhibit uniform peanut shape and submicron size with remarkably high protein entrapment efficiency of nearly 100%. Addition of HA has no influence on the protein entrapment efficiency or on morphology and size of the particles. These effects can be attributed to the strong interaction of Mn 2+ with proteins and much weaker interaction with HA. Therefore, entrapment efficiency, size and structure of biopolymer particles can be optimized by varying the mineral templates and additives. Copyright © 2017 Elsevier Inc. All rights reserved.
Structural and dielectric studies on Ag doped nano ZnSnO3

NASA Astrophysics Data System (ADS)

Deepa, K.; Angel, S. Lilly; Rajamanickam, N.; Jayakumar, K.; Ramachandran, K.

2018-04-01

Undoped and Ag-doped nano Zinc Stannate (ZSO) ternary oxide were prepared by co-precipitation method. The crystallographic, morphological and optical properties of the synthesized nanoparticles were studied using X-ray diffraction (XRD) and UV-Visible spectroscopy (UV-Vis) and Scanning electron microscopy (SEM). The electrical properties of the synthesized samples were studied by dielectric measurements. Higher concentration Ag doped ZSO nanoparticles exhibit higher dielectric constant at low frequency.
Acetone sensor based on zinc oxide hexagonal tubes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hastir, Anita, E-mail: anitahastir@gmail.com; Singh, Onkar, E-mail: anitahastir@gmail.com; Anand, Kanika, E-mail: anitahastir@gmail.com

2014-04-24

In this work hexagonal tubes of zinc oxide have been synthesized by co-precipitation method. For structural, morphological, elemental and optical analysis synthesized powders were characterized by using x-ray diffraction, field emission scanning microscope, EDX, UV-visible and FTIR techniques. For acetone sensing thick films of zinc oxide have been deposited on alumina substrate. The fabricated sensors exhibited maximum sensing response towards acetone vapour at an optimum operating temperature of 400°C.
The 170-kDa glucose-regulated stress protein is an endoplasmic reticulum protein that binds immunoglobulin.

PubMed Central

Lin, H Y; Masso-Welch, P; Di, Y P; Cai, J W; Shen, J W; Subjeck, J R

1993-01-01

Anoxia, glucose starvation, calcium ionophore A23187, EDTA, glucosamine, and several other conditions that adversely affect the function of the endoplasmic reticulum (ER) induce the synthesis of the glucose-regulated class of stress proteins (GRPs). The primary GRPs induced by these stresses migrate at 78 and 94 kDa (GRP78 and GRP94). In addition, another protein of approximately 150-170 kDa (GRP170) has been previously observed and is coordinately induced with GRP78 and GRP94. To characterize this novel stress protein, we have prepared an antisera against purified GRP170. Immunofluorescence, Endoglycosidase H sensitivity, and protease resistance of this protein in microsomes indicates that GRP170 is an ER lumenal glycoprotein retained in a pre-Golgi compartment. Immunoprecipitation of GRP170 with our antibody coprecipitates the GRP78 (also referred to as the B cell immunoglobulin-binding protein) and GRP94 members of this stress protein family in Chinese hamster ovary cells under stress conditions. ATP depletion, by immunoprecipitation in the presence of apyrase, does not affect the interaction between GRP78 and GRP170 but results in the coprecipitation of an unidentified 60-kDa protein. In addition, GRP170 is found to be coprecipitated with immunoglobulin (Ig) in four different B cell hybridomas expressing surface IgM, cytoplasmic Ig light chain only, cytoplasmic Ig heavy chain only, or an antigen specific secreted IgG. In addition, in IgM surface expressing WEHI-231 B cells, anti-IgM coprecipitates GRP78, GRP94, as well as GRP170; antibodies against GRP170 and GRP94 reciprocally coprecipitate GRP94/GRP170 as well as GRP78. Results suggest that this 170-kDa GRP is a retained ER lumenal glycoprotein that is constitutively present and that may play a role in immunoglobulin folding and assembly in conjunction or consecutively with GRP78 and GRP94. Images PMID:8305733
Particle size, charge and colloidal stability of humic acids coprecipitated with Ferrihydrite.

PubMed

Angelico, Ruggero; Ceglie, Andrea; He, Ji-Zheng; Liu, Yu-Rong; Palumbo, Giuseppe; Colombo, Claudio

2014-03-01

Humic acids (HA) have a colloidal character whose size and negative charge are strictly dependent on surface functional groups. They are able to complex large amount of poorly ordered iron (hydr)oxides in soil as a function of pH and other environmental conditions. Accordingly, with the present study we intend to assess the colloidal properties of Fe(II) coprecipitated with humic acids (HA) and their effect on Fe hydroxide crystallinity under abiotic oxidation and order of addition of both Fe(II) and HA. TEM, XRD and DRS experiments showed that Fe-HA consisted of Ferrihydrite with important structural variations. DLS data of Fe-HA at acidic pH showed a bimodal size distribution, while at very low pH a slow aggregation process was observed. Electrophoretic zeta-potential measurements revealed a negative surface charge for Fe-HA macromolecules, providing a strong electrostatic barrier against aggregation. Under alkaline conditions HA chains swelled, which resulted in an enhanced stabilization of the colloid particles. The increasing of zeta potential and size of the Fe-HA macromolecules, reflects a linear dependence of both with pH. The increase in the size and negative charge of the Fe-HA precipitate seems to be more affected by the ionization of the phenolic acid groups, than by the carboxylic acid groups. The main cause of negative charge generation of Fe/HA is due to increased dissociation of phenolic groups in more expanded structure. The increased net negative surface potential induced by coprecipitation with Ferrihydrite and the correspondent changes in configuration of the HA could trigger the inter-particle aggregation with the formation of new negative surface. The Fe-HA coprecipitation can reduce electrosteric repulsive forces, which in turn may inhibit the aggregation process at different pH. Therefore, coprecipitation of Ferrihydrite would be expected to play an important role in the carbon stabilization and persistence not only in organic soils, but also in waters containing dissolved organic matter. Copyright © 2013 Elsevier Ltd. All rights reserved.
Flame atomic absorption spectrometric determination of heavy metals in aqueous solution and surface water preceded by co-precipitation procedure with copper(II) 8-hydroxyquinoline

NASA Astrophysics Data System (ADS)

Ipeaiyeda, Ayodele Rotimi; Ayoade, Abisayo Ruth

2017-12-01

Co-precipitation procedure has widely been employed for preconcentration and separation of metal ions from the matrices of environmental samples. This is simply due to its simplicity, low consumption of separating solvent and short duration for analysis. Various organic ligands have been used for this purpose. However, there is dearth of information on the application of 8-hydroxyquinoline (8-HQ) as ligand and Cu(II) as carrier element. The use of Cu(II) is desirable because there is no contamination and background adsorption interference. Therefore, the objective of this study was to use 8-HQ in the presence of Cu(II) for coprecipitation of Cd(II), Co(II), Cr(III), Ni(II) and Pb(II) from standard solutions and surface water prior to their determinations by flame atomic absorption spectrometry (FAAS). The effects of pH, sample volume, amount of 8-HQ and Cu(II) and interfering ions on the recoveries of metal ions from standard solutions were monitored using FAAS. The water samples were treated with 8-HQ under the optimum experimental conditions and metal concentrations were determined by FAAS. The metal concentrations in water samples not treated with 8-HQ were also determined. The optimum recovery values for metal ions were higher than 85.0%. The concentrations (mg/L) of Co(II), Ni(II), Cr(III), and Pb(II) in water samples treated with 8-HQ were 0.014 ± 0.002, 0.03 ± 0.01, 0.04 ± 0.02 and 0.05 ± 0.02, respectively. These concentrations and those obtained without coprecipitation technique were significantly different. Coprecipitation procedure using 8-HQ as ligand and Cu(II) as carrier element enhanced the preconcentration and separation of metal ions from the matrix of water sample.
Synthesis of high capacity cathodes for lithium-ion batteries by morphology-tailored hydroxide co-precipitation

NASA Astrophysics Data System (ADS)

Wang, Dapeng; Belharouak, Ilias; Ortega, Luis H.; Zhang, Xiaofeng; Xu, Rui; Zhou, Dehua; Zhou, Guangwen; Amine, Khalil

2015-01-01

Nickel manganese hydroxide co-precipitation inside a continuous stirred tank reactor was studied with sodium hydroxide and ammonium hydroxide as the precipitation agents. The ammonium hydroxide concentration had an effect on the primary and secondary particle evolution. The two-step precipitation mechanism proposed earlier was experimentally confirmed. In cell tests, Li- and Mn-rich composite cathode materials based on the hydroxide precursors demonstrated good electrochemical performance in terms of cycle life over a wide range of lithium content.
CESIUM RECOVERY FROM AQUEOUS SOLUTIONS

DOEpatents

Schneider, R.A.

1961-06-20

Cesium may be precipitated from an aqueous solution whose acidity ranges between a pH of 1.5 and a molarity of 5 on cobaltous, zinc, cadmium, nickel, or ferrous cobalticyanide. This precipitation brings about a separation from most fission products. Ruthenium which coprecipitates to a great degree can be removed by dissolving in sulfuric acid and boiling the solution in the presence of periodic acid for volatilization; other coprecipitated fission products can then be precipitated from the sulfuric acid solution with a ferric hydroxide carrier.
[Entrapment of herbal extracts in biodegradable microcapsules].

PubMed

Borodina, T N; Rumsh, L D; Kunizhev, S M; Sukhorukov, G B; Vorozhtsov, G N; Fel'dman, B M; Rusanova, A V; Vasil'eva, T V; Strukova, S M; Markvicheva, E A

2007-01-01

The microcapsules with entrapped herbal water-soluble extracts Plantago major and Calendula officinalis L. (HE) were prepared by LbL-adsorption of carrageenan and modificated chitosan onto CaCO3 microparticles with their subsequent dissolving after the treatment of EDTA. Entrapment of HE was performed by adsorption and co-precipitation techniques. The co-precipitation provided better entrapment of HE compared to adsorption. In vitro release kinetics in an artificial gastric juice (AGJ) was studied. The HE release was shown to accelerate gastric ulcer treatment in a rat model.
Method for rapid screening analysis of Sr-90 in edible plant samples collected near Fukushima, Japan.

PubMed

Amano, Hikaru; Sakamoto, Hideaki; Shiga, Norikatsu; Suzuki, Kaori

2016-06-01

A screening method for measuring (90)Sr in edible plant samples by focusing on (90)Y in equilibrium with (90)Sr is reported. (90)Y was extracted from samples with acid, co-precipitated with iron hydroxide, and precipitated with oxalic acid. The dissolved oxalate precipitate was loaded on an extraction chromatography resin, and the (90)Y-enriched eluate was analyzed by Cherenkov counting with a TDCR liquid scintillation counter. (90)Sr ((90)Y) concentration was determined in plant samples collected near the damaged Fukushima Daiichi Nuclear Power Plants with this method. Copyright © 2016 Elsevier Ltd. All rights reserved.
Improvements in electrical and dielectric properties of substituted multiferroic LaMnO{sub 3} based nanostructures synthesized by co-precipitation method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mahmood, Azhar; Warsi, Muhammad Farooq, E-mail: Farooq.warsi@iub.edu.pk; Ashiq, Muhammad Naeem

2012-12-15

Graphical abstract: Display Omitted Highlights: ► Simultaneous double ion substitutions philosophy is introduced in LaMnO{sub 3}. ► La{sub 1−x}Gd{sub x}Mn{sub 1−y}Cr{sub y}O{sub 3} nanoparticles are not reported previously. ► La{sub 1−x}Gd{sub x}Mn{sub 1−y}Cr{sub y}O{sub 3} nanoparticles are synthesized by co-precipitation method. ► The 12 fold increase in resistivity of LaMnO{sub 3} nanostructures is observed. -- Abstract: A series of La{sub 1−x}Gd{sub x}Mn{sub 1−y}Cr{sub y}O{sub 3} nanoparticles (where x, y = 0, 0.25, 0.50, 0.75 and 1.0) has been synthesized by the chemical co-precipitation method, involving double ion substitution philosophy. The nanoparticles were characterized by thermo gravimetric analysis (TGA), X-ray fluorescencemore » spectrometry (XRF), X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, vibrating sample magnetometer (VSM), DC electrical resistivity and dielectric measurements. The XRD and FTIR analysis confirmed the single orthorhombic phase and the crystallite size were found in the range of 16–34 nm. DC resistivity exhibited very interesting behavior which increased from 1.41 × 10{sup 8} to 16.35 ± 0.2 × 10{sup 8} Ω cm upon complete double ions replacement of La and Mn with Gd and Cr, respectively. This very high resistivity variation upon substitution definitely would open new avenues for applications of these materials in microwave devices and other related areas. The dielectric properties of these nanoparticles were also studied at room temperature in the range of 6 kHz to 5 MHz and the maximum dielectric behavior (ε′ = 2.86 × 10{sup 3}, tan δ = 5.41, ε″ = 15.5 × 10{sup 3}) was exhibited by La{sub 0.75}Gd{sub 0.25}Mn{sub 0.75}Cr{sub 0.25}O{sub 3} at 6 kHz. Hysteresis loops measurements showed that the synthesized nanomaterials are paramagnetic in nature at room temperature.« less
Trace Metals in Groundwater and Vadose Zone Calcite: In Situ Containment and Stabilization of Stronthium-90 and Other Divalent Metals and Radionuclides at Arid Western DOE Sites: Final Report for Award Number DE-FG07-02ER63486 to the University of Idaho (RW Smith) Environmental Management Science Program Project Number 87016

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, Robert W.; Fujita, Yoshiko

2007-11-07

Radionuclide and metal contaminants are present in the vadose zone and groundwater throughout the U.S. Department of Energy (DOE) energy research and weapons complex. In situ containment and stabilization of these contaminants represents a cost-effective treatment strategy that minimizes workers’ exposure to hazardous substances, does not require removal or transport of contaminants, and generally does not generate a secondary waste stream. We have investigated an in situ bioremediation approach that immobilizes radionuclides or contaminant metals (e.g., strontium-90) by their microbially facilitated co-precipitation with calcium carbonate in groundwater and vadose zone systems. Calcite, a common mineral in many aquifers and vadosemore » zones in the arid west, can incorporate divalent metals such as strontium, cadmium, lead, and cobalt into its crystal structure by the formation of a solid solution. Collaborative research undertaken by the Idaho National Laboratory (INL), University of Idaho, and University of Toronto as part of this Environmental Management Science Program project has focused on in situ microbially-catalyzed urea hydrolysis, which results in an increase in pH, carbonate alkalinity, ammonium, calcite precipitation, and co-precipitation of divalent cations. In calcite-saturated aquifers, microbially facilitated co-precipitation with calcium carbonate represents a potential long-term contaminant sequestration mechanism. Key results of the project include: **Demonstrating the linkage between urea hydrolysis and calcite precipitation in field and laboratory experiments **Observing strontium incorporation into calcite precipitate by urea hydrolyzers with higher distribution coefficient than in abiotic **Developing and applying molecular methods for characterizing microbial urease activity in groundwater including a quantitative PCR method for enumerating ureolytic bacteria **Applying the suite of developed molecular methods to assess the feasibility of the proposed bioremediation technique at a contaminated site located within the 100-N area of the Hanford, Washington site **Assessing the role of nitrification on the persistence of precipitated calcite by modifying primers for identification of the amoA gene region of various ammonia oxidizing bacteria (AOB) for characterizing AOB in the field« less
Synthesis, characterization and magnetic property of maghemite (γ-Fe{sub 2}O{sub 3}) nanoparticles and their protective coating with pepsin for bio-functionalization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bandhu, A.; Sutradhar, S.; Mukherjee, S.

Highlights: • Maghemite nanoparticles were prepared by a modified co-precipitation method. • Nanoparticles were then successfully coated with pepsin for bio-functionlization. • XRD and Mössbauer spectra confirmed the maghemite phase of the nanoparticles. • Magnetic data were analysed to evaluate particle size, anisotropy etc. - Abstract: Maghemite nanoparticles (γ-Fe{sub 2}O{sub 3}) are prepared by co-precipitation method. To obtain bio-functionalized magnetic nanoparticles for magnetically controlled drug delivery, the prepared nanoparticles are successfully coated with pepsin, a bio-compatible polymer and digestive enzyme. Crystallographic phase of the nanoparticles is confirmed by X-ray diffractograms (XRD), high resolution transmission electron microscopy (HRTEM) and {sup 57}Femore » Mössbauer spectrometry. The average size of nanoparticles/nanocrystallites is estimated from the (3 1 1) peak of the XRD pattern using Debye–Scherrer formula. Results of HRTEM of coated and bare samples are in good agreement with those extracted from the XRD analysis. The dynamic magnetic properties are observed and different quantities viz., coercive field, magnetization, remanence, hysteresis losses etc., are estimated, which confirmed the presence of superparamagnetic relaxation of nanoparticles. Mössbauer spectra of the samples recorded at both 300 and 77 K, confirmed that the majority of particles are maghemite together with a very small fraction of magnetite nanoparticles.« less

Effects of Gd-Substitutions on the Microstructure, Electrical and Electromagnetic Behavior of M-Type Hexagonal Ferrites

NASA Astrophysics Data System (ADS)

Ahmad, Ishtiaq; Ahmad, Mahmood; Ali, Ihsan; Kanwal, M.; Awan, M. S.; Mustafa, Ghulam; Ahmad, Mukhtar

2015-07-01

A series of Gd-substituted Ba-Co-based (M-type) hexaferrites having the chemical compositions of Ba0.5Co0.5Gd x Fe12- x O19 ( x = 0.0, 0.2, 0.4, 0.6, 0.8, 1.0) were prepared by co-precipitation method. The pellets formed by co-precipitated powder were calcined at a temperature of 1200°C for 20 h. Final sintering was done at 1320°C for 4 h. From the x-ray diffraction analysis, it was revealed that all the samples showed M-type hexagonal structure as a major phase. The scanning electron microscope was used to examine the morphology of the sintered ferrites. The average grain size estimated by the line intercept method was found to be in the range of 2.8-1.0 μm. The room temperature DC resistivity increases with increasing Gd-contents to make these ferrites useful for high frequency applications and microwave devices. Lower values of coercivity ( H c) and higher saturation magnetization ( M s) may be suitable to enhance the permeability of these ferrites, which is favorable for impedance matching in microwave absorption. In addition, reflection coefficients for a sample was also measured from a frequency of 1 MHz to 3 GHz and a reflection peak was observed at about 2.2 GHz.
Semimicrodetermination of tantalum with selenous acid

USGS Publications Warehouse

Grimaldi, F.S.; Schnepfe, M.M.

1958-01-01

Tantalum is separated and determined gravimetrically by precipitation with selenous acid from a highly acidic solution containing oxalic and tartaric acids. The method is selective for the determination of up to 30 mg. of tantalum pentoxide, and tolerates relatively large amounts of scandium, yttrium, cerium, titanium, zirconium, thorium, vanadium, niobium, molybdenum, tungsten, uranium, iron, aluminum, gallium, tin, lead, antimony, and bismuth. The separation of tantalum from niobium and titanium is not strictly quantitative, and correction is made colorimetrically for the small amounts of niobium and titanium co-precipitating with the tantalum. The method was applied to the determination of tantalum in tantaloniobate ores.
Synthesis and characterization of graphene quantum dots/cobalt ferrite nanocomposite

NASA Astrophysics Data System (ADS)

Ramachandran, Shilpa; Sathishkumar, M.; Kothurkar, Nikhil K.; Senthilkumar, R.

2018-02-01

A facile method has been developed for the synthesis of a graphene quantum dots/cobalt ferrite nanocomposite. Graphene quantum dots (GQDs) were synthesized by a simple bottom-up method using citric acid, followed by the co-precipitation of cobalt ferrite nanoparticles on the graphene quantum dots. The morphology, structural analysis, optical properties, magnetic properties were investigated using transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), UV-vis absorption spectroscopy, fluorescence spectroscopy, vibrating sample magnetometry (VSM) measurements. The synthesized nanocomposite showed good fluorescence and superparamagnetic properties, which are important for biomedical applications.
Ceramic Technology for Advanced Heat Engines Project Semiannual Progress Report for Period October 1985 Through March 1986

DTIC Science & Technology

1986-08-01

materials (2.2 w/o and 3.0 w/o MgO). The other two batches (2.8 w/o and 3.1 w/o MgO), of higher purity, were made using E-10 zirconia powder from...CID) powders Two methods have been used for the coprecipitation of doped zirconia powders from solutions of chemical precursors. (4) Method I, for...of powder, approximate sample size 3.2 Kg (6.4 Kg for zirconia powder ); 342 3. Random selection of sample; 4. Partial drying of sample to reduce caking
Optimization principles for preparation methods and properties of fine ferrite materials

NASA Astrophysics Data System (ADS)

Borisova, N. M.; Golubenko, Z. V.; Kuz'micheva, T. G.; Ol'khovik, L. P.; Shabatin, V. P.

1992-08-01

The paper is devoted to the problems of development of fine materials based on Ba-ferrite for vertical magnetic recording in particular. Taking an analogue — BaFe 12-2 xCo xTe xO 19 — we have optimized the melt co-precipitation method and shown a new opportunity to provide chemical homogeneity of microcrystallites by means of cryotechnology. Magnetic characteristics of the magnetic tape experimental sample for digital video recording are presented. A series of principles of consistent control of ferrite powder properties are formulated and illustrated with specific developments.
Mercury (II) reduction and co-precipitation of metallic mercury on hydrous ferric oxide in contaminated groundwater.

PubMed

Richard, Jan-Helge; Bischoff, Cornelia; Ahrens, Christian G M; Biester, Harald

2016-01-01

Mercury (Hg) speciation and sorption analyses in contaminated aquifers are useful for understanding transformation, retention, and mobility of Hg in groundwater. In most aquifers hydrous ferric oxides (HFOs) are among the most important sorbents for trace metals; however, their role in sorption or mobilization of Hg in aquifers has been rarely analyzed. In this study, we investigated Hg chemistry and Hg sorption to HFO under changing redox conditions in a highly HgCl2-contaminated aquifer (up to 870μgL(-1) Hg). Results from aqueous and solid phase Hg measurements were compared to modeled (PHREEQC) data. Speciation analyses of dissolved mercury indicated that Hg(II) forms were reduced to Hg(0) under anoxic conditions, and adsorbed to or co-precipitated with HFO. Solid phase Hg thermo-desorption measurements revealed that between 55 and 93% of Hg bound to HFO was elemental Hg (Hg(0)). Hg concentrations in precipitates reached more than 4 weight %, up to 7000 times higher than predicted by geochemical models that do not consider unspecific sorption to and co-precipitation of elemental Hg with HFO. The observed process of Hg(II) reduction and Hg(0) formation, and its retention and co-precipitation by HFO is thought to be crucial in HgCl2-contaminated aquifers with variable redox-conditions regarding the related decrease in Hg solubility (factor of ~10(6)), and retention of Hg in the aquifer. Copyright © 2015 Elsevier B.V. All rights reserved.
Quality-by-Design (QbD): An integrated process analytical technology (PAT) approach for a dynamic pharmaceutical co-precipitation process characterization and process design space development.

PubMed

Wu, Huiquan; White, Maury; Khan, Mansoor A

2011-02-28

The aim of this work was to develop an integrated process analytical technology (PAT) approach for a dynamic pharmaceutical co-precipitation process characterization and design space development. A dynamic co-precipitation process by gradually introducing water to the ternary system of naproxen-Eudragit L100-alcohol was monitored at real-time in situ via Lasentec FBRM and PVM. 3D map of count-time-chord length revealed three distinguishable process stages: incubation, transition, and steady-state. The effects of high risk process variables (slurry temperature, stirring rate, and water addition rate) on both derived co-precipitation process rates and final chord-length-distribution were evaluated systematically using a 3(3) full factorial design. Critical process variables were identified via ANOVA for both transition and steady state. General linear models (GLM) were then used for parameter estimation for each critical variable. Clear trends about effects of each critical variable during transition and steady state were found by GLM and were interpreted using fundamental process principles and Nyvlt's transfer model. Neural network models were able to link process variables with response variables at transition and steady state with R(2) of 0.88-0.98. PVM images evidenced nucleation and crystal growth. Contour plots illustrated design space via critical process variables' ranges. It demonstrated the utility of integrated PAT approach for QbD development. Published by Elsevier B.V.
Structural stability of coprecipitated natural organic matter and ferric iron under reducing conditions

USGS Publications Warehouse

Henneberry, Yumiko K.; Kraus, Tamara E.C.; Nico, Peter S.; Horwath, William R.

2012-01-01

The objective was to assess the interaction of Fe coprecipitated with dissolved organic matter (DOM) and its effect on Fe (hydr)oxide crystallinity and DOM retention under abiotic reducing conditions. A Fe-based coagulant was reacted with DOM from an agricultural drain and the resulting precipitate (floc) was exposed to S(-II) and Fe(II). Solution concentrations of Fe(II/III) and DOM were monitored, floc crystallinity was determined using X-ray diffraction, and the composition and distribution of functional groups were assessed using scanning transmission X-ray microscopy (STXM) and near edge X-ray absorption fine structure (NEXAFS) spectroscopy. Results indicate coprecipitation of Fe(III) with DOM forms a non-crystalline floc that withstands crystallization regardless of change in pH, Fe:DOM ratio and type of reductant added. There was no evidence that exposure to reducing conditions led to release of DOM from the floc, indicating that coprecipitation with complex natural DOM in aquatic environments may stabilize Fe (hydr)oxides against crystallization upon reaction with reduced species and lead to long term sequestration of the DOM. STXM analysis identified spatially distinct regions with remarkable functional group purity, contrary to the model of DOM as a relatively uniform complex polymer lacking identifiable organic compounds. Polysaccharide-like OM was strongly and directly correlated with the presence of Fe but showed different Fe binding strength depending on the presence of carboxylic acid functional groups, whereas amide and aromatic functional groups were inversely correlated with Fe content.
Sorption and coprecipitation of trace concentrations of thorium with various minerals under conditions simulating an acid uranium mill effluent environment

USGS Publications Warehouse

Landa, Edward R.; Le, Anh H.; Luck, Rudy L.; Yeich, Philip J.

1995-01-01

Sorption of thorium by pre-existing crystals of anglesite (PbSO4), apatite (Ca5(PO4)3(HO)), barite (BaSO4), bentonite (Na0.7Al3.3Mg0.7Si8O20(OH)4), celestite (SrSO4), fluorite (CaF2), galena (PbS), gypsum (CaSO4·2H2O), hematite (Fe2O3), jarosite (KFe3(SO4)2(OH)6), kaolinite (Al2O3·2SiO2·2H2O), quartz (SiO2) and sodium feldspar (NaAlSi3O8) was studied under conditions that simulate an acidic uranium mill effluent environment. Up to 100% removal of trace quantitiees of thorim (approx. 1.00 ppm in 0.01 N H2SO4) from solution occurred within 3 h with fluorite and within 48 h in the case of bentonite. Quartz, jarosite, hematite, sodium feldspar, gypsum and galena removed less than 15% of the thorium from solution. In the coprecipitation studies, barite, anglesite, gypsum and celestite were formed in the presence of thorium (approx. 1.00 ppm). Approximately all of the thorium present in solution coprecipitated with barite and celestite; 95% coprecipitated with anglesite and less than 5% with gypsum under similar conditions. When jarosite was precipitated in the presence of thorium, a significant amount of thorium (78%) was incorporated in the precipitate.
Enabling Large Superalloy Parts Using Compact Coprecipitation of γ' and γ''

NASA Astrophysics Data System (ADS)

Detor, Andrew J.; DiDomizio, Richard; Sharghi-Moshtaghin, Reza; Zhou, Ning; Shi, Rongpei; Wang, Yunzhi; McAllister, Donald P.; Mills, Michael J.

2018-03-01

Next-generation gas turbines will require disk materials capable of operating at 923 K (650 °C) and above to achieve efficiencies well beyond today's 62 pct benchmark. This temperature requirement marks a critical turning point in materials selection. Current turbine disk alloys, such as 706 and 718, are limited by the stability of their major strengthening phase, γ'', which coarsens rapidly beyond 923 K (650 °C) resulting in significant degradation in properties. More capable γ' strengthened superalloys, such as those used in jet engine disks, are also limited due to the sheer size of gas turbine hardware; the γ' phase overages during the slow cooling rates inherent in processing thick-section parts. In the present work, we address this fundamental gap in available superalloy materials. Through careful control of Al, Ti, and Nb levels, we show that fine (<100 nm) γ' and compact γ'/γ'' coprecipitate structures can be formed even under extremely slow cooling rates from high temperature. The presence of Ti is shown to have a dominant effect on phase formation, dictating whether γ', γ'/γ'' coprecipitates, or other less desirable acicular phases form on cooling. Sensitivity to cooling rate and aging heat treatment is also explored. A custom phase field model along with commercial precipitation kinetics software is used to better understand the phase evolution and stability of compact coprecipitates. The alloying strategies discussed here enable a new class of superalloys suitable for applications requiring large parts operating at high temperature.
Macroscopic and microscopic investigation of Ni(II) sequestration on diatomite by batch, XPS, and EXAFS techniques.

PubMed

Sheng, Guodong; Yang, Shitong; Sheng, Jiang; Hu, Jun; Tan, Xiaoli; Wang, Xiangke

2011-09-15

Sequestration of Ni(II) on diatomite as a function of time, pH, and temperature was investigated by batch, XPS, and EXAFS techniques. The ionic strength-dependent sorption at pH < 7.0 was consistent with outer-sphere surface complexation, while the ionic strength-independent sorption at pH = 7.0-8.6 was indicative of inner-sphere surface complexation. EXAFS results indicated that the adsorbed Ni(II) consisted of ∼6 O at R(Ni-O) ≈ 2.05 Å. EXAFS analysis from the second shell suggested that three phenomena occurred at the diatomite/water interface: (1) outer-sphere and/or inner-sphere complexation; (2) dissolution of Si which is the rate limiting step during Ni uptake; and (3) extensive growth of surface (co)precipitates. Under acidic conditions, outer-sphere complexation is the main mechanism controlling Ni uptake, which is in good agreement with the macroscopic results. At contact time of 1 h or 1 day or pH = 7.0-8.0, surface coprecipitates occur concurrently with inner-sphere complexes on diatomite surface, whereas at contact time of 1 month or pH = 10.0, surface (co)precipitates dominate Ni uptake. Furthermore, surface loading increases with temperature increasing, and surface coprecipitates become the dominant mechanism at elevated temperature. The results are important to understand Ni interaction with minerals at the solid-water interface, which is helpful to evaluate the mobility of Ni(II) in the natural environment.
Simultaneous immobilization of borate, arsenate, and silicate from geothermal water derived from mining activity by co-precipitation with hydroxyapatite.

PubMed

Sasaki, Keiko; Hayashi, Yoshikazu; Toshiyuki, Kenta; Guo, Binglin

2018-09-01

The treatment of the geothermal water discharged through mining activity is a critical issue because the rate of discharge is 12,000 m 3 per day and the discharge contains high concentrations of borate (>20 mg/L) and arsenate (ca. 0.4 mg/L) as well as silicate and carbonate. The simultaneous reduction of borate and arsenate concentrations to acceptable levels was successfully performed by co-precipitation with hydroxyapatite (HAp). Although the coexisting high concentrations of carbonate act as a disturbing element, the co-precipitation equilibrium of borate was shifted to lower values by adjusting the P/Ca molar ratio, and the removal rate of borate was accelerated by using Al 3+ additives, resulting in the efficient reduction of borate within 1 h. The initially immobilized boron in HAp is in the tetragonal form, which probably occupies the hydroxyl sites in HAp, gradually transforming into the trigonal form in the solid state, as interpreted by 1 H NMR and 11 B-NMR. The coexisting silicate was also immobilized in an ellestadite form, as confirmed by 29 Si-NMR measurements. Arsenate and silicate were immobilized before borate in geothermal water. A dissolution assay of borate in the solid residues after co-precipitation with HAp verified the acceptable stability of borate, which is independent of the amount of added Al 3+ . Copyright © 2018 Elsevier Ltd. All rights reserved.
Synthesis of strontium hexaferrite nanoparticles prepared using co-precipitation method and microemulsion processing

NASA Astrophysics Data System (ADS)

Drmota, A.; Žnidaršič, A.; Košak, A.

2010-01-01

Strontium hexaferrite (SrFe12O19) nanoparticles have been prepared with co-precipitation in aqueous solutions and precipitation in microemulsion system water/SDS/n-butanol/cyclohexane, using iron and strontium nitrates in different molar rations as a starting materials. The mixed Sr2+, Fe3+ hydroxide precursors obtained during the reaction between corresponding metal nitrates and tetramethylammonium hydroxide (TMAH), which served as a precipitating reagent, were calcined in a wide temperature range, from 350 °C to 1000 °C in a static air atmosphere. The influence of the Sr2+/Fe3+ molar ratio and the calcination temperature to the chemistry of the product formation, its crystallite size, morphology and magnetic properties were investigated. It was found that the formation of single phase SrFe12O19 with relatively high specific magnetization (54 Am2/kg) was achieved at the Sr2+/Fe3+ molar ration of 6.4 and calcination at 800 °C for 3h with heating/cooling rate 5 °C/min. The prepared powders were characterized using X-ray diffractometry (XRD) and specific surface area measurements (BET). The specific magnetization (DSM-10, magneto-susceptometer) of the prepared samples was measured.
Curcumin-β-cyclodextrin inclusion complex: stability, solubility, characterisation by FT-IR, FT-Raman, X-ray diffraction and photoacoustic spectroscopy, and food application.

PubMed

Mangolim, Camila Sampaio; Moriwaki, Cristiane; Nogueira, Ana Claudia; Sato, Francielle; Baesso, Mauro Luciano; Neto, Antônio Medina; Matioli, Graciette

2014-06-15

Curcumin was complexed with β-CD using co-precipitation, freeze-drying and solvent evaporation methods. Co-precipitation enabled complex formation, as indicated by the FT-IR and FT-Raman techniques via the shifts in the peaks that were assigned to the aromatic rings of curcumin. In addition, photoacoustic spectroscopy and X-ray diffraction, with the disappearance of the band related to aromatic rings, by Gaussian fitting, and modifications in the spectral lines, respectively, also suggested complex formation. The possible complexation had an efficiency of 74% and increased the solubility of the pure colourant 31-fold. Curcumin-β-CD complex exhibited a sunlight stability 18% higher than the pure colourant. This material was stable to pH variations and storage at -15 and 4°C. With an isothermal heating at 100 and 150°C for 2h, the material exhibited a colour retention of approximately 99%. The application of curcumin-β-CD complex in vanilla ice creams intensified the colour of the products and produced a great sensorial acceptance. Copyright © 2013 Elsevier Ltd. All rights reserved.
Nano cube of CaSnO3: Facile and green co-precipitation synthesis, characterization and photocatalytic degradation of dye

NASA Astrophysics Data System (ADS)

Moshtaghi, Saeed; Gholamrezaei, Sousan; Salavati Niasari, Masoud

2017-04-01

In this work, nanocubes of CaSnO3 have been prepared by a simple and green co-precipitation method. In this technique, for preparation of calcium stannate, we have used from a complex structure of calcium as a new precursor and the synthesis of CaSnO3 have been done in water as a green solvent. Using of complexing precursors were created a congestion in reaction medium. Different conditions have been studied in synthetic approaches and optimized the effect of different parameters on the morphology of product such as precipitation agent (alkaline), pH, temperature, the rate of stirrer, surfactants and the mole ratio of surfactants for preparation product and obtain the best product in terms of quality and morphology. By using of this CaSnO3, two types of azo dyes (acid blue 92 and acid brown 14) have been degraded at presence of ultraviolet light from aqueous solution. Results display that the powder shows appropriate catalytic behavior for degradation of dyes (77% acid brown 14 and 67% acid black 92). Therefore these nano-cube structures have been used as photocatalysts in presence of UV light for degradation of azo dyes.
Effects of Precipitant and pH on Coprecipitation of Nanosized Co-Cr-V Alloy Powders.

PubMed

Chen, Xiaoyu; Li, Yongxia; Huang, Lan; Zou, Dan; Wu, Enxi; Liu, Yanjun; Xie, Yuanyan; Yao, Rui; Liao, Songyi; Wang, Guangrong; Zheng, Feng

2017-09-21

Nanosized Co-Cr-V alloy powders were synthesized via coprecipitation method. Effects of precipitants ((NH₄)₂C₂O₄·H₂O and Na₂CO₃) and pH were investigated by X-ray diffraction (XRD), Zeta potential analyzer, thermogravimetry-differential scanning calorimetry (TG-DSC), inductively coupled plasma-atomic emission spectrometry (ICP-AES) and scanning electron microscopy (SEM). Co-Cr-V alloy powders were consisted of major face-centered cubic Co (fcc Co) and minor hexagonal close-packed Co (hcp Co). Grain sizes of precursors and Co-Cr-V alloy powders were increased with pH value (7-10) within the ranges of 3~39 and 39~66 nm, respectively. Rod-like or granular Co-Cr-V alloy particles were assembled by interconnected nanograins. At pH = 7, Na₂CO₃ precipitant was found to be beneficial to maintain the desirable composition of Co-Cr-V powders. It was also found that lower pH favors the maintenance of pre-designed composition, while grain coarsens at higher pH. Effects of variation for precipitant and pH on the morphology and composition of Co-Cr-V alloy powder were discussed in detail and relevant mechanism was further proposed.
Fabrication of Tb3Al5O12 transparent ceramics using co-precipitated nanopowders

NASA Astrophysics Data System (ADS)

Dai, Jiawei; Pan, Yubai; Wang, Wei; Luo, Wei; Xie, Tengfei; Kou, Huamin; Li, Jiang

2017-11-01

Terbium aluminum garnet (TAG) precursor was synthesized by a co-precipitation method from a mixed solution of terbium and aluminum nitrates using ammonium hydrogen carbonate (AHC) as the precipitant. The powders calcined at different temperatures were investigated by XRD, FTIR and FESEM in order to choose the optimal calcination temperature. Fine and low-agglomerated TAG powders with average particle size of 88 nm were obtained by calcining the precursor at 1100 °C for 4 h. Using this powder as starting material, TAG transparent ceramics were fabricated by vacuum sintering combined with hot isostatic pressing (HIP) sintering. For the sample pre-sintered at 1700 °C for 20 h with HIP post-treated at 1700 °C for 3 h, the average grain size is about 3.9 μm and the in-line transmittance is beyond 55% in the region of 500-1600 nm, reaching a maximum transmittance of 64.2% at the wavelength of 1450 nm. The Verdet constant at 633 nm is measured to be -178.9 rad T-1 m-1, which is 33% larger than that of the commercial TGG single crystal (-134 rad T-1 m-1).
Synthesis of mesoporous TiO(2-x)N(x) spheres by template free homogeneous co-precipitation method and their photo-catalytic activity under visible light illumination.

PubMed

Parida, K M; Naik, Brundabana

2009-05-01

The article presents preparation, characterization and catalytic activity evaluation of an efficient nitrogen doped mesoporous titania sphere photo-catalyst for degradation of methylene blue (MB) and methyl orange (MO) under visible light illumination. Nitrogen doped titania was prepared by soft chemical route i.e. template free, slow and controlled homogeneous co-precipitation from titanium oxysulfate sulfuric acid complex hydrate, urea, ethanol and water. The molar composition of TiOSO(4) to urea was varied to prepare different atomic % nitrogen doped titania. Mesoporous anatase TiO(2-x)N(x) spheres with average crystallite size of 10 nm and formation of titanium oxynitride center were confirmed from HRTEM, XRD and XPS study. UV-vis DRS showed a strong absorption in the range of 400-500 nm which supports its use in visible spectrum of light. Nitrogen adsorption-desorption study supports the porous nature of the doped material. All the TiO(2-x)N(x) samples showed higher photo-catalytic activity than Degussa P(25) and undoped mesoporous titania. Sample containing around one atomic % nitrogen showed highest activity among the TiO(2-x)N(x) samples.
Composition and process for organic and metal contaminant fixation in soil

DOEpatents

Schwitzgebel, Klaus

1994-02-08

A method and compositions using a first ferrous iron containing solution with the iron concentration in excess of theoretical requirements to treat a contaminated site to reduce hexavalent chromium to trivalent chromium and coprecipitate trivalent chromium with other heavy metals and using a second solution of silicate containing a destabilizing salt to form a relatively impermeable gel in the contaminated site thereby fixing metals and organics to the extent that there should be no detectable ground water contamination.
Size dependence of magnetorheological properties of cobalt ferrite ferrofluid

DOE Office of Scientific and Technical Information (OSTI.GOV)

Radhika, B.; Sahoo, Rasmita; Srinath, S., E-mail: srinath@uohyd.ac.in

2015-06-24

Cobalt Ferrite nanoparticles were synthesized using co-precipitation method at reaction temperatures of 40°C and 80°C. X-Ray diffraction studies confirm cubic phase formation. The average crystallite sizes were found to be ∼30nm and ∼48nm for 40°C sample and 80°C sample respectively. Magnetic properties measured using vibrating sample magnetometer show higher coercivety and magnetization for sample prepared at 80°C. Magnetorheological properties of CoFe2O4 ferrofluids were measured and studied.

Coprecipitation of arsenate with metal oxides. 3. Nature, mineralogy, and reactivity of iron(III)-aluminum precipitates.

PubMed

Violante, Antonio; Pigna, Massimo; Del Gaudio, Stefania; Cozzolino, Vincenza; Banerjee, Dipanjan

2009-03-01

Coprecipitation involving arsenic with aluminum or iron has been studied because this technique is considered particularly efficient for removal of this toxic element from polluted waters. Coprecipitation of arsenic with mixed iron-aluminum solutions has received scant attention. In this work we studied (i)the mineralogy, surface properties, and chemical composition of mixed iron-aluminum oxides formed at initial Fe/Al molar ratio of 1.0 in the absence or presence of arsenate [As/ Fe+Al molar ratio (R) of 0, 0.01, or 0.1] and at pH 4.0, 7.0, and 10.0 and aged for 30 and 210 days at 50 degrees C and (ii) the removal of arsenate from the coprecipitates after addition of phosphate. The amounts of short-range ordered precipitates (ferrihydrite, aluminous ferrihydrite and/or poorly crystalline boehmite) were greater than those found in iron and aluminum systems (studied in previous works), due to the capacity of both aluminum and arsenate to retard or inhibitthe transformation of the initially formed precipitates into well-crystallized oxides (gibbsite, bayerite, and hematite). As a consequence, the surface areas of the iron-aluminum oxides formed in the absence or presence of arsenate were usually much larger than those of aluminum or iron oxides formed under the same conditions. Arsenate was found to be associated mainly into short-range ordered materials. Chemical composition of all samples was affected by pH, initial R, and aging. Phosphate sorption was facilitated by the presence of short-range ordered materials, mainly those richer in aluminum, but was inhibited by arsenate present in the samples. The quantities of arsenate replaced by phosphate, expressed as percentages of its total amount present in the samples, were particularly low, ranging from 10% to 26%. A comparison of the desorption of arsenate by phosphate from aluminum-arsenate and iron-arsenate (studied in previous works) and iron-aluminum-arsenate coprecipitates evidenced that phosphate has a greater capacity to desorb arsenate from aluminum than iron sites.
Evaluation of alternatives for best available technology treatment and retreatment of uranium-contaminated solutions at the Paducah Gaseous Diffusion Plant C-400 Facility

DOE Office of Scientific and Technical Information (OSTI.GOV)

Del Cul, G.D.

1991-02-01

The Paducah Gaseous Diffusion Plant C-400 Decontamination Facility generators aqueous solutions that originate in drum washing, machine parts and equipment cleaning, and other decontamination processes. In general, the waste contains uranyl, fluoride, carbonate, and nitrate ions, in addition to soaps, detergents, secondary contaminants, and particulate matter. The main contaminants are fluoride, technetium, uranium, and other heavy metals. In accordance with Department of Energy (DOE) Order 5400.5, the releases of radioactive materials must be as low as reasonably achievable and be below the derived concentration guide limits. To comply with the DOE order, an action plan was formulated. The action planmore » included a literature search to support best available technology evaluation of treatment alternatives, a quality assurance/quality control plan, suggestion of alternative treatment options, bench-scale test studies of the proposed treatment alternatives, and establishment of the final recommendation. Five major technologies were considered: precipitation/coprecipitation, reverse osmosis, ultrafiltration, supported liquid membranes, and ion exchange. Biosorption was also briefly considered. Based on C-400's requirements and facilities, the precipitation/coprecipitation process appears to be the best suited for use at the plant. Four different treatment options using the precipitation/coprecipitation technology were proposed. Bench-scale studies of all four options were suggested. Options 1 and 2 represent a combination of lime-softening and iron coprecipitation. Laboratory test evaluations were initiated and the results involving Options 1 and 2 reported here. 29 refs., 1 fig., 2 tabs.« less
Trace Metals in Groundwater & the Vadose Zone Calcite: In Situ Containment & Stabilization of Strontium-90 & Other Divalent Metals & Radionuclides at Arid West DOE

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, Robert W.

2004-12-01

Radionuclide and metal contaminants such as strontium-90 are present beneath U.S. Department of Energy (DOE) lands in both the groundwater (e.g., 100-N area at Hanford, WA) and vadose zone (e.g., Idaho Nuclear Technology and Engineering Center at the Idaho National Engineering and Environmental Laboratory). In situ containment and stabilization of these contaminants is a cost-effective treatment strategy. However, implementing in situ containment and stabilization approaches requires definition of the mechanisms that control contaminant sequestration. We are investigating the in situ immobilization of radionuclides or contaminant metals (e.g., strontium-90) by their facilitated co-precipitation with calcium carbonate in groundwater and vadose zonemore » systems. Our facilitated approach, shown schematically in Figure 1, relies upon the hydrolysis of introduced urea to cause the acceleration of calcium carbonate precipitation (and trace metal co-precipitation) by increasing pH and alkalinity. Subsurface urea hydrolysis is catalyzed by the urease enzyme, which may be either introduced with the urea or produced in situ by ubiquitous subsurface urea hydrolyzing microorganisms. Because the precipitation process tends to be irreversible and many western aquifers are saturated with respect to calcite, the co-precipitated metals and radionuclides will be effectively removed from the aqueous phase over the long-term. Another advantage of the ureolysis approach is that the ammonium ions produced by the reaction can exchange with radionuclides sorbed to subsurface minerals, thereby enhancing the availability of the radionuclides for re-capture in a more stable solid phase (co-precipitation rather than adsorption).« less
Laboratory study on coprecipitation of phosphate with ikaite in sea ice

NASA Astrophysics Data System (ADS)

Hu, Yu-Bin; Dieckmann, Gerhard S.; Wolf-Gladrow, Dieter A.; Nehrke, Gernot

2014-10-01

Ikaite (CaCO3·6H2O) has recently been discovered in sea ice, providing first direct evidence of CaCO3 precipitation in sea ice. However, the impact of ikaite precipitation on phosphate (PO4) concentration has not been considered so far. Experiments were set up at pH from 8.5 to 10.0, salinities from 0 to 105, temperatures from -4°C to 0°C, and PO4 concentrations from 5 to 50 µmol kg-1 in artificial sea ice brine so as to understand how ikaite precipitation affects the PO4 concentration in sea ice under different conditions. Our results show that PO4 is coprecipitated with ikaite under all experimental conditions. The amount of PO4 removed by ikaite precipitation increases with increasing pH. Changes in salinity (S ≥ 35) as well as temperature have little impact on PO4 removal by ikaite precipitation. The initial PO4 concentration affects the PO4 coprecipitation. These findings may shed some light on the observed variability of PO4 concentration in sea ice.
Thermoluminescence of nanocrystalline CaSO{sub 4}: Dy for gamma dosimetry and calculation of trapping parameters using deconvolution method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mandlik, Nandkumar, E-mail: ntmandlik@gmail.com; Patil, B. J.; Bhoraskar, V. N.

2014-04-24

Nanorods of CaSO{sub 4}: Dy having diameter 20 nm and length 200 nm have been synthesized by the chemical coprecipitation method. These samples were irradiated with gamma radiation for the dose varying from 0.1 Gy to 50 kGy and their TL characteristics have been studied. TL dose response shows a linear behavior up to 5 kGy and further saturates with increase in the dose. A Computerized Glow Curve Deconvolution (CGCD) program was used for the analysis of TL glow curves. Trapping parameters for various peaks have been calculated by using CGCD program.
Comparative investigations on ferrite nanocomposites for magnetic hyperthermia applications

NASA Astrophysics Data System (ADS)

El-Dek, S. I.; Ali, Maha A.; El-Zanaty, Sara M.; Ahmed, Shehab E.

2018-07-01

Superparamagnetic iron oxide nanoparticles (SPION) Fe3O4 nanoparticles were prepared using different approaches: co-precipitation and sonochemical methods. This article is a comparative study on how different synthesis techniques greatly affect the magnetic properties and heating efficiency of such nanomaterial. Another important issue addressed here is the correlation between microstructure, colloidal stability, magnetization and specific absorption rate (SAR) of the nanoparticles. The results reveal that the sonochemical method for polyethylene glycol (PEGylated) Fe3O4 with size 5 nm leads to pseudo single domain with smallest loop area. Additionally, large SAR values are obtained within 10-15 min using low magnetic field.
Thermoluminescence of nanocrystalline CaSO4: Dy for gamma dosimetry and calculation of trapping parameters using deconvolution method

NASA Astrophysics Data System (ADS)

Mandlik, Nandkumar; Patil, B. J.; Bhoraskar, V. N.; Sahare, P. D.; Dhole, S. D.

2014-04-01

Nanorods of CaSO4: Dy having diameter 20 nm and length 200 nm have been synthesized by the chemical coprecipitation method. These samples were irradiated with gamma radiation for the dose varying from 0.1 Gy to 50 kGy and their TL characteristics have been studied. TL dose response shows a linear behavior up to 5 kGy and further saturates with increase in the dose. A Computerized Glow Curve Deconvolution (CGCD) program was used for the analysis of TL glow curves. Trapping parameters for various peaks have been calculated by using CGCD program.
Synthesis of amino-silane modified superparamagnetic Fe{sub 3}O{sub 4} nanoparticles and its application in immobilization of lipase from Pseudomonas fluorescens Lp1

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kanimozhi, S., E-mail: skanimo@gmail.com; Perinbam, K.

2013-05-15

Highlights: ► Magnetic nanoparticles were synthesized by chemical co-precipitation method. ► Surface was functionalized with amino-silane and used for lipase immobilization. ► Characterized through TEM, SEM, XRD, FT-IR and VSM analysis. ► The functionalization and immobilization did not affect the magnetite properties. ► The immobilized lipase showed greater functional property than free lipase. - Abstract: Superparamagnetic nanoparticles (Fe{sub 3}O{sub 4}–magnetite) were prepared by chemical co-precipitation method and their surface was functionalized with 3-aminopropyltriethoxysilane via silanization reaction to obtain amino functionalized magnetic nanoparticles. The purified lipase from Pseudomonas fluorescens Lp1 was immobilized onto functionalized magnetite using glutaraldehyde as the coupling agent.more » The characterization of the nanoparticles was done by scanning electron microscopy, transmission electron microscopy, powder X-ray diffraction, vibrating sample magnetometry and Fourier transformed infrared spectroscopy. The size of the magnetite was measured about 10–30 nm. The results of characterization study revealed the successful immobilization of lipase on to functionalized magnetite. The saturation magnetization of magnetic nanoparticles was found to be 28.34 emu/g whereas the immobilized magnetic nanoparticle was 17.074 emu/g. The immobilized lipase had greater activity at 50 °C and thermal stability upto 70 °C. It exhibited excellent reusability for 4 cycles and storage stability upto 15 days by retaining 75% of its initial activity.« less
Structural and luminescence properties of CaTiO{sub 3}:Eu{sup 3+} phosphor synthesized by chemical co-precipitation method for the application of solid state lighting devices

DOE Office of Scientific and Technical Information (OSTI.GOV)

Singh, Dhananjay Kumar, E-mail: dksism89@gmail.com; Manam, J., E-mail: jairam.manam@gmail.com

2016-05-06

The present work report a series of trivalent Europium (Eu{sup 3+}) doped well crystallized perovskite CaTiO{sub 3} phosphors successfully synthesized by chemical co-precipitation method. The crystal structure was confirmed by X-ray diffraction (XRD) which is in good agreement with pure orthorhombic phase with space group Pbnm, and it also indicated that the incorporation of the dopant did not affect the crystal structure. The impact of doping on the photoluminescence performances of the sample has been investigated by emission, excitation, and diffuse reflectance spectra at the room temperature. Photoluminescence spectra of Eu{sup 3+} doped CaTiO{sub 3} nanophosphor revealed the characteristic emissionmore » peak around wavelength 618 nm in the visible region upon the excitation of near-UV light at wavelength 397 nm due to {sup 5}D{sub 0} → {sup 7}F{sub 2} transition in Eu{sup 3+}. It was further proved that the dipole– dipole interactions results in the concentration quenching of Eu{sup 3+} in CaTiO{sub 3}:Eu{sup 3+} nanophosphors. The elemental composition of sample carried out by energy dispersive spectroscopy (EDS). EDS analysis reveals that the Eu{sup 3+} doped successfully into host CaTiO{sub 3}. The experimental result reveals that prepared nanophosphor can be used in the application of solid state lighting devices.« less
Microstructure, magnetic and microwave absorptive behavior of doped W-type hexaferrite nanoparticles prepared by co-precipitation method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gordani, Gholam Reza, E-mail: gordani@gmail.com; Mohseni, Marzieh; Ghasemi, Ali

2016-04-15

Highlights: • High frequency properties of substituted W-type Sr-hexaferrite. • Saturation magnetization of samples is decreased with increasing of dopants content. • The ferrite sample covers about 6 GHz of bandwidth in K{sub u} band. • The optimum substituted samples can be used as a potential magnetic loss material. • Sample contain x = 0.4 of dopants have shown greater than 90% of reflection loss. - Abstract: Substituted W-type hexaferrite nanoparticles of SrZn{sub 2−x}Co{sub x/2}Ni{sub x/2}Fe{sub 16}O{sub 27} were synthesized by a chemical co-precipitation method. The X-ray diffraction results confirmed that W-type ferrite was identified as the main phase inmore » whole samples in the range of x = 0–0.4. According to magnetic hysteresis loops, with increasing of substituted cations, saturation of magnetization increased and coercivity decreased due to crystalline site occupation of Zn with Ni and Co cations. The microwave reflection loss analysis results in the K{sub u} band (12–18 GHz) show that the highest value of reflection loss of samples was −29.11 dB at frequency of 14.57 GHz with an absorption bandwidth of more than 6 GHz by choosing reflection loss value of −10 dB as a reference. The results indicate that, the sample with appropriate amount of substituted cations hold great promise for microwave device applications.« less
Structure and photoluminescence studies of CeO2·CuAlO2 mixed metal oxide fabricated by co-precipitation method.

PubMed

Subhan, Md Abdus; Ahmed, Tanzir; Awal, M R; Kim, B Moon

2015-01-25

A novel mixed metal oxide, CeO2·CuAlO2 was fabricated by co-precipitation method in aqueous medium. CeO2·CuAlO2 was characterized by XRD, SEM, EDS, TEM, FTIR and PL spectra. The optical properties of the nanoparticles were studied by photoluminescence (PL) spectra. PL spectra at different excitations were recorded. The composite showed emission in UV, visible and NIR region depending on the excitation wavelength. The special spectral feature observed for this composite is that it showed six emission bands at 364, 409, 434, 448, 465 and 481 nm when excited at 298 nm. The green and red emissions observed at 512 and 669 nm are originated from cubic CeO2 phase when excited at 450 nm. The PL spectra were found to be dependent on excitation wavelength violating Kasha's rule. The X-ray diffraction reveals a cubic CeO2 phase and hexagonal CuAlO2 phase. EDS spectra revealed the presence of cerium (Ce), copper (Cu), aluminum (Al) and oxygen (O) elements. The particle size of the CeO2·CuAlO2 mixed oxide was estimated using Scherrer's formula, which was found to be in the range of 17.2-34.2 nm. The TEM image showed particles are almost uniform size of approximately 15-50 nm with spherical morphology. Copyright © 2014 Elsevier B.V. All rights reserved.
Structure and photoluminescence studies of CeO2·CuAlO2 mixed metal oxide fabricated by co-precipitation method

NASA Astrophysics Data System (ADS)

Subhan, Md Abdus; Ahmed, Tanzir; Awal, M. R.; Kim, B. Moon

2015-01-01

A novel mixed metal oxide, CeO2·CuAlO2 was fabricated by co-precipitation method in aqueous medium. CeO2·CuAlO2 was characterized by XRD, SEM, EDS, TEM, FTIR and PL spectra. The optical properties of the nanoparticles were studied by photoluminescence (PL) spectra. PL spectra at different excitations were recorded. The composite showed emission in UV, visible and NIR region depending on the excitation wavelength. The special spectral feature observed for this composite is that it showed six emission bands at 364, 409, 434, 448, 465 and 481 nm when excited at 298 nm. The green and red emissions observed at 512 and 669 nm are originated from cubic CeO2 phase when excited at 450 nm. The PL spectra were found to be dependent on excitation wavelength violating Kasha's rule. The X-ray diffraction reveals a cubic CeO2 phase and hexagonal CuAlO2 phase. EDS spectra revealed the presence of cerium (Ce), copper (Cu), aluminum (Al) and oxygen (O) elements. The particle size of the CeO2·CuAlO2 mixed oxide was estimated using Scherrer's formula, which was found to be in the range of 17.2-34.2 nm. The TEM image showed particles are almost uniform size of approximately 15-50 nm with spherical morphology.
High coercivity Gd-substituted Ba hexaferrites, prepared by chemical coprecipitation

NASA Astrophysics Data System (ADS)

Litsardakis, G.; Manolakis, I.; Serletis, C.; Efthimiadis, K. G.

2008-04-01

A series of Gd-substituted Ba hexaferrites with nominal formula (Ba1-xGdx)Oṡ5.25 Fe2O3 (x=0-0.30) were prepared by the chemical coprecipitation method from nitrate precursors and heating at T =800-1200°C for 2h. The samples have been examined by x-ray diffraction, vibrating-sample magnetometer, and scanning electron microscopy methods. Gd substituted samples form single phase materials with the M-type hexaferrite structure at all heating temperatures, in the range of x ⩽0.10-0.20. The saturation magnetization (at 1.8T) varies slightly with x in most cases and, for x =0.05-0.10, it increases up to 66.7Am2/kg, exceeding the value of the unsubstituted hexaferrite. A strong enhancement of the coercivity is observed for all substituted samples, with maximum values Hc=457kA/m for the single-phase x =0.10 sample annealed at 1000°C and Hc=477kA/m for the x =0.25 sample annealed at 1100°C which contains Fe2O3 and GdFeO3 impurities. As the variation of coercivity with either substitution rate (x ) or annealing temperature is not monotonic, three different factors may account for the high coercivities that are obtained: (a) an inhibition of grain growth due to the presence of Gd, (b) a possible inherent effect on magnetocrystalline anisotropy, especially for single phase samples, and (c) a microstructural effect of secondary phases.
Synthesis and LPG sensing properties of nano-sized cadmium oxide.

PubMed

Waghulade, R B; Patil, P P; Pasricha, Renu

2007-04-30

This paper reports the synthesis and liquid petroleum gas (LPG) sensing properties of nano-sized cadmium oxide (CdO). The nano-sized CdO powder was successfully synthesized by using a chemical co-precipitation method using cadmium acetate and the ammonium hydroxide, as starting materials and water as a carrier. The resulting nano-sized powder was characterized by X-ray diffraction (XRD) measurements and the transmission electron microscopy (TEM). The LPG sensing properties of the synthesized nano-sized CdO were investigated at different operating temperatures and LPG concentrations. It was found that the calcination temperature and the operating temperature significantly affect the sensitivity of the nano-sized CdO powder to the LPG. The sensitivity is found to be maximum when the calcination temperature was 400 degrees C. The sensitivity to 75ppm of LPG is maximum at an operating temperature 450 degrees C and it was found to be approximately 341%. The response and recovery times were found to be nearly 3-5s and 8-10s, respectively. The synthesized nano-sized CdO powder is able to detect up to 25ppm for LPG with reasonable sensitivity at an operating temperature 450 degrees C and it can be reliably used to monitor the concentration of LPG over the range (25-75ppm). The experimental results of the LPG sensing studies reveal that the nano-sized CdO powder synthesized by a simple co-precipitation method is a suitable material for the fabrication of the LPG sensor.
Uniform Deposition of Protein Incorporated Mineral Layer on Three-Dimensional Porous Polymer Scaffolds

PubMed Central

Segvich, Sharon; Smith, Hayes C.; Luong, Linh N.; Kohn, David H.

2009-01-01

Inorganic–organic hybrid materials designed to facilitate bone tissue regeneration use a calcium phosphate mineral layer to encourage cell adhesion, proliferation, and osteogenic differentiation. Mineral formed on porous materials is often discontinuous through the thickness of the scaffold. This study aimed to uniformly coat the pores of three-dimensional (3D) porous, polymer scaffolds with a bone-like mineral layer in addition to uniformly incorporating a model protein within this mineral layer. A filtration system designed to induce simulated body fluid flow through the interstices of 3D polylactic-co-glycolic acid scaffolds (10-mm diameter × 2-mm thickness) illustrated that a uniform, continuous mineral layer can be precipitated on the pore surfaces of a 3D porous structure within 5 days. MicroCT analysis showed increased mineral volume percent (MV%) (7.86 ± 3.25 MV%, p = 0.029) and continuous mineralization of filtered scaffolds compared with two static control groups (floating, 0.16 ± 0.26 MV% and submerged, 0.20 ± 0.01 MV%). Furthermore, the system was effective in coprecipitating a model protein, bone sialoprotein (BSA), within the mineral layer. A 10-fold increase in BSA incorporation was seen when coprecipitated filtered scaffolds (1308 ± 464 μg) were compared to a submerged static control group (139 ± 45 μg), p < 0.001. Confocal microscopy visually confirmed uniform coprecipitation of BSA throughout the thickness of the filtration scaffolds. The designed system enables 3D mineralization through the thickness of porous materials, and provides the option of including coprecipitated biomolecular cues within the mineral layer. This approach of providing a 3D conductive and osteoinductive environment could be conducive to bone tissue regeneration. PMID:17618505
Co-precipitation of dissolved organic matter by calcium carbonate in Pyramid Lake, Nevada

USGS Publications Warehouse

Leenheer, Jerry A.; Reddy, Michael M.

2008-01-01

Our previous research has demonstrated that dissolved organic matter (DOM) influences calcium carbonate mineral formation in surface and ground water. To better understand DOM mediation of carbonate precipitation and DOM co-precipitation and/or incorporation with carbonate minerals, we characterized the content and speciation of DOM in carbonate minerals and in the lake water of Pyramid Lake, Nevada, USA. A 400-gram block of precipitated calcium carbonate from the Pyramid Lake shore was dissolved in 8 liters of 10% acetic acid. Particulate matter not dissolved by acetic acid was removed by centrifugation. DOM from the carbonate rock was fractionated into nine portions using evaporation, dialysis, resin adsorption, and selective precipitations to remove acetic acid and inorganic constituents. The calcium carbonate rock contained 0.23% DOM by weight. This DOM was enriched in polycarboxylic proteinaceous acids and hydroxy-acids in comparison with the present lake water. DOM in lake water was composed of aliphatic, alicyclic polycarboxylic acids. These compound classes were found in previous studies to inhibit calcium carbonate precipitation. DOM fractions from the carbonate rock were 14C-age dated at about 3,100 to 3,500 years before present. The mechanism of DOM co-precipitation and/or physical incorporation in the calcium carbonate is believed to be due to formation of insoluble calcium complexes with polycarboxylic proteinaceous acids and hydroxy-acids that have moderately large stability constants at the alkaline pH of the lake. DOM co-precipitation with calcium carbonate and incorporation in precipitated carbonate minerals removes proteinaceous DOM, but nearly equivalent concentrations of neutral and acidic forms of organic nitrogen in DOM remain in solution. Calcium carbonate precipitation during lime softening pretreatment of drinking water may have practical applications for removal of proteinaceous disinfection by-product precursors.
Co-precipitation of DEAE-dextran coated SPIONs: how synthesis conditions affect particle properties, stem cell labelling and MR contrast.

PubMed

Barrow, Michael; Taylor, Arthur; García Carrión, Jaime; Mandal, Pranab; Park, B Kevin; Poptani, Harish; Murray, Patricia; Rosseinsky, Matthew J; Adams, Dave J

2016-09-01

Superparamagnetic iron oxide nanoparticles (SPIONs) are widely used as contrast agents for stem cell tracking using magnetic resonance imaging (MRI). The total mass of iron oxide that can be internalised into cells without altering their viability or phenotype is an important criterion for the generation of contrast, with SPIONs designed for efficient labelling of stem cells allowing for an increased sensitivity of detection. Although changes in the ratio of polymer and iron salts in co-precipitation reactions are known to affect the physicochemical properties of SPIONs, particularly core size, the effects of these synthesis conditions on stem cell labelling and magnetic resonance (MR) contrast have not been established. Here, we synthesised a series of cationic SPIONs with very similar hydrodynamic diameters and surface charges, but different polymer content. We have investigated how the amount of polymer in the co-precipitation reaction affects core size and modulates not only the magnetic properties of the SPIONs but also their uptake into stem cells. SPIONs with the largest core size and lowest polymer content presented the highest magnetisation and relaxivity. These particles also had the greatest uptake efficiency without any deleterious effect on either the viability or function of the stem cells. However, for all particles internalised in cells, the T 2 and T 2 * relaxivity was independent of the SPION's core size. Our results indicate that the relative mass of iron taken up by cells is the major determinant of MR contrast generation and suggest that the extent of SPION uptake can be regulated by the amount of polymer used in co-precipitation reactions. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.
Recovery of indium ions by nanoscale zero-valent iron

NASA Astrophysics Data System (ADS)

Chen, Wen; Su, Yiming; Wen, Zhipan; Zhang, Yalei; Zhou, Xuefei; Dai, Chaomeng

2017-03-01

Indium and its compounds have plenty of industrial applications and high demand. Therefore, indium recovery from various industrial effluents is necessary. It was sequestered by nanoscale zero-valent iron (nZVI) whose size mainly ranged from 50 to 70 nm. Adsorption kinetics and isotherm, influence of pH, and ionic strength were thoroughly investigated. The reaction process was well fitted to a pseudo second-order model, and the maximum adsorption capacity of In(III) was 390 mg In(III)/g nZVI similar to 385 mg In(III)/g nZVI at 298 K calculated by Langmuir model. The mole ratio of Fe(II) released to In(III) immobilized was 3:2, which implied a special chemical process of co-precipitation combined Fe(OH)2 with In(OH)3. Transmission electron microscopy with an energy-disperse X-ray (TEM-EDX), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS) were used to characterize surface morphology, corrosion products, and valence state of indium precipitate formed on nanoparticles. The structural evolution changed from core-shell structure of iron oxide to sheet structure of co-precipitation, to sphere structure that hydroxide gradually dissolved as the pH decreased, and to cavity structures for the pH continually decreased. Furthermore, below pH 4.7, the In(III) enrichment was inhibited for the limited capacity of co-precipitation. Also, it was found that Ca2+ and HPO4 2- have more negative influence on In(III) recovery compared with Na+, NO3 -, HCO3 -, and SO4 2-. Therefore, the In(III) recovery can be described by a mechanism which consists of adsorption, co-precipitation, and reduction and was over 78% even after 3 cycles. The results confirmed that it was applicable to employ nZVI for In(III) immobilization.
Method of producing .sup.67 Cu

DOEpatents

O'Brien, Jr., Harold A.; Barnes, John W.; Taylor, Wayne A.; Thomas, Kenneth E.; Bentley, Glenn E.

1984-01-01

A method of producing carrier-free .sup.67 Cu by proton spallation combined with subsequent chemical separation and purification is disclosed. A target consisting essentially of pressed zinc oxide is irradiated with a high energy, high current proton beam to produce a variety of spallogenic nuclides, including .sup.67 Cu and other copper isotopes. The irradiated target is dissolved in a concentrated acid solution to which a palladium salt is added. In accordance with the preferred method, the spallogenic copper is twice coprecipitated with palladium, once with metallic zinc as the precipitating agent and once with hydrogen sulfide as the precipitating agent. The palladium/copper precipitate is then dissolved in an acid solution and the copper is separated from the palladium by liquid chromatography on an anion exchange resin.
Simultaneous separation of copper, cadmium and cobalt from sea-water by co-flotation with octadecylamine and ferric hydroxide as collectors.

PubMed

Cabezon, L M; Caballero, M; Cela, R; Perez-Bustamante, J A

1984-08-01

A method is proposed for the simultaneous quantitative separation of traces ofCu(II), Cd(II) and Co(II) from sea-water samples by means of the co-flotation (adsorbing colloid flotation) technique with ferric hydroxide as co-precipitant and octadecylamine as collector. The experimental parameters have been studied and optimized. The drawbacks arising from the low solubility of octadecylamine and the corresponding sublates in water have been avoided by use of a 6M hydrochloric acid-MIBK-ethanol (1:2:2 v v ) mixture. The results obtained by means of the proposed method have been compared with those given by the usual ammonium pyrrolidine dithiocarbamate/MIBK extraction method.

Method for producing /sup 67/Cu

DOEpatents

O'Brien, H.A. Jr.; Barnes, J.W.; Taylor, W.A.; Thomas, K.E.; Bentley, G.E.

A method of producing carrier-free /sup 67/Cu by proton spallation combined with subsequent chemical separation and purification is disclosed. A target consisting essentially of pressed zinc oxide is irradiated with a high energy, high current proton beam to produce a variety of spallogenic nuclides, including /sup 67/Cu and other copper isotopes. The irradiated target is dissolved in a concentrated acid solution to which a palladium salt is added. In accordance with the preferred method, the spallogenic copper is twice coprecipitated with palladium, once with metallic zinc as the precipitating agent and once with hydrogen sulfide as the precipitating agent. The palladium/copper precipitate is then dissolved in an acid solution and the copper is separated from the palladium by liquid chromatography on an anion exchange resin.
Magnetic Properties of Copper Doped Nickel Ferrite Nanoparticles Synthesized by Co Precipitation Method

NASA Astrophysics Data System (ADS)

Anjana, V.; John, Sara; Prakash, Pooja; Nair, Amritha M.; Nair, Aravind R.; Sambhudevan, Sreedha; Shankar, Balakrishnan

2018-02-01

Nickel ferrite nanoparticles with copper atoms as dopant have been prepared using co-precipitation method with general formula Ni1-xCuxFe2O4 (x=0.2, 0.4, 0.6, 0.8 and 1) and are sintered at quite ambient temperature. Structural and magnetic properties were examined using Fourier Transform Infrared Spectroscopy (FTIR), X-ray Diffraction method (XRD) and Vibrating Sample Magnetometer (VSM) to study the influence of copper doping in nickel ferrite magnetic nanoparticles. X-ray studies proves that the particles are possessing single phase spinel structure with an average particle size calculated using Debye Scherer formula. Magnetic measurements reveal that saturation magnetization value (Ms) decreases while magnetic coercivity (Hc) increases upon doping.
Synthesis of composite nanoparticles using co-precipitation of a magnetic iron-oxide shell onto core nanoparticles

NASA Astrophysics Data System (ADS)

Primc, Darinka; Belec, Blaž; Makovec, Darko

2016-03-01

Composite nanoparticles can be synthesized by coating a shell made of one material onto core nanoparticles made of another material. Here we report on a novel method for coating a magnetic iron oxide onto the surface of core nanoparticles in an aqueous suspension. The method is based on the heterogeneous nucleation of an initial product of Fe3+/Fe2+ co-precipitation on the core nanoparticles. The close control of the supersaturation of the precipitating species required for an exclusively heterogeneous nucleation and the growth of the shell were achieved by immobilizing the reactive Fe3+ ions in a nitrate complex with urea ([Fe((CO(NH2)2)6](NO3)3) and by using solid Mg(OH)2 as the precipitating reagent. The slow thermal decomposition of the complex at 60 °C homogeneously releases the reactive Fe3+ ions into the suspension of the core nanoparticles. The key stage of the process is the thermal hydrolysis of the released Fe3+ ions prior to the addition of Mg(OH)2. The thermal hydrolysis results in the formation of γ-FeOOH, exclusively at the surfaces of the core nanoparticles. After the addition of the solid hydroxide Mg(OH)2, the pH increases and at pH 5.7 the Fe2+ precipitates and reacts with the γ-FeOOH to form magnetic iron oxide with a spinel structure (spinel ferrite) at the surfaces of the core nanoparticles. The proposed low-temperature method for the synthesis of composite nanoparticles is capable of forming well-defined interfaces between the two components, important for the coupling of the different properties. The procedure is environmentally friendly, inexpensive, and appropriate for scaling up to mass production.
Surface-engineered core-shell nano-size ferrites and their antimicrobial activity

DOE Office of Scientific and Technical Information (OSTI.GOV)

Baraliya, Jagdish D., E-mail: jdbaraliya@yahoo.co.in; Joshi, Hiren H., E-mail: jdbaraliya@yahoo.co.in

We report the results of biological study on core-shell structured MFe{sub 2}O{sub 4} (where M = Co, Mn, Ni) nanoparticles and influence of silica- DEG dual coating on their antimicrobial activity. Spherical MFe{sub 2}O{sub 4} nanoparticles were prepared via a Co-precipitation method. The microstructures and morphologies of these nanoparticles were studied by x-ray diffraction and FTIR. The antimicrobial activity study carried out in nutrient agar medium with addition of antimicrobial synthesis compound which is tested for its activity against different types of bacteria.
[Preparation and characterization of a polyvinylpyrrolidone water-based magnetic fluid].

PubMed

Xie, Jian-feng; Zhang, Yang-de; Zeng, Zhao-wu; Wang, Xiao-li; Liu, Xing-yan; Zhou, Wei-hua

2008-03-01

To prepare a stable water-based magnetic fluid. A water-based magnetic fluid was prepared by addition of polyvinylpyrrolidone (PVP) as the coating agent for the magnetic particles. After preparation of Fe3O4 by co-precipitation method, PVP was added for its coating, followed by ultrasonic agitation and purification. The magnetic nanoparticles of homogeneously small size and water-based magnetic fluid were obtained, which had good dispersion in water with strong magnetism. PVP can be used as a surfactant to stabilize the magnetic fluid.
Effect of preparation conditions on the nanostructure of hydroxyapatite and brushite phases

NASA Astrophysics Data System (ADS)

Mansour, S. F.; El-dek, S. I.; Ahmed, M. A.; Abd-Elwahab, S. M.; Ahmed, M. K.

2016-10-01

Hydroxyapatite (HAP) and dicalcium phosphate dihydrate (brushite) nanoparticles were prepared by co-precipitation method. The obtained products were characterized by X-ray powder diffraction (XRD), Fourier transformation infra-red spectroscopy (FTIR) and thermo-gravimetric analysis (TGA). Scanning electron microscopy (SEM) and transmission electron microscope (TEM) were used to investigate the morphology of the powdered samples as well as their microstructure, respectively. Brushite samples were obtained in a spherical shape, while hydroxyapatite was formed in a needle and rice shape depending on the pH value.
Viscosity studies of water based magnetite nanofluids

DOE Office of Scientific and Technical Information (OSTI.GOV)

Anu, K.; Hemalatha, J.

2016-05-23

Magnetite nanofluids of various concentrations have been synthesized through co-precipitation method. The structural and topographical studies made with the X-Ray Diffractometer and Atomic Force Microscope are presented in this paper. The density and viscosity studies for the ferrofluids of various concentrations have been made at room temperature. The experimental viscosities are compared with theoretical values obtained from Einstein, Batchelor and Wang models. An attempt to modify the Rosensweig model is made and the modified Rosensweig equation is reported. In addition, new empirical correlation is also proposed for predicting viscosity of ferrofluid at various concentrations.
Surface-engineered core-shell nano-size ferrites and their antimicrobial activity

NASA Astrophysics Data System (ADS)

Baraliya, Jagdish D.; Joshi, Hiren H.

2014-04-01

We report the results of biological study on core-shell structured MFe2O4 (where M = Co, Mn, Ni) nanoparticles and influence of silica- DEG dual coating on their antimicrobial activity. Spherical MFe2O4 nanoparticles were prepared via a Co-precipitation method. The microstructures and morphologies of these nanoparticles were studied by x-ray diffraction and FTIR. The antimicrobial activity study carried out in nutrient agar medium with addition of antimicrobial synthesis compound which is tested for its activity against different types of bacteria.
Influencing factors in the CO-precipitation process of superparamagnetic iron oxide nano particles: A model based study

NASA Astrophysics Data System (ADS)

Roth, Hans-Christian; Schwaminger, Sebastian P.; Schindler, Michael; Wagner, Friedrich E.; Berensmeier, Sonja

2015-03-01

The study, presented here, focuses on the impact of synthesis parameters on the co-precipitation process of superparamagnetic iron oxide nanoparticles. Particle diameters between 3 and 17 nm and saturation magnetizations from 26 to 89 Am2 kg-1 were achieved by variation of iron salt concentration, reaction temperature, ratio of hydroxide ions to iron ions and ratio of Fe3+/Fe2+. All synthesis assays were conceived according to the "design of experiments" method. The results were fitted to significant models. Subsequent validation experiments could confirm the models with an accuracy>95%. The characterization of the chemical composition, as well as structural and magnetic properties was carried out using powder X-ray diffraction, transmission electron microscopy, Raman and Mössbauer spectroscopy and superconducting quantum interference device magnetometry. The results reveal that the particles' saturation magnetization can be enhanced by the employment of high iron salt concentrations and a molar ratio of Fe3+/Fe2+ below 2:1. Furthermore, the particle size can be increased by higher iron salt concentrations and a hyperstoichiometric normal ratio of hydroxide ions to iron ions of 1.4:1. Overall results indicate that the saturation magnetization is directly related to the particle size.
Pronounced effects of the nominal concentrations of WO3 and Ag: WO3 nano-plates (obtained by a co-precipitation method) on their structural, morphological and optical properties

NASA Astrophysics Data System (ADS)

Rajendran, V.; Deepa, B.

2018-03-01

Tungsten oxide and different concentration of silver (Ag)-doped tungsten oxide nano material were synthesized by co-precipitation technique. The functional vibrations, structure, and morphology of as-prepared nano material were studied by Fourier transmission infrared spectroscopy, X-ray diffraction, scanning electron microscopy (SEM) and High-resolution transmission electron microscopy (HR-TEM) techniques. The SEM and HR-TEM analysis revealed the formation of nano-plate/nano rods with an average diameter of 40-80 nm diameter and 1-1.5 mm length. Fluorescence (PL) and UV-visible absorption techniques have been used to study the optical properties of the prepared nanoparticles. The observed red shift in the visible absorption spectra confirmed the promoted electron-phonon interaction in WO3 and Ag: WO3 nanoparticles compared to bulk structures. The photoluminescence of nanocrystalline Ag2+ doped WO3 exhibited a strong violet-blue, blue-green emission. Concentration dependence of the emission intensity of Ag2+ in WO3 was studied, and the significant concentration was found to be 0.5% of Ag: WO3. The effluent dye degradation executed for the 0.5% of Ag: WO3 sample under the visible light which reveals the highest degradation efficiency in appropriate time.
Preparation of core-shell Ti-Nb oxide nanocrystals

NASA Astrophysics Data System (ADS)

Simakov, David S. A.; Tsur, Yoed

2008-01-01

Nanosized powders of Ti-Nb oxide core-shell nanocrystals with atomic ratios of Nb/Ti = 0.11, 0.25, and 0.38 have been prepared by two preparation routes. The first route was co-precipitation, followed by␣annealing, using NbCl5 as a source of Nb. The second route was coating of pure TiO2 nanocrystals by Nb-isopropoxide in liquid medium, followed by impregnation of the Nb into the nanoparticles by annealing. Both methods yielded anatase nanocrystals with a Nb-rich shell and a core, which had much lower Nb loadings. The anatase structure solid solution (with Nb incorporated) was stable under annealing up to 760°C. The particle size remained within the nanometric scale ( <50 nm) under heat-treatment up to 760°C. It has been shown that the fabricated powders can be redispersed in aqueous media by simple ultrasound treatment, resulting in nanosized dispersions. Using a variety of analytical techniques, including depth profiling of single nanocrystallites by AES combined with sputtering by Ar ions, the mechanism of the core-shell structure creation was studied. It is proposed that the formation of the core-shell structure is governed by solubility limitations in the co-precipitation route and by solubility and diffusion limitations in the coating-incorporation route.
Effects of Precipitant and pH on Coprecipitation of Nanosized Co-Cr-V Alloy Powders

PubMed Central

Chen, Xiaoyu; Li, Yongxia; Huang, Lan; Zou, Dan; Wu, Enxi; Liu, Yanjun; Xie, Yuanyan; Yao, Rui; Liao, Songyi; Wang, Guangrong

2017-01-01

Nanosized Co-Cr-V alloy powders were synthesized via coprecipitation method. Effects of precipitants ((NH4)2C2O4·H2O and Na2CO3) and pH were investigated by X-ray diffraction (XRD), Zeta potential analyzer, thermogravimetry-differential scanning calorimetry (TG-DSC), inductively coupled plasma-atomic emission spectrometry (ICP-AES) and scanning electron microscopy (SEM). Co-Cr-V alloy powders were consisted of major face-centered cubic Co (fcc Co) and minor hexagonal close-packed Co (hcp Co). Grain sizes of precursors and Co-Cr-V alloy powders were increased with pH value (7–10) within the ranges of 3~39 and 39~66 nm, respectively. Rod-like or granular Co-Cr-V alloy particles were assembled by interconnected nanograins. At pH = 7, Na2CO3 precipitant was found to be beneficial to maintain the desirable composition of Co-Cr-V powders. It was also found that lower pH favors the maintenance of pre-designed composition, while grain coarsens at higher pH. Effects of variation for precipitant and pH on the morphology and composition of Co-Cr-V alloy powder were discussed in detail and relevant mechanism was further proposed. PMID:28934147
Structural and magnetic properties of calcium doped nickel ferrite nanoparticles by co-precipitation method

NASA Astrophysics Data System (ADS)

Vigneswari, T.; Raji, P.

2017-01-01

It is a truism that a sequence of calcium doped nickel ferrite (with x = 0.0, 0.2, 0.4, 0.6, 0.8 and 1.0) nanoparticles are combined by co-precipitation technique. X-Ray Diffraction (XRD) and Fourier Transform Infrared (FTIR) scrutinize the formation of single-phase inverse spinel structure in all the compositions. The lattice framework increases with the increase in calcium concentration and it exhibits the development of unit cell. Crystallite size in the range of 22-34 nm is viewed and also augmented the level of calcium. The elemental composition of pure and calcium doped nickel ferrite has been procured from Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) and Energy Dispersive X-ray analysis (EDX). It is interesting to note that the substitution of calcium increasingly exerts influence on the magnetic characteristics. These observations paved the way for the room temperature of magnetization measurements. The saturation magnetization and the experimental value of magnetic moment are noticed to enlarge initially up to x = 0.2, and then decrease incessantly with increase in the Ca content x. The increase and the decrease of saturation magnetization have widely been expounded by Neel's collinear two-sublattice model and Yafet-Kittel (Y-K) three-sub lattice model.
Effect of CTAB on structural and optical properties of CuO nanoparticles prepared by coprecipitation route

NASA Astrophysics Data System (ADS)

Varghese, Donna; Tom, Catherine; Krishna Chandar, N.

2017-11-01

CuO (Copper Oxide) nanoparticles were synthesized by a simple coprecipitation route by using copper acetate, sodium hydroxide as precursors and cetyltrimethyl ammonium bromide (CTAB) as surfactant. For the purpose of the study, the surfactant-CTAB treated and non-treated samples were synthesized separately. Both the synthesized samples were studied to understand their structural and optical properties. The formation of CuO and its crystallinity was confirmed by XRD. Further, the optical studies showed a defined blue shift in CTAB treated sample which is clear evidence that the particles undergo confinement when they are nano-regime.
Oxalate co-precipitation synthesis of calcium zirconate and calcium titanate powders.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hernandez-Sanchez, Bernadette A.; Tuttle, Bruce Andrew

2009-06-01

Fine powders of calcium zirconate (CaZrO{sub 3}, CZ) and calcium titanate (CaTiO{sub 3}, CT) were synthesized using a nonaqueous oxalate co-precipitation route from Ca(NO{sub 3}){sub 2}{center_dot}4 H{sub 2}O and group(IV) n-butoxides (Ti(OBu{sup n}){sub 4} or Zr(OBu{sup n}){sub 4}). Several reaction conditions and batch sizes (2-35 g) were explored to determine their influence on final particle size, morphology, and phase. Characterization of the as-prepared oxalate precursors, oven dried oxalate precursors (60-90 C), and calcined powders (635-900 C) were analyzed with TGA/DTA, XRD, TEM, and SEM. Densification and sintering studies on pressed CZ pellets at 1375 and 1400 C were also performed.more » Through the developed oxalate co-precipitation route, densification temperatures for CZ were lowered by 125 C from the 1500 C firing temperature required for conventional mixed oxide powders. Low field electrical tests of the CZ pellets indicated excellent dielectric properties with dielectric constants of {approx}30 and a dissipation factor of 0.0004 were measured at 1 kHz.« less
Intimate association of Thy-1 and the T-cell antigen receptor with the CD45 tyrosine phosphatase

DOE Office of Scientific and Technical Information (OSTI.GOV)

Volarevic, S.; Burns, C.M.; Sussman, J.J.

1990-09-01

Immunoprecipitation of Thy-1 from Triton X-100 detergent lysates of surface-iodinated and chemically cross-linked T cells precipitated at least first major and discrete bands. Four of these bands were identified as Thy-1, CD45 (a trasmembrane tyrosine phosphatase), a major histocompatibility complex-encoded class I molecule, and {beta}{sub 2}-microglobulin. Similar analyses revealed that CD45 was coprecipitated from lysates of cross-linker-treated cells by antibodies to the T-cell antigen receptor (TCR). The same pattern of coprecipitated bands was observed when digitonin was used to lyse untreated cells. Immunoprecipitation of Thy-1 or the TCR from lysates of cross-linked T cells precipitated CD45 tyrosine phosphatase activity. Calculationsmore » based upon the amounts of coprecipitated enzymatic activity or TCR {zeta} chain indicate that a substantial fraction of Thy-1 and TCR complexes can be cross-linked to CD45. These data support a model in which the dependence of Thy-1 signaling on TCR coexpression is due to their common interaction with a tyrosine phosphatase and provide a possible structural basis for the influence of CD45 on TCR-mediated signaling.« less
Co-precipitation of phosphate and iron limits mitochondrial phosphate availability in Saccharomyces cerevisiae lacking the yeast frataxin homologue (YFH1).

PubMed

Seguin, Alexandra; Santos, Renata; Pain, Debkumar; Dancis, Andrew; Camadro, Jean-Michel; Lesuisse, Emmanuel

2011-02-25

Saccharomyces cerevisiae cells lacking the yeast frataxin homologue (Δyfh1) accumulate iron in the mitochondria in the form of nanoparticles of ferric phosphate. The phosphate content of Δyfh1 mitochondria was higher than that of wild-type mitochondria, but the proportion of mitochondrial phosphate that was soluble was much lower in Δyfh1 cells. The rates of phosphate and iron uptake in vitro by isolated mitochondria were higher for Δyfh1 than wild-type mitochondria, and a significant proportion of the phosphate and iron rapidly became insoluble in the mitochondrial matrix, suggesting co-precipitation of these species after oxidation of iron by oxygen. Increasing the amount of phosphate in the medium decreased the amount of iron accumulated by Δyfh1 cells and improved their growth in an iron-dependent manner, and this effect was mostly transcriptional. Overexpressing the major mitochondrial phosphate carrier, MIR1, slightly increased the concentration of soluble mitochondrial phosphate and significantly improved various mitochondrial functions (cytochromes, [Fe-S] clusters, and respiration) in Δyfh1 cells. We conclude that in Δyfh1 cells, soluble phosphate is limiting, due to its co-precipitation with iron.
Potential for U sequestration with select minerals and sediments via base treatment.

PubMed

Emerson, Hilary P; Di Pietro, Silvina; Katsenovich, Yelena; Szecsody, Jim

2018-06-13

Temporary base treatment is a potential remediation technique for heavy metals through adsorption, precipitation, and co-precipitation with minerals. Manipulation of pH with ammonia gas injection may be especially useful for vadose zone environments as it does not require addition of liquids that would increase the flux towards groundwater. In this research, we conducted laboratory batch experiments to evaluate the changes in uranium mobility and mineral dissolution with base treatments including sodium hydroxide, ammonium hydroxide, and ammonia gas. Our data show that partitioning of uranium to the solid phase increases by several orders of magnitude following base treatment in the presence of different minerals and natural sediments from the Hanford site. The presence of dissolved calcium and carbonate play an important role in precipitation and co-precipitation of uranium at elevated pH. In addition, significant incongruent dissolution of bulk mineral phases occurs and likely leads to precipitation of secondary mineral phases. These secondary phases may remove uranium via adsorption, precipitation, and co-precipitation processes and may coat uranium phases with low solubility minerals as the pH returns to natural conditions. Copyright © 2018 Elsevier Ltd. All rights reserved.
Co-precipitation of radium with barium and strontium sulfate and its impact on the fate of radium during treatment of produced water from unconventional gas extraction.

PubMed

Zhang, Tieyuan; Gregory, Kelvin; Hammack, Richard W; Vidic, Radisav D

2014-04-15

Radium occurs in flowback and produced waters from hydraulic fracturing for unconventional gas extraction along with high concentrations of barium and strontium and elevated salinity. Radium is often removed from this wastewater by co-precipitation with barium or other alkaline earth metals. The distribution equation for Ra in the precipitate is derived from the equilibrium of the lattice replacement reaction (inclusion) between the Ra(2+) ion and the carrier ions (e.g., Ba(2+) and Sr(2+)) in aqueous and solid phases and is often applied to describe the fate of radium in these systems. Although the theoretical distribution coefficient for Ra-SrSO4 (Kd = 237) is much larger than that for Ra-BaSO4 (Kd = 1.54), previous studies have focused on Ra-BaSO4 equilibrium. This study evaluates the equilibria and kinetics of co-precipitation reactions in Ra-Ba-SO4 and Ra-Sr-SO4 binary systems and the Ra-Ba-Sr-SO4 ternary system under varying ionic strength (IS) conditions that are representative of brines generated during unconventional gas extraction. Results show that radium removal generally follows the theoretical distribution law in binary systems and is enhanced in the Ra-Ba-SO4 system and restrained in the Ra-Sr-SO4 system by high IS. However, the experimental distribution coefficient (Kd') varies widely and cannot be accurately described by the distribution equation, which depends on IS, kinetics of carrier precipitation and does not account for radium removal by adsorption. Radium removal in the ternary system is controlled by the co-precipitation of Ra-Ba-SO4, which is attributed to the rapid BaSO4 nucleation rate and closer ionic radii of Ra(2+) with Ba(2+) than with Sr(2+). Carrier (i.e., barite) recycling during water treatment was shown to be effective in enhancing radium removal even after co-precipitation was completed. Calculations based on experimental results show that Ra levels in the precipitate generated in centralized waste treatment facilities far exceed regulatory limits for disposal in municipal sanitary landfills and require careful monitoring of allowed source term loading (ASTL) for technically enhanced naturally occurring materials (TENORM) in these landfills. Several alternatives for sustainable management of TENORM are discussed.
Mechanisms of iron-silica aqueous interaction and the genesis of Precambrian iron formation

NASA Astrophysics Data System (ADS)

Chemtob, S. M.; Catalano, J. G.; Moynier, F.; Pringle, E. A.

2015-12-01

Iron formations (IFs), Fe- and Si-rich chemical sediments common in Precambrian successions, preserve key information about the compositional, biological, and oxidative evolution of the Precambrian ocean. Stable Si isotopes (δ30Si) of IF have been used to infer paleo-oceanic composition, and secular variations in δ30Si may reflect ancient biogeochemical cycles. The δ30Si of primary Fe-Si precipitates that formed IF depends not only on the δ30Si of aqueous silica but also on the precipitation mechanism. Multiple formation mechanisms for these primary precipitates are plausible. Aqueous Si may have adsorbed on newly precipitated iron oxyhydroxide surfaces; alternatively, Fe and Si may have coprecipitated as a single phase. Here we explore variations in the Si isotope fractionation factor (ɛ) with Fe-Si aqueous interaction mechanism (adsorption vs. coprecipitation). In adsorption experiments, sodium silicate solutions (pH 8.1, 125-2000 µM Si) were reacted with iron oxide particles (hematite, ferrihydrite, goethite, and magnetite) for 24 to 72 hours. Resultant solutions had δ30Si between 0 and +6‰. Calculated ɛ varied significantly with oxide mineralogy and morphology. For ferrihydrite, ɛ = -1.7‰; for hematite, ɛ = -2 to -5‰, depending on particle morphology. Apparent ɛ decreased upon surface site saturation, implying a smaller isotope effect for polymeric Si adsorption than monomeric adsorption. In coprecipitation experiments, solutions of Na-silicate and Fe(II) chloride (0.4-10 mM) were prepared anaerobically, then air-oxidized for 3 days to induce precipitation. At low Si concentrations, magnetite formed; near silica saturation, lepidocrocite and ferrihydrite formed. The Si isotope fractionation factor for coprecipitation was within the range of ɛ observed for adsorption (ɛ = -2.3 ± 1.0‰). These results indicate that the mechanism of Fe-Si interaction affects ɛ, presumably due to varying silicate coordination environments. These isotopic analyses will be paired with Si K-edge and Fe K-edge X-ray absorption spectra of the solids to illustrate how Si bonding environment affects ɛ. Effective reconstruction of paleo-oceanic δ30Si may require additional constraints on the relative importance of Si adsorption and Fe-Si coprecipitation in the production of IF primary precipitates.

Ferrihydrite-associated organic matter (OM) stimulates reduction by Shewanella oneidensis MR-1 and a complex microbial consortia

NASA Astrophysics Data System (ADS)

Cooper, Rebecca Elizabeth; Eusterhues, Karin; Wegner, Carl-Eric; Totsche, Kai Uwe; Küsel, Kirsten

2017-11-01

The formation of Fe(III) oxides in natural environments occurs in the presence of natural organic matter (OM), resulting in the formation of OM-mineral complexes that form through adsorption or coprecipitation processes. Thus, microbial Fe(III) reduction in natural environments most often occurs in the presence of OM-mineral complexes rather than pure Fe(III) minerals. This study investigated to what extent does the content of adsorbed or coprecipitated OM on ferrihydrite influence the rate of Fe(III) reduction by Shewanella oneidensis MR-1, a model Fe(III)-reducing microorganism, in comparison to a microbial consortium extracted from the acidic, Fe-rich Schlöppnerbrunnen fen. We found that increased OM content led to increased rates of microbial Fe(III) reduction by S. oneidensis MR-1 in contrast to earlier findings with the model organism Geobacter bremensis. Ferrihydrite-OM coprecipitates were reduced slightly faster than ferrihydrites with adsorbed OM. Surprisingly, the complex microbial consortia stimulated by a mixture of electrons donors (lactate, acetate, and glucose) mimics S. oneidensis under the same experimental Fe(III)-reducing conditions suggesting similar mechanisms of electron transfer whether or not the OM is adsorbed or coprecipitated to the mineral surfaces. We also followed potential shifts of the microbial community during the incubation via 16S rRNA gene sequence analyses to determine variations due to the presence of adsorbed or coprecipitated OM-ferrihydrite complexes in contrast to pure ferrihydrite. Community profile analyses showed no enrichment of typical model Fe(III)-reducing bacteria, such as Shewanella or Geobacter sp., but an enrichment of fermenters (e.g., Enterobacteria) during pure ferrihydrite incubations which are known to use Fe(III) as an electron sink. Instead, OM-mineral complexes favored the enrichment of microbes including Desulfobacteria and Pelosinus sp., both of which can utilize lactate and acetate as an electron donor under Fe(III)-reducing conditions. In summary, this study shows that increasing concentrations of OM in OM-mineral complexes determines microbial Fe(III) reduction rates and shapes the microbial community structure involved in the reductive dissolution of ferrihydrite. Similarities observed between the complex Fe(III)-reducing microbial consortia and the model Fe(III)-reducer S. oneidensis MR-1 suggest electron-shuttling mechanisms dominate in OM-rich environments, including soils, sediments, and fens, where natural OM interacts with Fe(III) oxides during mineral formation.
Isotopic analysis of uranium in natural waters by alpha spectrometry

USGS Publications Warehouse

Edwards, K.W.

1968-01-01

A method is described for the determination of U234/U238 activity ratios for uranium present in natural waters. The uranium is coprecipitated from solution with aluminum phosphate, extracted into ethyl acetate, further purified by ion exchange, and finally electroplated on a titanium disc for counting. The individual isotopes are determined by measurement of the alpha-particle energy spectrum using a high resolution low-background alpha spectrometer. Overall chemical recovery of about 90 percent and a counting efficiency of 25 percent allow analyses of water samples containing as little as 0.10 ?g/l of uranium. The accuracy of the method is limited, on most samples, primarily by counting statistics.
Investigations on structural and optical properties of starch capped ZnS nanoparticles synthesized by microwave irradiation method

NASA Astrophysics Data System (ADS)

Lalithadevi, B.; Mohan Rao, K.; Ramananda, D.

2018-05-01

Following a green synthesis method, zinc sulfide (ZnS) nanoparticles were prepared by chemical co-precipitation technique using starch as capping agent. Microwave irradiation was used as heating source. X-ray diffraction studies indicated that nanopowders obtained were polycrystalline possessing ZnS simple cubic structure. Transmission electron microscopic studies indicated that starch limits the agglomeration by steric stabilization. Interaction between ZnS and starch was confirmed by Fourier transform infrared spectroscopy as well as Raman scattering studies. Quantum size effects were observed in optical absorption studies while quenching of defect states on nanoparticles was improved with increase in starch addition as indicated by photoluminescence spectra.
Synthesis, characterization, and controlled release anticorrosion behavior of benzoate intercalated Zn-Al layered double hydroxides

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Yi; Zhang, Dun, E-mail: zhangdun@qdio.ac.cn

2011-11-15

Graphical abstract: The benzoate anion released from Zn-Al LDHs provides a more effective long-term protection against corrosion of Q235 carbon steel in 3.5% NaCl solution. Highlights: {yields} A benzoate anion corrosion inhibitor intercalated Zn-Al layered double hydroxides (LDHs) has been assembled by coprecipitation method. {yields} The kinetic simulation indicates that the ion-exchange one is responsible for the release process and the diffusion through particle is the rate limiting step. {yields} A significant reduction of the corrosion rate is observed when the LDH nanohybrid is present in the corrosive media. -- Abstract: Corrosion inhibitor-inorganic clay composite including benzoate anion intercalated Zn-Almore » layered double hydroxides (LDHs) are assembled by coprecipitation. Powder X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectrum analyses indicate that the benzoate anion is successfully intercalated into the LDH interlayer and the benzene planes are vertically bilayer-positioned as a quasi-guest ion-pair form in the gallery space. Kinetic simulation for the release data, XRD and FT-IR analyses of samples recovered from the release medium indicate that ion-exchange is responsible for the release process and diffusion through the particle is also indicated to be the rate-limiting step. The anticorrosion capabilities of LDHs loaded with corrosion inhibitor toward Q235 carbon steel are analyzed by polarization curve and electrochemical impedance spectroscopy methods. Significant reduction of corrosion rate is observed when the LDH nanohybrid is present in the corrosive medium. This hybrid material may potentially be applied as a nanocontainer in self-healing coatings.« less
Photocatalytic removal of 2,4-dichlorophenoxyacetic acid herbicide on copper oxide/titanium dioxide prepared by co-precipitation method

NASA Astrophysics Data System (ADS)

Lee, Shu Chin; Hasan, Norhasnita; Lintang, Hendrik O.; Shamsuddin, Mustaffa; Yuliati, Leny

2016-02-01

In this work, suppression of the charge recombination on the titanium dioxide (TiO2) was reported by the addition of copper oxide (CuO), which led to a higher activity of TiO2 for removal of 2,4-dichlorophenoxyacetic acid (2,4-D) herbicide. A series of CuO/TiO2 with CuO loadings of 0.1-1 wt% was prepared through a co-precipitation method. X-ray diffraction patterns revealed that the presence of CuO could not be detected as the low loading amount of CuO might have good dispersion on the surface of TiO2. Diffuse reflectance UV-visible spectra suggested that low loading amount of CuO did not influence the optical property of TiO2. Fluorescence spectroscopy revealed that TiO2 possessed a dominant emission peak of 407 nm at an excitation wavelength of 218 nm. The increasing loading amount of CuO decreased the emission intensity of TiO2, suggesting the successful reduction of charge recombination. After irradiation under UV light for 1 h, CuO(0.1 wt%)/TiO2 gave the highest percentage removal of the herbicide among the samples. The optimum loading amount of CuOmight improve the charge separation and reduce the electron-hole recombination on TiO2 without blocking the active sites, thus leading to the improved photocatalytic activity. This work showed that CuO/TiO2 is a potential photocatalyst for environmental remediation.
Electrochemical performance of Li[Ni0.7Co0.1Mn0.2]O2 cathode materials using a co-precipitation method.

PubMed

Kim, Jeong-Min; Jin, Bong-Soo; Koo, Hoe-Jin; Choi, Jae-Man; Kim, Hyun-Soo

2013-05-01

The Li[Ni0.7Co0.1Mn0.2]O2 cathode material synthesized using a co-precipitation method was investigated as a function of various pH level in terms of its microstructure and electrochemical properties. From the XRD pattern analysis, the Li[Ni0.7Co0.1Mn0.2]O2 cathode material prepared in this study are found to well coincide with typically hexagonal alpha-NaFeO2 structure. The primary particle size was about 100-300 nm at all compositions while secondary particle size increased as pH level increased from 10.34 microm (pH 10.3) to 14 microm (pH 12.5). The initial discharge capacity increased up to 165 mAh/g (0.1 C) at pH 11, and then decreased down to 144 mAh/g with further increasing pH level. The capacity retention of the cathode (pH 11) showed 90% at 0.2 C and 15% at 5 C respectively compared with the discharge capacity at 0.1 C. The capacity retention of the cathode (pH 10.3) performed 94% of the initial capacity after 22 cycles at 0.5 C charge/discharge test. Therefore, it is thought to be that pH 10.3 is optimized condition of the Li[Ni0.7Co0.1Mn0.2]O2 cathode material in this study because pH 10.3 shows better cycle performance than other conditions.
Drug delivery system for an anticancer agent, chlorogenate-Zn/Al-layered double hydroxide nanohybrid synthesised using direct co-precipitation and ion exchange methods

NASA Astrophysics Data System (ADS)

Barahuie, Farahnaz; Hussein, Mohd Zobir; Arulselvan, Palanisamy; Fakurazi, Sharida; Zainal, Zulkarnain

2014-09-01

A nano-structured drug-inorganic clay hybrid involving an active anticancer compound, which is chlorogenic acid (CA) intercalated into Zn/Al-layered double hydroxide, has been assembled via ion-exchange and co-precipitation methods to form a nanohybrid CZAE (a chlorogenic acid-Zn/Al nanohybrid synthesised using an ion-exchange method) and CZAC (a chlorogenic acid-Zn/Al nanohybrid synthesised using a direct method), respectively. The X-ray diffraction (XRD) results confirmed that the CA-LDH had a hybrid structure in which the anionic chlorogenate is arranged between the interlayers as a horizontal monolayer at 90 and 20° angles from the x axis for CZAE and CZAC, respectively. Both nanohybrids have the properties of mesoporous materials. The high loading percentage of chlorogenic acid (approximately 43.2% for CZAE and 45.3% for CZAC) with basal spacings of 11.7 and 12.6 Å for CZAE and CZAC, respectively, corroborates the successful intercalation of chlorogenic acid into the interlayer gallery of layered double hydroxides. Free chlorogenic acid and the synthesised nanocomposites (CZAE, CZAC) were assessed for their cytotoxicity against various cancer cells. The Fourier transform infrared data supported the formation of both nanohybrids, and a thermal analysis showed that the nanohybrids are more thermally stable than their counterparts. The chlorogenate shows a sustained release, and the release rate of chlorogenate from CZAE and CZAC nanohybrids at pH 7.4 is remarkably lower than that at pH 4.8 due to their different release mechanisms. The release rate of chlorogenate from both nanohybrids can be described as pseudo-second order. The present investigation revealed the potential of the nanohybrids to enhance the in vitro anti-tumour effect of chlorogenic acid in liver and lung cancer cells in vitro.
Effect of Co-Contaminants Uranium and Nitrate on Iodine Remediation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Szecsody, James E.; Lee, Brady D.; Lawter, Amanda R.

The objective of this study is to evaluate the significance of co-contaminants on the migration and transformation of iodine species in the Hanford subsurface environment. These impacts are relevant because remedies that target individual contaminants like iodine, may not only impact the fate and transport of other contaminants in the subsurface, but also inhibit the effectiveness of a targeted remedy. For example, iodine (as iodate) co-precipitates with calcite, and has been identified as a potential remedy because it immobilizes iodine. Since uranium also co-precipitates with calcite in field sediments, the presence of uranium may also inhibit iodine co-precipitation. Another potentiallymore » significant impact from co-existing contaminants is iodine and nitrate. The presence of nitrate has been shown to promote biogeochemical reduction of iodate to iodide, thereby increasing iodine species subsurface mobility (as iodide exhibits less sorption). Hence, this study reports on both laboratory batch and column experiments that investigated a) the change in iodate uptake mass and rate of uptake into precipitating calcite due to the presence of differing amounts of uranium, b) the amount of change of the iodate bio-reduction rate due to the presence of differing nitrate concentrations, and c) whether nitrite can reduce iodate in the presence of microbes and/or minerals acting as catalysts.« less
Effects of Residual Lithium in the precursors of Li[Ni1/3Co1/3Mn1/3]O2 on their lithium-ion battery performance

NASA Astrophysics Data System (ADS)

Jo, Minsang; Ku, Heesuk; Park, Sanghyuk; Song, Junho; Kwon, Kyungjung

2018-07-01

Li[Ni1/3Co1/3Mn1/3]O2 cathode active materials are synthesized from co-precipitated hydroxide precursors Lix[Ni1/3Co1/3Mn1/3]1-x(OH)2, and the effect of residual Li in the precursors on the lithium-ion battery (LIB) performance of their corresponding cathode active materials is investigated. Three kinds of precursors that contain different amounts of Li are selected depending on different conditions of the solution composition for the co-precipitation and washing process. It is confirmed that the introduction of Li to the precursors reduces the degree of structural perfection by X-ray diffraction analysis. Undesirable cation mixing occurs with the increasing Li content of the precursors, which is inferred from a decline in lattice parameters and the calculated intensity ratio of (003) and (104) peaks. In the voltage range of 3.0-4.3 V, the initial charge/discharge capacities and the rate capability of the cathode active materials are aggravated when Li exists in the precursors. Therefore, it could be concluded that the strict control of Li in a solution for co-precipitation of precursors is necessary in the resynthesis of cathode active materials from spent LIBs.
Intercalation of amino acids and oligopeptides into Zn Al layered double hydroxide by coprecipitation reaction

NASA Astrophysics Data System (ADS)

Aisawa, Sumio; Sasaki, Shuji; Takahashi, Satoshi; Hirahara, Hidetoshi; Nakayama, Hirokazu; Narita, Eiichi

2006-05-01

The coprecipitation of amino acids and oligopeptides with the Zn Al LDH was investigated using phenylalanine (Phe), phenylalanyl-phenylalanine (Phe-Phe), glycyl-phenylalanine (Gly Phe), glycine (Gly), glycyl-glycine (Gly Gly), glycyl-glycyl-glycine (Gly Gly Gly) and N-(N-γ-glutamyl-cysteinyl)-glycine (GSH) as guest species. The coprecipitation behavior of amino acids and oligopeptides was found to be influenced by the solution pH and the kind of their side chain groups, and reached the maximum at pH 8 or 9. The basal spacing, d003, of the Phe, Phe-Phe and GSH/LDH was 1.81, 2.41 and 1.64 nm, supporting that guests were arranged vertical to the LDH basal layer. Acceding to the basal spacing of the Gly, Gly Gly and Gly Gly Gly/LDH (d003=0.84 0.88 nm), these guests were oriented horizontal to the LDH basal layer with the co-intercalated NO3-. Moreover, the amount of Phe-Phe, Gly Gly and Gly Gly Gly intercalated was almost the same as that of Phe and Gly despite increasing the number peptide bond and the molecular size. GSH was intercalated into the LDH interlayer space as GSH oxidized form with bridged LDH layers by their carboxylate groups.
URANIUM RECOVERY PROCESS

DOEpatents

Bailes, R.H.; Long, R.S.; Olson, R.S.; Kerlinger, H.O.

1959-02-10

A method is described for recovering uranium values from uranium bearing phosphate solutions such as are encountered in the manufacture of phosphate fertilizers. The solution is first treated with a reducing agent to obtain all the uranium in the tetravalent state. Following this reduction, the solution is treated to co-precipitate the rcduced uranium as a fluoride, together with other insoluble fluorides, thereby accomplishing a substantially complete recovery of even trace amounts of uranium from the phosphate solution. This precipitate usually takes the form of a complex fluoride precipitate, and after appropriate pre-treatment, the uranium fluorides are leached from this precipitate and rccovered from the leach solution.
Synthesis of Ce doped ZnO nanoparticles coupled with graphene oxide as efficient photocatalyst for the degradation of dye under day light

NASA Astrophysics Data System (ADS)

Labhane, P. K.; Patle, L. B.; Huse, V. R.; Sonawane, G. H.

2018-05-01

Ce doped ZnO nanoparticles coupled with graphene oxide (Ce-ZnO/GO) photocatalyst was prepared by co-precipitation and wet impregnation method. The effect of Ce doping on ZnO and ZnO-GO composite has been evaluated by using XRD, Williamson-Hall Plot, FESEM and EDX data. Solar light photocatalytic activities of samples were evaluated spectrophotometrically by the degradation of methylene blue (MB). Ce doped ZnO coupled with GO shows excellent catalytic efficiency compared to other samples, degrading MB completely within 120 min under day light.
Effect of La3+ Substitution on Electric, Dielectric and Magnetic Properties of Cobalt Nano-Ferrite

NASA Astrophysics Data System (ADS)

Kumar, Pawan; Singh, M.

2011-07-01

Ultrafine particles of CoLaxFe2-xO4 (x = 0, 0.20) were prepared by using co-precipitation method. X-ray diffraction studies show that the samples have cubic spinel structure and average crystallite size of x = 0 and x = 0.2 are 49.84 nm and 27.73 nm respectively. Dielectric and magnetic properties have been studied by impedance analyzer and magnetic properties of the ferrite system were studied using VSM respectively. La3+ ions modulate significantly the electric, dielectric and magnetic properties of cobalt spinel ferrites.
Investigation of photoluminescence and dielectric properties of pure and Fe doped nickel oxide nanoparticles

NASA Astrophysics Data System (ADS)

Gupta, Jhalak; Ahmad, Arham S.

2018-05-01

The nanocrystallites of pure and Fe doped Nickel Oxide (NiO) were synthesized by the cost effective co-precipitation method using nickel nitrate as the initial precursor. The synthesized nickel oxide nanoparticles were characterized by X-Ray Diffraction (XRD), Photoluminiscence Spectroscopy (PL), LCR meter. The crystallite size of synthesized pure Nickel Oxide nanoparticles obtained by XRD using Debye Scherer's formula was found to be 21.8nm and the size decreases on increasing the dopant concentration. The optical properties were analyzed by PL and dielectric ones by using LCR meter.
Facile synthesis and paramagnetic properties of Fe3O4@SiO2 core-shell nanoparticles

NASA Astrophysics Data System (ADS)

Yang, Lili; Zou, Ping; Cao, Jian; Sun, Yunfei; Han, Donglai; Yang, Shuo; Chen, Gang; Kong, Xiangwang; Yang, Jinghai

2014-12-01

The Fe3O4@SiO2 core-shell nanoparticles (NPs) had been successfully fabricated via direct decomposition of tetraethyl orthosilicate (TEOS) in solution under the presence of as-synthesized Fe3O4 NPs prepared by chemical coprecipitation method. The structure and magnetic properties of Fe3O4@SiO2 NPs were characterized and the result indicated that Fe3O4@SiO2 NPs are about 12 nm in size with paramagnetic property. The possible growth and magnetic mechanism was discussed in detail.
Single and combined effects of phosphate, silicate, and natural organic matter on arsenic removal from soft and hard groundwater using ferric chloride

NASA Astrophysics Data System (ADS)

Chanpiwat, Penradee; Hanh, Hoang Thi; Bang, Sunbaek; Kim, Kyoung-Woong

2017-06-01

In order to assess the effects of phosphate, silicate and natural organic matter (NOM) on arsenic removal by ferric chloride, batch coprecipitation experiments were conducted over a wide pH range using synthetic hard and soft groundwaters, similar to those found in northern Vietnam. The efficiency of arsenic removal from synthetic groundwater by coprecipitation with FeCl3 was remarkably decreased by the effects of PO4 3-, SiO4 4- and NOM. The negative effects of SiO4 4- and NOM on arsenic removal were not as strong as that of PO4 3-. Combining PO4 3- and SiO4 4- increased the negative effects on both arsenite (As3+) and arsenate (As5+) removal. The introduction of NOM into the synthetic groundwater containing both PO4 3- and SiO4 4- markedly magnified the negative effects on arsenic removal. In contrast, both Ca2+ and Mg2+ substantially increased the removal of As3+ at pH 8-12 and the removal of As5+ over the entire pH range. In the presence of Ca2+ and Mg2+, the interaction of NOM with Fe was either removed or the arsenic binding to Fe-NOM colloidal associations and/or dissolved complexes were flocculated. Removal of arsenic using coprecipitation by FeCl3 could not sufficiently reduce arsenic contents in the groundwater (350 μg/L) to meet the WHO guideline for drinking water (10 μg/L), especially when the arsenic-rich groundwater also contains co-occurring solutes such as PO4 3-, SiO4 4- and NOM; therefore, other remediation processes, such as membrane technology, should be introduced or additionally applied after this coprecipitation process, to ensure the safety of drinking water.
Development of high T(sub c) (greater than 110 K) Bi, Tl, and Y-based materials as superconducting circuit elements

NASA Technical Reports Server (NTRS)

Haertling, Gene H.; Grabert, Gregory; Gilmour, Phillip

1992-01-01

Experimental work has continued on the development and characterization of bulk and hot pressed powders and tapecast materials in the Bi-Sr-Ca-Cu-O and Tl-Ba-Ca-Cu-O systems. A process for producing warp-free, sintered, superconducting tapes of Bi composition Bi2Sr2Ca2Cu3O(x) with a mixed oxide process was established. This procedure required a triple calcination at 830 C for 24 hours and sintering at 845 C from 20 to 200 hours. Hot pressing the triple calcined powder at 845 C for 6 hours at 5000 psi yielded a dense material which on further heat treatment at 845 C for 24 hours exhibited a Tc of 108.2 K. A further improvement in the processing of the bismuth materials was achieved via a chemical coprecipitation process wherein the starting nitrate materials were coprecipitated with oxalic acid, thus yielding a more chemically homogeneous, more reactive powder. With the coprecipitated powders, only one calcine at 830 C for 12 hours and a final sinter at 845 C for 30 hours was sufficient to produce a bulk superconducting material with a Tc of 108.4 K. SAFIRE-type grounding links were successfully fabricated from sintered, tapecast, coprecipitated BSCCO 2223 powders. Compositional and processing investigations were continued on the Tl-based superconductors. Manganese and lithium additions and sintering temperature and time were examined to determine their influence on superconducting properties. It was found that lithium substitutions for copper enhance the transition temperatures while manganese additions produced deleterious effects on the superconducting properties. A suitable procedure for producing reproducible bulk and tapecast material of Tl composition Tl2Ba2Ca2Cu3O(x) was developed and used in fabricating uniform superconducting tapes. The highest transition temperature for Tl-based tapes was measured at 110.2 K. Thallium superconducting SAFIRE-type grounding links were fabricated from the tapes.
Transformation of Strontium during formation of biogenic calcium carbonate

NASA Astrophysics Data System (ADS)

Ohnuki, T.; Kozai, N.; Sakamoto, F.; Yamashita, M.; Horiieke, T.; Utsunomiya, S.

2016-12-01

Some amounts of radionuclides contaminated water containing 90Sr generated in the Fukushima Daiichi Nuclear Power Plant were leaked to sea water in the port. One of the possible method to eliminate 90Sr is co-precipitated with biogenic carbonates minerals (CCM). Specific bacteria are known to form biogenic CCM in groundwater. In the present study, we have screened specific bacterium to form CCM in saline water, and studied transformation of Sr during biogenic CCM. A marine microbe of strain TK2d, which is screened from Tokyo bay to form CCM in saline solution, was grown in the medium solution contained urea and Sr. The concentratuion of Sr2+ in the solution was monitored by ICP-OES (ICP-OES; 720 Agilent Technologies, Inc., USA) during the formation of biogenic CCM. The precipitates were analyzed by SEM, TEM, and XAFS. When 1.0 mM Sr was dissolved in the medium solution, the concentration of Sr decreased up to 0.02 mM within 10 days, indicating that most of Sr in the solution was eliminated within 10 days. SEM and TEM analyses showed that needle shaped CCM containing Ca and Sr were formed. The CCM was not single crystalline, but poly-crystalline of calcite and aragonite. The elemental mapping showed that Sr was present at the same position of Ca, indicating that Sr was coprecipitated with Ca. The XANES analysis of Sr in the precipitates showed that the XANES spectrum was not the same as that of Sr coprecipitated with an abiotic Ca carbonates. Linear combination fitting of XANES spectra by those of SrCl2 and SrCO3 showed that both Sr2+ and SrCO3 were present in CCM. Longer contact time resulted in higher content of SrCO3, indicating that Sr was incorporated gradually with time into CCM structure. Thus, Sr was changed its chemical species from adsorbed one to the incorporated one in biogenic CCM in saline solution. This work was partially supported by a research grant from the Japan Science and Technology Agency, Japan (research grant No. 260502).
Influence of adsorption versus coprecipitation on the retention of rice straw-derived dissolved organic carbon and subsequent reducibility of Fe-DOC systems

NASA Astrophysics Data System (ADS)

Sodano, Marcella; Lerda, Cristina; Martin, Maria; Celi, Luisella; Said-Pullicino, Daniel

2016-04-01

The dissimilatory reduction of Fe oxides is the main organic C-consuming process in paddy soils under anoxic conditions. The contribution of Fe(III) reduction to anaerobic C mineralization depends on many factors, but most importantly on the bioavailability of labile organic matter and a reducible Fe pool as electron donors and acceptors, respectively. On the other hand, the strong affinity of these minerals for organic matter and their capability of protecting it against microbial decomposition is well known. Natural Fe oxides in these soils may therefore play a key role in determining the C source/sink functions of these agro-ecosystems. Apart from contributing to C stabilization, the interaction between Fe oxides and dissolved organic C (DOC) may influence the structure and reactivity of these natural oxides, and selectively influence the chemical properties of DOC. Indeed, Fe-DOC associations may not only reduce the availability of DOC, but may also limit the microbial reduction of Fe oxides under anoxic conditions. In fact, the accessibility of these minerals to microorganisms, extracellular enzymes, redox active shuttling compound or reducing agents may be impeded by the presence of sorbed organic matter. In soils that are regularly subjected to fluctuations in redox conditions the interaction between DOC and Fe oxides may not only involve organic coatings on mineral surfaces, but also Fe-DOC coprecipitates that form during the rapid oxidation of soil solutions containing important amounts of DOC and Fe(II). However, little is known on how these processes influence DOC retention, and the structure and subsequent reducibility of these Fe-DOC associations. We hypothesized that the nature and extent of the interaction between DOC and Fe oxides may influence the accessibility of the bioavailable Fe pool and consequently its reducibility. We tested this hypothesis by synthesizing a series of Fe-DOC systems with increasing C:Fe ratios prepared by either surface adsorption or coprecipitation, DOC was obtained by incubating a suspension of rice straw in water (straw-solution ratio of 1:30) under oxic conditions at 25° C for 30 days to simulate the decomposition of rice straw in the field. Increasing amounts of DOC were equilibrated (pH = 6) with a known mass of ferrihydrite (initial molar C:Fe ratios of 1, 5 and 10) to obtain surface coated Fe-DOC systems with increasing C loading. On the other hand, coprecipitates with similar initial C:Fe ratios were obtained by oxidation of a Fe(II) solution in the presence of increasing amounts of DOC at pH = 6. A natural Fe-DOC coprecipitate was also obtained by in situ sampling of a paddy soil solution from the topsoil during a cropping season, and subsequent oxidation in the laboratory. The surface and chemical properties of all substrates were subsequently evaluated and compared. We hereby present the first results of the influence of adsorption vs coprecipitation on the selective retention of DOC, structure and surface charge, as well as their susceptibility to chemical reduction with ascorbic acid.
Specific solubilization of impurities in culture media: Arg solution improves purification of pH-responsive tag CspB50 with Teriparatide.

PubMed

Oki, Shogo; Nonaka, Takahiro; Shiraki, Kentaro

2018-06-01

Protein purification using non-chromatographic methods is a simple technique that avoids costly resin. Recently, a cell surface protein B (CspB) tag has been developed for a pH-responsive tag for protein purification by solid-liquid separation. Proteins fused with the CspB tag show reversible insolubilization at acidic pH that can be used in solid-liquid separation for protein purification. However, brown-color impurities from co-precipitation hamper further analysis of the target proteins. In this study, we investigated the effect of additives on the co-precipitation of CspB-tagged Teriparatide (CspB50TEV-Teriparatide) expressed in Corynebacterium glutamicum and associated impurities. Arginine (Arg) at 1.0 M was found to be the most effective additive for removing impurities, particularly carotenoids and nucleic acids. Furthermore, all impurities detected in the fluorescence and absorbance spectra were successfully removed by the repetition of precipitation-redissolution in the Arg solution. The precipitation yield of the CspB50TEV-Teriparatide did not change with the addition of Arg and the repetition of the precipitation-redissolution process. Collectively, our findings indicate that the specific desorption of π-electron rich compounds by Arg may be useful in conjunction with the pH-responsive CspB tag for solid-liquid protein purification. Copyright © 2018 Elsevier Inc. All rights reserved.

P41IDENTIFICATION OF GLIOMA SPECIFIC APTAMER TARGETS

PubMed Central

Arora, Mohit; Alder, Jane; Lawrence, Clare; Davis, Charles; Dawson, Tim; Hall, Greg; Shaw, Lisa

2014-01-01

INTRODUCTION: Aptamers are in vitro generated DNA and RNA sequences which are randomly created as a library, with multiple permutations and combinations. These are then exposed to the target structure against which we want an aptamer ‘selected’ using Sequential Enumeration of Ligands by Exponential enrichment (SELEX). METHOD: Commercially available glioma and glial cell lines and in-house generated primary glioma cultures were used. Modified aptamers based on published sequences against glioma cell lines and newly generated sequences were used in the project to identify their binding targets. Cy3 or biotin- conjugated aptamers were incubated with live glioma cell cultures and imaged using confocal or light microscopy.To determine the target ligand, aptamers were then reacted with glial cell lysate and subjected to precipitation using streptavidin agarose beads and SDS polyacrylamide electrophoresis. Proteins were analysed by mass spectroscopy. RESULTS: Known and unknown aptamer protein ligands were co-precipitated. Ku70, Ku80 were precipitated along with nucleolin and related proteins. CONCLUSION: The aptamer has shown preferential binding to glioma cells and could act as a delivery system for therapeutic payloads. The aptamer targets Ku70 and Ku80, which are known to be over expressed in other forms of cancer but their role in gliomagenesis has not been fully elucidated. Other novel proteins have also been identified. Thus the aptamer co-precipitation technique has identified potential glioma biomarkers that may be of clinical significance.
Structural, optical and morphological characterization of Cu-doped α-Fe2O3 nanoparticles synthesized through co-precipitation technique

NASA Astrophysics Data System (ADS)

Lassoued, Abdelmajid; Lassoued, Mohamed Saber; Dkhil, Brahim; Gadri, Abdellatif; Ammar, Salah

2017-11-01

Pure and copper (Cu concentration varying from 2 to 8%) doped hematite (α-Fe2O3) nanocrystals were synthesized through co-precipitation method using simple equipment. X-ray Diffraction (XRD), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Fourier Transform Infra-Red (FT-IR), Raman spectroscopy, Differential Thermal Analysis (DTA), Thermo Gravimetric Analysis (TGA) and Ultraviolet-Visible (UV-Vis) techniques were used to characterize the synthesized samples. XRD measurements confirm that all the prepared nanocrystals consist only in nanocrystalline hematite phase. These results along with TEM and SEM show that the size of the nanoparticles decreases with Cu-doping down to 21 nm. FT-IR confirm the phase purity of the nanoparticles synthesized. The Raman spectroscopy was used not only to prove that we synthesized pure and Cu-doped hematite but also to identify their phonon modes. The TGA showed three mass losses, whereas DTA resulted in three endothermic peaks. The UV-Vis absorption measurements confirm that the decrease of particle size is accompanied by a decrease in the band gap value from 2.12 eV for pure α-Fe2O3 down to 1.91 eV for 8% Cu-doped α-Fe2O3. 8% Cu-doped hematite had the smallest size, the best crystallinity and the lowest band gap.
The relationship between structural stability and electrochemical performance of multi-element doped alpha nickel hydroxide

NASA Astrophysics Data System (ADS)

Miao, Chengcheng; Zhu, Yanjuan; Huang, Liangguo; Zhao, Tengqi

2015-01-01

The multi-element doped alpha nickel hydroxide has been prepared by supersonic co-precipitation method. Three kinds of samples A, B and C are prepared by chemically coprecipitating Ni/Al, Ni/Al/Mn and Ni/Al/Mn/Yb, respectively. Inductively coupled plasma atomic emission spectroscopy (ICP-AES), Particle size distribution (PSD) measurement, X-ray diffraction (XRD), scanning electron microscope (SEM) and Fourier transform infrared spectroscopy (FT-IR) are used to characterize the physical properties of the synthesized α-Ni(OH)2 samples, such as chemical composition, morphology, structural stability of the crystal. The results show that all samples are nano-sized materials and the interlayer spacing becomes larger and the structural stability becomes better with the increase of doped elements and doped ratio. The prepared alpha nickel hydroxide samples are added into micro-sized beta nickel hydroxide to form biphase electrode materials for Ni-MH battery. The electrochemical characterization of the biphase electrodes, including cyclic voltammetry (CV) and charge/discharge test, are also performed. The results demonstrate that the biphase electrode with sample C exhibits better electrochemical reversibility and cyclic stability, higher charge efficient and discharge potential, larger proton diffusion coefficient (5.81 × 10-12 cm2 s-1) and discharge capacity (309.0 mAh g-1). Hence, it indicates that all doped elements can produce the synergic effect and further improve the electrochemical properties of the alpha nickel hydroxide.
Synthesis of cristobalite from silica sands of Tuban and Tanah Laut

NASA Astrophysics Data System (ADS)

Nurbaiti, U.; Pratapa, S.

2018-03-01

Synthesis of SiO2 cristobalite powders has been successfully carried out by a coprecipitation method by making use of local silica sands from districts of Tuban and Tanah Laut, Indonesia. Cristobalite is a phase of SiO2 polymorphs which can be used as a composite filler, a coating material, a surface finishing media, and structural ceramics. In the first stage of the synthesis, the as-received sands were processed by a magnetic separation, grinding, and soaking with HCl to increase the purity of silica content. X-ray fluorescence (XRF) spectroscopy showed that the atomic content of Si (excluding oxygen) in both powders reached 95.3 and 97.4%. A coprecipitation process was then performed by dissolving the silica powders in a 7M NaOH solution followed by a titration with 2M HCl to achieve a normal pH and to form a gel. Furthermore, the silica gel is washed, dried and then calcined at a temperature of between 950-1200 °C with a variation of holding time for 1, 4 dan 10 hrs to produce white powders. X-ray diffraction (XRD) data analyses showed that the powder with calcination temperature of 1150 °C for 4 hrs exhibited the highest cristobalite content of up to 95wt%. Its scanning electron microscopy (SEM) image showed that its grain morphology was relatively homogeneous.
Synthesis and characterization of sulfate and dodecylbenzenesulfonate intercalated zinc iron layered double hydroxides by one-step coprecipitation route

NASA Astrophysics Data System (ADS)

Zhang, Hui; Wen, Xing; Wang, Yingxia

2007-05-01

Inorganic sulfate- and organic dodecylbenzenesulfonate (DBS)-intercalated zinc-iron layered double hydroxides (LDHs) materials were prepared by one-step coprecipitation method from a mixed salt solutions containing Zn(II), Fe(II) and Fe(III) salts. The as-prepared samples have been characterized by X-ray powder diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), low-temperature nitrogen adsorption, scanning electron microscopy (SEM), inductively coupled plasma emission spectroscopy (ICP), and Mössbauer spectroscopy (MS). The XRD analyses demonstrate the typical LDH-like layered structural characteristics of both products. The room temperature MS results reveal the characteristics of both the Fe(II) and Fe(III) species for SO 42--containing product, while only the Fe(III) characteristic for DBS-containing one. The combination characterization results and Rietveld analysis illustrate that the SO 42--containing product possesses the Green Rust two (GR2)-like crystal structure with an approximate chemical composition of [Zn 0.435·Fe II0.094·Fe III0.470·(OH) 2]·(SO 42-) 0.235·1.0H 2O, while the DBS-containing one exhibits the common LDH compound-like structure. The contact angle measurement indicates the evident hydrophobic properties of DBS-containing nanocomposite, compared with SO 42--containing product, due to the modification of the internal and external surface of LDHs by the organic hydrophobic chain of DBS.
Preparation of Sm-doped ceria (SDC) nanowires and tubes by gas-liquid co-precipitation at room temperature

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gu Lina; School of Chemistry and Chemical Engineering, Anhui University, 230039 Hefei; Meng Guangyao

Sm-doped cerium dioxide (SDC) with fcc structure was formed using a gas-liquid chemical co-precipitation process at room temperature. Morphology and structure of the as-prepared samples were characterized using TG, XRD, TEM, HRTEM and SAED techniques. Under our specific experimental conditions, two kinds of 1D nano-structures SDC have been mainly obtained. SDC nanowires are 0.3-1.2 {mu}m in lengths and 5-20 nm in diameters. SDC nanotubes have outer diameters in 10-40 nm with lengths up to 2 {mu}m. The as-prepared SDC shows very strong UV absorption ability and the maximum absorption peak redshifts compared with that of SDC nanoparticles.
An efficient method for purifying high quality RNA from wheat pistils.

PubMed

Manickavelu, A; Kambara, Kumiko; Mishina, Kohei; Koba, Takato

2007-02-15

Many methods are available for total RNA extraction from plants, except the floral organs like wheat pistils containing high levels of polysaccharides that bind/or co-precipitate with RNA. In this protocol, a simple and effective method for extracting total RNA from small and feathery wheat pistils has been developed. Lithium chloride (LiCl) and phenol:chloroform:isoamylalcohol (PCI) were employed and the samples were ground in microcentrifuge tube using plastic pestle. A jacket of liquid nitrogen and simplified procedures were applied to ensure thorough grinding of the pistils and to minimize the samples loss. These measures substantially increased the recovery of total RNA (approximately 50%) in the extraction process. Reliable differential display by cDNA-AFLP was successfully achieved with the total RNA after DNase treatment and reverse transcription. This method is also practicable for gene expression and gene regulation studies in floral parts of other plants.
Microwave acid digestion and preconcentration neutron activation analysis of biological and diet samples for iodine.

PubMed

Rao, R R; Chatt, A

1991-07-01

A simple preconcentration neutron activation analysis (PNAA) method has been developed for the determination of low levels of iodine in biological and nutritional materials. The method involves dissolution of the samples by microwave digestion in the presence of acids in closed Teflon bombs and preconcentration of total iodine, after reduction to iodide with hydrazine sulfate, by coprecipitation with bismuth sulfide. The effects of different factors such as acidity, time for complete precipitation, and concentrations of bismuth, sulfide, and diverse ions on the quantitative recovery of iodide have been studied. The absolute detection limit of the PNAA method is 5 ng of iodine. Precision of measurement, expressed in terms of relative standard deviation, is about 5% at 100 ppb and 10% at 20 ppb levels of iodine. The PNAA method has been applied to several biological reference materials and total diet samples.
Synthesis and characterization of nanocomposite polymer blend electrolyte thin films by spin-coating method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chapi, Sharanappa; Niranjana, M.; Devendrappa, H., E-mail: dehu2010@gmail.com

2016-05-23

Solid Polymer blend electrolytes based on Polyethylene oxide (PEO) and poly vinyl pyrrolidone (PVP) complexed with zinc oxide nanoparticles (ZnO NPs; Synthesized by Co-precipitation method) thin films have prepared at a different weight percent using the spin-coating method. The complexation of the NPs with the polymer blend was confirmed by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR). The variation in film morphology was examined by polarized optical micrographs (POMs). The thermal behavior of blends was investigated under non-isothermal conditions by differential thermal analyses (DTA). A single glass transition temperature for each blend was observed, which supports the existence ofmore » compatibility of such system. The obtained results represent that the ternary based thin films are prominent materials for battery and optoelectronic device applications.« less
Antibodies against toluene diisocyanate protein conjugates. Three methods of measurement.

PubMed

Patterson, R; Harris, K E; Zeiss, C R

1983-12-01

With the use of canine antisera against toluene diisocyanate (TDI)-dog serum albumin (DSA), techniques for measuring antibody against TDI-DSA were evaluated. The use of an ammonium sulfate precipitation assay showed suggestive evidence of antibody binding but high levels of TDI-DSA precipitation in the absence of antibody limit any usefulness of this technique. Double-antibody co-precipitation techniques will measure total antibody or Ig class antibody against 125I-TDI-DSA. These techniques are quantitative. The polystyrene tube radioimmunoassay is a highly sensitive method of detecting and quantitatively estimating IgG antibody. The enzyme linked immunosorbent assay is a rapidly adaptable method for the quantitative estimation of IgG, IgA, and IgM against TDI-homologous proteins. All these techniques were compared and results are demonstrated by using the same serum sample for analysis.
Synthesis, Properties and Application of Glucose Coated Fe3O4 Nanoparticles Prepared by Co-precipitation Method

NASA Astrophysics Data System (ADS)

Sari, Ayu Y.; Eko, A. S.; Candra, K.; Hasibuan, Denny P.; Ginting, M.; Sebayang, P.; Simamora, P.

2017-07-01

Synthesis of glucose coated Fe3O4 magnetic nanoparticles have been successfully prepared with co-precipitation method. Raw material of natural iron-sand was obtained from Buaya River, Deliserdang, Indonesia. The milled iron-sand was dissolved in HCl (37 mole %), and stirred in 300 rpm at 70°C for 90 minutes. Glucose was added to the filtered powder with varied content of 0.01, 0.02, and 0.03 mole, and precipitated by NH3 (25 mole%). After drying process, the final product subsequently was glucose coated magnetite (Fe3O4) nanoparticles. The characterizations performed were true density measurement, FTIR, VSM, XRD, BET, and adsorbent performance by AAS. The FTIR analysis showed that M-O (bending) with M=Fe (stretching vibration) with υ = 570.92 and 401.19 cm-1. While glucose coated well on nanoparticle Fe3O4, proved by functional groups C=O (stretching), M-O (stretching) and C-H (bending) with υ = 1404.17, 570.92, and 2368.58 cm-1, respectively. Single phase of magnetite (Fe3O4) structure was determined from XRD analysis with cubic spinel structure and lattice parameter of 8.396 Å. The optimum conditions, obtained on the Fe3O4 nanoparticles with 0.01 mole of glucose addition, which has true density value of 4.57 g/cm3, magnetic saturation, M s = 35,41 emu/g, coercivity, H cJ = 83.58 Oe, average particle size = 12.3 nm and surface area = 124.88 m2/g. This type magnetic nanoparticles of glucose-coated Fe3O4 was capable to adsorbed 93.78 % of ion Pb. Therefore, the glucose-coated Fe3O4 nanoparticle is a potential candidate to be used as heavy metal removal from wastewater.
Magnetic studies of CuFe{sub 2}O{sub 4} nanoparticles prepared by co-precipitation method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Subha, A.; Shalini, M. Govindaraj; Sahoo, Subasa C., E-mail: subasa@cukerala.ac.in

2016-05-06

Cu-ferrite nanoparticles were synthesized by co-precipitation method and were annealed at different temperatures ranging from 400 to l000°C in air for 4 hours. The as-prepared sample and the sample annealed at 400°C showed small peaks of cubic Cu-ferrite in X-ray diffraction studies. For the intermediate temperature 600°C, some additional peaks of α-Fe{sub 2}O{sub 3} were observed. As the annealing temperature increased further only tetragonal Cu-ferrite peaks were observed. In all the samples some traces of CuO was noted. Grain size was increased from 2lnm for the as prepared sample to 42nm for the sample annealed at l000°C. Spontaneous magnetization valuemore » was found to be very small for the as prepared sample and it was increased monotonically with the increase in annealing temperature. Maximum magnetization of 29.7emu/g was observed at 300K for the sample annealed at l000°C. The remanent magnetization was increased with the increase in annealing temperature up to 900°C and then decreased whereas for the coercivity a peak was observed for the sample annealed at 800°C. The highest coercivity of l402 Oe was observed at 300K for the sample annealed at 800°C. As the measurement temperature decreased from 300K to 60K, magnetization and coercivity values were increased. The observed magnetic behaviour may be understood on the basis of phase transformation, grain growth with the increase in annealing temperature and reduced thermal energy at low measurement temperature.« less
Ex-Situ Synthesis of Polyvinyl alcohol(PVA)-coated Fe3O4 Nanoparticles by Coprecipitation-Ultrasonication Method

NASA Astrophysics Data System (ADS)

Riva'i, Imam; Oktavia Wulandari, Ika; Sulistyarti, Hermin; Sabarudin, Akhmad

2018-01-01

In this study, the synthesis of Fe3O4 nanoparticles was done with surface modification using PVA with coprecipitation-ultrasonication method. Time variations and PVA concentrations were added to determine the effect on crystallite size and lattice parameters on the synthesis of Fe3O4-PVA nanoparticles. Fe3O4 characterization was done using X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FTIR) instruments. FTIR was employed to determine PVA coating on the surface of Fe3O4 nanoparticles. The crystallite size and lattice parameters were analyzed using XRD. From the FTIR data, it is known that the interaction between PVA and Fe3O4 nanoparticles is characterized by Fe-O-C group at 1100 cm-1 region which is characteristic of Fe3O4-PVA nanoparticles, C-H groups of PVA in the range of 2950 cm-1 wave number, C-C of PVA regions of wave number 1405 cm-1, Fe3O4 and Fe3O4-PVA samples are in the range of 565 cm-1. In addition, the variation of ultrasonication time and the addition of PVA concentration have an effect on the crystallite size change and the lattice parameter observed from the XRD data. The use of ultrasonication time will affect the size of the crystallite become smaller and the grating lattice parameters obtained are wider. The effect of addition of PVA showed that higher concentration of PVA resulted in smaller crystallite size and larger lattice parameters. These results indicated that ultrasonication time and addition of PVA concentration greatly affect the characteristics of nanoparticles.
Improved photocatalytic activities of CuxCo0.5-xNi0.5Fe2O4 nanoparticles through co-precipitation method in degrading methylene blue

NASA Astrophysics Data System (ADS)

Lassoued, Abdelmajid; Lassoued, Mohamed Saber; Dkhil, Brahim; Ammar, Salah; Gadri, Abdellatif

2018-07-01

We report the synthesis of CuxCo0.5-xNi0.5Fe2O4 with x = (0.1, 0.2, 0.3, 0.4) nanoparticles using the co-precipitation method in the presence of oleic acid as a surfactant and coating material. The X-ray diffraction analysis with Rietveld refinement technique confirmed the formation of cubic phase with Fd-3m space group of all the prepared nano-ferrites. The average crystallite size varies in the range of 21-38 nm with varying concentration of copper. The lattice parameter was found to decrease with increase in copper substitution. This may be attributed to larger ionic radius of cobalt as compared to that of copper. TEM and SEM analysis showed the monodispersion and cubic-like nanostructure. Two prominent stretching bands were observed in FT-IR spectra around 400-600 cm-1. These two bands confirmed the spinel structure of the prepared nanoparticles. Raman spectroscopy is used to verify that we have synthesized ferrite spinels and determines their phonon modes. The thermal decomposition of CuxCo0.5-xNi0.5Fe2O4 was investigated by TGA∖DTA. The optical study UV-visible is used to calculate the optical band gap energies. The products exhibited the attractive magnetic properties with high saturation magnetization, which were examined by a vibrating sample magnetometer (VSM). On the other part, the photocatalytic activity of our compounds was studied using methylene blue (MB) as model organic pollutants, where the results showed that an appropriate amount of copper (Cu2+) could greatly increase the amount of hydroxyl radicals generated by the ferrite nanoparticles, which were responsible for the obvious increase in the photocatalytic activity.
Study of structural phase transformation and hysteresis behavior of inverse-spinel α-ferrite nanoparticles synthesized by co-precipitation method

NASA Astrophysics Data System (ADS)

Dabagh, Shadab; Chaudhary, Kashif; Haider, Zuhaib; Ali, Jalil

2018-03-01

Substitution of cobalt (Co2+) ions in cobalt ferrite (CoFe2O4) with copper (Cu2+) and aluminum (Al3+) ions allows variations in their electric and magnetic properties which can be optimized for specific applications. In this article, synthesis of inverse-spinel Co1-xCuxFe2-xAlxO4 (0.0 ≤ x ≤ 0.8) nanoparticles by substituting Cu2+ and Al3+ ions in CoFe2O4 via co-precipitation method is reported. By controlling copper and aluminum (Cu-Al) substituent ratio, the magnetic moment and coercivity of synthesized cobalt ferrite nanoparticles is optimized. The role of substituents on the structure, particle size, morphology, and magnetic properties of nano-crystalline ferrite is investigated. The Co1-xCuxFe2-xAlxO4 (0.0 ≤ x≤ 0.8) nanoparticles with crystallite size in the range of 23.1-26.5 nm are observed, 26.5 nm for x = 0.0-23.1 nm for x = 0.8. The inverse-spinel structure of synthesized Co1-xCuxFe2-xAlxO4 (0.0 ≤ x ≤ 0.8) nano-particles is confirmed by characteristic vibrational bands at tetrahedral and octahedral sites using Fourier transform infrared spectroscopy. A decreases in coercive field and magnetic moment is observed as Cu-Al contents are increased (x = 0.0-0.8). The positive anisotropy of synthesized particles Co1-xCuxFe2-xAlxO4 (0.0 ≤ x ≤ 0.8) is obtained in the range 1.96 × 105 J/m3 for x = 0.0 to 0.29 × 105 J/m3 for x = 0.8.
Deproteinization assessment using isotopically enriched compounds to trace the coprecipitation of low-molecular-weight selenium species with proteins.

PubMed

Godin, Simon; Bouzas-Ramos, Diego; Fontagné-Dicharry, Stéphanie; Bouyssière, Brice; Bueno, Maïté

2017-08-01

Studies have shown that information related to the presence of low-molecular-weight metabolites is frequently lost after deproteinization of complex matrices, such as blood and plasma, during sample preparation. Therefore, the effect of several deproteinization reagents on low-molecular-weight selenium species has been compared by species-specific isotope labeling. Two isotopically enriched selenium tracers were used to mimic models of small inorganic anionic ( 77 Se-selenite) and organic zwitterionic ( 76 Se-selenomethionine) species. The results presented here show that the use of a methanol-acetonitrile-acetone (1:1:1 v/v/v) mixture provided approximately two times less tracer loss from plasma samples in comparison with the classic procedure using acetonitrile, which may not be optimal as it leads to important losses of low-molecular-weight selenium species. In addition, the possible interactions between selenium tracers and proteins were investigated, revealing that both coprecipitation phenomena and association with proteins were potentially responsible for selenite tracer losses during protein precipitation in blood samples. However, coprecipitation phenomena were found to be fully responsible for losses of both tracers observed in plasma samples and of the selenomethionine tracer in blood samples. This successfully applied strategy is anticipated to be useful for more extensive future studies in selenometabolomics. Copyright © 2017 Elsevier Inc. All rights reserved.
Treatment of low level radioactive liquid waste containing appreciable concentration of TBP degraded products.

PubMed

Valsala, T P; Sonavane, M S; Kore, S G; Sonar, N L; De, Vaishali; Raghavendra, Y; Chattopadyaya, S; Dani, U; Kulkarni, Y; Changrani, R D

2011-11-30

The acidic and alkaline low level radioactive liquid waste (LLW) generated during the concentration of high level radioactive liquid waste (HLW) prior to vitrification and ion exchange treatment of intermediate level radioactive liquid waste (ILW), respectively are decontaminated by chemical co-precipitation before discharge to the environment. LLW stream generated from the ion exchange treatment of ILW contained high concentrations of carbonates, tributyl phosphate (TBP) degraded products and problematic radio nuclides like (106)Ru and (99)Tc. Presence of TBP degraded products was interfering with the co-precipitation process. In view of this a modified chemical treatment scheme was formulated for the treatment of this waste stream. By mixing the acidic LLW and alkaline LLW, the carbonates in the alkaline LLW were destroyed and the TBP degraded products got separated as a layer at the top of the vessel. By making use of the modified co-precipitation process the effluent stream (1-2 μCi/L) became dischargeable to the environment after appropriate dilution. Based on the lab scale studies about 250 m(3) of LLW was treated in the plant. The higher activity of the TBP degraded products separated was due to short lived (90)Y isotope. The cement waste product prepared using the TBP degraded product was having good chemical durability and compressive strength. Copyright Â© 2011 Elsevier B.V. All rights reserved.
Structure and reactivity of ferrihydrite-soil organic carbon-calcium ternary complexes

NASA Astrophysics Data System (ADS)

Yang, Y.; Adhikari, D.; Sowers, T.; Stuckey, J.; Poulson, S.; Sparks, D. L.

2017-12-01

Complete understanding about the interactions between soil organic carbon (SOC) and minerals is important for predicting the stability of SOC and its response to climate change. Recent studies have shown the importance of calcium (Ca)-bearing minerals and iron (Fe) oxide in associating with and stabilizing SOC. In this study, we have investigated the formation and reactivity of ferrihydrite-SOC-Ca ternary complexes. During the co-precipitation of ferrihydrite with SOC in the presence of Ca2+, 60% of SOC can be co-precipitated with ferrihydrite at a C/Fe (molar ratio) of up to 10, whereas the Ca/Fe ratio was saturated at 0.2. Increasing amount of Ca2+ did not affect the co-precipitation of SOC with ferrihydrite or the lability of ferrihydrite-bound SOC. In addition, microbial reduction of ferrihydrite and reductive release of ferrihydrite-bound SOC were not influenced by the presence of Ca, but the pathway for Fe mineral transformation during the reduction was affected by Ca. In the meantime, Fe reduction selectively released carboxylic-enriched SOC. As a comparison, the presence of SOC increased the incorporation of Ca into the structure of ferrihydrite. Our results indicate the formation of ferrihydrite-SOC-Ca complexes, with organic carbon bridging the ferrihydrite and Ca. Such ternary complexes potentially play an important role in regulating the interactions between SOC and mineral phases in soil.
Co-precipitation of tobramycin into biomimetically coated orthopedic fixation pins employing submicron-thin seed layers of hydroxyapatite.

PubMed

Sörensen, Jan H; Lilja, Mirjam; Åstrand, Maria; Sörensen, Torben C; Procter, Philip; Strømme, Maria; Steckel, Hartwig

2014-01-01

The migration, loosening and cut-out of implants and nosocomial infections are current problems associated with implant surgery. New innovative strategies to overcome these issues are emphasized in today's research. The current work presents a novel strategy involving co-precipitation of tobramycin with biomimetic hydroxyapatite (HA) formation to produce implant coatings that control local drug delivery to prevent early bacterial colonization of the implant. A submicron- thin HA layer served as seed layer for the co-precipitation process and allowed for incorporation of tobramycin in the coating from a stock solution of antibiotic concentrations as high as 20 mg/ml. Concentrations from 0.5 to 20 mg/ml tobramycin and process temperatures of 37 °C and 60 °C were tested to assess the optimal parameters for a thin tobramycin- delivering HA coating on discs and orthopedic fixation pins. The morphology and thickness of the coating and the drug-release profile were evaluated via scanning electron microscopy and high performance liquid chromatography. The coatings delivered pharmaceutically relevant amounts of tobramycin over a period of 12 days. To the best of our knowledge, this is the longest release period ever observed for a fast-loaded biomimetic implant coating. The presented approach could form the foundation for development of combination device/antibiotic delivery vehicles tailored to meet well-defined clinical needs while combating infections and ensuring fast implant in-growth.
Synthesis of aqueous suspensions of magnetic nanoparticles with the co-precipitation of iron ions in the presence of aspartic acid

NASA Astrophysics Data System (ADS)

Pušnik, Klementina; Goršak, Tanja; Drofenik, Miha; Makovec, Darko

2016-09-01

There is increasing demand for the production of large quantities of aqueous suspensions of magnetic iron-oxide nanoparticles. Amino acids are one possible type of inexpensive, nontoxic, and biocompatible molecules that can be used as the surfactants for the preparation of stable suspensions. This preparation can be conducted in a simple, one-step process based on the co-precipitation of Fe3+/Fe2+ ions in the presence of the amino acid. However, the presence of this amino acid changes the mechanism of the magnetic nanoparticles' formation. In this investigation we analyzed the influence of aspartic amino acid (Asp) on the formation of magnetic iron-oxide nanoparticles during the co-precipitation. The process of the nanoparticles' formation was followed using a combination of TEM, x-ray diffractometry, magnetic measurements, in-situ FT-IR spectroscopy, and chemical analysis, and compared with the formation of nanoparticles without the Asp. The Asp forms a coordination complex with the Fe3+ ions, which impedes the formation of the intermediate iron oxyhydroxide phase and suppresses the growth of the final magnetic iron-oxide nanoparticles. Slower reaction kinetics can lead to the formation of nonmagnetic secondary phases. The aspartic-acid-absorbed nanoparticles can be dispersed to form relatively concentrated aqueous suspensions displaying a good colloidal stability at an increased pH.

The coprecipitation of Pu and other radionuclides with CaCO[sub 3

DOE Office of Scientific and Technical Information (OSTI.GOV)

Meece, D.E.; Benninger, L.K.

1993-04-01

The record of fallout plutonium concentrations in annual bands of corals is strikingly similar to the record of atmospheric deposition of [sup 90]Sr. This similarity implies that corals may incorporate Pu from seawater with a constant partition coefficient (constant discrimination). To investigate physicochemical aspects of Pu incorporation, the following have been coprecipitated with CaCO[sub 3] (calcite and aragonite): oxidized and reduced Pu; americium, thorium, and uranium as analogs to Pu oxidation states (III, IV, VI), respectively; and [sup 210]Pb as a particle-reactive nuclide which may be incorporated by corals with constant discrimination. Americium, thorium, and lead adsorb onto both calcitemore » and aragonite, with more than 99% of the recovered activity found associated with the solids. Uranium exhibits a behavior consistent with lattice substitution. Partition coefficients for U in aragonite range from 1.8 to 9.8 and vary inversely with pH and/or rate of precipitation. The partition coefficient for U in calcite is less than 0.2 and may be as low as 0.046. Reduced Pu sorbs with 3 to 4% remaining in solution. Oxidized Pu may both sorb and coprecipitate. The coral record for Pb and U results primarily from biological, rather than physicochemical, effects; it is likely that the PU coral record also reflects biological discrimination. 50 refs., 4 figs., 5 tabs.« less
Facile Synthesis of Radial-Like Macroporous Superparamagnetic Chitosan Spheres with In-Situ Co-Precipitation and Gelation of Ferro-Gels

PubMed Central

Yang, Chih-Hui; Wang, Chih-Yu; Huang, Keng-Shiang; Yeh, Chen-Sheng; Wang, Andrew H. -J.; Wang, Wei-Ting; Lin, Ming-Yu

2012-01-01

Macroporous chitosan spheres encapsulating superparamagnetic iron oxide nanoparticles were synthesized by a facile and effective one-step fabrication process. Ferro-gels containing ferrous cations, ferric cations and chitosan were dropped into a sodium hydroxide solution through a syringe pump. In addition, a sodium hydroxide solution was employed for both gelation (chitosan) and co-precipitation (ferrous cations and ferric cations) of the ferro-gels. The results showed that the in-situ co-precipitation of ferro-ions gave rise to a radial morphology with non-spheroid macro pores (large cavities) inside the chitosan spheres. The particle size of iron oxide can be adjusted from 2.5 nm to 5.4 nm by tuning the concentration of the sodium hydroxide solution. Using Fourier Transform Infrared Spectroscopy and X-ray diffraction spectra, the synthesized nanoparticles were illustrated as Fe3O4 nanoparticles. In addition, the prepared macroporous chitosan spheres presented a super-paramagnetic behaviour at room temperature with a saturation magnetization value as high as ca. 18 emu/g. The cytotoxicity was estimated using cell viability by incubating doses (0∼1000 µg/mL) of the macroporous chitosan spheres. The result showed good viability (above 80%) with alginate chitosan particles below 1000 µg/mL, indicating that macroporous chitosan spheres were potentially useful for biomedical applications in the future. PMID:23226207
One Ion to Rule Them All: Combined Antibacterial, Osteoinductive and Anticancer Properties of Selenite-Incorporated Hydroxyapatite

PubMed Central

Uskoković, Vuk; Iyer, Maheshwar Adiraj; Wu, Victoria M.

2017-01-01

Although hydroxyapatite (HAp) has been doped with dozens of different ions, the quest for an ion imparting a combination of properties conducive to bone healing is still ongoing. Because of its protean potency and the similarity in size and shape to the phosphate tetrahedron, selenite ion presents a natural ionic substitute in HAp. The incorporation of selenite into synthetic HAp using two different methods – co-precipitation and ion-exchange sorption - was studied for its effect on crystal properties and on a triad of biological responses: antibacterial, anticancer and osteoinductive. Co-precipitation yielded HAp with higher selenite contents than sorption and the stoichiometry of HAp richest in selenite was represented as Ca9.75(PO4)5.75(SeO3)0.25(OH)1.75. Crystallinity of HAp decreased in direct proportion with the amount of selenite incorporated. Because of their lower selenite content, HAp powders prepared by ion-exchange exhibited a consistently higher crystallinity compared to the co-precipitated ones. Annealing partially recovered the crystallinity, yet the difference in crystallinity between powders prepared by co-precipitation and by ion-exchange remained, suggesting that the amorphization is mainly due to structural incorporation of selenite, not its effect on the crystal growth kinetics. The addition of selenite changed the morphology of HAp nanoparticles from acicular to rounded and affected the crystal lattice parameters in different ways depending on whether the powders were annealed or not. As for the annealed powders, the incorporation of selenite contracted the lattice in both a and c crystallographic directions. In the agar diffusion assay, the effectiveness of HAp was more dependent on the presence or absence of selenite in it than on its concentration and was highest against E. coli and S. aureus, moderately high against S. enteritidis and ineffective against P. aeruginosa. In liquid inoculation tests, on the other hand, the antibacterial activity of HAp was directly proportional to the amount of selenite contained in it. The viability of K7M2 osteosarcoma cells decreased in direct proportion with the amount of selenite in HAp and was significantly different from the untreated control and from pure HAp at contents equal to or higher than 1.9 wt.%. In contrast, no reduction was observed in the viability of primary fibroblasts treated with HAp incorporating different amounts of selenite ions, suggesting their potentially selective anticancer activity: lethal for the cancer cells and harmless for the healthy cells. Finally, mRNA expression of bone gamma-carboxyglutamate protein (BGLAP3) was higher in differentiated MC3T3-E1 osteoblastic cells treated with selenite-incorporated HAp particles than in cells treated with pure HAp. The osteoinductive effect was due to an overall higher metabolic activity of cells treated with the particles and not due to increased proliferation. In such a way, a triad of antibacterial, osteoinductive and anticancer activities was attributed to selenite-incorporated HAp. PMID:28944060
Magnetic properties of Zn0.9(Mn0.05,Ni0.05)O nanoparticle: Experimental and theoretical investigation

NASA Astrophysics Data System (ADS)

Mounkachi, O.; Lakhal, M.; Labrim, H.; Hamedoun, M.; Benyoussef, A.; El Kenz, A.; Loulidi, M.; Bhihi, M.

2012-06-01

The crystalline and magnetic properties of 5% Mn and 5% Ni co-doped nanocrystalline ZnO particles, obtained by the co-precipitation method, are performed. X-ray diffraction data revealed that Zn0.90Mn0.05Ni0.05O crystallizes in the monophasic wurtzite structure. DC magnetization measurement showed that the samples are paramagnetic at room temperature. However, a large increase in the magnetization is observed below 50 K. This behavior, along with the negative value of Weiss constant obtained from the linear fit of magnetic susceptibility data below room temperature, indicates ferrimagnetic behavior. The ferrimagnetic properties observed at low temperature are explained and confirmed from ab-initio calculations using the Korringa-Kohn-Rostoker method combined with the coherent potential approximation.
Preparation of Nanocrystalline Powders of ZrO2, Stabilized by Y2O3 Dobs for Ceramics

NASA Astrophysics Data System (ADS)

Petrunin, V. F.; Korovin, S. A.

The purpose of this study was to develop a synthesis conditions and produce samples of nanocrystalline zirconia powder in a high-temperature phase state. To increase the stability of this state at room temperature, Y2O3 was used as a dop in the two-stages chemical method including coprecipitation mixture of the corresponding hydroxides and air drying. To reduce agglomeration of nanoparticles during heat treatment of precursors the microwave oven instead of a muffle was used. Different characterisation methods have been used to determine that the obtained powders are nano-scale corresponds to a high-temperature tetragonal phase of ZrO2. It is shown that such nanocrystalline powders may be used to produce highly-dense nanoceramics.
Functional Iron Oxide-Silver Hetero-Nanocomposites: Controlled Synthesis and Antibacterial Activity

NASA Astrophysics Data System (ADS)

Trang, Vu Thi; Tam, Le Thi; Van Quy, Nguyen; Huy, Tran Quang; Thuy, Nguyen Thanh; Tri, Doan Quang; Cuong, Nguyen Duy; Tuan, Pham Anh; Van Tuan, Hoang; Le, Anh-Tuan; Phan, Vu Ngoc

2017-06-01

Iron oxide-silver nanocomposites are of great interest for their antibacterial and antifungal activities. We report a two-step synthesis of functional magnetic hetero-nanocomposites of iron oxide nanoparticles and silver nanoparticles (Fe3O4-Ag). Iron oxide nanoparticles were prepared first by a co-precipitation method followed by the deposition of silver nanoparticles via a hydrothermal route. The prepared Fe3O4-Ag hetero-nanocomposites were characterized by x-ray diffraction, transmission electron microscopy, high resolution transmission electron microscopy and vibrating sample magnetometry. Their antibacterial activities were investigated by using paper-disc diffusion and direct-drop diffusion methods. The results indicate that the Fe3O4-Ag hetero-nanocomposites exhibit excellent antibacterial activities against two Gram-negative bacterial strains ( Salmonella enteritidis and Klebsiella pneumoniae).
Optical and electrical studies of cerium mixed oxides

NASA Astrophysics Data System (ADS)

Sherly, T. R.; Raveendran, R.

2014-10-01

The fast development in nanotechnology makes enthusiastic interest in developing nanomaterials having tailor made properties. Cerium mixed oxide materials have received great attention due to their UV absorption property, high reactivity, stability at high temperature, good electrical property etc and these materials find wide applications in solid oxide fuel cells, solar control films, cosmetics, display units, gas sensors etc. In this study cerium mixed oxide compounds were prepared by co-precipitation method. All the samples were doped with Zn (II) and Fe (II). Preliminary characterizations such as XRD, SEM / EDS, TEM were done. UV - Vis, Diffuse reflectance, PL, FT-IR, Raman and ac conductivity studies of the samples were performed.
Free-standing ultrathin CoMn2O4 nanosheets anchored on reduced graphene oxide for high-performance supercapacitors.

PubMed

Gao, Guoxin; Lu, Shiyao; Xiang, Yang; Dong, Bitao; Yan, Wei; Ding, Shujiang

2015-11-21

Ultrathin CoMn2O4 nanosheets supported on reduced graphene oxide (rGO) are successfully synthesized through a simple co-precipitation method with a post-annealing treatment. With the assistance of citrate, the free-standing CoMn2O4 ultrathin nanosheets can form porous overlays on both sides of the rGO sheets. Such a novel hybrid nanostructure can effectively promote charge transport and accommodate volume variation upon prolonged charge/discharge cycling. When evaluated as a promising electrode for supercapacitors in a 6 M KOH solution electrolyte, the hybrid nanocomposites demonstrate highly enhanced capacitance and excellent cycling stability.
Development of space stable thermal control coatings for use on large space vehicles. [effects of ultraviolet radiation

NASA Technical Reports Server (NTRS)

Gilligan, J. E.; Harada, Y.

1974-01-01

The development of a large scale manufacturing method for the production of a stable zinc orthotitanate pigment is discussed. Major emphasis was placed on the evaluation of ultraviolet radiation stability tests of pigments derived from coprecipitated and individually precipitated oxalates. Emphasis was also placed on an investigation of the conditions (time and temperature) leading to high reflectance and high optical stability. Paints were formulated in OI-650 and in OI-650G vehicles from pigments which were prepared at various temperatures. Analyses of ultraviolet irradiation test data were conducted regarding optimum pigment preparation parameters and treatment conditions.
Effect of solvent on the synthesis of SnO{sub 2} nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Virender; Singh, Karamjit; Singh, Kulwinder

Tin oxide (SnO{sub 2}) nanoparticles have been synthesized by co-precipitation method. The synthesized nanoparticles have been characterized by X-ray diffraction (XRD) and Ultraviolet-Visible spectroscopy (UV-VIS). XRD analysis confirmed the formation of single phase of SnO{sub 2} nanoparticles. It has been found that solvents played important role in controlling the crystallite size of SnO{sub 2} nanoparticles. The XRD analysis showed well crystallized tetragonal SnO{sub 2} nanoparticles. The crystallite size of SnO{sub 2} nanoparticles varies with the solvent. Tauc plot showed that optical band gap was also tailored by controlling the solvent during synthesis.
Synthesis of optically transparent ceramic of CaF2 doped with Mn and Ce for thermoluminescent dosimetry

NASA Astrophysics Data System (ADS)

Sen, Shashwati; Singh, S. G.; Patra, G. D.; Shinde, S.; Bhattacharya, S.; Gadkari, S. C.

2012-06-01

Nano-particles of CaF2: Mn were synthesized by a co-precipitation method. Optically transparent ceramics were obtained by vacuum hot-pressing at 1000°C under 20 MPa pressure for 2 h. The duration of pressure and dehydration of the initial powder was found important to achieve the transparency. 50% transparency was observed for a polished disc of 1 mm thickness. SEM micrographs revealed the absence of voids in hot pressed samples. These samples were found to be highly sensitive and linear for TLD and can measure doses from mGy to kGy.
Applications of Ferro-Nanofluid on a Micro-Transformer

PubMed Central

Tsai, Tsung-Han; Kuo, Long-Sheng; Chen, Ping-Hei; Lee, Da-sheng; Yang, Chin-Ting

2010-01-01

An on-chip transformer with a ferrofluid magnetic core has been developed and tested. The transformer consists of solenoid-type coil and a magnetic core of ferrofluid, with the former fabricated by MEMS technology and the latter by a chemical co-precipitation method. The performance of the MEMS transformer with a ferrofluid magnetic core was measured and simulated with frequencies ranging from 100 kHz to 100 MHz. Experimental results reveal that the presence of the ferrofluid increases the inductance of coils and the coupling coefficient of transformer; however, it also increases the resistance owing to the lag between the external magnetic field and the magnetization of the material. PMID:22163647
Applications of ferro-nanofluid on a micro-transformer.

PubMed

Tsai, Tsung-Han; Kuo, Long-Sheng; Chen, Ping-Hei; Lee, Da-Sheng; Yang, Chin-Ting

2010-01-01

An on-chip transformer with a ferrofluid magnetic core has been developed and tested. The transformer consists of solenoid-type coil and a magnetic core of ferrofluid, with the former fabricated by MEMS technology and the latter by a chemical co-precipitation method. The performance of the MEMS transformer with a ferrofluid magnetic core was measured and simulated with frequencies ranging from 100 kHz to 100 MHz. Experimental results reveal that the presence of the ferrofluid increases the inductance of coils and the coupling coefficient of transformer; however, it also increases the resistance owing to the lag between the external magnetic field and the magnetization of the material.
Effect of sintering on structure and magnetic properties of Mn-doped Zn ferrite

NASA Astrophysics Data System (ADS)

Farheen, Atiya; Singh, Rajender

2018-05-01

The Mn-doped zinc ferrites, MnxZn1-xFe2O4 (x= 0 and 0.1) were prepared using co-precipitation method. The as-prepared samples were sintered at different temperatures. The x-ray diffraction pattern for all the samples confirms single phase spinel structure with Fd-3m space group. The lattice parameters have been estimated using Rietveld fitting. The magnetic moment is found to increase with Mn-doping. The magnetization increases as the sintering temperature increases up to 1200°C. The as-prepared samples are super paramagnetic, while the sintered samples are ferrimagnetic in nature.
Photoluminescence studies on Cd(1-x)Zn(x)S:Mn2+ nanocrystals.

PubMed

Sethi, Ruchi; Kumar, Lokendra; Pandey, A C

2009-09-01

Highly monodispersed, undoped and doped with Mn2+, binary and ternary (CdS, ZnS, Cd(1-x)Zn(x)S) compound semiconductor nanocrystals have been synthesized by co-precipitation method using citric acid as a stabilizer. As prepared sample are characterized by X-ray diffraction, Small angle X-ray scattering, Transmission electron microscope, Optical absorption and Photoluminescence spectroscopy, for their optical and structural properties. X-ray diffraction, Small angle X-ray scattering and Transmission electron microscope results confirm the preparation of monodispersed nanocrystals. Photoluminescence studies show a significant blue shift in the wavelength with an increasing concentration of Zn in alloy nanocrystals.
Synthesis and characterization of rod like C doped ZnO nanoparticles with enhanced photocatalytic activities

NASA Astrophysics Data System (ADS)

Labhane, P. K.; Sapkal, B. M.; Sonawane, G. H.

2018-05-01

Carbon (C) doped ZnO rod like nanoparticles were prepared by simple co-precipitation method. The effect of C doping on ZnO has been evaluated by using XRD, Williamson-Hall Plot, FESEM and EDX data. UV light assisted photocatalytic activities of prepared samples were evaluated spectrophotometrically by the degradation of methylene blue (MB). C doped ZnO shows excellent catalytic efficiency compared to pure ZnO, degrading MB completely within 100 min under UV light. Photocatalysis follows the first order kinetics law and the calculated apparent reaction kinetics rate constant suggest the better activity of C-ZnO.
Doped sesquioxide ceramic for eye-safe solid state laser materials

NASA Astrophysics Data System (ADS)

Kim, Woohong; Baker, Colin; Florea, Catalin; Frantz, Jesse; Villalobos, Guillermo; Shaw, Brandon; Bowman, Steve; O'Connor, Shawn; Sadowski, Bryan; Hunt, Michael; Aggalwar, Ishwar; Sanghera, Jasbinder

2013-03-01

In this paper, we present our recent results in the development of Ho3+ doped sesquioxides for eye-safe solid state lasers. We have synthesized optical quality Lu2O3 nanopowders doped with concentrations of 0.1, 1.0, 2.0, and 5% Ho3+. The powders were synthesized by a co-precipitation method beginning with nitrates of holmium and lutetium. The nanopowders were hot pressed into optical quality ceramic discs. The optical transmission of the ceramic discs is excellent, nearly approaching the theoretical limit. The optical, spectral and morphological properties as well as the lasing performance from highly transparent ceramics are presented.
Inclusion compound of vitamin B6 in β-CD. Physico-chemical and structural investigations

NASA Astrophysics Data System (ADS)

Borodi, Gheorghe; Kacso, Irina; Farcaş, Sorin I.; Bratu, Ioan

2009-08-01

Structural and physico-chemical characterization of supramolecular assembly of vitamin B6 with β-cyclodextrin (β-CD) prepared by different methods (kneading, co-precipitation and freeze-drying) has been performed by using several spectroscopic techniques (FTIR, 1H NMR, UV-Vis), powder X-ray diffraction and DSC in order to evidence the inclusion compound formation. An analysis of the chemical shifts observed in the 1H-NMR spectra and of the vibrational frequency shifts led to the tentative conclusion that the vitamin B6 probably enters the cyclodextrin torus when forming the β-CD-vitamin B6 inclusion complex.
Synthesis and characterization of lanthanum doped zinc oxide nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Vinod; Sonia,; Suman,

La doped ZnO (Zn{sub 1-x}La{sub x}O, x = 0, 3, 6 and 9) were prepared via chemical co-precipitation method using Zinc Acetate, Lanthanum Acetate and Sodium Hydroxide at 50°C. Hydrate nanoparticles were annealed in air at 300°C for 3 hours. The synthesized samples have been characterized by powder X-ray diffraction and UV–Visible spectrophotometer. The XRD measurement revealsthat the prepared nanoparticles have different microstructure without changing a hexagonal wurtzite structure. The result shows the change in nanoparticles size with the increment of lanthanum concentration for lower concentration for x = 0 to 6 and decreases at x = 9.
Structural and dielectric studies of Ce doped BaSnO3 perovskite nanostructures

NASA Astrophysics Data System (ADS)

Angel, S. Lilly; Deepa, K.; Rajamanickam, N.; Jayakumar, K.; Ramachandran, K.

2018-04-01

Undoped and Cerium (Ce) doped BaSnO3(BSO) nanostructures were synthesized by co-precipitation method. The cubic structure and perovskite phase were confirmed by X-ray diffraction (XRD). The crystallite size of BSO is 41nm and when Ce ion concentration is increased, the crystallite sizesdecreased. The nanocube, nanocuboids and nanorods are observed from SEM analysis. The purity of the undoped and doped samples are confirmed by EDS spectrum. For larger defects, wide band gap was obtained from UV-Vis and PL spectrum. The dielectric constants are increased at low frequencies when Ce impurities are introduced in the BSO matrix at Sn site.

Nanocrystalline NiNd0.01Fe1.99O4 as a gas sensor

NASA Astrophysics Data System (ADS)

Shinde, Tukaram J.; Gadkari, Ashok B.; Jadhav, Sarjerao R.; Kumar, Surender; Dalawai, Sanjeev P.; Vasambekar, Pramod N.

2015-06-01

Nanocrystalline NiNd0.01Fe1.99O4 has been synthesized by oxalate co-precipitation method and was characterized by X-ray diffraction technique. X-ray diffraction analysis confirms the formation of single phase cubic spinel structure. Crystallite size of the ferrite lies in the nano-particle range. The gas sensing properties of nanocrystalline ferrite were studied for gases like Cl2, LPG and C2H5OH. It was observed that NiNd0.01Fe1.99O4 is more sensitive towards chlorine followed by LPG at an operating temperature 277 °C compared to ethanol.
Synthesis, characterizations and catalytic activities of CoFe2O4 nanoparticles

NASA Astrophysics Data System (ADS)

Verma, Divya; Sharma, Vikash; Parmar, Sarita; Okram, Gunadhor Singh; Jain, Shubha

2018-05-01

We report the synthesis of CoFe2O4 nanoparticles (NPs) through a novel one-step coprecipitation method. These NPs were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), Fourier transform infrared (FTIR), and Raman spectroscopy. These nano ferrites were successfully used for the synthesis of 3, 4-dihydropyrimidin-2(1H)-ones and thiones. They can be easily recovered by simple filtration and their catalytic activity remains nearly unaltered even after 4 consecutive cycles, making them ecofriendly and widely applicable due to their efficiency, ease of handling, and cost effectiveness.
Structure, optical and phonon properties of bulk and nanocrystalline Al2-xScx(WO4)3 solid solutions doped with Cr3+

NASA Astrophysics Data System (ADS)

Mączka, M.; Hermanowicz, K.; Pietraszko, A.; Yordanova, A.; Koseva, I.

2014-01-01

Pure and Cr3+ doped nanosized Al2-xScx(WO4)3 solid solutions were prepared by co-precipitation method as well as Al2-xScx(WO4)3 single crystals were grown by high-temperature flux method. The obtained samples were characterized by X-ray, Raman, IR, absorption and luminescence methods. Single crystal X-ray diffraction showed that AlSc(WO4)3 is orthorhombic at room temperature with space group Pnca and trivalent cations are statistically distributed. Raman and IR studies showed that Al2-xScx(WO4)3 solid solutions show "two mode" behavior. They also showed that vibrational properties of nanosized samples have been weakly modified in comparison with the bulk materials. The luminescence and absorption spectra revealed that chromium ions occupy two sites of weak and strong crystal field strength.
A green approach to the synthesis of novel ``Desert rose stone''-like nanobiocatalytic system with excellent enzyme activity and stability

NASA Astrophysics Data System (ADS)

Wang, Min; Bao, Wen-Jing; Wang, Jiong; Wang, Kang; Xu, Jing-Juan; Chen, Hong-Yuan; Xia, Xing-Hua

2014-10-01

3D hierarchical layer double hydroxides (LDHs) have attracted extensive interest due to their unique electronic and catalytic properties. Unfortunately, the existing preparation methods require high temperature or toxic organic compounds, which limits the applications of the 3D hierarchical LDHs in biocatalysis and biomedicine. Herein, we present a green strategy to synthesize ``Desert Rose Stone''-like Mg-Al-CO3 LDH nanoflowers in situ deposited on aluminum substrates via a coprecipitation method using atmospheric carbon dioxide. Using this method, we construct a novel ``Desert Rose Stone''-like nanobiocatalytic system by using HRP as the model enzyme. Compared with the free HRP, the HRP/Mg-Al-LDH nanobiocatalytic system exhibits higher catalytic activity and stability. A smaller apparent Michaelis-Menten constant (0.16 mM) of this system suggests that the encapsulated HRP shows higher affinity towards H2O2.
Emerging investigator series: As( v ) in magnetite: incorporation and redistribution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huhmann, Brittany L.; Neumann, Anke; Boyanov, Maxim I.

2017-01-01

As coprecipitated with magnetite remained incorporated over time whereas sorbed As was redistributed and became increasingly incorporated into magnetite, both the absence and presence of aqueous Fe(ii).
Enhanced UVB emission and analysis of chemical states of Ca5(PO4)3OH:Gd3+,Pr3+ phosphor prepared by co-precipitation

NASA Astrophysics Data System (ADS)

Mokoena, P. P.; Nagpure, I. M.; Kumar, Vinay; Kroon, R. E.; Olivier, E. J.; Neethling, J. H.; Swart, H. C.; Ntwaeaborwa, O. M.

2014-08-01

Hydroxyapatite (Ca5(PO4)3OH) is a well-known bioceramic material used in medical applications because of its ability to form direct chemical bonds with living tissues. This mineral is currently used as a host for rare-earth ions (e.g. Gd3+, Pr3+, Tb3+, etc.) to prepare phosphors that can be used in light emitting devices of different types. In this study Ca5(PO4)3OH:Gd3+,Pr3+ phosphors were prepared by the co-precipitation method and were characterised by x-ray diffraction, x-ray photoelectron spectroscopy, scanning electron microscopy, high resolution transmission electron microscopy, energy dispersive x-ray spectroscopy and photoluminescence spectroscopy. The x-ray diffraction pattern was consistent with the hexagonal phase of Ca5(PO4)3OH referenced in JCPDS card number 73-0293. The x-ray photoelectron spectroscopy data indicated that Ca2+ occupied two different lattice sites, referred to as Ca1 and Ca2. The photoluminescence data exhibited a narrowband emission located at 313 nm, which is associated with the 6P7/2→8S7/2 transition of the Gd3+ ion. This emission is classified as ultraviolet B and it is suitable for use in phototherapy lamps to treat various skin diseases. The photoluminescence intensity of the 313 nm emission was enhanced considerably by Pr3+ co-doping.
DOE Office of Scientific and Technical Information (OSTI.GOV)

Pratapa, S.; Susanti, L.; Insany, Y. A. S.

Simple coprecipitation method has been used to produce nanoparticles of MgO (magnesia), MgO{center_dot}Al{sub 2}O{sub 3}(spinel), Y{sub 2}O{sub 3}(yttria) and Fe{sub 3}O{sub 4}(ferrite). The raw materials were, in respective, magnesium powder, magnesium and aluminium powders, ytrria powder, and natural sand. The coprecipitation included the use of suitable acid and base to dissolve the powders or sand and to produce precipitates, as well as the use of water to wash and purify the precipitates, and drying at relatively low temperatures, namely lower than 100 deg. C, followed by heating at 450 deg. C, 750 deg. C, 600 deg. C and 200 deg.more » C to produce magnesia, spinel, yttria and ferrite nanopowders, respectively. X-ray diffractometry was used to characterise the purity and nanocrystallinity of the final powders. It was found qualitatively that the powders were of high purity. Further line-broadening analysis using single-line and Rietveld-based softwares was performed to reveal the nanocrystallinity of the powders. Different line breadth values were found for the powders, indicating different crystallite sizes. It was also found that, particularly for spinel and yttria, the diffraction peaks exhibited 'longer' tails, indicating broader crystallite size distribution. The average crystallite size for the powders ranged from 3 to 70 nm. The results could then be used as 'fingerprints' for nanocrystallinity using x-ray diffractometry. The XRD crystallite sizes for yttria and ferrite nanocrystals are in fair agreement with their counterparts from electron microscopy observation.« less
Mesoporous composite nickel cobalt oxide/graphene oxide synthesized via a template-assistant co-precipitation route as electrode material for supercapacitors

NASA Astrophysics Data System (ADS)

Xu, Yanjie; Wang, Lincai; Cao, Peiqi; Cai, Chuanlin; Fu, Yanbao; Ma, Xiaohua

2016-02-01

A simple co-precipitation method utilizing SDS (sodium dodecyl sulfate) as template and ammonia as precipitant is successfully employed to synthesize nickel cobalt oxide/graphene oxide (NiCo2O4/GO) composite. The as-prepared composite (NCG-10) exhibits a high capacitance of 1211.25 F g-1, 687 F g-1 at the current density of 1 A g-1, 10 A g-1 and good cycling ability which renders NCG-10 as promising electrode material for supercapacitors. An asymmetric supercapacitor (ASC) (full button cell) has been constructed with NCG-10 as positive electrode and lab-made reduced graphene oxide (rGO) as negative electrode. The fabricated NCG-10//rGO with an extended stable operational voltage of 1.6 V can deliver a high specific capacitance of 144.45 F g-1 at a current density of 1 A g-1. The as-prepared NCG-10//rGO demonstrates remarkable energy density (51.36 W h kg-1 at 1 A g-1), high power density (50 kW kg-1 at 20 A g-1). The retention of capacitance is 88.6% at the current density of 8 A g-1 after 2000 cycles. The enhanced capacitive performance can be attributed to the improved specific surface area and 3D open area of NCG-10 generated by the pores and channels with the substantial function of SDS.
Hybrid nanomaterials based on gum Arabic and magnetite for hyperthermia treatments.

PubMed

Horst, M Fernanda; Coral, Diego F; Fernández van Raap, Marcela B; Alvarez, Mariana; Lassalle, Verónica

2017-05-01

In this study, one-step co-precipitation method was conveniently adapted to obtain novel nanomaterials based on Gum Arabic and magnetite. Two synthesis procedures were evaluated: one employing the solid biopolymer in the co-precipitation media; a second using an aqueous solution of the polysaccharide. An exhaustive characterization of both formulations was performed using several specific techniques. The obtained data confirmed the successful incorporation of the gum Arabic on the magnetic core. Values of hydrodynamic diameters, measured by dynamic light scattering, in aqueous dispersions were about 70-80nm, while sizes lower than 20nm were registered by TEM microscopy. Surface charge of gum Arabic coated magnetic nanoparticles was significantly different from the corresponding to raw materials (magnetite and GA). This fact confirmed the formation of hybrid nanosystems with novel and specific properties. The potential utility of these materials was tested regarding to magnetic hyperthermia therapy under radiofrequency fields. Magnetocalorimetric measurements were performed in a wide range of field amplitude and frequency. Specific absorption rate of 218W/gFe was determined at field frequency of 260kHz and amplitude of 52kA/m. These results demonstrate their viability to be applied in tumor ablation treatments. Using the linear response theory and restricting field parameters to the accepted biomedical window, maximum useful value of 74w/gFe is predicted at 417kHz and 12kA/m. Copyright © 2016 Elsevier B.V. All rights reserved.
Structural, vibrational and luminescence properties of the (1−x)CaWO{sub 4}−xCdWO{sub 4} system

DOE Office of Scientific and Technical Information (OSTI.GOV)

Taoufyq, A.; Laboratoire Matériaux et Environnement LME, Faculté des Sciences, Université Ibn Zohr, BP 8106, Cité Dakhla, Agadir, Maroc; CEA/DEN, Département d’Études des Réacteurs, Laboratoire Dosimétrie Capteurs Instrumentation, CEA Cadarache, 13108, Saint-Paul-lez-Durance

2014-11-15

In the present work, we investigate the structural, microstructural, vibrational and luminescence properties of the system (1−x)CaWO{sub 4}−xCdWO{sub 4} with x ranging between 0 and 1. Polycrystalline samples were elaborated using a coprecipitation technique followed by thermal treatment at 1000 °C. The samples were then characterized using X-ray diffraction, scanning electron microscopy, Raman spectroscopy and luminescence analyses. X-ray diffraction profile analyses using Rietveld method showed that two kinds of solid solutions Ca{sub 1−x}Cd{sub x}WO{sub 4} having scheelite and wolframite structures, with respectively tetragonal and monoclinic crystal cells, were observed, with a biphasic system for compositions x=0.6 and 0.7. The scanningmore » electron microscopy experiments showed a complex evolution of morphologies and crystallite sizes as x increased. The vibration modes of Raman spectra were characteristic of composition-dependent disordered solid solutions with decreasing wavenumbers as x increased. Luminescence experiments were performed under UV-laser light irradiation. The energies of emission bands increased linearly with cadmium composition x. The integrated intensity of luminescence reached a maximum value for the substituted wolframite phase with composition x=0.8. - Graphical abstract: Luminescence on UV excitation (364.5 nm) of (1−x)CaWO{sub 4−x}CdWO{sub 4} system, elaborated from coprecipitation technique at 1000 °C, with 0« less
Recovery of nickel and cobalt as MHP from limonitic ore leaching solution: Kinetics analysis and precipitate characterization

NASA Astrophysics Data System (ADS)

Safitri, Nina; Mubarok, M. Zaki; Winarko, Ronny; Tanlega, Zela

2018-05-01

In the present study, precipitation of nickel and cobalt as mixed hydroxide precipitate (MHP) from pregnant leach solution of nickel limonite ore from Soroako after iron removal stage was carried out. A series of MHP precipitation experiments was conducted by using MgO slurry as neutralizing agent and the effects of pH, temperature, duration of precipitation and the addition of MHP seed on the precipitation behavior of nickel, cobalt, as well as iron and manganese was studied. Characterization of MHP product was performed by particle size analyzer (PSA) as well as X-Ray Fluorescence (XRF), X-Ray Diffractometer (XRD) and Scanning Electron Microscope (SEM) analyses. Kinetics analysis was made by using differential-integral method for the rate of homogenous reaction. Precipitation at pH 7, temperature 50°C for 30 minute, without seed addition resulted in nickel and cobalt recoveries of 82.8% and 92%, respectively with co-precipitated iron and manganese of 70% and 24.2%, respectively. The seed addition increases nickel and cobalt precipitations significantly to 99.9% and 99.1%, respectively. However, the addition of seed into led to a significant increase of manganese co-precipitation from 24.2% without seed addition to 39.5% at the addition of 1 g seed per 200 mL of PLS. Kinetics analysis revealed that Ni precipitation to form MHP follows the second-order reaction kinetics with activation energy of 94.6 kJ/mol.
21 CFR 82.3 - Definitions.

Code of Federal Regulations, 2013 CFR

2013-04-01

... hydroxide. (h) The term blanc fixe means a suspension in water of precipitated barium sulfate. (i) The term gloss white means a suspension in water of co-precipitated aluminum hydroxide and barium sulfate. (j...
21 CFR 82.3 - Definitions.

Code of Federal Regulations, 2012 CFR

2012-04-01

... hydroxide. (h) The term blanc fixe means a suspension in water of precipitated barium sulfate. (i) The term gloss white means a suspension in water of co-precipitated aluminum hydroxide and barium sulfate. (j...
21 CFR 82.3 - Definitions.

Code of Federal Regulations, 2014 CFR

2014-04-01

... hydroxide. (h) The term blanc fixe means a suspension in water of precipitated barium sulfate. (i) The term gloss white means a suspension in water of co-precipitated aluminum hydroxide and barium sulfate. (j...
Development of the Ion Exchange-Gravimetric Method for Sodium in Serum as a Definitive Method

PubMed Central

Moody, John R.; Vetter, Thomas W.

1996-01-01

An ion exchange-gravimetric method, previously developed as a National Committee for Clinical Laboratory Standards (NCCLS) reference method for the determination of sodium in human serum, has been re-evaluated and improved. Sources of analytical error in this method have been examined more critically and the overall uncertainties decreased. Additionally, greater accuracy and repeatability have been achieved by the application of this definitive method to a sodium chloride reference material. In this method sodium in serum is ion-exchanged, selectively eluted and converted to a weighable precipitate as Na2SO4. Traces of sodium eluting before or after the main fraction, and precipitate contaminants are determined instrumentally. Co-precipitating contaminants contribute less than 0.1 % while the analyte lost to other eluted ion-exchange fractions contributes less than 0.02 % to the total precipitate mass. With improvements, the relative expanded uncertainty (k = 2) of the method, as applied to serum, is 0.3 % to 0.4 % and is less than 0.1 % when applied to a sodium chloride reference material. PMID:27805122
Thermodynamic stability of CoOOH and its coprecipitation with manganese

USGS Publications Warehouse

Hem, J.D.; Roberson, C.E.; Lind, Carol J.

1985-01-01

A precipitate of cobalt oxyhydroxides formed by bubbling oxygen through a dilute solution of Co(NO3)2 held at pH 9.0 and 25??C was aged for 23 months in contact with the original solution, with access to atmospheric oxygen. Co3O4 and CoOOH were identified in the precipitate by X-ray diffraction. Chemical equilibria involving these solids were evaluated by measurements of solution pH and Co2+ activities and by redox potential measurements and gave a ??GcoOOH0 of -92.3 ?? 0.5 kcal/mole. This value and other thermodynamic data show relative feasibility of hypothetical reaction steps and changes in reaction paths during automated coprecipitation titrations and subsequent aging of a precipitate that finally contained ??MnOOH, MnO2 (birnessite) and CoOOH. ?? 1985.
Oxidation of aqueous EDTA and associated organics and coprecipitation of inorganics by ambient iron-mediated aeration.

PubMed

Englehardt, James D; Meeroff, Daniel E; Echegoyen, Luis; Deng, Yang; Raymo, Françisco M; Shibata, Tomoyuki

2007-01-01

Cationic metal and radionuclide contaminants can be extracted from soils to groundwater with sequestering agents such as EDTA. However, EDTA must then be removed fromthe groundwater, by advanced oxidation or specialized biological treatment. In this work, aqueous individual metal-EDTA solutions were aerated with steel wool for 25 h, at ambient pH, temperature, and pressure. Removal of approximately 99% of EDTA (0.09-1.78 mM); glyoxylic acid (0.153 mM); chelated Cd2+ (0.94 and 0.0952 mM), Pb2+ (0.0502 mM), and Hg2+ (0.0419 mM); and free chromate and vanadate was shown. EDTA was oxidized to glyoxylic acid and formaldehyde, and metals/metalloids were coprecipitated together with iron oxyhydroxide floc. Free arsenite and arsenate were each removed at 99.97%. Free Sr2+, and chelated Ni2+ were removed at 92% and 63%, respectively. Similar removals were obtained from mixtures, including 99.996+/-0.004% removal of total arsenic (95% confidence). Traces of iminodiacetic acid, nitrilotriacetic acid, and ethylenediaminetriacetic acid were detected after 25 h. Results are consistent with first-order, solution-phase oxidation of EDTA and glyoxylic acid by ferryl ion and H202, respectively, with inhibition due to sludge accumulation, and equilibrium metal coprecipitation. This ambient process, to our knowledge previously unknown, agrees with recently reported findings and shows promise for remediation of metals, metalloids, and radionuclides in wastewater, soil, and sediment.
ENVIRONMENTALMANAGEMENT SCIENCE PROGRAM PROJECT NUMBER 87016 CO-PRECIPITATION OF TRACEMETALS INGROUNDWATER AND VADOSE ZONE CALCITE: IN SITU CONTAINMENT AND STABILIZATION OF STRONTIUM-90 ANDOTHER DIVALENT METALS AND RADIONUCLIDES AT ARIDWESTERN DOE SITES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ferris, F. Grant; Fujita, Yoshiko; Smith, Robert W.

2004-06-15

Radionuclide and metal contaminants are present in the vadose zone and groundwater throughout the U.S. Department of Energy (DOE) weapons complex. In situ containment and stabilization of these contaminants in vadose zones or groundwater is a cost-effective treatment strategy. Our facilitated approach relies upon the hydrolysis of introduced urea to cause the acceleration of calcium carbonate precipitation (and trace metal coprecipitation) by increasing groundwater pH and alkalinity (Fujita et al., 2000; Warren et al., 2001). Subsurface urea hydrolysis is catalyzed by the urease enzyme, which may be either introduced with the urea or produced in situ by ubiquitous subsurface ureamore » hydrolyzing microorganisms. Because the precipitation processes are irreversible and many western aquifers are saturated with respect to calcite, the co-precipitated metals and radionuclides will be effectively removed from groundwater. The rate at which trace metals are incorporated into calcite is a function of calcite precipitation kinetics, adsorption interactions between the calcite surface and the trace metal in solution (Zachara et al., 1991), solid solution properties of the trace metal in calcite (Tesoriero and Pankow, 1996), and also the surfaces upon which the calcite is precipitating. A fundamental understanding of the coupling of calcite precipitation and trace metal partitioning, and how this occurs in aquifers and vadose environments is lacking. This report summarizes work undertaken during the second year of this project.« less
A New Superalloy Enabling Heavy Duty Gas Turbine Wheels for Improved Combined Cycle Efficiency

DOE Office of Scientific and Technical Information (OSTI.GOV)

Detor, Andrew; DiDomizio, Richard; McAllister, Don

The drive to increase combined cycle turbine efficiency from 62% to 65% for the next-generation advanced cycle requires a new heavy duty gas turbine wheel material capable of operating at 1200°F and above. Current wheel materials are limited by the stability of their major strengthening phase (gamma double prime), which coarsens at temperatures approaching 1200°F, resulting in a substantial reduction in strength. More advanced gamma prime superalloys, such as those used in jet engine turbine disks, are also not suitable due to size constraints; the gamma prime phase overages during the slow cooling rates inherent in processing thick-section turbine wheels.more » The current program addresses this need by screening two new alloy design concepts. The first concept exploits a gamma prime/gamma double prime coprecipitation reaction. Through manipulation of alloy chemistry, coprecipitation is controlled such that gamma double prime is used only to slow the growth of gamma prime during slow cooling, preventing over-aging, and allowing for subsequent heat treatment to maximize strength. In parallel, phase field modeling provides fundamental understanding of the coprecipitation reaction. The second concept uses oxide dispersion strengthening to improve on two existing alloys that exhibit excellent hold time fatigue crack growth resistance, but have insufficient strength to be considered for gas turbine wheels. Mechanical milling forces the dissolution of starting oxide powders into a metal matrix allowing for solid state precipitation of new, nanometer scale oxides that are effective at dispersion strengthening.« less
Determination of (210)Po in drinking water and urine samples using copper sulfide microprecipitation.

PubMed

Guérin, Nicolas; Dai, Xiongxin

2014-06-17

Polonium-210 ((210)Po) can be rapidly determined in drinking water and urine samples by alpha spectrometry using copper sulfide (CuS) microprecipitation. For drinking water, Po in 10 mL samples was directly coprecipitated onto the filter for alpha counting without any purification. For urine, 10 mL of sample was heated, oxidized with KBrO3 for a short time (∼5 min), and subsequently centrifuged to remove the suspended organic matter. The CuS microprecipitation was then applied to the supernatant. Large batches of samples can be prepared using this technique with high recoveries (∼85%). The figures of merit of the methods were determined, and the developed methods fulfill the requirements for emergency and routine radioassays. The efficiency and reliability of the procedures were confirmed using spiked samples.

Hydrogenolysis of Glycerol to Propylene Glycol on Nanosized Cu-Zn-Al Catalysts Prepared Using Microwave Process.

PubMed

Kim, Dong Won; Ha, Sang Ho; Moon, Myung Jun; Lim, Kwon Taek; Ryu, Young Bok; Lee, Sun Do; Lee, Man Sig; Hong, Seong-Soo

2015-01-01

Cu-Zn-Al catalysts were prepared using microwave-assisted process and co-precipitation methods. The prepared catalysts were characterized by XRD, BET, XPS and TPD of ammonia and their catalytic activity for the hydrogenolysis of glycerol to propylene glycol was also examined. The XRD patterns of Cu/Zn/Al mixed catalysts show CuO and ZnO crystalline phase regardless of preparation method. The highest glycerol hydrogenolysis conversion is obtained with the catalyst having a Cu/Zn/Al ratio of 2:2:1. Hydrogen pre-reduction of catalysts significantly enhanced both glycerol conversions and selectivity to propylene glycol. The glycerol conversion increased with an increase of reaction temperature. However, the selectivity to propylene glycol increased with an increase of temperature, and then declined to 30.5% at 523 K.
Determination of (210)Pb and (210)Po in water using the extractive scintillation cocktail Polex™.

PubMed

Landstetter, Claudia; Hiegesberger, Bernd; Sinojmeri, Merita; Katzlberger, Christian

2014-11-01

Method validation was performed to achieve the accreditation for our determination method of (210)Pb and (210)Po in water. A Pb(NO3)2 carrier is added to the sample and lead is precipitated with Na2SxH2O. (210)Po is co-precipitated and the extractive scintillation cocktail Polex(™) is used to determine (210)Po and (210)Pb. Uranium is also extracted by Polex(™). It can be removed by washing the precipitate with 1% HNO3. The ingrowth of (210)Pb from (222)Rn during transportation time must be calculated. It has to be subtracted from the original (210)Pb in the sample and taken into account for the calculation of the lower limit of detection. Copyright © 2014 Elsevier Ltd. All rights reserved.
Dye adsorption into transition metal-doped zinc oxide nanoparticles supported on natural zeolites to solve wastewater issue

NASA Astrophysics Data System (ADS)

Indra Pratiwi, Margaretha; Afifah, Nur; Saleh, Rosari

2017-03-01

In this work, Fe-doped zinc oxide/natural zeolite (Fe:ZnO/NZ) nanocomposites were prepared using the co-precipitation method with various NZ amounts. The nanocomposites were characterized by X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) surface area analysis and thermogravimetric analysis (TGA). The nanocomposites were used to remove methylene blue (MB) dye from an aqueous solution. The effect of various NZ amounts and initial MB concentration were tested. The Pseudo-first-order and pseudo-second-order kinetic models were used to explain the adsorption mechanism. The Langmuir and the Freundlich isotherm models were used to fit the adsorption isotherms of the nanocomposites.
Structural, optical and dielectric properties of pure and chromium (Cr) doped nickel oxide nanoparticles

NASA Astrophysics Data System (ADS)

Gupta, Jhalak; Ahmed, Arham S.

2018-05-01

The pure and Cr doped nickel oxide (NiO) nanoparticles have been synthesized by cost effective co-precipitation method having nickel nitrate as initial precursor. The synthesized samples were characterized by X-Ray diffraction (XRD), UV-Visible Spectroscopy(UV-Vis) and LCR meter for structural, optical and dielectric properties respectively. The crystallite size of pure nickel oxide nanoparticles characterized by XRD using Debye Scherer's formula was found to be 21.7nm and the same decreases on increasing Cr concentration whereas optical and dielectric properties were analyzed by UV-Vis and LCR meter respectively. The energy band gaps were determined by UV-Vis using Tauc relation.
Synthesis and characterization of magnesium doped cerium oxide for the fuel cell application

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Amit; Kumari, Monika; Kumar, Mintu

2016-05-06

Cerium oxide has attained much attentions in global nanotechnology market due to valuable application for catalytic, fuel additive, and widely as electrolyte in solid oxide fuel cell. Doped cerium oxide has large oxygen vacancies that allow for greater reactivity and faster ion transport. These properties make cerium oxide suitable material for SOFCs application. Cerium oxide electrolyte requires lower operation temperature which shows improvement in processing and the fabrication technique. In our work, we synthesized magnesium doped cerium oxide by the co-precipitation method. With the magnesium doping catalytic reactivity of CeO{sub 2} was increased. Synthesized nanoparticle were characterized by the XRDmore » and UV absorption techniques.« less
Low temperature synthesis and characterization of carbonated hydroxyapatite nanocrystals

NASA Astrophysics Data System (ADS)

Anwar, Aneela; Asghar, Muhammad Nadeem; Kanwal, Qudsia; Kazmi, Mohsin; Sadiqa, Ayesha

2016-08-01

Carbonate substituted hydroxyapatite (CHA) nanorods were synthesized via coprecipitation method from aqueous solution of calcium nitrate tetrahydrate and diammonium hydrogen phosphate (with urea as carbonate ion source) in the presence of ammonium hydroxide solution at 70 °C at the conditions of pH 11. The obtained powders were physically characterized using transmission electron microscopy (TEM), X-ray powder diffraction analysis (XRD), and FTIR and Raman spectroscopy. The particle size was evaluated by Dynamic light scattering (DLS). The chemical structural analysis of as prepared sample was performed using X-ray photoelectron spectroscopy (XPS). After ageing for 12 h, and heat treatment at 1000 °C for 1 h, the product was obtained as highly crystalline nanorods of CHA.
Erbium induced magnetic properties of Er/ZnO nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jayachandraiah, C.; Divya, A.; Sivakumar, K.

Pure and Er (2, 3 and 4 at. %) doped ZnO nanoparticles have been synthesized by chemical co-precipitation method. EDS spectrum confirmed the presence of Zn, O and Er in the synthesized samples. The XRD measurements confirmed the hexagonal wurtzite structure of ZnO for all samples. The crystallite size of the samples decreases with increase in concentration and are compatible with the results that obtained from TEM analysis.EPR spectra exhibitedferromagnetic signals the substitution Er The possible ferromagnetic zinc interstials signal is appeared for 2 at. % of Er dopant. The room temperature ferromagnetic is observed only for 2 at. %more » of Er while all other samples exhibiting weak ferromagnetic nature.« less
Efficient MgO-based mesoporous CO2 trapper and its performance at high temperature.

PubMed

Han, Kun Kun; Zhou, Yu; Chun, Yuan; Zhu, Jian Hua

2012-02-15

A novel MgO-based porous adsorbent has been synthesized in a facile co-precipitation method for the first time, in order to provide a candidate for trapping CO(2) in flue gas at high temperature. The resulting composite exhibits a mesoporous structure with a wide pore size distribution, due to the even dispersion and distribution of microcrystalline MgO in the framework of alumina to form a concrete-like structure. These sorbents can capture CO(2) at high temperature (150-400°C), possessing high reactivity and stability in cyclic adsorption-desorption processes, providing competitive candidates to control CO(2) emission. Copyright © 2011 Elsevier B.V. All rights reserved.
Preparation and characterization of Ag-doped In2O3 nanoparticles gas sensor

NASA Astrophysics Data System (ADS)

Anand, Kanica; Kaur, Jasmeet; Singh, Ravi Chand; Thangaraj, Rengasamy

2017-08-01

Pure and Ag-doped In2O3 nanoparticles are synthesized by the co-precipitation method and are characterized by X-ray diffraction, transmission electron microscopy and photoluminescence spectroscopy. Gas sensing properties of the sensors has been investigated towards methanol, ethanol, acetone and LPG at different operating temperatures. It is found that the sensor response magnitude of the 3% Ag-doped In2O3 nanoparticles sensors is higher to 50 ppm of ethanol at 300 °C, to acetone at 350 °C and to LPG at 400 °C. This is mainly attributed to the large number of oxygen vacancies and defects in doped sensors as corroborated by the photoluminescence studies.
Microstress, strain, band gap tuning and photocatalytic properties of thermally annealed and Cu-doped ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Prasad, Neena; V. M. M, Saipavitra; Swaminathan, Hariharan; Thangaraj, Pandiyarajan; Ramalinga Viswanathan, Mangalaraja; Balasubramanian, Karthikeyan

2016-06-01

ZnO nanoparticles and Cu-doped ZnO nanoparticles were prepared by co-precipitation method. Also, a part of the pure ZnO nanoparticles were annealed at 750 °C for 3, 6, and 9 h. X-ray diffraction studies were carried out and the lattice parameters, unit cell volume, interplanar spacing, and Young's modulus were calculated for all the samples, and also the crystallite size was found using the Scherrer method. X-ray peak broadening analysis was used to estimate the crystallite sizes and the strain using the Williamson-Hall (W-H) method and the size-strain plot (SSP) method. Stress and the energy density were calculated using the W-H method assuming different models such as uniform deformation model, uniform strain deformation model, uniform deformation energy density model, and the SSP method. Optical absorption properties of the samples were understood from their UV-visible spectra. Photocatalytic activities of ZnO and 5 % Cu-doped ZnO were observed by the degradation of methylene blue dye in aqueous medium under the irradiation of 20-W compact fluorescent lamp for an hour.
Effect of Morphology and Manganese Valence on the Voltage Fade and Capacity Retention of Li[Li 2/12Ni 3/12Mn 7/12]O 2

DOE PAGES

Verde, Michael G.; Liu, Haodong; Carroll, Kyler J.; ...

2014-10-02

We have determined the electrochemical characteristics of the high voltage, high capacity Li-ion battery cathode material Li[Li 2/12Ni 3/12Mn 7/12]O 2 prepared using three different synthesis routes: sol-gel, hydroxide co-precipitation, and carbonate co-precipitation. Each route leads to distinct morphologies and surface areas while maintaining the same crystal structures. X-ray photoelectron spectroscopy (XPS) measurements reveal differences in their surface chemistries upon cycling, which correlate with voltage fading. As expected, we observed the valence state of Mn on the surface to decrease upon lithiation, and this reduction is specifically correlated to discharging below 3.6V. Furthermore, the data shows a correlation of themore » formation of Li 2CO 3 with Mn oxidation state from the« less
Effect of trace metals and sulfite oxidation of adipic acid degradation in FGD systems. Final report Dec 81-May 82

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jarvis, J.B.; Terry, J.C.; Schubert, S.A.

The report gives results of the measurement of the adipic acid degradation rate in a bench-scale flue gas desulfurization (FGD) system, designed to simulate many of the important aspects of full-scale FGD systems. Results show that the adipic acid degradation rate depends on the sulfite oxidation rate, the adipic acid concentration, the presence of manganese in solution, and temperature. The degradation rate is also affected by pH, but only when manganese is present. Adipic acid degradation products identified in the liquid phase include valeric, butyric, propionic, succinic, and glutaric acids. When manganese was present, the predominant degradation products were succinicmore » and glutaric acids. Analysis of solids from the bench scale tests shows large concentrations of coprecipitated adipic acid in low oxidation sulfite solids. By contrast, low quantities of coprecipitated adipic acid were found in high oxidation gypsum solids.« less
[Inclusion of proteins into polyelectrolyte microcapsules by coprecipitation and adsorption].

PubMed

Kochetkova, O Iu; Kazakova, L I; Moshkov, D A; Vinokurov, M G; Shabarchina, L I

2013-01-01

In present study microcapsules composed of synthetic (PSS and PAA) and biodegradable (DS and PAr) polyelectrolytes on calcium carbonate microparticles were obtained. The ultrastructural organization of biodegradable microcapsules was studied using transmission electron microscopy. The envelope of such capsules consisting of six polyelectrolyte layers is already well-formed, having the average thickness of 44 ± 3.0 nm, and their internal polyelectrolyte matrix is sparser compared to the synthetic microcapsules. Spectroscopy was employed to evaluate the efficiency of incorporation of FITC-labeled BSA into synthetic microcapsules by adsorption, depending on the number of polyelectrolyte layers. It was shown that the maximal amount of protein incorporated into the capsules with 6 or 7 polyelectrolyte layers (4 and 2 pg/capsule, correspondingly). As a result we conclude that, in comparison with co-precipitation, the use of adsorption allows to completely avoid the loss of protein upon encapsulation.
MSFIA-LOV system for (226)Ra isolation and pre-concentration from water samples previous radiometric detection.

PubMed

Rodríguez, Rogelio; Borràs, Antoni; Leal, Luz; Cerdà, Víctor; Ferrer, Laura

2016-03-10

An automatic system based on multisyringe flow injection analysis (MSFIA) and lab-on-valve (LOV) flow techniques for separation and pre-concentration of (226)Ra from drinking and natural water samples has been developed. The analytical protocol combines two different procedures: the Ra adsorption on MnO2 and the BaSO4 co-precipitation, achieving more selectivity especially in water samples with low radium levels. Radium is adsorbed on MnO2 deposited on macroporous of bead cellulose. Then, it is eluted with hydroxylamine to transform insoluble MnO2 to soluble Mn(II) thus freeing Ra, which is then coprecipitated with BaSO4. The (226)Ra can be directly detected in off-line mode using a low background proportional counter (LBPC) or through a liquid scintillation counter (LSC), after performing an on-line coprecipitate dissolution. Thus, the versatility of the proposed system allows the selection of the radiometric detection technique depending on the detector availability or the required response efficiency (sample number vs. response time and limit of detection). The MSFIA-LOV system improves the precision (1.7% RSD), and the extraction frequency (up to 3 h(-1)). Besides, it has been satisfactorily applied to different types of water matrices (tap, mineral, well and sea water). The (226)Ra minimum detectable activities (LSC: 0.004 Bq L(-1); LBPC: 0.02 Bq L(-1)) attained by this system allow to reach the guidance values proposed by the relevant international agencies e.g. WHO, EPA and EC. Copyright © 2016 Elsevier B.V. All rights reserved.
ENVIRONMENTAL MANAGEMENT SCIENCE PROGRAM PROJECT NUMBER 87016 CO-PRECIPITATION OF TRACE METALS IN GROUNDWATER AND VADOSE ZONE CALCITE: IN SITU CONTAINMENT AND STABILIZATION OF STRONTIUM-90 AND OTHER DIVALENT METALS AND RADIONUCLIDES AT ARID WESTERN DOE SITES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ferris, F. Grant; Fujita, Yoshiko; Smith, Robert W.

2004-06-15

Radionuclide and metal contaminants are present in the vadose zone and groundwater throughout the U.S. Department of Energy (DOE) weapons complex. In situ containment and stabilization of these contaminants in vadose zones or groundwater is a cost-effective treatment strategy. Our facilitated approach relies upon the hydrolysis of introduced urea to cause the acceleration of calcium carbonate precipitation (and trace metal coprecipitation) by increasing groundwater pH and alkalinity (Fujita et al., 2000; Warren et al., 2001). Subsurface urea hydrolysis is catalyzed by the urease enzyme, which may be either introduced with the urea or produced in situ by ubiquitous subsurface ureamore » hydrolyzing microorganisms. Because the precipitation processes are irreversible and many western aquifers are saturated with respect to calcite, the co-precipitated metals and radionuclides will be effectively removed from groundwater. The rate at which trace metals are incorporated into calcite is a function of calcite precipitation kinetics, adsorption interactions between the calcite surface and the trace metal in solution (Zachara et al., 1991), solid solution properties of the trace metal in calcite (Tesoriero and Pankow, 1996), and also the surfaces upon which the calcite is precipitating. A fundamental understanding of the coupling of calcite precipitation and trace metal partitioning, and how this occurs in aquifers and vadose environments is lacking. This report summarizes work undertaken during the second year of this project.« less
Trace Metals in Groundwater & Vadose Zone Calcite: In Situ Containment & Stabilization of Stronthium-90 & Other Divalent Metals & Radionuclides at Arid West DOE

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, Robert W.

2005-06-01

Radionuclide and metal contaminants such as strontium-90 are present beneath U.S. Department of Energy (DOE) lands in both the groundwater (e.g., 100-N area at Hanford, WA) and vadose zone (e.g., Idaho Nuclear Technology and Engineering Center [INTEC] at the Idaho National Laboratory [INL]). In situ containment and stabilization of these contaminants is a cost-effective treatment strategy. However, implementing in situ containment and stabilization approaches requires definition of the mechanisms that control contaminant sequestration. We are investigating the in situ immobilization of radionuclides or contaminant metals (e.g., strontium-90) by their facilitated co-precipitation with calcium carbonate (primarily calcite) in groundwater and vadosemore » zone systems. Our facilitated approach relies upon the hydrolysis of introduced urea to cause the acceleration of calcium carbonate precipitation (and trace metal co-precipitation) by (a) increasing pH and alkalinity and (b) liberating cations from the aquifer matrix by cation exchange reactions. Subsurface urea hydrolysis is catalyzed by the urease enzyme, which is produced in situ by native urea hydrolyzing microorganisms. Because the precipitation process tends to be irreversible and many western aquifers are saturated with respect to calcite, the co-precipitated metals and radionuclides will be effectively removed from the aqueous phase over the long term. We are currently conducting field based activities at both the INL Vadose Zone Research Park (VZRP), an uncontaminated surrogate site for the strontium-90 contaminated vadose zone at INTEC and at the strontium-90 contaminated aquifer of 100-N area of the Hanford site.« less
Co-Precipitation Synthesis and Optical Properties of Mn4+-Doped Hexafluoroaluminate w-LED Phosphors

PubMed Central

Geitenbeek, Robin G.; Meijerink, Andries

2017-01-01

Mn4+-activated hexafluoroaluminates are promising red-emitting phosphors for white light emitting diodes (w-LEDs). Here, we report the synthesis of Na3AlF6:Mn4+, K3AlF6:Mn4+ and K2NaAlF6:Mn4+ phosphors through a simple two-step co-precipitation method. Highly monodisperse large (~20 μm) smoothed-octahedron shaped crystallites are obtained for K2NaAlF6:Mn4+. The large size, regular shape and small size distribution are favorable for application in w-LEDs. All Mn4+-doped hexafluoroaluminates show bright red Mn4+ luminescence under blue light excitation. We compare the optical properties of Na3AlF6:Mn4+, K3AlF6:Mn4+ and K2NaAlF6:Mn4+ at room temperature and 4 K. The luminescence measurements reveal that multiple Mn4+ sites exist in M3AlF6:Mn4+ (M = Na, K), which is explained by the charge compensation that is required for Mn4+ on Al3+ sites. Thermal cycling experiments show that the site distribution changes after annealing. Finally, we investigate thermal quenching and show that the luminescence quenching temperature is high, around 460–490 K, which makes these Mn4+-doped hexafluoroaluminates interesting red phosphors for w-LEDs. The new insights reported on the synthesis and optical properties of Mn4+ in the chemically and thermally stable hexafluoroaluminates can contribute to the optimization of red-emitting Mn4+ phosphors for w-LEDs. PMID:29149083
Preparation of Superparamagnetic Zn0.5Mn0.5Fe2O4 Particle by Coprecipitation-Sonochemical Method for Radar Absorbing Material

NASA Astrophysics Data System (ADS)

Taufiq, A.; Bahtiar, S.; Sunaryono; Hidayat, N.; Hidayat, A.; Mufti, N.; Diantoro, M.; Fuad, A.; Munasir; Rahmawati, R.; Adi, W. A.; Pratapa, S.; Darminto

2017-05-01

One of many applications of spinel ferrite nanoparticles is related to their performance as radar absorbing materials. In this work, we report developing synthesis method through combined coprecipitation-sonochemical routes in preparing Zn0.5Mn0.5Fe2O4 nanoparticle from iron sand in Indonesia as a vital raw material. The structure, size, morphology, and elements of the Zn0.5Mn0.5Fe2O4 nanoparticle were investigated via X-Ray diffractometry and Transmission/Scanning Electron Microscopy (TEM/SEM) combining Energy Dispersive Spectroscopy (EDS). The magnetic properties of the Zn0.5Mn0.5Fe2O4 nanoparticle were characterized by using Vibrating Sample Magnetometer (VSM). Furthermore, the reflection loss character of the Zn0.5Mn0.5Fe2O4 nanoparticle was determined via Vector Network Analyzer (VNA). From the qualitative and quantitative analysis of the XRD data, it can be identified that the Zn0.5Mn0.5Fe2O4 particle formed a spinel cubic structure in a single phase with the lattice parameter of approximately 8.401 Å. It is known from the TEM image that the Zn0.5Mn0.5Fe2O4 particle had a size of about 9.7 nm and tended to agglomerate. Furthermore, the data analysis of the M(H) curve presented that the Zn0.5Mn0.5Fe2O4 nanoparticle has a superparamagnetic behavior with the saturation magnetization of approximately 43 emu/g. Finally, the data analysis of the reflection loss as a function of frequency showed that the Zn0.5Mn0.5Fe2O4 nanoparticle performs as a radar absorbing material with the absorption performance of approximately -11.0 dB at the frequency of 10.8 GHz
In situ synthesis of magnesium-substituted biphasic calcium phosphate and in vitro biodegradation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kim, Tae-Wan; Lee, Hyeong-Shin; Kim, Dong-Hyun

Highlights: ► Mg–BCP were successfully prepared through in situ aqueous co-precipitation method. ► The amount of β-TCP phase was changed with the magnesium substitution level. ► The substitution of magnesium led to a decrease in the unit cell volume. ► Mg–BCP could be able to develop a new apatite phase on the surface faster than BCP. -- Abstract: In situ preparation of magnesium (Mg) substituted biphasic calcium phosphate (BCP) of hydroxyapatite (HAp)/β-tricalcium phosphate (β-TCP) were carried out through aqueous co-precipitation method. The concentrations of added magnesium were varied with the calcium in order to obtain constant (Ca + Mg)/P ratiosmore » of 1.602. X-ray diffraction (XRD) and Fourier transformed infrared (FTIR) spectroscopy were used to characterize the structure of synthesized magnesium substituted BCP powders. The results have shown that substitution of magnesium in the calcium deficient apatites revealed the formation of biphasic mixtures of different HAp/β-TCP ratios after heating at 1000 °C. The ratios of the formation of phase mixtures were dependent on the content of magnesium. After immersing in Hanks’ balanced salt solution (HBSS) for 1 week, 1 wt% magnesium substituted BCP powders were degraded and precipitation started to be formed with small granules consisting of number of flake-like crystal onto the surface of synthesized powders. On the other hand, in the case of pure BCP powders, the formation of new precipitates was detected after immersion in HBSS for 2 weeks. On the basis of these results, magnesium substituted BCP could be able to develop a new apatite phase on the surface in contact with physiological fluids faster than BCP does. In addition, the retention time to produce the new apatite phase in implantation operation for the BCP powder could be controlled by the amount of magnesium substitution.« less
Preparation and Characterization of Chitosan-coated Fe3O4 Nanoparticles using Ex-Situ Co-Precipitation Method and Tripolyphosphate/Sulphate as Dual Crosslinkers

NASA Astrophysics Data System (ADS)

Wulandari, Ika O.; Mardila, Vita T.; Santjojo, D. J. Djoko H.; Sabarudin, Akhmad

2018-01-01

The unique properties of nanomaterial provide great opportunities to develop in several fields. Several types of nanoparticles have been proven beneficial for biomedical and therapeutic agent development. Particularly for clinical use, nanoparticles must be biocompatible and non-toxic. Iron oxide nanoparticles consist of either magnetite (Fe3O4) or maghemite (γ-Fe2O3) was eligible to use for in vivo application including targeting drug delivery. Due to their distinct properties, these nanoparticles could be directed to the specific target under external magnetic field. However, nanoparticles have a tendency to form agglomeration. Therefore, surface modification was required to reduce the agglomeration. In this study, nanoparticles of Fe3O4 were produced and coated by biomaterial (chitosan) using ex-situ co-precipitation method. Nanoparticles of Fe3O4 were synthesized by adding ammonia water into iron ferric and ferrous solution. Synthesis process of Fe3O4 was conducted prior to adding chitosan. Chitosan was then cross-linked by a combination of tripolyphosphate/sulphate. The different composition ratio and crosslinking time provide the different physical and magnetic characteristics of nanoparticles. Particle and crystallite size was determined by using Scanning Electron Microscopy (SEM) and X-Ray Diffraction (XRD) respectively, whereas magnetic characteristic was determined by Electron Spin Resonance (ESR). The results showed that the ratio enhancement between chitosan: Fe3O4 increase the particle size, while decreased the crystallite size. Morphology and particle size were influenced by the ratio of crosslinkers. It was found that the higher tripolyphosphate content was contributed to the small size and more spherical morphology. In addition, the influence of crosslinking time toward crystallite size was determined by altering stirring time. The longer duration of crosslinking time, provide the larger crystallite size of chitosan-Fe3O4. There was an interesting correlation between particle size and amount of Fe3O4 phase with ESR curve.

Structural Characterization of Poorly-Crystalline Scorodite, Iron (III)-arsenate Co-precipitates and Uranium Millneutralized Raffinate Solids using X-ray Absorption Fine Structure Spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, N.; Jiang, D; Cutler, J

X-ray absorption fine structure (XAFS) is used to characterize the mineralogy of the iron(III)-arsenate(V) precipitates produced during the raffinate (aqueous effluent) neutralization process at the McClean Lake uranium mill in northern Saskatchewan, Canada. To facilitate the structural characterization of the precipitated solids derived from the neutralized raffinate, a set of reference compounds were synthesized and analyzed. The reference compounds include crystalline scorodite, poorly-crystalline scorodite, iron(III)-arsenate co-precipitates obtained under different pH conditions, and arsenate-adsorbed on goethite. The poorly-crystalline scorodite (prepared at pH 4 with Fe/As = 1) has similar As local structure as that of crystalline scorodite. Both As and Femore » K-edge XAFS of poorly-crystalline scorodite yield consistent results on As-Fe (or Fe-As) shell. From As K-edge analysis the As-Fe shell has an inter-atomic distance of 3.33 {+-} 0.02 A and coordination number of 3.2; while from Fe K-edge analysis the Fe-As distance and coordination number are 3.31 {+-} 0.02 A and 3.8, respectively. These are in contrast with the typical arsenate adsorption on bidentate binuclear sites on goethite surfaces, where the As-Fe distance is 3.26 {+-} 0.03 A and coordination number is close to 2. A similar local structure identified in the poorly-crystalline scorodite is also found in co-precipitation solids (Fe(III)/As(V) = 3) when precipitated at the same pH (pH = 4): As-Fe distance 3.30 {+-} 0.03 A and coordination number 3.9; while at pH = 8 the co-precipitate has As-Fe distance of 3.27 {+-} 0.03 A and coordination number about 2, resembling more closely the adsorption case. The As local structure in the two neutralized raffinate solid series (precipitated at pH values up to 7) closely resembles that in the poorly-crystalline scorodite. All of the raffinate solids have the same As-Fe inter-atomic distance as that in the poorly-crystalline scorodite, and a systematic decrease in the As-Fe coordination is observed when pH is progressively increased; the basic poorly-crystalline scorodite structural feature remains in the raffinate solid up to pH 7.« less
Structural characterization of poorly-crystalline scorodite, iron(III)-arsenate co-precipitates and uranium mill neutralized raffinate solids using X-ray absorption fine structure spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, N; Jiang, D T; Cutler, J

X-ray absorption fine structure (XAFS) is used to characterize the mineralogy of the iron(III)-arsenate(V) precipitates produced during the raffinate (aqueous effluent) neutralization process at the McClean Lake uranium mill in northern Saskatchewan, Canada. To facilitate the structural characterization of the precipitated solids derived from the neutralized raffinate, a set of reference compounds were synthesized and analyzed. The reference compounds include crystalline scorodite, poorly-crystalline scorodite, iron(III)-arsenate co-precipitates obtained under different pH conditions, and arsenate-adsorbed on goethite. The poorly-crystalline scorodite (prepared at pH 4 with Fe/As = 1) has similar As local structure as that of crystalline scorodite. Both As and Femore » K-edge XAFS of poorly-crystalline scorodite yield consistent results on As-Fe (or Fe-As) shell. From As K-edge analysis the As-Fe shell has an inter-atomic distance of 3.33 ± 0.02 Å and coordination number of 3.2; while from Fe K-edge analysis the Fe-As distance and coordination number are 3.31 ± 0.02 Å and 3.8, respectively. These are in contrast with the typical arsenate adsorption on bidentate binuclear sites on goethite surfaces, where the As-Fe distance is 3.26 ± 0.03 Å and coordination number is close to 2. A similar local structure identified in the poorly-crystalline scorodite is also found in co-precipitation solids (Fe(III)/As(V) = 3) when precipitated at the same pH (pH = 4): As-Fe distance 3.30 ± 0.03 Å and coordination number 3.9; while at pH = 8 the co-precipitate has As-Fe distance of 3.27 ± 0.03 Å and coordination number about 2, resembling more closely the adsorption case. The As local structure in the two neutralized raffinate solid series (precipitated at pH values up to 7) closely resembles that in the poorly-crystalline scorodite. All of the raffinate solids have the same As-Fe inter-atomic distance as that in the poorly-crystalline scorodite, and a systematic decrease in the As-Fe coordination is observed when pH is progressively increased; the basic poorly-crystalline scorodite structural feature remains in the raffinate solid up to pH 7.« less
Synthesis, strctural and electrochemical characterizations of lithium- manganese- rich composite cathode materials for lithium ion batteries

NASA Astrophysics Data System (ADS)

Wang, Dapeng

The electrification trend for transportation systems requires alternative cathode materials to LiCoO2 with improved safety, lowered cost and extended cycle life. Lithium- manganese- rich composite cathode materials, which can be presented in a two component notation as xLi2MnO3·(1-x)LiMO 2, (M= Ni, Co or Mn) have superior cost and energy density advantages. These cathode materials have shown success in laboratory scale experiments, but are still facing challenges such as voltage fade, moderate rate capacity and tap density for commercialization. The synthesis of precursors with high packing density and suitable physical properties is critical to achieve high energy density as well as the other acceptable electrochemical performance for the next generation lithium ion batteries. The aim of this study is to correlate the electrochemical properties of materials to their structural, morphological, and physical properties by coordinating the science of synthesis with the science of function, in order to enable the use of these compounds in vehicle technologies. Three different precursors including carbonate, hydroxide and oxalate were synthesized by co-precipitation reactions using continuous stirred tank reactor (CSTR) under various conditions. Research focused on areas such as nucleation and growth mechanisms, synthesis optimizations, and intrinsic limitations of each co-precipitation method. A combination of techniques such as PSA, BET, SEM, EDX FIB, TEM, Raman, FTIR, TGA-DSC, XRD, and ICP-MS, as well as electrochemical test methods such as cycling, CV, EIS and HPPC tests were used in correlation with each other in order to deepen our understanding to these materials. Related topics such as the composite structure formation process during the solid state reaction, lithium and nickel content effects on the cathode properties were also discussed. Additionally, the side reactions between the active materials and electrolyte as a result of the high charge potential were mitigated through a simple wet chemical surface coating method, and the positive effect of the surface coating on the cells' performance was also discussed.
Simple and Rapid Synthesis of Magnetite/Hydroxyapatite Composites for Hyperthermia Treatments via a Mechanochemical Route

PubMed Central

Iwasaki, Tomohiro; Nakatsuka, Ryo; Murase, Kenya; Takata, Hiroshige; Nakamura, Hideya; Watano, Satoru

2013-01-01

This paper presents a simple method for the rapid synthesis of magnetite/hydroxyapatite composite particles. In this method, superparamagnetic magnetite nanoparticles are first synthesized by coprecipitation using ferrous chloride and ferric chloride. Immediately following the synthesis, carbonate-substituted (B-type) hydroxyapatite particles are mechanochemically synthesized by wet milling dicalcium phosphate dihydrate and calcium carbonate in a dispersed suspension of magnetite nanoparticles, during which the magnetite nanoparticles are incorporated into the hydroxyapatite matrix. We observed that the resultant magnetite/hydroxyapatite composites possessed a homogeneous dispersion of magnetite nanoparticles, characterized by an absence of large aggregates. When this material was subjected to an alternating magnetic field, the heat generated increased with increasing magnetite concentration. For a magnetite concentration of 30 mass%, a temperature increase greater than 20 K was achieved in less than 50 s. These results suggest that our composites exhibit good hyperthermia properties and are promising candidates for hyperthermia treatments. PMID:23629669
Synthesis of SiO2-coated ZnMnFe2O4 nanospheres with improved magnetic properties.

PubMed

Wang, Jun; Zhang, Kai; Zhu, Yuejin

2005-05-01

A core-shell structured composite, SiO2 coated ZnMnFe2O4 spinel ferrite nanoparticles (average diameter of approximately 80 nm), was prepared by hydrolysis of tetraethyl orthosilicate (TEOS) in the presence of ZnMnFe2O4 nanoparticles (average diameter of approximately 10 nm) synthesized by a hydrothermal method. The obtained samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and field emission scanning electron microscopy (FESEM). The magnetic measurements were carried out on a vibrating sample magnetometer (VSM), and the measurement results indicate that the core-shell samples possess better magnetic properties at room temperature, compared with paramagnetic colloids with a magnetic core by a coprecipitation method. These core-shell nanospherical particles with self-assembly under additional magnetic fields could have potential application in biomedical systems.
Cu-doped Cd1- x Zn x S alloy: synthesis and structural investigations

NASA Astrophysics Data System (ADS)

Yadav, Indu; Ahlawat, Dharamvir Singh; Ahlawat, Rachna

2016-03-01

Copper doped Cd1- x Zn x S ( x ≤ 1) quantum dots have been synthesized using chemical co-precipitation method. Structural investigation of the synthesized nanomaterials has been carried out by powder XRD method. The XRD results have confirmed that as-prepared Cu-doped Cd1- x Zn x S quantum dots have hexagonal structure. The average nanocrystallite size was estimated in the range 2-12 nm using Debye-Scherrer formula. The lattice constants, lattice plane, d-spacing, unit cell volume, Lorentz factor and dislocation density were also calculated from XRD data. The change in particle size was observed with the change in Zn concentration. Furthermore, FTIR spectra of the prepared samples were observed for identification of COO- and O-H functional groups. The TEM study has also reported the same size range of nanoparticles. The increase in agglomeration has been observed with the increase in Zn concentration in the prepared samples.
Tannic acid assisted synthesis of flake-like hydroxyapatite nanostructures at room temperature

NASA Astrophysics Data System (ADS)

Vázquez, Maricela Santana; Estevez, O.; Ascencio-Aguirre, F.; Mendoza-Cruz, R.; Bazán-Díaz, L.; Zorrila, C.; Herrera-Becerra, R.

2016-09-01

A simple and non-expensive procedure was performed to synthesize hydroxyapatite (HAp) flake-like nanostructures, by using a co-precipitation method with tannic acid as stabilizing agent at room temperature and freeze drying. Samples were synthesized with two different salts, Ca(NO3)2 and CaCl2. X-ray diffraction analysis, Raman spectroscopy, scanning and transmission electron microscopy characterizations reveal Ca10(PO4)6(OH)2 HAp particles with hexagonal structure and P63/m space group in both cases. In addition, the particle size was smaller than 20 nm. The advantage of this method over the works reported to date lies in the ease for obtaining HAp particles with a single morphology (flakes), in high yield. This opens the possibility of expanding the view to the designing of new composite materials based on the HAp synthesized at room temperature.
Air trichloroethylene oxidation in a corona plasma-catalytic reactor

NASA Astrophysics Data System (ADS)

Masoomi-Godarzi, S.; Ranji-Burachaloo, H.; Khodadadi, A. A.; Vesali-Naseh, M.; Mortazavi, Y.

2014-08-01

The oxidative decomposition of trichloroethylene (TCE; 300 ppm) by non-thermal corona plasma was investigated in dry air at atmospheric pressure and room temperature, both in the absence and presence of catalysts including MnOx, CoOx. The catalysts were synthesized by a co-precipitation method. The morphology and structure of the catalysts were characterized by BET surface area measurement and Fourier Transform Infrared (FTIR) methods. Decomposition of TCE and distribution of products were evaluated by a gas chromatograph (GC) and an FTIR. In the absence of the catalyst, TCE removal is increased with increases in the applied voltage and current intensity. Higher TCE removal and CO2 selectivity is observed in presence of the corona and catalysts, as compared to those with the plasma alone. The results show that MnOx and CoOx catalysts can dissociate the in-plasma produced ozone to oxygen radicals, which enhances the TCE decomposition.
Intrinsic dependence of the magnetic properties of CoFe2O4 nanoparticles prepared via chemical methods with addition of chelating agents

NASA Astrophysics Data System (ADS)

Mendonça, E. C.; Tenório, Mayara A.; Mecena, S. G.; Zucolotto, B.; Silva, L. S.; Jesus, C. B. R.; Meneses, C. T.; Duque, J. G. S.

2015-12-01

In this work, the effect of addition of different chelating agents on the magnetic properties of cobalt ferrite nanoparticles produced by the combining of both co-precipitation and hydrothermal methods is reported. The Rietveld analyses of X-ray diffraction patterns reveal that our samples are single phase (space group: Fd-3m) with small average sizes. The weight losses observed in the thermogravimetric measurements together with the M×H curves show that the organic contamination coming from chelating agent decomposition can give rise to misinterpretation of the magnetization measurements. Besides, analyses of the zero-field-cooled (ZFC) and field-cooled (FC) magnetization measurements and the M×H curves measured at room temperature allows us to state that both the average blocking temperature and particles size distribution are sensitive to the kind of chelating agent.
MnFe2O4: Synthesis, morphology and electrochemical properties

NASA Astrophysics Data System (ADS)

Kulkarni, Shrikant; Thombare, Balu; Patil, Shankar

2017-05-01

MnFe2O4 has been synthesized by simple ammonia assisted co-precipitation method to obtain nanocrystalline powder. X-ray diffraction studies confirmed its crystallinity and phase purity. The MnFe2O4 calcined at 1000°C for 4 h has spinel crystal structure with Fd3m space group and lattice constant 8.511 Å. The electrode was prepared by dip coating method on stainless steel substrate and fired at 600°C for 2 h. Random shape grains of 0.2 to 1.5 micron with pores of 1-2 micron dimensions were observed in SEM images. The electrochemical studies of MnFe2O4 were carried out with 1 mole Na2SO4 electrolyte. The MnFe2O4 electrode shows highest specific capacitance of 27.53 F.g-1 and interfacial capacitance of 0.83 F.cm-2.
Simulation and experimental results of optical and thermal modeling of gold nanoshells.

PubMed

Ghazanfari, Lida; Khosroshahi, Mohammad E

2014-09-01

This paper proposes a generalized method for optical and thermal modeling of synthesized magneto-optical nanoshells (MNSs) for biomedical applications. Superparamagnetic magnetite nanoparticles with diameter of 9.5 ± 1.4 nm are fabricated using co-precipitation method and subsequently covered by a thin layer of gold to obtain 15.8 ± 3.5 nm MNSs. In this paper, simulations and detailed analysis are carried out for different nanoshell geometry to achieve a maximum heat power. Structural, magnetic and optical properties of MNSs are assessed using vibrating sample magnetometer (VSM), X-ray diffraction (XRD), UV-VIS spectrophotometer, dynamic light scattering (DLS), and transmission electron microscope (TEM). Magnetic saturation of synthesized magnetite nanoparticles are reduced from 46.94 to 11.98 emu/g after coating with gold. The performance of the proposed optical-thermal modeling technique is verified by simulation and experimental results. Copyright © 2014 Elsevier B.V. All rights reserved.
Possible treatments for arsenic removal in Latin American waters for human consumption.

PubMed

Litter, Marta I; Morgada, Maria E; Bundschuh, Jochen

2010-05-01

Considering the toxic effects of arsenic, the World Health Organization recommends a maximum concentration of 10 microg L(-1) of arsenic in drinking water. Latin American populations present severe health problems due to consumption of waters with high arsenic contents. The physicochemical properties of surface and groundwaters are different from those of other more studied regions of the planet, and the problem is still publicly unknown. Methods for arsenic removal suitable to be applied in Latin American waters are here summarized and commented. Conventional technologies (oxidation, coagulation-coprecipitation, adsorption, reverse osmosis, use of ion exchangers) are described, but emphasis is made in emergent decentralized economical methods as the use of inexpensive natural adsorbents, solar light technologies or biological treatments, as essential to palliate the situation in poor, isolated and dispersed populations of Latin American regions. Copyright 2010 Elsevier Ltd. All rights reserved.
Preconcentration and Spectrophotometric Determination of a Naphthalene Analog of Medetomidine Using Modified Maghemite Nanoparticles

NASA Astrophysics Data System (ADS)

Maddah, B.; Hosseini, F.; Ahmadi, M.; Rajabi, A. Asghar; Beik-Mohammadlood, Z.

2016-05-01

A novel and sensitive extraction procedure using sodium dodecyl sulfate (SDS) modified maghemite nanoparticles (MNPs) as an efficient solid phase has been developed for removal, preconcentration, and spectrophotometric determination of trace amounts of a naphthalene analog of dexmedetomidine (4-(1-(na phthalene-1-yl)ethyl)-1Himidazole, NMED). The MNPs were obtained by a coprecipitation method, and their surfaces were furthermore modified by SDS. The size and morphological properties of the synthesized MNPs were determined by X-ray diffraction analysis, FT-IR, vibrating sample magnetometry, and scanning electron microscopy. NMED was adsorbed at pH 3.0. The adsorbed drug was then desorbed and determined by spectrophotometry at 280 nm. The calibration graph was linear in the range 1 × 10-6-1 × 10-4 mol/L of NMED with a correlation coefficient of 0.989. The detection limit of the method for NMED determination was 3.7 × 10-7 mol/L. The method was successfully applied to the determination of NMED in human urine samples.
SEPARATION OF FISSION PRODUCTS FROM PLUTONIUM BY PRECIPITATION

DOEpatents

Seaborg, G.T.; Thompson, S.G.; Davidson, N.R.

1959-09-01

Fission product separation from hexavalent plutonium by bismuth phosphate precipitation of the fission products is described. The precipitation, according to this invention, is improved by coprecipitating ceric and zirconium phosphates (0.05 to 2.5 grams/liter) with the bismuth phosphate.
Synthesis, crystal structure and spectroscopy properties of Na 3AZr(PO 4) 3 ( A=Mg, Ni) and Li 2.6Na 0.4NiZr(PO 4) 3 phosphates

NASA Astrophysics Data System (ADS)

Chakir, M.; El Jazouli, A.; de Waal, D.

2006-06-01

Na 3AZr(PO 4) 3 ( A=Mg, Ni) phosphates were prepared at 750 °C by coprecipitation route. Their crystal structures have been refined at room temperature from X-ray powder diffraction data using Rietveld method. Li 2.6Na 0.4NiZr(PO 4) 3 was synthesized through ion exchange from the sodium analog. These materials belong to the Nasicon-type structure. Raman spectra of Na 3AZr(PO 4) 3 ( A=Mg, Ni) phosphates present broad peaks in favor of the statistical distribution in the sites around PO 4 tetrahedra. Diffuse reflectance spectra indicate the presence of octahedrally coordinated Ni 2+ ions.
A process for the chemical preparation of high-field ZnO varistors

DOEpatents

Brooks, R.A.; Dosch, R.G.; Tuttle, B.A.

1986-02-19

Chemical preparation techniques involving co-precipitation of metals are used to provide microstructural characteristics necessary in order to produce ZnO varistors and their precursors for high field applications. The varistors produced have homogeneous and/or uniform dopant distributions and a submicron average grain size with a narrow size distribution. Precursor powders are prepared via chemical precipitation techniques and varistors made by sintering uniaxially and/or isostatically pressed pellets. Using these methods, varistors were made which were suitable for high-power applications, having values of breakdown field, E/sub B/, in the 10 to 100 kV/cm range, ..cap alpha.. > 30 and densities in the range of 65 to 99% of theoretical, depending on both composition and sintering temperature.
Nanocrystalline NiNd{sub 0.01}Fe{sub 1.99}O{sub 4} as a gas sensor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shinde, Tukaram J., E-mail: pshindetj@yahoo.co.in; Gadkari, Ashok B.; Jadhav, Sarjerao R.

2015-06-24

Nanocrystalline NiNd{sub 0.01}Fe{sub 1.99}O{sub 4} has been synthesized by oxalate co-precipitation method and was characterized by X-ray diffraction technique. X-ray diffraction analysis confirms the formation of single phase cubic spinel structure. Crystallite size of the ferrite lies in the nano-particle range. The gas sensing properties of nanocrystalline ferrite were studied for gases like Cl{sub 2}, LPG and C{sub 2}H{sub 5}OH. It was observed that NiNd{sub 0.01}Fe{sub 1.99}O{sub 4} is more sensitive towards chlorine followed by LPG at an operating temperature 277 °C compared to ethanol.
Process for the chemical preparation of high-field ZnO varistors

DOEpatents

Brooks, Robert A.; Dosch, Robert G.; Tuttle, Bruce A.

1987-01-01

Chemical preparation techniques involving co-precipitation of metals are used to provide micro-structural characteristics necessary in order to produce ZnO varistors and their precursors for high field applications. The varistors produced have homogeneous and/or uniform dopant distributions and a submicron average grain size with a narrow size distribution. Precursor powders are prepared via chemical precipitation techniques and varistors made by sintering uniaxially and/or isostatically pressed pellets. Using these methods, varistors were made which were suitable for high-power applications, having values of breakdown field, E.sub.B, in the 10-100 kV/cm range, .alpha.>30 and densities in the range of 65-99% of theoretical, depending on both composition and sintering temperature.
In situ surface treatment of nanocrystalline MFe2O4 (M = Co, Mg, Mn, Ni) spinel ferrites using linseed oil

NASA Astrophysics Data System (ADS)

Gherca, Daniel; Cornei, Nicoleta; Mentré, Olivier; Kabbour, Houria; Daviero-Minaud, Sylvie; Pui, Aurel

2013-12-01

This paper reports the synthesis by coprecipitation method of MFe2O4 nanoparticles using linseed oil as the in-situ surfactant. The decomposition process of the precursors and the formation process of MFe2O4 were investigated by thermogravimetric analysis and differential thermal analysis (TG-DTA). The crystal structure and surface morphology were examined by means of X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM) analysis. The results demonstrate that the surface of MFe2O4 with a diameter in the range 5-13 nm, is activated with hydrophilic groups of the surfactant which coat them and enhance the stability. Magnetic properties are discussed.
Comparative studies on structural properties and antimicrobial potential of spinel ferrite nanoparticles synthesized using various methods

NASA Astrophysics Data System (ADS)

Baraliya, Jagdish D.; Rakhashiya, Purvi M.; Patel, Pooja P.; Thaker, Vrinda S.; Joshi, Hiren H.

2017-05-01

In this study, novel multifunctional magnetic iron-based nanoparticles (CoFe2O4) coated with silica, silica-DEG (diethylene glycol), PEG (polyethylene glycol) were synthesized using Auto Combustion Method (ACM), Co-precipitation Method (COPM), Citrate Precursor Method (CPM), Flash Combustion Method (FCM). These spinel ferrite nanoparticles also contain very high antibacterial properties to fulfill the requirements of a drug delivery system so that the antibiotic concentration could be minimized. A potential delivery system could be based on a ferromagnetic fluid. The effects of various preparation methods on the physical properties of the nanoparticles were examined. The nanoparticles were also tested against four human pathogenic bacteria (Gram negative E.coli, P. aeruginosa, Gram positive S. aureus, S. pyogenus) and two fungi (C. albicans, A.niger). It was revealed that a nanoparticle has strong antibacterial activity as compared to antifungal. Further, Gram positive bacteria are more affected than Gram negative bacteria. It was also clear that different methods of coating have great influence on the antimicrobial properties. It was observed that these nanoparticles have significantly different but potentially very high antimicrobial activities against the tested organisms than found elsewhere by other nanoparticles on the same organisms.

ARSENIC TRANSPORT AND FATE IN SULFIDIC ENVIRONMENTS: AS(III) - FES INTERACTIONS

EPA Science Inventory

Arsenic mobility in groundwater and retention in aquifer materials at contaminated sites is often linked to redox processes, especially iron and sulfur cycling at redox boundaries. Important processes include adsorption or co-precipitation reactions of arsenate, arsenite, or th...
Uranium Isotopes in Calcium Carbonate: A Possible Proxy for Paleo-pH and Carbonate Ion Concentration?

NASA Astrophysics Data System (ADS)

Chen, X.; Romaniello, S. J.; Herrmann, A. D.; Wasylenki, L. E.; Anbar, A. D.

2015-12-01

Natural variations of 238U/235U in marine carbonates are being explored as a paleoredox proxy. However, in order for this proxy to be robust, it is important to understand how pH and alkalinity affect the fractionation of 238U/235U during coprecipitation with calcite and aragonite. Recent work suggests that the U/Ca ratio of foraminiferal calcite may vary with seawater [CO32-] concentration due to changes in U speciation[1]. Here we explore analogous isotopic consequences in inorganic laboratory co-precipitation experiments. Uranium coprecipitation experiments with calcite and aragonite were performed at pH 8.5 ± 0.1 and 7.5 ± 0.1 using a constant addition method [2]. Dissolved U in the remaining solution was periodically collected throughout the experiments. Samples were purified with UTEVA resin and 238U/235U was determined using a 233U-236U double-spike and MC-ICP-MS, attaining a precision of ± 0.10 ‰ [3]. Small but resolvable U isotope fractionation was observed in aragonite experiments at pH ~8.5, preferentially enriching heavier U isotopes in the solid phase. 238U/235U of the dissolved U in these experiments can be fit by Rayleigh fractionation curves with fractionation factors of 1.00002 - 1.00009. In contrast, no resolvable U isotope fractionation was detected in an aragonite experiment at pH ~7.5 or in calcite experiments at either pH. Equilibrium isotope fractionation among dissolved U species is the most likely mechanism driving these isotope effects. Our quantitative model of this process assumes that charged U species are preferentially incorporated into CaCO3 relative to the neutral U species Ca2UO2(CO3)3(aq), which we hypothesize to have a lighter equilibrium U isotope composition than the charged U species. According to this model, the magnitude of U isotope fractionation should scale with the fraction of the neutral U species in the solution, in agreement with our experimental results. These findings suggest that U isotope variations in abiotic CaCO3 reflect changes in aqueous U(VI) speciation, which are in turn a function of carbonate ion chemistry and pH. Hence, the door is opened to the development of a possible 238U/235U proxy for the carbonate ion system. [1] DeCarlo et al., (2015), GCA, 162,151-165. [2] Reeder et a., (2001), GCA, 65, 3491-3503. [3] Weyer et al., (2008) GCA 72, 345-359.
A practical grinding-assisted dry synthesis of nanocrystalline NiMoO{sub 4} polymorphs for oxidative dehydrogenation of propane

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen Miao, E-mail: chenmiao@sinochem.com; Zhejiang Chemical Industry Research Institute, Hangzhou 310023; Wu Jialing

2011-12-15

A practical two-stage reactive grinding-assisted pathway waste-free and cost-effective for the synthesis of NiMoO{sub 4} has been successfully developed. It was demonstrated that proper design in synthetic strategy for grinding plays a crucial role in determining the ultimate polymorph of NiMoO{sub 4}. Specifically, direct grinding (DG) of MoO{sub 3} and NiO rendered {alpha}-NiMoO{sub 4} after annealing, whereas sequential grinding (SG) of the two independently pre-ground oxides followed by annealing generated {beta}-NiMoO{sub 4} solid solution. Characterizations in terms of Raman and X-ray diffraction suggest the creation of {beta}-NiMoO{sub 4} precursor in the latter alternative is the key aspect for the formationmore » of {beta}-NiMoO{sub 4}. The DG-derived {alpha}-NiMoO{sub 4} tested by oxidative dehydrogenation of propane exhibited superior activity in contrast to its analog synthesized via conventional coprecipitation. It is suggested that the favorable chemical composition facilely obtained via grinding in contrast to that by coprecipitation was essential for achieving a more selective production of propylene. - Graphical Abstract: Grinding-assisted synthesis of NiMoO{sub 4} offers higher and more reproducible activities in contrast to coprecipitation for oxidative dehydrogenation of propane, and both {alpha}- and {beta}-NiMoO{sub 4} can be synthesized. Highlights: Black-Right-Pointing-Pointer NiMoO{sub 4} was prepared through grinding-assisted pathway. Black-Right-Pointing-Pointer Direct/sequential grinding rendered {alpha}-, {beta}-NiMoO{sub 4}, respectively. Black-Right-Pointing-Pointer Grinding-derived {alpha}-NiMoO{sub 4} showed high and reproducible activity for oxidative dehydrogenation of propane.« less
Kinetic and mechanism studies of the adsorption of lead onto waste cow bone powder (WCBP) surfaces.

PubMed

Cha, Jihoon; Cui, Mingcan; Jang, Min; Cho, Sang-Hyun; Moon, Deok Hyun; Khim, Jeehyeong

2011-01-01

This study examines the adsorption isotherms, kinetics and mechanisms of Pb²(+) sorption onto waste cow bone powder (WCBP) surfaces. The concentrations of Pb²(+) in the study range from 10 to 90 mg/L. Although the sorption data follow the Langmuir and Freundlich isotherm, a detailed examination reveals that surface sorption or complexation and co-precipitation are the most important mechanisms, along with possibly ion exchange and solid diffusion also contributing to the overall sorption process. The co-precipitation of Pb²(+) with the calcium hydroxyapatite (Ca-HAP) is implied by significant changes in Ca²(+) and PO₄³⁻ concentrations during the metal sorption processes. The Pb²(+) sorption onto the WCBP surface by metal complexation with surface functional groups such as ≡ POH. The major metal surface species are likely to be ≡ POPb(+). The sorption isotherm results indicated that Pb²(+) sorption onto the Langmuir and Freundlich constant q(max) and K( F ) is 9.52 and 8.18 mg g⁻¹, respectively. Sorption kinetics results indicated that Pb²(+) sorption onto WCBP was pseudo-second-order rate constants K₂ was 1.12 g mg⁻¹ h⁻¹. The main mechanism is adsorption or surface complexation (≡POPb(+): 61.6%), co-precipitation or ion exchange [Ca₃(.)₉₃ Pb₁(.)₀₇ (PO₄)₃ (OH): 21.4%] and other precipitation [Pb 50 mg L⁻¹ and natural pH: 17%). Sorption isotherms showed that WCBP has a much higher Pb²(+) removal rate in an aqueous solution; the greater capability of WCBP to remove aqueous Pb²(+) indicates its potential as another promising way to remediate Pb²(+)-contaminated media.
Evaluation of alternatives for best available technology treatment and retreatment of uranium-contaminated wastewater at the Paducah Gaseous Diffusion Plant C-400 Facility

DOE Office of Scientific and Technical Information (OSTI.GOV)

Del Cul, G.D.; Osborne, P.E.; Beck, D.E.

1991-01-01

The Paducah Gaseous Diffusion Plant (PGDP) C-400 Decontamination Facility generates aqueous solutions that originate in drum washing, machine parts and equipment cleaning, and other decontamination processes. The chemical composition of the waste depends on the particular operation involved. In general, the waste contains uranyl, fluoride, carbonate, and nitrate ions, plus soaps, detergents, secondary contaminants, and particulate matter. The uranium content is rather variable ranging between 0.5 and 30 g/l. The main contaminants are fluoride, technetium, uranium, and other heavy metals. The plan included (1) a literature search to support best available technology (BAT) evaluation of treatment alternatives, (2) a qualitymore » assurance/quality control plan, (3) suggestion of alternative treatment options, (4) bench-scale tests studies of the proposed treatment alternatives, and (5) establishment of the final recommendation. The following report records the evaluation of items (1) to (3) of the action plan for the BAT evaluation of alternatives for the treatment and retreatment of uranium-contaminated wastewater at the PGDP C-400 treatment facility. After a thorough literature search, five major technologies were considered: (1) precipitation/coprecipitation, (2) reverse osmosis, (3) ultrafiltration, (4) supported liquid membranes, and (5) ion exchange. Biosorption was also considered, but as it is a fairly new technology with few demonstrations of its capabilities, it is mentioned only briefly in the report. Based on C-400's requirements and facilities, the precipitation/coprecipitation process appears to be the best suited for use at the plant. Four different treatment options using the precipitation/coprecipitation technology are proposed. Bench-scale studies of the four options are suggested. 37 refs.« less
Preparation and characterization of host-guest system between inosine and β-cyclodextrin through inclusion mode

NASA Astrophysics Data System (ADS)

Prabu, Samikannu; Sivakumar, Krishnamurty; Swaminathan, Meenakshisundaram; Rajamohan, Rajaram

2015-08-01

Inosine is a nucleoside that is formed when hypoxanthine is attached to a ribose ring (also known as a ribofuranose) via a β-N9-glycosidic bond. Inosine is commonly found in tRNAs. Inosine (INS) has been used widely as an antiviral drug. The inclusion complex of INS with β-CDx in solution phase is studied by ground and excited state with UV-visible and fluorescence spectroscopy, respectively. A binding constant and stoichiometric ratio between INS and β-CDx are calculated by BH equation. The lifetime and relative amplitude of INS is increases with increasing the concentrations of β-CDx, confirms the formation of inclusion complex in liquid state. The solid complexes are prepared by kneading method (KM) and co-precipitation method (CP). The solid complex is characterized by Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), powder X-ray diffraction (XRD) and differential scanning colorimetry (DSC). CP method gives the solid product with good yield than that of physical mixture and KM method. The structure of complex is proposed based on the study of Patch - Dock server.
ARSENIC CONTAMINATION AT THE INDUSTRI-PLEX SUPERFUND SITE, WOBURN, MA

EPA Science Inventory

Arsenate coprecipitated with hydrous ferric oxide (HFO) was stabilized against dissolution during transformation of HFO to more crystalline iron (hydr)oxides. The rate of arsenate stabilization approximately coincided with the rate of HFO transformation at pH 6 and 40 ?C. Compa...
THE SIGNIFICANCE OF ARSENIC-BOUND SOLIDS IN DRINKING WATER DISTRIBUTION SYSTEMS

EPA Science Inventory

Sorption, co-precipitation, and oxidation-reduction reactions of arsenic at the sorbent-water interface are importent factors affecting the fate and transport of arsenic in aqueous systems. Numerous studies have concluded that arsenite (As(III) is more soluble and mobile than ar...
Enhanced terrestrial carbon preservation promoted by reactive iron in deltaic sediments

NASA Astrophysics Data System (ADS)

Shields, Michael R.; Bianchi, Thomas S.; Gélinas, Yves; Allison, Mead A.; Twilley, Robert R.

2016-02-01

We examined the role of reactive iron (FeR) in preserving organic carbon (OC) across a subaerial chronosequence of the Wax Lake Delta, a prograding delta within the Mississippi River Delta complex. We found that ~15.0% of the OC was bound to FeR, and the dominant binding mechanisms varied from adsorption in the youngest subaerial region to coprecipitation at the older, vegetated sites. The δ13C of the iron-associated OC was more negative than the total OC (mean = -2.6‰), indicating greater preference for terrestrial material and/or compounds with more negative δ13C values. However, only the adsorbed OC displayed preferential binding of lignin phenols. We estimate that ~8% of the OC initially deposited in deltaic systems is bound to FeR (equivalent to 6 × 1012 gC yr-1), and this percentage increases postdepositionally, as coprecipitation of FeR and OC allows for an even greater amount of OC to be bound to FeR.
Surface Chemical Studies on Pyrite in the Presence of Polysaccharide-Based Flotation Depressants.

PubMed

Rath; Subramanian; Pradeep

2000-09-01

The interaction of dextrin and guar gum with pyrite has been investigated through adsorption, flotation, and electrokinetic measurements. The adsorption densities of the polysaccharides onto pyrite reveal a region of higher adsorption density in the pH range 7.5-11, with a maximum around pH 10 for both polymers. The isotherms exhibit Langmuirian behavior. The adsorption density of guar gum onto pyrite is higher than that of dextrin. Electrokinetic measurements indicate a decrease in the electrophoretic mobility values in proportion to the concentration of the polymer added. Co-precipitation tests confirm polymer-ferric species interaction in the bulk solution, especially in the pH range 5.5-8.5. The pH range for higher adsorption, significant co-precipitation, and appreciable depression of pyrite encompass each other. XPS and FTIR spectroscopic studies provide evidence in support of chemical interaction between hydroxylated pyrite and the hydroxyl groups of the polymeric depressants. Copyright 2000 Academic Press.
Room Temperature Co-Precipitation Synthesis of Magnetite Nanoparticles in a Large pH Window with Different Bases.

PubMed

Mascolo, Maria Cristina; Pei, Yongbing; Ring, Terry A

2013-11-28

Magnetite nanoparticles (Fe₃O₄) represent the most promising materials in medical applications. To favor high-drug or enzyme loading on the nanoparticles, they are incorporated into mesoporous materials to form a hybrid support with the consequent reduction of magnetization saturation. The direct synthesis of mesoporous structures appears to be of interest. To this end, magnetite nanoparticles have been synthesized using a one pot co-precipitation reaction at room temperature in the presence of different bases, such as NaOH, KOH or (C₂H₅)₄NOH. Magnetite shows characteristics of superparamagnetism at room temperature and a saturation magnetization (Ms) value depending on both the crystal size and the degree of agglomeration of individual nanoparticles. Such agglomeration appears to be responsible for the formation of mesoporous structures, which are affected by the pH, the nature of alkali, the slow or fast addition of alkaline solution and the drying modality of synthesized powders.
Highly transparent Tb3Al5O12 magneto-optical ceramics sintered from co-precipitated powders with sintering aids

NASA Astrophysics Data System (ADS)

Dai, Jiawei; Pan, Yubai; Xie, Tengfei; Kou, Huamin; Li, Jiang

2018-04-01

Highly transparent terbium aluminum garnet (Tb3Al5O12, TAG) magneto-optical ceramics were fabricated from co-precipitated nanopowders with tetraethoxysilane (TEOS) as sintering aid by vacuum sintering combined with hot isostatic pressing (HIP) post-treatment. The ball milled TAG powder shows better dispersity than the as-synthesized powder, and its average particle size is about 80 nm. For the ceramic sample pre-sintered at 1720 °C for 20 h with HIP post-treated at 1700 °C for 3 h, the in-line transmittance exceeds 76% in the region of 400-1580nm (except the absorption band), reaching a maximum value of 81.8% at the wavelength of 1390 nm. The microstructure of the TAG ceramic is homogeneous and its average grain size is approximately 19.7 μm. The Verdet constant of the sample is calculated to be -182.7 rad·T-1·m-1 at room temperature.
Size-dependent magnetic anisotropy of PEG coated Fe3O4 nanoparticles; comparing two magnetization methods

NASA Astrophysics Data System (ADS)

Nayek, C.; Manna, K.; Imam, A. A.; Alqasrawi, A. Y.; Obaidat, I. M.

2018-02-01

Understanding the size dependent magnetic anisotropy of iron oxide nanoparticles is essential for the successful application of these nanoparticles in several technological and medical fields. PEG-coated iron oxide (Fe3O4) nanoparticles with core diameters of 12 nm, 15 nm, and 16 nm were synthesized by the usual co-precipitation method. The morphology and structure of the nanoparticles were investigated using transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), and X-ray diffraction (XRD). Magnetic measurements were conducted using a SQUID. The effective magnetic anisotropy was calculated using two methods from the magnetization measurements. In the first method the zero-field-cooled magnetization versus temperature measurements were used at several applied magnetic fields. In the second method we used the temperature-dependent coercivity curves obtained from the zero-field-cooled magnetization versus magnetic field hysteresis loops. The role of the applied magnetic field on the effective magnetic anisotropy, calculated form the zero-field-cooled magnetization versus temperature measurements, was revealed. The size dependence of the effective magnetic anisotropy constant Keff obtained by the two methods are compared and discussed.
Efficient production of recombinant adeno-associated viral vector, serotype DJ/8, carrying the GFP gene.

PubMed

Hashimoto, Haruo; Mizushima, Tomoko; Chijiwa, Tsuyoshi; Nakamura, Masato; Suemizu, Hiroshi

2017-06-15

The purpose of this study was to establish an efficient method for the preparation of an adeno-associated viral (AAV), serotype DJ/8, carrying the GFP gene (AAV-DJ/8-GFP). We compared the yields of AAV-DJ/8 vector, which were produced by three different combination methods, consisting of two plasmid DNA transfection methods (lipofectamine and calcium phosphate co-precipitation; CaPi) and two virus DNA purification methods (iodixanol and cesium chloride; CsCl). The results showed that the highest yield of AAV-DJ/8-GFP vector was accomplished with the combination method of lipofectamine transfection and iodixanol purification. The viral protein expression levels and the transduction efficacy in HEK293 and CHO cells were not different among four different combination methods for AAV-DJ/8-GFP vectors. We confirmed that the AAV-DJ/8-GFP vector could transduce to human and murine hepatocyte-derived cell lines. These results show that AAV-DJ/8-GFP, purified by the combination of lipofectamine and iodixanol, produces an efficient yield without altering the characteristics of protein expression and AAV gene transduction. Copyright © 2017 Elsevier B.V. All rights reserved.
Effects of Mg substitution on the structural and magnetic properties of Co0.5Ni0.5-x Mg x Fe2O4 nanoparticle ferrites

NASA Astrophysics Data System (ADS)

R, M. Rosnan; Z, Othaman; R, Hussin; Ali, A. Ati; Alireza, Samavati; Shadab, Dabagh; Samad, Zare

2016-04-01

In this study, nanocrystalline Co-Ni-Mg ferrite powders with composition Co0.5Ni0.5-x Mg x Fe2O4 are successfully synthesized by the co-precipitation method. A systematic investigation on the structural, morphological and magnetic properties of un-doped and Mg-doped Co-Ni ferrite nanoparticles is carried out. The prepared samples are characterized using x-ray diffraction (XRD) analysis, Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FESEM), and vibrating sample magnetometry (VSM). The XRD analyses of the synthesized samples confirm the formation of single-phase cubic spinel structures with crystallite sizes in a range of ˜ 32 nm to ˜ 36 nm. The lattice constant increases with increasing Mg content. FESEM images show that the synthesized samples are homogeneous with a uniformly distributed grain. The results of IR spectroscopy analysis indicate the formation of functional groups of spinel ferrite in the co-precipitation process. By increasing Mg2+ substitution, room temperature magnetic measurement shows that maximum magnetization and coercivity increase from ˜ 57.35 emu/g to ˜ 61.49 emu/g and ˜ 603.26 Oe to ˜ 684.11 Oe (1 Oe = 79.5775 A·m-1), respectively. The higher values of magnetization M s and M r suggest that the optimum composition is Co0.5Ni0.4Mg0.1Fe2O4 that can be applied to high-density recording media and microwave devices. Project supported by the Ibnu Sina Institute for Scientific and Industrial Research, Physics Department of Universiti Teknologi Malaysia and the Ministry of Education Malaysia (Grant Nos. Q.J130000.2526.04H65).
Could binary mixture of Nd-Ni ions control the electrical behavior of strontium-barium M-type hexaferrite nanoparticles?

DOE Office of Scientific and Technical Information (OSTI.GOV)

Iqbal, Muhammad Javed, E-mail: mjiqauchem@yahoo.com; Farooq, Saima

2011-05-15

Research highlights: {yields} Strontium-barium hexaferrites (Sr{sub 0.5}Ba{sub 0.5}Fe{sub 12}O{sub 19}) in single magnetoplumbite phase solid structure are synthesized by the co-precipitation method. {yields} Structural and electrical properties of Nd-Ni substituted ferrites are investigated. {yields} These ferrite materials possess high electrical resistivity (108 {Omega} cm) that is essential to curb the eddy current loss, which is pre-requisite for surface mount devices. -- Abstract: Cationic substitution in M-type hexaferrites is considered to be an important tool for modification of their electrical properties. This work is part of our comprehensive study on the synthesis and characterization of Nd-Ni doped strontium-barium hexaferrite nanomaterials ofmore » nominal composition Sr{sub 0.5}Ba{sub 0.5-x}Nd{sub x}Fe{sub 12-y}Ni{sub y}O{sub 19} (x = 0.00-0.10; y = 0.00-1.00). Doping with this binary mixture modulates the physical and electrical properties of strontium-barium hexaferrite nanoparticles. Structural and electrical properties of the co-precipitated ferrites are investigated using state-of-the-art techniques. The results of X-ray diffraction analysis reveal that the lattice parameters and cell volume are inversely related to the dopant content. Temperature dependent DC-electrical resistivity measurements infer that resistivity of strontium-barium hexaferrites decreases from 1.8 x 10{sup 10} to 2.0 x 10{sup 8} {Omega} cm whereas the drift mobility, dielectric constant and dielectric loss tangent are directly related to the Nd-Ni content. The results of the study demonstrate a relationship between the modulation of electrical properties of substituted ferrites and nature of cations and their lattice site occupancy.« less
Treatment Of Metal-Mine Effluents By Limestone Neutralization And Calcite Co-Precipitation

EPA Science Inventory

The U.S. Geological Survey - Leetown Science Center and the Colorado School of Mines have developed a remediation process for the treatment of metals in circumneutral mining influenced waters. The process involves treatment with a pulsed limestone bed (PLB) system, followed by c...
40 CFR 141.66 - Maximum contaminant levels for radionuclides.

Code of Federal Regulations, 2010 CFR

2010-07-01

... quality range andconsiderations. 1 1. Ion exchange (IE) (a) Intermediate All ground waters. 2. Point of.... Lime softening (d) Advanced All waters. 6. Green sand filtration (e) Basic. 7. Co-precipitation with Barium sulfate (f) Intermediate to Advanced Ground waters with suitable water quality. 8. Electrodialysis...
ARSENIC UPTAKE PROCESSES IN REDUCING ENVIRONMENTS: IMPLICATIONS FOR ACTIVE REMEDIATION AND NATURAL ATTENUATION

EPA Science Inventory

Reductive dissolution of iron oxyhydr(oxides) and release of adsorbed or coprecipitated arsenic is often implicated as a key process that controls the mobility and bioavailability of arsenic in anoxic environments. Yet a complete assessment of arsenic transport and fate requires...
Synthesis and Luminescence Properties of Rare Earth Activated Phosphors for near UV-Emitting LEDs for Efficacious Generation of White Light

NASA Astrophysics Data System (ADS)

Han, Jinkyu

Solid state white-emitting lighting devices based on LEDs outperform conventional light sources in terms of lifetime, durability, and luminous efficiency. Near UV-LEDs in combination with blue-, green-, and red-emitting phosphors show superior luminescence properties over the commercialized blue-emitting LED with yellow-emitting phosphors. However, phosphor development for near UV LEDs is a challenging problem and a vibrant area of research. In addition, using the proper synthesis technique is an important consideration in the development of phosphors. In this research, efficient blue-, green-yellow, red-emitting, and color tunable phosphors for near UV LEDs based white light are identified and prepared by various synthetic methods such as solid state reaction, sol-gel/Pechini, co-precipitation, hydrothermal, combustion and spray-pyrolysis. Blue-emittingLiCaPO4:Eu2+, Green/yellow-emitting (Ba,Sr)2SiO4:Eu2+, color tunable solid solutions of KSrPO4-(Ba,Ca)2SiO4:Eu 2+, and red-emitting (Ba,Sr,Ca)3MgSi2O 8:Eu2+,Mn2+ show excellent excitation profile in the near UV region, high quantum efficiency, and good thermal stability for use in solid state lighting applications. In addition, different synthesis methods are analyzed and compared, with the goal of obtaining ideal phosphors, which should have not only have high luminous output but also optimal particle size (˜150--400 nm) and spherical morphology. For Sr2SiO 4:Eu2+, the sol-gel method appears to be the best method. For Ba2SiO4:Eu2+, the co-precipitation method is be the best. Lastly, the fabrication of core/SiO2 shell particles alleviate surface defects and improve luminescence output and moisture stability of nano and micron sized phosphors. For nano-sized Y2O 3:Eu3+, Y2SiO5:Ce3+,Tb 3+, and (Ba,Sr)2SiO4, the luminescence emission intensity of the core/shell particles were significantly higher than that of bare cores. Additionally, the moisture stability is also improved by SiO 2 shells, the luminescence output of SiO2 coated green emitting Ca3SiO4Cl2:Eu2+ and blue emitting Ca2PO4Cl:Eu2+ phosphors is comparable to that of fresh phosphors although bare phosphors shows significant luminescence quenching after water exposure.

Gd-DTPA Adsorption on Chitosan/Magnetite Nanocomposites

NASA Astrophysics Data System (ADS)

Pylypchuk, Ie. V.; Kołodyńska, D.; Kozioł, M.; Gorbyk, P. P.

2016-03-01

The synthesis of the chitosan/magnetite nanocomposites is presented. Composites were prepared by co-precipitation of iron(II) and iron(III) salts by aqueous ammonia in the 0.1 % chitosan solution. It was shown that magnetite synthesis in the chitosan medium does not affect the magnetite crystal structure. The thermal analysis data showed 4.6 % of mass concentration of chitosan in the hybrid chitosan/magnetite composite. In the concentration range of initial Gd-DTPA solution up to 0.4 mmol/L, addition of chitosan to magnetite increases the adsorption capacity and affinity to Gd-DTPA complex. The Langmuir and Freundlich adsorption models were applied to describe adsorption processes. Nanocomposites were characterized by scanning electron microscopy (SEM), differential thermal analysis (DTA), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and specific surface area determination (ASAP) methods.
Synthesis, characterization, microstructure, optical and magnetic properties of strontium cobalt carbonate precursor and Sr2Co2O5 oxide material

NASA Astrophysics Data System (ADS)

Agilandeswari, K.; Ruban Kumar, A.

2014-04-01

Sr2Co2O5 ceramic synthesized by the coprecipitation of strontium cobalt carbonate method. XRD analysis shows the single phase strontianite precursor and decomposed oxide product as orthorhombic structure of Sr2Co2O5. Thermal analysis proves the Sr2Co2O5 phase formation temperature of 800 °C. SEM image indicates crystalline rod shaped carbonate precursor transformed to oxide as porous diffused sphere shape particles. Optical band gap it reveals the strontium cobalt carbonate precursor as insulating material and the Sr2Co2O5 as semiconducting nature. The room temperature magnetic study indicates the carbonate precursor as paramagnetic but its oxide Sr2Co2O5 as superparamagnetic behavior.
Synthesis and electrochemical characterization of TixTayAlzN1-δOγ for fuel cell catalyst supports

NASA Astrophysics Data System (ADS)

Wakabayashi, Ryo H.; Abruña, Héctor D.; DiSalvo, Francis J.

2017-02-01

Quinary TixTayAlzN1-δOγ of various compositions have been prepared by a co-precipitation method followed by ammonolysis. The nitride samples were examined as potential catalyst supports in polymer electrolyte membrane fuel cells. The nitride products crystallized in the rock salt (NaCl) structure over a wide range of compositions. The addition of Ta and Al was highly beneficial towards improving the chemical and electrochemical stability of TiN, without a significant loss of electrical conductivity. Platinum particles were successfully deposited on the (oxy)nitride samples, and the composite samples at some compositions were found to be comparable to Pt/carbon in their stability and catalytic activity even without optimizing the Pt deposition and dispersion processes.
Conductivity and Dielectric Relaxation Properties of Annealed Cr-Substituted Ni-Ferrite Nanoparticles

NASA Astrophysics Data System (ADS)

El-Ghazzawy, E. H.

2017-10-01

Nanocrystalline NiCr x Fe2- x O4 spinel samples with x = 0.1 and 0.2 have been synthesized by coprecipitation method and annealed at 620°C and 1175°C for 4 h. Their electrical properties were investigated as functions of frequency in the range of 100 Hz to 100 kHz and temperature in the range of 308 K to 358 K. The dielectric constant ( ɛ^' } ) and dielectric loss factor ( {tan} δ ) appeared to decrease with increasing frequency, while the alternating-current (AC) conductivity ( σ^' } ) increased. These dielectric parameters increased with increasing temperature. On the other hand, impedance spectroscopy gave Cole-Cole plots with only one semicircular arc for all the samples, indicating that the grain-boundary contribution was dominant in the conduction mechanism.
In vitro simulation studies of silica deposition induced by lignin from rice*

PubMed Central

Fang, Jiang-Yu; Ma, Xue-Long

2006-01-01

To reveal the possible mechanism of silica deposition in higher plants, lignin was isolated from rice straw following a modified method to conduct a simulation experiment in vitro. UV and infrared absorption spectra showed that the substance had the unique characteristics of pure lignin. The presence of silicon in the precipitation was revealed by TEM (transmission electron microscopy) with EDXA (energy dispersive X-ray analysis) device. It was found that in the borax solution where lignin precipitation occurred silica-lignin co-precipitation was produced but not in the DMSO solution where lignin was broken into its composition compounds and did not precipitate. This means that it is macromolecular lignin itself but not its compounds that could induce silica deposition in higher plants. PMID:16532527
DOE Office of Scientific and Technical Information (OSTI.GOV)

Dubey, P., E-mail: purushd@barc.gov.in; Sharma, V. K.; Mitra, S.

Synthetic hydroxyapatite (HAp) is an important material in biomedical engineering due to its excellent biocompatibility and bioactivity. Here we report dynamics of cetyltrimethylammonium bromide (CTAB) in HAp composite, prepared by co-precipitation method, as studied by quasielastic neutron scattering (QENS) technique. It is found that the observed dynamics involved two time scales associated with fast torsional motion and segmental motion of the CTAB monomers. In addition to segmental motion of the hydrogen atoms, few undergo torsional motion as well. Torsional dynamics was described by a 2-fold jump diffusion model. The segmental dynamics of CTAB has been described assumimg the hydrogen atomsmore » undergoing diffusion inside a sphere of confined volume. While the diffusivity is found to increase with temperature, the spherical volumes within which the hydrogen atoms are undergoing diffusion remain almost unchanged.« less
In vitro genotoxicity and cytotoxicity of polydopamine-coated magnetic nanostructures.

PubMed

Woźniak, Anna; Walawender, Magdalena; Tempka, Dominika; Coy, Emerson; Załęski, Karol; Grześkowiak, Bartosz F; Mrówczyński, Radosław

2017-10-01

Synthesis of magnetic nanoparticles and magnetic nanoclusters was performed by the co-precipitation method or solvothermal synthesis, respectively, followed by oxidative polymerization of dopamine, resulting in a polydopamine (PDA) shell. The nanomaterials obtained were described using TEM, FTIR and magnetic measurements. For the first time, cyto- and genotoxicity studies of polydopamine-coated nanostructures were performed on cancer and normal cell lines, providing in-depth insight into the toxicity of such materials. The tests conducted, e.g. ROS, apoptosis and DNA double-break of the nanomaterials obtained revealed the low toxicity of these structures. Thus, these results prove the biocompatibility and low genotoxicity of these materials and provide new data on the toxicity of PDA-coated materials, which is of great importance for their biomedical application. Copyright © 2017 Elsevier Ltd. All rights reserved.
Thermoluminescent properties of ZnS:Mn nanocrystalline powders.

PubMed

Ortiz-Hernández, Arturo Agustín; Méndez García, Víctor Hugo; Pérez Arrieta, María Leticia; Ortega Sígala, José Juan; Araiza Ibarra, José de Jesús; Vega-Carrillo, Héctor Rene; Falcony Guajardo, Ciro

2015-05-01

Thermoluminescent ZnS nanocrystals doped with Mn(2+) ions were synthesized by chemical co-precipitation method. From X-ray diffraction studies it was observed that the synthesized nanoparticles have cubic zinc blende structure with average sizes of about 40-50nm. Morphology was analyzed by TEM. Photoluminescence studies showed two transitions, one of them close to 396nm and other close to 598nm, which is enhanced with increasing dopant concentration, this behavior was also observed in the cathodoluminescence spectrum. The thermoluminescence gamma dose-response has linear behavior over dose range 5-100mGy, the glow curve structure shows two glow peaks at 436K and at 518K that were taken into account to calculate the kinetic parameters using the Computerized Glow Curve Deconvolution procedure. Copyright © 2015 Elsevier Ltd. All rights reserved.
Lignin-based Biochar/graphene Oxide Composites as Supercapacitor Electrode Materials

NASA Astrophysics Data System (ADS)

Cai, Z.; Jiang, C.; Xiao, X. F.; Zhang, Y. S.; Liang, L.

2018-05-01

The lignin-based biochar/graphene composites were effectively obtained via an easy and rapid co-precipitation method. The chemical structure, microstructure, electrochemical properties of lignin/graphene oxide composites before and after carbonization were investigated by Fourier transformation infrared spectrum (FTIR), Scanning electron microscope (SEM), x-ray diffraction (XRD) and cyclic voltammetry (CV). FTIR results confirmed that the oxygen-containing groups of lignin, GO and their composites were partly removed after 800 °C carbonization and GO had a positive impact on the formation of graphitic structure for lignin. XRD results showed that lignin could completely block the restacking of GO sheets. The electrochemical test presented that lignin/graphene oxide composites exhibited a typical CV curve and the specific capacitance reached ∼103F/g at a scan rate of 20mv/s.
Bio-Diesel Production from Deoxygenation Reaction Over Ce0.6Zr0.4O2 Supported Transition Metal (Ni, Cu, Co, and Mo) Catalysts.

PubMed

Shim, Jae-Oh; Jeong, Dae-Woon; Jang, Won-Jun; Jeon, Kyung-Won; Jeon, Byong-Hun; Kim, Seong-Heon; Roh, Hyun-Seog; Na, Jeong-Geol; Han, Sang Sup; Ko, Chang Hyun

2016-05-01

Ce0.6Zr0.4O2 supported transition metal (Me = Ni, Cu, Co, and Mo) catalysts have been investigated to screen for the catalytic activity and selectivity for deoxygenation reaction of oleic acid. Me-Ce0.6Zr0.4O2 catalysts were prepared by a co-precipitation method. Ni-Ce0.6Zr0.4O2 catalyst exhibited much higher oleic acid conversion, selectivity for C9 to C17 compounds, and oxygen removal efficiency than the others. This is mainly ascribed to the presence of free Ni species, synergy effects between Ni and Ce0.6Zr0.4O2, and the highest BET surface area.
Influence of Fabrication Conditions on the Structural and the Magnetic Properties of Co-doped BaFe12O19 Hexaferrites

NASA Astrophysics Data System (ADS)

Tran, Ngo; Kim, Deok Hyeon; Lee, Bo Wha

2018-03-01

BaFe11CoO19 hexaferrites were prepared by using a co-precipitation method and heat treatment. By changing the ion molar ratio of (Fe + Co)/Ba = ( x + 1)/1, we found a clear difference in the crystalline structural and magnetic properties. Particularly, the magnetic properties became optimal at x = 11 - 13 based on the saturation magnetization and coercivity values. The effects of heat treatment on the morphological, structural and magnetic properties were assessed. With the results of thermal gravimetric analyses, X-ray diffraction patterns, and magnetic-field-dependent magnetization, we found that M-type hexaferrite nanocrystals start being formed at a temperature of 650°C, which was much lower than temperatures reported previously.
Fe3O4 nanoparticles decorated MWCNTs @ C ferrite nanocomposites and their enhanced microwave absorption properties

NASA Astrophysics Data System (ADS)

Zhang, Kaichuang; Gao, Xinbao; Zhang, Qian; Chen, Hao; Chen, Xuefang

2018-04-01

Fe3O4 nanoparticles decorated MWCNTs @ C ferrite nanocomposites were synthesized using a co-precipitation method and a calcination process. As one kind absorbing material, we researched the electromagnetic absorption properties of the composites that were mixed with a filler loading of 80 wt% paraffin. In addition, we studied the influence of the magnetic nanoparticle content on the absorbing properties. The results showed that the frequency corresponding to the maximum absorptions shifted to lower frequency when the magnetic nanoparticles content increased. The Fe3O4 nanoparticles decorated MWCNTs @ C ferrite nanocomposites with approximately 60% Fe3O4 nanoparticles showed the best electromagnetic absorption properties. The maximum reflection loss was -52.47 dB with a thickness of 2.0 mm at 10.4 GHz.
Characterization and synergetic antibacterial properties of ZnO and CeO2 supported by halloysite

NASA Astrophysics Data System (ADS)

Shu, Zhan; Zhang, Yi; Ouyang, Jing; Yang, Huaming

2017-10-01

A novel antibacterial nanocomposite, CeO2-ZnO/HNTs was prepared by a homogeneous co-precipitation method in ethanol solution. ZnO and CeO2 nanoparticles with sizes of approximately 8 and 4 nm, respectively, were dispersively precipitated onto the surface of halloysite nanotubes (HNTs). HNTs served as a template for reducing the agglomeration of ZnO nanoparticles and improving the interface reactions between the nanocomposite and bacteria cells. CeO2 nanoparticles were introduced to suppress the recombination of electron-hole pairs, and narrow the energy gap of ZnO nanoparticles. The synergistic effects of ZnO, CeO2 nanoparticles and HNTs led to the superior antibacterial activity of the CeO2-ZnO/HNTs nanocomposite against gram-negative Escherichia coli.
Hierarchical La0.7Ce0.3FeO3/halloysite nanocomposite for photocatalytic degradation of antibiotics

NASA Astrophysics Data System (ADS)

Li, Xiazhang; Zhu, Wei; Yan, Xiangyu; Lu, Xiaowang; Yao, Chao; Ni, Chaoying

2016-08-01

The hierarchical La0.7Ce0.3FeO3/halloysite nanotubes (HNTs) composites have been successfully prepared via sol-gel method. XRD and TEM characterizations indicated that the sheet-like La0.7Ce0.3FeO3 coupled with the co-precipitated CeO2 were evenly deposited onto the surface of halloysite. The photocatalytic degradation of chlortetracycline under visible light irradiation using La0.7Ce0.3FeO3/HNTs as catalyst was evaluated by high-performance liquid chromatography, which exhibited remarkable photocatalytic activity with the removal rate up to 99 % in 90 min, due to the formation of "solid solution/co-precipitation" heterostructure as well as the excellent adsorptive capability of halloysite for antibiotics.
Sodium Dodecyl Sulphate-Supported Nanocomposite as Drug Carrier System for Controlled Delivery of Ondansetron.

PubMed

Sharma, Gaurav; Naushad, Mu; Thakur, Bharti; Kumar, Amit; Negi, Poonam; Saini, Reena; Chahal, Anterpreet; Kumar, Ashok; Stadler, Florian J; Aqil, U M H

2018-02-27

Sodium dodecyl sulphate-supported iron silicophosphate (SDS/FeSP) nanocomposite was successfully fabricated by the co-precipitation method. The SDS/FeSP nanocomposite was investigated as a drug carrier for ondansetron. The cumulative drug release of ondansetron was observed at various pH values for different time intervals, i.e., from 20 min to 48 h. A ranking of the drug release was observed at different pHs; pH 2.2 > saline (pH 5.5) > pH 7.4 > pH 9.4 > distilled water. Maximum release of encapsulated drug was found to be about 45.38% at pH 2.2. The cell viability tests of SDS/FeSP nanocomposite concluded that SDS/FeSP nanocomposite was non-cytotoxic in nature.
Treatment Of Metal-Mine Effluents By Limestone Neutralization And Calcite Co-Precipitation (Presentation)

EPA Science Inventory

The U.S. Geological Survey - Leetown Science Center and the Colorado School of Mines have developed a remediation process for the treatment of metals in circumneutral mining influenced waters. The process involves treatment with a pulsed limestone bed (PLB) system, followed by c...
AN INVESTIGATION OF ARSENIC MOBILITY FROM IRON OXIDE SOLIDS PRODUCED DURING DRINKING WATER TREATMENT

EPA Science Inventory

The Arsenic Rule under the Safe Drinking Water Act will require certain drinking water suppliers to add to or modify their existing treatment in order to comply with the regulations. One of the treatment options is iron co-precipitation. This treatment is attractive because ars...
ARSENIC MOBILITY FROM IRON OXIDE SOLIDS PRODUCED DURING WATER TREATMENT

EPA Science Inventory

The Arsenic Rule under the Safe Drinking Water Act will require certain drinking water suppliers to add to or modify their existing treatment in order to comply with the new 10 ppb arsenic standard. One of the treatment options is co-precipitation of arsenic with iron. This tre...
THE INFLUENCE OF IRON AND SULFUR CYCLING ON ARSENIC PARTITIONING IN SOILS AND SEDIMENTS

EPA Science Inventory

Field evidence suggests that arsenic solid-solution partitioning in natural systems is often tied to iron and sulfur cycling. This is likely due to the coprecipitation of arsenic as a trace component in poorly crystalline iron oxides and monosulfides. However, there is limited ...
A novel method for the elaboration of hydroxyapatite with high purity by sol-gel using the albumin and comparison with the classical methods

NASA Astrophysics Data System (ADS)

Mohammed, Eddya; Bouazza, Tbib; Khalil, El-Hami

2018-02-01

In this paper, we report the first synthesis of hydroxyapatite (Hap) by sol-gel using the albumin (egg white) compared with the four classical elaboration methods such as co-precipitation, solid state, and solid-liquid samples of hydroxyapatite. We use a reference sample of hydroxyapatite bought from Fluka Chemika company (Lot and Filling code 385330/1 14599). All samples are characterized by X-ray diffraction (XRD), Uv-visible spectroscopy (Uv-Vis), and Fourier transforms infrared spectroscopy (FT-IR). The XRD study showed the existence of a Hexagonal phase for all our samples prepared in our laboratory and an orthorhombic phase for the Fulka Chemika sample of Hap (Lot and Filling code 385330/1 14599). The study by Uv-visible spectroscopy was performed to determine and compare the optical gap and the disorder of each sample of Hap. The FT-IR spectroscopy demonstrated that all our Hap samples had a similar mode of vibration of the chemical bonds (OH-) and (PO4)3-.

Photoluminescence properties and energy transfer of color tunable MgZn₂(PO₄)₂:Ce³⁺,Tb³⁺ phosphors.

PubMed

Xu, Mengjiao; Wang, Luxiang; Jia, Dianzeng; Zhao, Hongyang

2015-11-21

A series of Ce(3+)/Tb(3+) co-doped MgZn2(PO4)2 phosphors have been synthesized by the co-precipitation method. Their structure, morphology, photoluminescence properties, decay lifetime, thermal stability and luminous efficiency were investigated. The possible energy transfer mechanism was proposed based on the experimental results and detailed luminescence spectra and decay curves of the phosphors. The critical distance between Ce(3+) and Tb(3+) ions was calculated by both the concentration quenching method and the spectral overlap method. The energy transfer mechanism from the Ce(3+) to Tb(3+) ion was determined to be dipole-quadrupole interaction, and the energy transfer efficiency was 85%. By utilizing the principle of energy transfer and appropriate tuning of Ce(3+)/Tb(3+) contents, the emission color of the obtained phosphors can be tuned from blue to green light. The MgZn2(PO4)2:Ce(3+),Tb(3+) phosphor is proved to be a promising UV-convertible material capable of green light emitting in UV-LEDs due to its excellent thermal stability and luminescence properties.
Improvement of sulfur resistance of Pd/Ce-Zr-Al-O catalysts for CO oxidation

NASA Astrophysics Data System (ADS)

Shin, Haebin; Baek, Minsung; Ro, Youngsoo; Song, Changyeol; Lee, Kwan-Young; Song, In Kyu

2018-01-01

Two kinds of mesoporous ceria-zirconia-alumina supports were prepared by a single-step epoxide-driven sol-gel method (SGCZA) and by a co-precipitation method (PCZA). Palladium catalysts supported on these materials were then prepared by a wet impregnation method (Pd/SGCZA and Pd/PCZA). The prepared catalysts were applied to the CO oxidation reaction before and after sulfur aging. XRD and N2 adsorption-desorption analyses revealed that these two catalysts retained different physicochemical properties. Pd/SGCZA had higher surface area and larger pore volume than Pd/PCZA before and after sulfur aging. TPR (Temperature-programmed reduction), CO chemisorption, FT-IR, and XPS analyses showed that the catalysts were differently influenced by sulfur species. Pd/SGCZA formed less sulfate and retained higher palladium dispersion than Pd/PCZA after sulfur aging. In the CO oxidation, Pd/PCZA showed better activity than Pd/SGCZA before sulfur aging. However, Pd/SGCZA showed higher CO conversion than Pd/PCZA after sulfur aging. We concluded that Pd/SGCZA was less poisoned by sulfur species than Pd/PCZA.
Different preparation methods and characterization of magnetic maghemite coated with chitosan

NASA Astrophysics Data System (ADS)

Hojnik Podrepšek, Gordana; Knez, Željko; Leitgeb, Maja

2013-06-01

The preparation of maghemite (γ-Fe2O3) micro- and nanoparticles coated with chitosan, used as carriers for immobilized enzymes, was investigated. γ-Fe2O3 nanoparticles were synthesized by coprecipitation of Fe2+ and Fe3+ ions in the presence of ammonium. They were coated with chitosan by the microemulsion process, suspension cross-linking technique, and covalent binding of chitosan on the γ-Fe2O3 surface. The methods distinguished the concentration of chitosan, concentration of acetic acid solution, concentration of a cross-linking agent, temperature of synthesis, pH of the medium, and time of synthesis. γ-Fe2O3 micro- and nanoparticles coated with chitosan prepared after three preparation methods were evaluated by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy analysis, energy dispersive spectrometry, thermogravimetric analysis, differential scanning calorimetry analysis, vibrating sample magnetometry, dynamic light scattering, laser diffraction granulometry, and X-ray diffractometry. These positive attributes demonstrated that these magnetic micro- and nanoparticles coated with chitosan may be used as a promising carrier for further diverse biomedical applications.
Two micro-scale protocols for the isolation of DNA from polysaccharide-rich plant tissue.

PubMed

Shepherd, Lara D; McLay, Todd G B

2011-03-01

The high polysaccharide content of some plant species hinders the successful isolation of their DNA. As an alternative to the macro-extraction methods previously published for polysaccharide-rich plants, we present two techniques (STE/CTAB and HEPES/CTAB), which are performed in microcentrifuge tubes. These protocols are suitable for small amounts of silica gel-preserved plant tissue such as are commonly available from endangered plants. The critical step to remove polysaccharides was performing initial washes in either STE (0.25 M sucrose, 0.03 M Tris, 0.05 M EDTA) or HEPES (2% β-mercaptoethanol, 0.2% PVP, 0.1 M HEPES, pH 8.0) buffer. Precipitating the DNA at room temperature with isopropanol also aided in decreasing polysaccharide co-precipitation. Of the two protocols we present the STE/CTAB method has the advantages of being more cost-effective and avoiding the use of the hazardous chemical β-mercaptoethanol.
Gene Transfer in Eukaryotic Cells Using Activated Dendrimers

NASA Astrophysics Data System (ADS)

Dennig, Jörg

Gene transfer into eukaryotic cells plays an important role in cell biology. Over the last 30 years a number of transfection methods have been developed to mediate gene transfer into eukaryotic cells. Classical methods include co-precipitation of DNA with calcium phosphate, charge-dependent precipitation of DNA with DEAE-dextran, electroporation of nucleic acids, and formation of transfection complexes between DNA and cationic liposomes. Gene transfer technologies based on activated PAMAM-dendrimers provide another class of transfection reagents. PAMAM-dendrimers are highly branched, spherical molecules. Activation of newly synthesized dendrimers involves hydrolytic removal of some of the branches, and results in a molecule with a higher degree of flexibility. Activated dendrimers assemble DNA into compact structures via charge interactions. Activated dendrimer - DNA complexes bind to the cell membrane of eukaryotic cells, and are transported into the cell by non-specific endocytosis. A structural model of the activated dendrimer - DNA complex and a potential mechanism for its uptake into cells will be discussed.
The Microstructure Analysis of Barium M- Hexaferrite Particles Coated by Pani Conducting Material with In Situ Polymerization Process

NASA Astrophysics Data System (ADS)

Zainuri, M.; Amalia, L.

2017-05-01

Barium M-Hexaferrite (BaM) was synthesized by coprecipitation method and doped with Zn. Polyaniline (PANI) was synthesized by chemically and doped DBSA. The composite of PANI/BaM was synthesized by in situ polymerization method. The phase identification of the sample was performed by XRD, FTIR and SEM. Based on XRD data, the phase composition of BaM and hematite are 85.52 % and 14.48%. The characteristic peaks of PANI occur at 3435, 1637, 1473, 1298, 1127, 1009, and 799 cm-1. The characteristic metal oxide stretching peaks of BaM occurs at 575 and 437 cm-1. There is no phase changing in PANI/BaM composite. Based on SEM photography, the shape of BaM is hexagonal. The particle size of BaM powder ranges from 400-700 nm. The qualitative interfacial bonding between PANI and BaM particles are conducted very well and the both materials have good wettability.
[The progress in speciation analysis of trace elements by atomic spectrometry].

PubMed

Wang, Zeng-Huan; Wang, Xu-Nuo; Ke, Chang-Liang; Lin, Qin

2013-12-01

The main purpose of the present work is to review the different non-chromatographic methods for the speciation analysis of trace elements in geological, environmental, biological and medical areas. In this paper, the sample processing methods in speciation analysis were summarized, and the main strategies for non-chromatographic technique were evaluated. The basic principles of the liquid extractions proposed in the published literatures recently and their advantages and disadvantages were discussed, such as conventional solvent extraction, cloud point extraction, single droplet microextraction, and dispersive liquid-liquid microextraction. Solid phase extraction, as a non-chromatographic technique for speciation analysis, can be used in batch or in flow detection, and especially suitable for the online connection to atomic spectrometric detector. The developments and applications of sorbent materials filled in the columns of solid phase extraction were reviewed. The sorbents include chelating resins, nanometer materials, molecular and ion imprinted materials, and bio-sorbents. Other techniques, e. g. hydride generation technique and coprecipitation, were also reviewed together with their main applications.
Study of lattice strain and optical properties of nanocrystalline SnO2

NASA Astrophysics Data System (ADS)

Ahmad, Naseem; Khan, Shakeel; Bhargava, Richa; Ansari, Mohd Mohsin Nizam

2018-05-01

Nanocrystalline SnO2 has been synthesized by co-precipitation method by using two solvents (water and ethylene glycol). The structure and surface morphology were investigated using XRD and scanning electron microscope (SEM). The optical properties were studied using diffused reflectance spectroscopy (DRS). From the XRD analysis, the prepared materials are found to be pure crystalline with tetragonal rutile structure. The lattice strain and crystallite size, were calculated using Williamson-Hall method, are found to be 0.00413 & 16.3 nm in water assisted SnO2 and 0.00495 & 35.6 nm for EG assisted SnO2. Study of surface morphology of the samples was carried out using SEM. It has been seen that the solvents which are used in synthesis can also alter the optical properties of the materials. The optical band gap of the water based SnO2 and EG based SnO2 are found to be 3.92eV and 3.86eV respectively.
Effect of reducing agents on low-temperature synthesis of nanostructured LiFePO4

NASA Astrophysics Data System (ADS)

Kulka, Andrzej; Walczak, Katarzyna; Zając, Wojciech; Molenda, Janina

2017-09-01

Simple co-precipitation synthesis procedure yielding nanometric LiFePO4 with enhanced electrochemical properties without any post-synthesis heat treatment is presented. XRD, SEM and TEM analysis of the obtained powders revealed platelet crystallites and well crystalized bulk structure. Effective way of decreasing amount of Fe3+ containing phases by addition of reducing agents (KI, (NH4)2S2O3, glucose and the atmosphere of 5%H2-95%Ar) during low-temperature (107 °C) synthesis is described. The traditional analytical chemistry methods or the Mӧssbauer spectroscopy methods revealed that utilization of selected reducing agents diminished Fe3+ concentration from 25 to 12 at%. The constructed cells with optimized LiFePO4 as a cathode material showed superior electrochemical performances, including high reversible capacity up to 162 mAh/g at C/10 current discharge rate, flat voltage plateau with a value close to 3.45 V vs. Li0/+.
Preparation and characterization of functional material based on hybrid polymer composites

NASA Astrophysics Data System (ADS)

Agusu, La; Amiruddin; Taswito, Chen Chen; Herdianto; Zamrun, Muh.

2016-08-01

The microstructures and properties of hybrid polymer composites based on polyaniline (PANi)/γ-Fe2O3 nanoparticles/TiO2/carbon have been investigated for multifunctional applications such as heavy metal removal and initial study for radar absorbing material application. γ-Fe2O3 nanoparticles with spherical shape were synthetized by a coprecipitation method from iron sand. By activating the polyethylene glycol (PEG-400) coated carbon of coconut shell, the homogenous shape and size of carbon was achieved. Then, γ- Fe2O3, TiO2, and carbon were mixed with PANi by an in situ polymerization method at low temperature 0-5 oC. Characterization process involved XRD, SEM, FTIR, VSM, and DC conductivity measurements. For radar absorber application, the functionalized polymer composites showed good electrical conductivity 0.45 S/cm to absorb the incoming electromagnetic energy. An efficient and effective reduction of Pb2+ ion from the water has been achieved by using this material.
A comparison of corrosion inhibition of magnesium aluminum and zinc aluminum vanadate intercalated layered double hydroxides on magnesium alloys

NASA Astrophysics Data System (ADS)

Guo, Lian; Zhang, Fen; Lu, Jun-Cai; Zeng, Rong-Chang; Li, Shuo-Qi; Song, Liang; Zeng, Jian-Min

2018-04-01

The magnesium aluminum and zinc aluminum layered double hydroxides intercalated with NO3 -(MgAl-NO3-LDH and ZnAl-NO3-LDH) were prepared by the coprecipitation method, and the magnesium aluminum and the zinc aluminum layered double hydroxides intercalated with VO x -(MgAl-VO x -LDH and ZnAl-VO x -LDH) were prepared by the anion-exchange method. Morphologies, microstructures and chemical compositions of LDHs were investigated by SEM, EDS, XRD, FTIR, Raman and TG analyses. The immersion tests were carried to determine the corrosion inhibition properties of MgAl-VO x -LDH and ZnAl-VO x -LDH on AZ31 Mg alloys. The results showed that ZnAl-VO x -LDH possesses the best anion-exchange and inhibition abilities. The influence of treatment parameters on microstructures of LDHs were discussed. Additionally, an inhibition mechanism for ZnAl-VO x -LDH on the AZ31 magnesium alloy was proposed and discussed.
Magnetic liposomes based on nickel ferrite nanoparticles for biomedical applications.

PubMed

Rodrigues, Ana Rita O; Gomes, I T; Almeida, Bernardo G; Araújo, J P; Castanheira, Elisabete M S; Coutinho, Paulo J G

2015-07-21

Nickel ferrite nanoparticles with superparamagnetic behavior at room temperature were synthesized using a coprecipitation method. These magnetic nanoparticles were either covered with a lipid bilayer, forming dry magnetic liposomes (DMLs), or entrapped in liposomes, originating aqueous magnetoliposomes (AMLs). A new and promising method for the synthesis of DMLs is described. The presence of the lipid bilayer in DMLs was confirmed by FRET (Förster Resonance Energy Transfer) measurements between the fluorescent-labeled lipids NBD-C12-HPC (NBD acting as a donor) included in the second lipid layer and rhodamine B-DOPE (acceptor) in the first lipid layer. An average donor-acceptor distance of 3 nm was estimated. Assays of the non-specific interactions of magnetoliposomes with biological membranes (modeled using giant unilamellar vesicles, GUVs) were performed. Membrane fusion between both aqueous and dry magnetoliposomes and GUVs was confirmed by FRET, which is an important result regarding applications of these systems both as hyperthermia agents and antitumor drug nanocarriers.
The Influence of Al+++ Substitution for Fe+++ in M-Type Ba Ferrite Powder on the Intrinsic Coercivity HcJ

NASA Astrophysics Data System (ADS)

Zheng, Zong-Yu; Feng, Jie; Mei, Xue-Ming; Guo, Bi-Jun; Zhang,

1990-05-01

The influence of Al+++ Substitution for Fe+++ in M-type Ba ferrite on the magnetocrystalline anisotropy field HA and the critical single-domain radius Rc has been studied by Haneda and Kojima. It is difficult to obtain HcJ values agreeing with theoretical results for the reason that the HcJ is very sensitive to the preparation method. We have been developing a new method called “coprecipitation combined with high-temperature melting.” It offers a suitable condition for studying the rule of HcJ of Ba Fe12-xAlxO19. Our results conformed to the effects calculated by Haneda and Kojima. The highest level of HcJ in our experiment reached 16000 Oe. We have fabricated plastic sheet magnets from the superhigh HcJ ferrite powder and padded the soft ferrite core with this sheet magnet to adjust the bias magnetic field. This ferrite core can be improved and the weight and size of the device can be reduced.
Polymeric phase change nanocomposite (PMMA/Fe:ZnO) for electronic packaging application

NASA Astrophysics Data System (ADS)

Maji, Pranabi; Choudhary, Ram Bilash; Majhi, Malati

2018-01-01

This paper reported the effect of Fe-doped ZnO (Fe:ZnO) nanoparticles on the structural, morphological, thermal, optical and dielectric properties of PMMA matrix. Fe-doped ZnO nanoparticle was synthesized by co-precipitation method, after its surface modification incorporated into the PMMA matrix by free radical polymerization method. The phase analysis and crystal structure were investigated by XRD and FTIR technique. These studies confirmed the chemical structure of the PMMA/Fe:ZnO nanocomposite. FESEM image showed the pyramidal shape and high porosity of PMMA/Fe:ZnO nanocomposite. Thermal analysis of the sample was carried out by thermo-gravimetric analyzer. PMMA/Fe:ZnO nanocomposite was found to have better thermal stability compared to pure one. Broadband dielectric spectroscopic technique was used to investigate the transition of electrical properties of Fe-doped ZnO nanoparticle reinforced PMMA matrix in temperature range 313-373 K. The results elucidated a phase transition from glassy to rubbery state at 344 K.
Size and shape effects in β-NaGdF4: Yb3+, Er3+ nanocrystals

NASA Astrophysics Data System (ADS)

Noculak, Agnieszka; Podhorodecki, Artur

2017-04-01

Three sets of β-NaGdF4:Yb3+, Er3+ nanocrystals (NCs) with different shapes (spherical and more complex flower shapes), different sizes (6-17 nm) and Yb3+ concentrations (2%-15%) were synthesized by a co-precipitation method using oleic acid as a stabilizing agent. The uncommon, single-crystalline flower-shaped NCs were obtained by simply adjusting the fluorine-to-lanthanides molar ratio. Additionally, some of the NCs with different sizes have been covered by the un-doped shell. The crystal phase, shapes and sizes of all NCs were examined using transmission electron microscopy and x-ray diffraction methods. Simultaneously, upconversion luminescence and lifetimes, under 980 nm excitation, were measured and the changes in green to red (G/R) emission ratios as well as emission decay times were correlated with the evolution of nanocrystal sizes and surface to volume ratios. Three different mechanisms responsible for the changes in G/R ratios were presented and discussed.
Hematite from Natural Iron Stones as Microwave Absorbing Material on X-Band Frequency Ranges

NASA Astrophysics Data System (ADS)

Zainuri, Mochamad

2017-05-01

This study has been investigated the effect of hematite as microwave absorbing materials (RAM) on X-Band frequency ranges. Hematite was succesfully processed by coprecipitation method and calcined at 500 °C for 5 hour. It was synthesized from natural iron stones from Tanah Laut, South Kalimantan, Indonesia. The products were characterized by X-ray diffraxtion (XRD), conductivity measurement, Vibrating Sample Magnetometer (VSM), and Vector Network Analyzer (VNA). The result was shown that hematite has conductivity value on (2.5-3).10-7 S/cm and be included as dielectric materials. The hysterisis curve was shown that hematite was a super paramagnetic materials. The product was mixed on paint with procentage 10% of total weight and coated on steel grade AH36 with spray methods. Then, the maximum of reflection loss on x - band’s frequency range (8,2-12,4) GHz was -7 dB on frequency of 10.5 GHz. It mean that almost 50% electromagnetic energy was absorbed by hematite.
Method for making fine and ultrafine spherical particles of zirconium titanate and other mixed metal oxide systems

DOEpatents

Hu, Michael Z.

2006-05-23

Disclosed is a method for making amorphous spherical particles of zirconium titanate and crystalline spherical particles of zirconium titanate comprising the steps of mixing an aqueous solution of zirconium salt and an aqueous solution of titanium salt into a mixed solution having equal moles of zirconium and titanium and having a total salt concentration in the range from 0.01 M to about 0.5 M. A stearic dispersant and an organic solvent is added to the mixed salt solution, subjecting the zirconium salt and the titanium salt in the mixed solution to a coprecipitation reaction forming a solution containing amorphous spherical particles of zirconium titanate wherein the volume ratio of the organic solvent to aqueous part is in the range from 1 to 5. The solution of amorphous spherical particles is incubated in an oven at a temperature .ltoreq.100.degree. C. for a period of time .ltoreq.24 hours converting the amorphous particles to fine or ultrafine crystalline spherical particles of zirconium titanate.
Synthesis and characterization of a magnetic adsorbent from negatively-valued iron mud for methylene blue adsorption.

PubMed

Liu, Jiancong; Yu, Yang; Zhu, Suiyi; Yang, Jiakuan; Song, Jian; Fan, Wei; Yu, Hongbin; Bian, Dejun; Huo, Mingxin

2018-01-01

With increasing awareness of reduction of energy and CO2 footprint, more waste is considered recyclable for generating value-added products. Here we reported the negatively-valued iron mud, a waste from groundwater treatment plant, was successfully converted into magnetic adsorbent. Comparing with the conventional calcination method under the high temperature and pressure, the synthesis of the magnetic particles (MPs) by Fe2+/Fe3+ coprecipitation was conducted at environment-friendly condition using ascorbic acid (H2A) as reduction reagent and nitric acid (or acid wastewater) as leaching solution. The MPs with major component of Fe3O4 were synthesized at the molar ratio (called ratio subsequently) of H2A to Fe3+ of iron mud ≥ 0.1; while amorphous ferrihydrite phase was formed at the ratio ≤ 0.05, which were confirmed by vibrating sample magnetometer (VSM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). With the ratio increased, the crystalline size and the crystallization degree of MPs increased, and thus the Brunauer-Emmett-Teller (BET) surface and the cation-exchange capacity (CEC) decreased. MPs-3 prepared with H2A to Fe3+ ratio of 0.1 demonstrated the highest methylene blue (MB) adsorption of 87.3 mg/g and good magnetic response. The adsorption of MB onto MPs agreed well with the non-linear Langmuir isotherm model and the pseudo-second-order model. Pilot-scale experiment showed that 99% of MB was removed by adding 10 g/L of MPs-3. After five adsorption-desorption cycles, MPs-3 still showed 62% removal efficiency for MB adsorption. When nitric acid was replaced by acid wastewater from a propylene plant, the synthesized MPs-3w showed 3.7 emu/g of saturation magnetization (Ms) and 56.7 mg/g of MB adsorption capacity, 2.8 times of the widely used commercial adsorbent of granular active carbon (GAC). The major mechanism of MPs adsorption for MB was electrostatic attraction and cation exchange. This study synthesized a magnetic adsorbent from the negatively-valued iron mud waste by using an environment-friendly coprecipitation method, which had a potential for treatment of dye wastewater.
Effect of Co2+ Ions Doping on the Structural and Optical Properties of Magnesium Aluminate

NASA Astrophysics Data System (ADS)

Kanwal, Kiran; Ismail, Bushra; Rajani, K. S.; Kissinger, N. J. Suthan; Zeb, Aurang

2017-07-01

Cobalt-doped nanosized magnesium aluminate (Mg1-xCoxAl2O4) samples having different compositions ( x = 0.2, 0.4, 0.6, 0.8, 1.0) were synthesized by a chemical co-precipitation method. All samples were characterized by means of x-ray diffraction (XRD), scanning electron microscopy, Fourier transform infrared spectroscopy, ultra violet-visible spectroscopy, photoluminescence and diffused reflectance spectroscopy. The results of XRD revealed that the samples were spinel single phase cubic close packed crystalline materials. The lattice constant and x-ray density were found to be affected by the ionic radii of the doped metal cations. Using the Debye-Scherrer formula, the calculated crystalline size was found to be Co2+ ion concentration-dependent and varied between 32 nm and 40 nm. Nano-dimensions and phase of the Mg1-xCoxAl2O4 samples were analyzed and the replacement of Mg2+ ions with Co2+ ions was confirmed by elemental analysis. Three strong absorption bands at 540 nm, 580 nm and 630 nm were observed for the doped samples which are attributed to the three spin-allowed 4T1g (4F) → 4T2g, 4A2g, 4T1g (4P) electronic transitions of Co2+ at tetrahedral lattice sites. Nanophosphors have optical properties different from bulk because of spatial confinement and non-radiative relaxation. Decreases in particle size can increase the surface area and the defects, which can in turn increase the luminescent efficiency to make it very useful for tunable laser operations, persistent phosphorescence, color centers, photoconductivity and luminescence for display technology. MgAl2O4 was doped with Co2+ ions using a co-precipitation method and the optical absorption studies revealed that there is a decrease of band gap due to the increase of Co2+ content. The emission intensity of this phosphor is observed at 449 nm with a sharp peak attributed to the smaller size of the particles and the homogeneity of the powder.
Synthesis and characterization of a magnetic adsorbent from negatively-valued iron mud for methylene blue adsorption

PubMed Central

Liu, Jiancong; Yu, Yang; Yang, Jiakuan; Song, Jian; Fan, Wei; Yu, Hongbin; Bian, Dejun; Huo, Mingxin

2018-01-01

With increasing awareness of reduction of energy and CO2 footprint, more waste is considered recyclable for generating value-added products. Here we reported the negatively-valued iron mud, a waste from groundwater treatment plant, was successfully converted into magnetic adsorbent. Comparing with the conventional calcination method under the high temperature and pressure, the synthesis of the magnetic particles (MPs) by Fe2+/Fe3+ coprecipitation was conducted at environment-friendly condition using ascorbic acid (H2A) as reduction reagent and nitric acid (or acid wastewater) as leaching solution. The MPs with major component of Fe3O4 were synthesized at the molar ratio (called ratio subsequently) of H2A to Fe3+ of iron mud ≥ 0.1; while amorphous ferrihydrite phase was formed at the ratio ≤ 0.05, which were confirmed by vibrating sample magnetometer (VSM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). With the ratio increased, the crystalline size and the crystallization degree of MPs increased, and thus the Brunauer-Emmett-Teller (BET) surface and the cation-exchange capacity (CEC) decreased. MPs-3 prepared with H2A to Fe3+ ratio of 0.1 demonstrated the highest methylene blue (MB) adsorption of 87.3 mg/g and good magnetic response. The adsorption of MB onto MPs agreed well with the non-linear Langmuir isotherm model and the pseudo-second-order model. Pilot-scale experiment showed that 99% of MB was removed by adding 10 g/L of MPs-3. After five adsorption-desorption cycles, MPs-3 still showed 62% removal efficiency for MB adsorption. When nitric acid was replaced by acid wastewater from a propylene plant, the synthesized MPs-3w showed 3.7 emu/g of saturation magnetization (Ms) and 56.7 mg/g of MB adsorption capacity, 2.8 times of the widely used commercial adsorbent of granular active carbon (GAC). The major mechanism of MPs adsorption for MB was electrostatic attraction and cation exchange. This study synthesized a magnetic adsorbent from the negatively-valued iron mud waste by using an environment-friendly coprecipitation method, which had a potential for treatment of dye wastewater. PMID:29394262

Microemulsion flame pyrolysis for hopcalite nanoparticle synthesis: a new concept for catalyst preparation.

PubMed

Biemelt, T; Wegner, K; Teichert, J; Kaskel, S

2015-04-07

A new route to highly active hopcalite catalysts via flame spray pyrolysis of an inverse microemulsion precursor is reported. The nitrate derived nanoparticles are around 15 nm in diameter and show excellent conversion of CO under ambient conditions, outperforming commercial reference hopcalite materials produced by co-precipitation.
40 CFR 142.65 - Variances and exemptions from the maximum contaminant levels for radionuclides.

Code of Federal Regulations, 2010 CFR

2010-07-01

... Raw water quality range &considerations 1 1. Ion exchange (IE) (a) Intermediate All ground waters. 2...-filtration. 5. Lime softening (d) Advanced All waters. 6. Green sand filtration (e) Basic. 7. Co-precipitation with barium sulfate (f) Intermediate to Advanced Ground waters with suitable water quality. 8...
ENVIRONMENTAL TECHNOLOGY VERIFICATION REPORT, REMOVAL OF ARSENIC IN DRINKING WATER: DELTA INDUSTRIAL SERVICES, INC., CAMPWATER PORTA-5 SYSTEM

EPA Science Inventory

The CampWater system uses ozonation followed by cartridge filtration to remove arsenic via co-precipitation. The system utilizes ozone to oxidize iron and arsenic (III) to arsenic (V). The arsenic bound to the iron precipitates is then removed by cartridge filtration. No additi...
A comparative study of the properties of five-layered Aurivillius oxides A2Bi4Ti5O18 (A = Ba, Pb, and Sr) synthesized by different wet chemical routes

NASA Astrophysics Data System (ADS)

Dubey, Shivangi; Subohi, Oroosa; Kurchania, Rajnish

2018-07-01

This paper reports the detailed study of the effect of different wet chemical synthesis routes (solution combustion, co-precipitation, and sol-gel route) on the microstructure, phase formation, dielectric, electrical, and ferroelectric properties of five-layered Aurivillius oxides: A2Bi4Ti5O18 (A = Ba, Pb, and Sr). Different synthesis parameters like the precursors used, synthesis temperature, and reaction time affects the morphology of the ceramics. Microstructure in turn influences the dielectric and ferroelectric properties. It was observed that the sol-gel-synthesized ceramics possess higher dielectric constant and remanent polarization, low dielectric loss due to lower conductivity in these samples as a result of higher density in these compounds as compared to those synthesized by other wet chemical synthesis routes such as solution combustion route and co-precipitation technique. The XRD data are used for phase analysis and surface morphology is studied using SEM images. Dielectric and electrical properties are investigated as a function of frequency and temperature.
a Calorimetric Study of the Precipitation Hardening Mechanisms in AN Al-Cu-Mg-Si Alloy

NASA Astrophysics Data System (ADS)

Hayoune, Abdelali

2013-08-01

The precipitation phenomena and the related hardening in an Al-Cu-Mg-Si alloy were studied by calorimetry, X-ray diffraction analysis and microhardness measurements. The main calorimetric peaks were identified to be due to β‧‧, θ‧ and Q‧ phases precipitation. The hardening during aging at room temperature and 160°C, was respectively, explained by atomic clusters and GP zones formation and by GP zones and β‧‧/θ‧ phases coprecipitation. Although the mechanical properties variation during aging at 200°C is simple, the corresponding microstructural evolution is complex: on the basis of the DSC results, the increasing of microhardness values, is mainly due to the coprecipitation of GP zones and β‧‧/θ‧ phases, however, the maximum hardening is explained by the coexistence of β‧‧/θ‧ and θ‧‧ phases. Another important conclusion is that during aging at 160°C and 200°C, the θ‧ phase is essentially developed from GP zones.
Effects of the synthesis temperature on the crystalline structure and the magnetic properties of cobalt ferrite nanoparticles prepared via coprecipitation

NASA Astrophysics Data System (ADS)

Hutamaningtyas, Evangelin; Utari; Suharyana; Purnama, Budi; Wijayanta, Agung Tri

2016-08-01

The effects of the synthesis temperature on the crystalline structure and the magnetic properties of cobalt ferrite (CoFe2O4) nanoparticles prepared via coprecipitation are discussed. The synthesis was conducted at temperatures of 75 °C, 85 °C and 95 °C. Fourier transform infrared spectroscopy characterization related to a stretching vibration at a wavenumber of 590 cm-1 indicated the formation of a CoFe2O4 metal oxide. In addition, powder X ray diffraction (XRD) characterization proved that the metal oxide was CoFe2O4. Crystallite sizes calculated using the Scherer formula at the strongest peak of the XRD spectra of the samples synthesized at 75 °C, 85 °C and 95 °C were 32 nm, 43 nm and 50.4 nm, respectively. Finally, the results of the vibrating sample magnetometer characterization showed that the saturation magnetization decreased with increasing synthesis temperature, which is related to the dominant preference of Co2+ over Fe3+ cations at the octahedral sites.
Impedance response and dielectric relaxation in co-precipitation derived ferrite (Ni,Zn)Fe{sub 2}O{sub 4} ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, D. G.; Tang, X. G.; Liu, Q. X.

2013-06-07

Dielectric spectra and magnetization hysteresis loops were used to investigate the grain size effect with temperature on the electrical and magnetic response of co-precipitation derived spinel (Ni{sub 0.5}Zn{sub 0.5})Fe{sub 2}O{sub 4} (NZFO) ceramics. Remarkable dielectric relaxation phenomena of non-Debye type have been observed in each NZFO ceramics as confirmed by two kinds of Cole-Cole plots of the 1100 Degree-Sign C sintered samples, mainly due to the electron-hopping mechanism between n-type and p-type carriers and interfacial ion effect when applied an increase of temperature. The high and low response of grain and grain-boundary regions were determined by modeling the impedance experimentalmore » results on two equivalent RC circuits taking into account grain deep trap states. By employing the modified Arrhenius equation, activation energy values of different sintering temperatures were calculated and analyzed in combination with oxygen vacancy. In addition, the magnetization of various sintering temperature samples is dominated by cation distribution and surface effect in different particle ranges.« less
Structural characterization, formation mechanism and stability of curcumin in zein-lecithin composite nanoparticles fabricated by antisolvent co-precipitation.

PubMed

Dai, Lei; Sun, Cuixia; Li, Ruirui; Mao, Like; Liu, Fuguo; Gao, Yanxiang

2017-12-15

Curcumin (Cur) exhibits a range of bioactive properties, but its application is restrained due to its poor water solubility and sensitivity to environmental stresses. In this study, zein-lecithin composite nanoparticles were fabricated by antisolvent co-precipitation technique for delivery of Cur. The result showed that the encapsulation efficiency of Cur was significantly enhanced from 42.03% in zein nanoparticles to 99.83% in zein-lecithin composite nanoparticles. The Cur entrapped in the nanoparticles was in an amorphous state confirmed by differential scanning calorimetry and X-ray diffraction. Fourier transform infrared analysis revealed that hydrogen bonding, electrostatic interaction and hydrophobic attraction were the main interactions among zein, lecithin, and Cur. Compared with single zein and lecithin nanoparticles, zein-lecithin composite nanoparticles significantly improved the stability of Cur against thermal treatment, UV irradiation and high ionic strength. Therefore, zein-lecithin composite nanoparticles could be a potential delivery system for water-insoluble bioactive compounds with enhanced encapsulation efficiency and chemical stability. Copyright © 2017 Elsevier Ltd. All rights reserved.
Speciation of Mn(II), Mn(VII) and total manganese in water and food samples by coprecipitation-atomic absorption spectrometry combination.

PubMed

Citak, Demirhan; Tuzen, Mustafa; Soylak, Mustafa

2010-01-15

A speciation procedure based on the coprecipitation of manganese(II) with zirconium(IV) hydroxide has been developed for the investigation of levels of manganese species. The determination of manganese levels was performed by flame atomic absorption spectrometry (FAAS). Total manganese was determined after the reduction of Mn(VII) to Mn(II) by ascorbic acid. The analytical parameters including pH, amount of zirconium(IV), sample volume, etc., were investigated for the quantitative recoveries of manganese(II). The effects of matrix ions were also examined. The recoveries for manganese(II) were in the range of 95-98%. Preconcentration factor was calculated as 50. The detection limit for the analyte ions based on 3 sigma (n=21) was 0.75 microg L(-1) for Mn(II). The relative standard deviation was found to be lower than 7%. The validation of the presented procedure was performed by analysis of certified reference material having different matrices, NIST SRM 1515 (Apple Leaves) and NIST SRM 1568a (Rice Flour). The procedure was successfully applied to natural waters and food samples.
Selective isolation of gold facilitated by second-sphere coordination with α-cyclodextrin.

PubMed

Liu, Zhichang; Frasconi, Marco; Lei, Juying; Brown, Zachary J; Zhu, Zhixue; Cao, Dennis; Iehl, Julien; Liu, Guoliang; Fahrenbach, Albert C; Botros, Youssry Y; Farha, Omar K; Hupp, Joseph T; Mirkin, Chad A; Fraser Stoddart, J

2013-01-01

Gold recovery using environmentally benign chemistry is imperative from an environmental perspective. Here we report the spontaneous assembly of a one-dimensional supramolecular complex with an extended {[K(OH₂)₆][AuBr₄](α-cyclodextrin)₂}n chain superstructure formed during the rapid co-precipitation of α-cyclodextrin and KAuBr₄ in water. This phase change is selective for this gold salt, even in the presence of other square-planar palladium and platinum complexes. From single-crystal X-ray analyses of six inclusion complexes between α-, β- and γ-cyclodextrins with KAuBr₄ and KAuCl₄, we hypothesize that a perfect match in molecular recognition between α-cyclodextrin and [AuBr₄](-) leads to a near-axial orientation of the ion with respect to the α-cyclodextrin channel, which facilitates a highly specific second-sphere coordination involving [AuBr₄](-) and [K(OH₂)₆](+) and drives the co-precipitation of the 1:2 adduct. This discovery heralds a green host-guest procedure for gold recovery from gold-bearing raw materials making use of α-cyclodextrin-an inexpensive and environmentally benign carbohydrate.
In situ TPR XANES study of the partial oxidation of methane using a Ni-substituted hexaaluminate catalyst

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kugler, E.L.; Gardner, T.H.; Campos, Andrew

2008-04-01

Metallic Ni formation near the mirror cation site, Ba in this study, is believed to cause the partial oxidation activity observed in Ni-substituted hexaaluminate catalysts. The BaNi1.0Al11.6O19-d catalyst was prepared by coprecipitation with nitrate salt precursors; following the coprecipitation procedure, the catalyst was calcined at 1400°C to create the hexaaluminate structure. TPR XANES in fluorescence was used to probe the local structure of the BaNi1.0Al11.6O19-d catalyst to determine whether metallic nickel forms at different temperatures: 825°C, 875°C, 925°C. The XANES results indicate that the Ni in the hexaaluminate catalyst only reduces if the temperature is maintained at 925°C. Once themore » metallic state is formed, the oxidation state is stable; even in the POX environment. Future work using a theoretical approach to the XANES data using FEFF 8.4 gives information on the interactions between Ni and Ba, which will be used to further optimize the catalyst.« less
Synthesis and magnetic characterization of nickel ferrite nanoparticles prepared by co-precipitation route

NASA Astrophysics Data System (ADS)

Maaz, K.; Karim, S.; Mumtaz, A.; Hasanain, S. K.; Liu, J.; Duan, J. L.

2009-06-01

Magnetic nanoparticles of nickel ferrite (NiFe 2O 4) have been synthesized by co-precipitation route using stable ferric and nickel salts with sodium hydroxide as the precipitating agent and oleic acid as the surfactant. X-ray diffraction (XRD) and transmission electron microscope (TEM) analyses confirmed the formation of single-phase nickel ferrite nanoparticles in the range 8-28 nm depending upon the annealing temperature of the samples during the synthesis. The size of the particles ( d) was observed to be increasing linearly with annealing temperature of the sample while the coercivity with particle size goes through a maximum, peaking at ˜11 nm and then decreases for larger particles. Typical blocking effects were observed below ˜225 K for all the prepared samples. The superparamagnetic blocking temperature ( T B) was found to be increasing with increasing particle size that has been attributed to the increased effective anisotropy energy of the nanoparticles. The saturation moment of all the samples was found much below the bulk value of nickel ferrite that has been attributed to the disordered surface spins or dead/inert layer in these nanoparticles.
Synthesis and properties of precipitated cobalt ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Ristic, Mira; Krehula, Stjepko; Reissner, Michael; Jean, Malick; Hannoyer, Beatrice; Musić, Svetozar

2017-07-01

The formation and properties of cobalt ferrite were investigated with XRD, FT-IR, FE-SEM, Mössbauer and magnetometry. Cobalt ferrite samples were prepared (a) by combining coprecipitation Co(OH)2/2Fe(OH)3, using NaOH between pH 5.2 and 11.4 and autoclaving, and (b) by autoclaving the Co(OH)2/2Fe(OH)3 coprecipitate in a very strong alkaline medium. XRD and FE SEM showed that both CoFe2O4 crystallites and particles were in the nanosize range. The FT-IR spectra were typical of spinel ferrites. Cobalt ferrite precipitated at pH 7.2 and at 11.4 contained a small fraction of α-Fe2O3, whereas in the sample precipitated at pH 11.4 a very small amount (traces) of α-FeOOH were detected by FT-IR, additionally. Parameters obtained by Mössbauer spectroscopy suggested a structural migration of cobalt and iron ions in prepared cobalt ferrite spinels with the prolonged time of autoclaving. Magnetic measurements showed the magnetic behaviour typical of spinel ferrite nanoparticles.
Comparative evaluation of ibuprofen/beta-cyclodextrin complexes obtained by supercritical carbon dioxide and other conventional methods.

PubMed

Hussein, Khaled; Türk, Michael; Wahl, Martin A

2007-03-01

The preparation of drug/cyclodextrin complexes is a suitable method to improve the dissolution of poor soluble drugs. The efficacy of the Controlled Particle Deposition (CPD) as a new developed method to prepare these complexes in a single stage process using supercritical carbon dioxide is therefore compared with other conventional methods. Ibuprofen/beta-cyclodextrin complexes were prepared with different techniques and characterized using FTIR-ATR spectroscopy, powder X-ray diffractometry (PXRD), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). In addition, the influences of the processing technique on the drug content (HPLC) and the dissolution behavior were studied. Employing the CPD-process resulted in a drug content of 2.8+/-0.22 wt.% in the carrier. The material obtained by CPD showed an improved dissolution rate of ibuprofen at pH 5 compared with the pure drug and its physical mixture with beta-cyclodextrin. In addition CPD material displays the highest dissolution (93.5+/- 2.89% after 75 min) compared to material obtained by co-precipitation (61.3 +/-0.52%) or freeze-drying (90.6 +/-2.54%). This study presents the CPD-technique as a well suitable method to prepare a drug/beta-cyclodextrin complex with improved drug dissolution compared to the pure drug and materials obtained by other methods.
A rapid silica spin column-based method of RNA extraction from fruit trees for RT-PCR detection of viruses.

PubMed

Yang, Fan; Wang, Guoping; Xu, Wenxing; Hong, Ni

2017-09-01

Efficient recovery of high quality RNA is very important for successful RT-PCR detection of plant RNA viruses. High levels of polyphenols and polysaccharides in plant tissues can irreversibly bind to and/or co-precipitate with RNA, which influences RNA isolation. In this study, a silica spin column-based RNA isolation method was developed by using commercially available silica columns combined with the application of a tissue lysis solution, and binding and washing buffers with high concentration guanidinium thiocyanate (GuSCN, 50% w/v), which helps remove plant proteins, polysaccharides and polyphenolic compounds. The method was successfully used to extract high quality RNA from citrus (Citrus aurantifolia), grapevine (Vitis vinifera), peach (Prunus persica), pear (Pyrus spp.), taro (Colocosia esculenta) and tobacco (Nicotiana benthamiana) samples. The method was comparable to conventional CTAB method in RNA isolation efficiency, but it was more sample-adaptable and cost-effective than commercial kits. High quality RNA isolated using silica spin column-based method was successfully used for the RT-PCR and/or multiplex RT-PCR amplification of woody fruit tree viruses and a viroid. The study provided a useful tool for the detection and characterization of plant viruses. Copyright © 2017 Elsevier B.V. All rights reserved.
Arsenic Removal from Groundwater by Solar Driven Inline-Electrolytic Induced Co-Precipitation and Filtration-A Long Term Field Test Conducted in West Bengal.

PubMed

Otter, Philipp; Malakar, Pradyut; Jana, Bana Bihari; Grischek, Thomas; Benz, Florian; Goldmaier, Alexander; Feistel, Ulrike; Jana, Joydev; Lahiri, Susmita; Alvarez, Juan Antonio

2017-10-02

Arsenic contamination in drinking water resources is of major concern in the Ganga delta plains of West Bengal in India and Bangladesh. Here, several laboratory and field studies on arsenic removal from drinking water resources were conducted in the past and the application of strong-oxidant-induced co-precipitation of arsenic on iron hydroxides is still considered as the most promising mechanism. This paper suggests an autonomous, solar driven arsenic removal setting and presents the findings of a long term field test conducted in West Bengal. The system applies an inline-electrolytic cell for in situ chlorine production using the natural chloride content of the water and by that substituting the external dosing of strong oxidants. Co-precipitation of As(V) occurs on freshly formed iron hydroxide, which is removed by Manganese Greensand Plus ® filtration. The test was conducted for ten months under changing source water conditions considering arsenic (187 ± 45 µg/L), iron (5.5 ± 0.8 mg/L), manganese (1.5 ± 0.4 mg/L), phosphate (2.4 ± 1.3 mg/L) and ammonium (1.4 ± 0.5 mg/L) concentrations. Depending on the system setting removal rates of 94% for arsenic (10 ± 4 µg/L), >99% for iron (0.03 ± 0.03 mg/L), 96% for manganese (0.06 ± 0.05 mg/L), 72% for phosphate (0.7 ± 0.3 mg/L) and 84% for ammonium (0.18 ± 0.12 mg/L) were achieved-without the addition of any chemicals/adsorbents. Loading densities of arsenic on iron hydroxides averaged to 31 µgAs/mgFe. As the test was performed under field conditions and the here proposed removal mechanisms work fully autonomously, it poses a technically feasible treatment alternative, especially for rural areas.
Arsenic Removal from Groundwater by Solar Driven Inline-Electrolytic Induced Co-Precipitation and Filtration—A Long Term Field Test Conducted in West Bengal

PubMed Central

Malakar, Pradyut; Jana, Bana Bihari; Benz, Florian; Goldmaier, Alexander; Feistel, Ulrike; Jana, Joydev; Lahiri, Susmita; Alvarez, Juan Antonio

2017-01-01

Arsenic contamination in drinking water resources is of major concern in the Ganga delta plains of West Bengal in India and Bangladesh. Here, several laboratory and field studies on arsenic removal from drinking water resources were conducted in the past and the application of strong-oxidant-induced co-precipitation of arsenic on iron hydroxides is still considered as the most promising mechanism. This paper suggests an autonomous, solar driven arsenic removal setting and presents the findings of a long term field test conducted in West Bengal. The system applies an inline-electrolytic cell for in situ chlorine production using the natural chloride content of the water and by that substituting the external dosing of strong oxidants. Co-precipitation of As(V) occurs on freshly formed iron hydroxide, which is removed by Manganese Greensand Plus® filtration. The test was conducted for ten months under changing source water conditions considering arsenic (187 ± 45 µg/L), iron (5.5 ± 0.8 mg/L), manganese (1.5 ± 0.4 mg/L), phosphate (2.4 ± 1.3 mg/L) and ammonium (1.4 ± 0.5 mg/L) concentrations. Depending on the system setting removal rates of 94% for arsenic (10 ± 4 µg/L), >99% for iron (0.03 ± 0.03 mg/L), 96% for manganese (0.06 ± 0.05 mg/L), 72% for phosphate (0.7 ± 0.3 mg/L) and 84% for ammonium (0.18 ± 0.12 mg/L) were achieved—without the addition of any chemicals/adsorbents. Loading densities of arsenic on iron hydroxides averaged to 31 µgAs/mgFe. As the test was performed under field conditions and the here proposed removal mechanisms work fully autonomously, it poses a technically feasible treatment alternative, especially for rural areas. PMID:28974053
Optimization of synthesis and peptization steps to obtain iron oxide nanoparticles with high energy dissipation rates

NASA Astrophysics Data System (ADS)

Mérida, Fernando; Chiu-Lam, Andreina; Bohórquez, Ana C.; Maldonado-Camargo, Lorena; Pérez, María-Eglée; Pericchi, Luis; Torres-Lugo, Madeline; Rinaldi, Carlos

2015-11-01

Magnetic Fluid Hyperthermia (MFH) uses heat generated by magnetic nanoparticles exposed to alternating magnetic fields to cause a temperature increase in tumors to the hyperthermia range (43-47 °C), inducing apoptotic cancer cell death. As with all cancer nanomedicines, one of the most significant challenges with MFH is achieving high nanoparticle accumulation at the tumor site. This motivates development of synthesis strategies that maximize the rate of energy dissipation of iron oxide magnetic nanoparticles, preferable due to their intrinsic biocompatibility. This has led to development of synthesis strategies that, although attractive from the point of view of chemical elegance, may not be suitable for scale-up to quantities necessary for clinical use. On the other hand, to date the aqueous co-precipitation synthesis, which readily yields gram quantities of nanoparticles, has only been reported to yield sufficiently high specific absorption rates after laborious size selective fractionation. This work focuses on improvements to the aqueous co-precipitation of iron oxide nanoparticles to increase the specific absorption rate (SAR), by optimizing synthesis conditions and the subsequent peptization step. Heating efficiencies up to 1048 W/gFe (36.5 kA/m, 341 kHz; ILP=2.3 nH m2 kg-1) were obtained, which represent one of the highest values reported for iron oxide particles synthesized by co-precipitation without size-selective fractionation. Furthermore, particles reached SAR values of up to 719 W/gFe (36.5 kA/m, 341 kHz; ILP=1.6 nH m2 kg-1) when in a solid matrix, demonstrating they were capable of significant rates of energy dissipation even when restricted from physical rotation. Reduction in energy dissipation rate due to immobilization has been identified as an obstacle to clinical translation of MFH. Hence, particles obtained with the conditions reported here have great potential for application in nanoscale thermal cancer therapy.
Cation-Dependent Gold Recovery with α-Cyclodextrin Facilitated by Second-Sphere Coordination.

PubMed

Liu, Zhichang; Samanta, Avik; Lei, Juying; Sun, Junling; Wang, Yuping; Stoddart, J Fraser

2016-09-14

Herein, we report an alkali metal cation-dependent approach to gold recovery, facilitated by second-sphere coordination with eco-friendly α-cyclodextrin (α-CD). Upon mixing eight salts composed of Na(+), K(+), Rb(+), or Cs(+) cations and [AuX4](-) (X = Cl/Br) anions with α-, β-, or γ-CD in water, co-precipitates form selectively from the three (out of 24) aqueous solutions containing α-CD with KAuBr4, RbAuBr4, and CsAuBr4, from which the combination of α-CD and KAuBr4 affords the highest yield. Single-crystal X-ray analyses reveal that in 20 of the 24 adducts CD and [AuX4](-) anions form 2:1 sandwich-type second-sphere adducts driven partially by [C-H···X-Au] interactions between [AuX4](-) anions and the primary faces of two neighboring CDs. In the adduct formed between α-CD and KAuBr4, a [K(OH2)6](+) cation is encapsulated inside the cavity between the secondary faces of two α-CDs, leading to highly efficient precipitation owing to the formation of a cation/anion alternating ion wire residing inside a continuous α-CD nanotube. By contrast, in the other 19 adducts, the cations are coordinated by OH groups and glucopyranosyl ring O atoms in CDs. The strong coordination of Rb(+) and Cs(+) cations by these ligands, in conjunction with the stereoelectronically favorable binding of [AuBr4](-) anions with two α-CDs, facilitates the co-precipitation of the two adducts formed between α-CD with RbAuBr4 and CsAuBr4. In order to develop an efficient process for green gold recovery, the co-precipitation yield of α-CD and KAuBr4 has been optimized regarding both the temperature and the molar ratio of α-CD to KAuBr4.
Li1.2Mn0.6Ni0.1Co0.1O2 microspheres constructed by hierarchically arranged nanoparticles as lithium battery cathode with enhanced electrochemical performance

NASA Astrophysics Data System (ADS)

Remith, P.; Kalaiselvi, N.

2014-11-01

Novel lithium-rich layered Li1.2Mn0.6Ni0.1Co0.1O2 microspheres containing hierarchically arranged and interconnected nanostructures have been synthesized by a combination of template-free co-precipitation and solid-state methods. The in situ formed γ-MnO2 spherical template upon co-precipitation gets sacrificed during the course of solid-state fusion of cobalt, nickel and lithium precursors to produce the title compound in the form of microspheres constructed by nanoparticles as building blocks. Porous and hollow microspheres of Li1.2Mn0.6Ni0.1Co0.1O2 are formed out of the spontaneous aggregation of nanoparticles, obtained from the custom-designed synthesis protocol. The growth mechanism of Li1.2Mn0.6Ni0.1Co0.1O2 spheres could be understood in terms of the Kirkendall effect and Ostwald ripening. The nanocrystalline Li1.2Mn0.6Ni0.1Co0.1O2 compound is obtained as a solid solution consisting of rhombohedral R3&cmb.macr;m and monoclinic C2/m group symmetries, as evidenced by XRD, Raman spectra and HRTEM equipped with FFT and STEM. The currently synthesized Li1.2Mn0.6Ni0.1Co0.1O2 cathode exhibits an appreciable discharge capacity of 242 mA h g-1 at a current density of 50 mA g-1, due to the synergistic effect of the capacity obtained from the rhombohedral and monoclinic phases.Novel lithium-rich layered Li1.2Mn0.6Ni0.1Co0.1O2 microspheres containing hierarchically arranged and interconnected nanostructures have been synthesized by a combination of template-free co-precipitation and solid-state methods. The in situ formed γ-MnO2 spherical template upon co-precipitation gets sacrificed during the course of solid-state fusion of cobalt, nickel and lithium precursors to produce the title compound in the form of microspheres constructed by nanoparticles as building blocks. Porous and hollow microspheres of Li1.2Mn0.6Ni0.1Co0.1O2 are formed out of the spontaneous aggregation of nanoparticles, obtained from the custom-designed synthesis protocol. The growth mechanism of Li1.2Mn0.6Ni0.1Co0.1O2 spheres could be understood in terms of the Kirkendall effect and Ostwald ripening. The nanocrystalline Li1.2Mn0.6Ni0.1Co0.1O2 compound is obtained as a solid solution consisting of rhombohedral R3&cmb.macr;m and monoclinic C2/m group symmetries, as evidenced by XRD, Raman spectra and HRTEM equipped with FFT and STEM. The currently synthesized Li1.2Mn0.6Ni0.1Co0.1O2 cathode exhibits an appreciable discharge capacity of 242 mA h g-1 at a current density of 50 mA g-1, due to the synergistic effect of the capacity obtained from the rhombohedral and monoclinic phases. Electronic supplementary information (ESI) available: Fig. S1 represents the STEM elemental mapping of pristine Li1.2Mn0.6Ni0.1Co0.1O2. Fig. S2 is the EDX spectrum obtained from HRTEM and Fig. S3 is the SAED pattern. Fig. S4 shows the room temperature conductivity plot and Fig. S5 shows the comparison of the discharge capacity values of LiMn1/3Ni1/3Co1/3O2 and Li1.2Mn0.6Ni0.1Co0.1O2 cathodes and Table 1 shows the d spacing values corresponding to different space group symmetries, derived from XRD and TEM studies. See DOI: 10.1039/c4nr04314f

In vitro cytotoxicity of iron oxide nanoparticles: effects of chitosan and polyvinyl alcohol as stabilizing agents

NASA Astrophysics Data System (ADS)

Tran, Phong A.; Nguyen, Hiep T.; Fox, Kate; Tran, Nhiem

2018-03-01

Iron oxide magnetic nanoparticles have significant potential in biomedical applications such as in diagnosis, imaging and therapeutic agent delivery. The choice of stabilizers and surface functionalization is important as it is known to strongly influence the cytotoxicity of the nanoparticles. The present study aimed at investigating the effects of surface charges on the cytotoxicity of iron oxide nanoparticles. We used a co-precipitation method to synthesize iron oxide nanoparticles which were then stabilized with either chitosan (CS) or polyvinyl alcohol (PVA) which have net positive charge and zero charge at physiological pH, respectively. The nanoparticles were characterized in terms of size, charges and chemical oxidation state. Cytotoxicity of the nanoparticles was assessed using mouse fibroblast cells and was correlated with surface charges of the nanoparticles and their aggregation.
Preparation, structural and dielectric characteristics of Y0.5La0.95PO4 nanoparticles

NASA Astrophysics Data System (ADS)

Raina, Bindu; Verma, Seema; Gupta, Vandana; Bamzai, K. K.

2018-05-01

Nanoparticles of yttrium substituted lanthanum phosphate having formulae Y0.5La0.95PO4 were successfully prepared through co-precipitation method. The phase, purity and crystallinity of 5% yttrium substituted lanthanum phosphate (Y: LaP 5%) powder was characterized by X-ray diffraction technique which suggests the sample belonging to monoclinic monazite crystal system. The spherical morphology with partial agglomeration having grain size in the nano scale range was observed with transmission electron microscopy. FTIR analysis depicts the presence of water molecule along with the phosphate group. The electrical properties of the grown composition show dependence of dielectric constant and dielectric loss on frequency and temperature. The continuous decrease in dielectric constant with increase in frequency suggests that the conduction mechanism is due to hopping of the charge carriers from one site to another.
From biowaste to magnet-responsive materials for water remediation from polycyclic aromatic hydrocarbons.

PubMed

Nisticò, Roberto; Cesano, Federico; Franzoso, Flavia; Magnacca, Giuliana; Scarano, Domenica; Funes, Israel G; Carlos, Luciano; Parolo, Maria E

2018-07-01

Composted urban biowaste-derived substances (BBS-GC) are used as carbon sources for the preparation of carbon-coated magnet-sensitive nanoparticles obtained via co-precipitation method and the subsequent thermal treatment at 550 °C under nitrogen atmosphere. A multitechnique approach has been applied to investigate the morphology, magnetic properties, phase composition, thermal stability of the obtained magnet-sensitive materials. In particular, pyrolysis-induced modifications affecting the BBS-GC/carbon shell were highlighted. The adsorption capacity of such bio-derivative magnetic materials for the removal of hydrophobic contaminants such as polycyclic aromatic hydrocarbons was evaluated in order to verify their potential application in wastewater remediation process. The promising results suggest their use as a new generation of magnet-responsive easily-recoverable adsorbents for water purification treatments. Copyright © 2018 Elsevier Ltd. All rights reserved.
Fabrication of PDMS-Based Microfluidic Devices: Application for Synthesis of Magnetic Nanoparticles

NASA Astrophysics Data System (ADS)

Thu, Vu Thi; Mai, An Ngoc; Le The Tam; Van Trung, Hoang; Thu, Phung Thi; Tien, Bui Quang; Thuat, Nguyen Tran; Lam, Tran Dai

2016-05-01

In this work, we have developed a convenient approach to synthesize magnetic nanoparticles with relatively high magnetization and controllable sizes. This was realized by combining the traditional co-precipitation method and microfluidic techniques inside microfluidic devices. The device was first designed, and then fabricated using simplified soft-lithography techniques. The device was utilized to synthesize magnetite nanoparticles. The synthesized nanomaterials were thoroughly characterized using field emission scanning electron microscopy and a vibrating sample magnetometer. The results demonstrated that the as-prepared device can be utilized as a simple and effective tool to synthesize magnetic nanoparticles with the sizes less than 10 nm and magnetization more than 50 emu/g. The development of these devices opens new strategies to synthesize nanomaterials with more precise dimensions at narrow size-distribution and with controllable behaviors.
A simple and facile synthesis of MPA capped CdSe and CdSe/CdS core/shell nanoparticles

NASA Astrophysics Data System (ADS)

Sukanya, D.; Sagayaraj, P.

2015-06-01

II-VI semiconductor nanostructures, in particular, CdSe quantum dots have drawn a lot of attention because of their promising potential applications in biological tagging, photovoltaic, display devices etc. due to their excellent optical properties, high emission quantum yield, size dependent emission wavelength and high photostability. In this paper, we describe the synthesis and properties of mercaptopropionic acid capped CdSe and CdSe/CdS nanoparticles through a simple and efficient co-precipitation method followed by hydrothermal treatment. The growth process, characterization and the optical absorption as a function of wavelength for the synthesized MPA capped CdSe and CdSe/CdS nanoparticles have been determined using X-ray diffraction study (XRD), Ultraviolet-Visible spectroscopy (UV-Vis), Fourier transform infrared spectroscopy (FT-IR) and High Resolution Transmission Electron Microscopy (HRTEM).
Magnetite Nanoparticles Coated with Rifampicin and Chlortetracycline for Drug Delivery Applications

NASA Astrophysics Data System (ADS)

Nǎdejde, Claudia; Ciurlicǎ, Ecaterina Foca-nici; Creangǎ, Dorina; Cârlescu, Aurelian; Bǎdescu, Vasile

2010-12-01

Four types of biocompatible magnetic fluids based on superparamagnetic nanoparticles with Fe3O4 cores were functionalized with antibiotics (rifampicin or chlortetracycline) as potential candidates for in vivo biomedical applications, such as magnetically controlled drug delivery. The synthesis consisted in coprecipitation of iron oxide in basic, as well as in acid medium, followed by the dispersion of the resulted magnetite nanoparticles in aqueous solution containing the antibiotic. The chosen method to prepare the magnetite-core/drug-shell systems avoided intermediate organic coating of the magnetic nanoparticles. Comparative analysis of the rheological features of the aqueous magnetic fluid samples was performed. The structural features of the coated magnetic particles were investigated by X-Ray Diffraction (XRD), Transmission Electron Microscopy (TEM) and Vibrating Sample Magnetometry (VSM). Good crystallinity and adequate stability in time were evidenced. Drug delivery curves were spectrophotometrically provided.
Micro structural analysis and magnetic characteristics of rare earth substituted cobalt ferrite

NASA Astrophysics Data System (ADS)

Tapdiya, Swati; Singh, Sarika; Kulshrestha, Shobha; Shrivastava, A. K.

2018-05-01

A series of ultrafine nanoparticles of Gd3+ doped Co-ferrites CoGdxFe2-xO4 (x=0.0, 0.05 and 0.10) were prepared by wet chemical co-precipitation method using nitrates of respective metal ions. Structural and morphology studies were performed using XRD, SEM and EDAX. Indexed XRD patterns confirm the formation of cubic spinel phase. Average crystallite sizes found to be decreases with trivalent rare earth ion substitution. Lattice constant (a) and lattice strain increases with increase in Gd3+ concentration due to large ionic radii (0.94nm) of Gd3+ replacing Fe3+ (0.64nm). SEM images show the spherical morphology and uniform growth of nanoparticles. Magnetic studies show that magnetization (Ms), decreases with increase in Gd3+ concentration from 50.16 emu/gm to 31.26 emu/gm.
Photoluminescence study of ZnS and ZnS:Pb nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Virpal,, E-mail: virpalsharma.sharma@gmail.com; Hastir, Anita; Kaur, Jasmeet

2015-05-15

Photoluminescence (PL) study of pure and 5wt. % lead doped ZnS prepared by co-precipitation method was conducted at room temperature. The prepared nanoparticles were characterized by X-ray Diffraction (XRD), UV-Visible (UV-Vis) spectrophotometer, Photoluminescence (PL) and Raman spectroscopy. XRD patterns confirm cubic structure of ZnS and PbS in doped sample. The band gap energy value increased in case of Pb doped ZnS nanoparticles. The PL spectrum of pure ZnS was de-convoluted into two peaks centered at 399nm and 441nm which were attributed to defect states of ZnS. In doped sample, a shoulder peak at 389nm and a broad peak centered atmore » 505nm were observed. This broad green emission peak originated due to Pb activated ZnS states.« less
Aqueous synthesis of polyhedral “brick-like” iron oxide nanoparticles for hyperthermia and T2 MRI contrast enhancement†

PubMed Central

Worden, Matthew; Bruckman, Michael A.; Kim, Min-Ho; Steinmetz, Nicole F.; Kikkawa, James M.; LaSpina, Catherine

2015-01-01

A low temperature, aqueous synthesis of polyhedral iron oxide nanoparticles (IONPs) is presented. The modification of the co-precipitation hydrolysis method with Triton X surfactants results in the formation of crystalline polyhedral particles. The particles are herein termed iron oxide “nanobricks” (IONBs) as the variety of particles made are all variations on a simple “brick-like” rhombohedral shape as evaluated by TEM. These IONBs can be easily coated with hydrophilic silane ligands, allowing them to be dispersed in aqueous media. The dispersed particles are investigated for potential applications as hyperthermia and T2 MRI contrast agents. The results demonstrate that the IONBs perform better than comparable spherical IONPs in both applications, and show r2 values amongst the highest for iron oxide based materials reported in the literature. PMID:26693011
Versatile Poly(Diallyl Dimethyl Ammonium Chloride)-Layered Nanocomposites for Removal of Cesium in Water Purification.

PubMed

Jang, Sung-Chan; Kang, Sung-Min; Kim, Gi Yong; Rethinasabapathy, Muruganantham; Haldorai, Yuvaraj; Lee, Ilsong; Han, Young-Kyu; Renshaw, Joanna C; Roh, Changhyun; Huh, Yun Suk

2018-06-12

In this work, we elucidate polymer-layered hollow Prussian blue-coated magnetic nanocomposites as an adsorbent to remove radioactive cesium from environmentally contaminated water. To do this, Fe₃O₄ nanoparticles prepared using a coprecipitation method were thickly covered with a layer of cationic polymer to attach hollow Prussian blue through a self-assembly process. The as-synthesized adsorbent was confirmed through various analytical techniques. The adsorbent showed a high surface area (166.16 m²/g) with an excellent cesium adsorbent capacity and removal efficiency of 32.8 mg/g and 99.69%, respectively. Moreover, the superparamagnetism allows effective recovery of the adsorbent using an external magnetic field after the adsorption process. Therefore, the magnetic adsorbent with a high adsorption efficiency and convenient recovery is expected to be effectively used for rapid remediation of radioactive contamination.
Biocatalytic response of multi-layer assembled collagen/hyaluronic acid nanoengineered capsules.

PubMed

Sousa, Fernanda; Kreft, Oliver; Sukhorukov, Gleb B; Möhwald, Helmuth; Kokol, Vanja

2014-01-01

Biodegradable hollow capsules filled with fluorescently labelled bovine serum albumin (BSA) as a model drug were prepared via layer-by-layer (LbL) self-assembly of type-I collagen (COL) and hyaluronic acid (HA) using calcium carbonate micro-particles and co-precipitation method. Capsules loaded with fluorescein isothiocyanate (FITC)-BSA, tetramethylrhodamin isothiocyanate (TRITC)-BSA or Alex-Fluor-488-BSA, respectively, were characterised before and after core removal using Confocal Laser Scanning Microscopy (CLSM), whilst the morphologies of individual hollow capsules were assessed using Atomic Force Microscopy (AFM). The sustained release of the encapsulated FITC-BSA protein was attained using enzymatic degradation of the capsule shells by collagenase. The released profile of the fluorescently-labelled BSA indicated that it could be successfully controlled by modulating the number of layers and/or by collagen crosslinking either before or after the capsule's assembly.
Nanoparticles: synthesis and applications in life science and environmental technology

NASA Astrophysics Data System (ADS)

Luong Nguyen, Hoang; Nguyen, Hoang Nam; Hai Nguyen, Hoang; Quynh Luu, Manh; Hieu Nguyen, Minh

2015-03-01

This work focuses on the synthesis, functionalization, and application of gold and silver nanoparticles, magnetic nanoparticles Fe3O4, combination of 4-ATP-coated silver nanoparticles and Fe3O4 nanoparticles. The synthesis methods such as chemical reduction, seeding, coprecipitation,and inverse microemulsion will be outlined. Silica- and amino-coated nanoparticles are suitable for several applications in biomedicine and the environment. The applications of the prepared nanoparticles for early detection of breast cancer cells, basal cell carcinoma, antibacterial test, arsenic removal from water, Herpes DNA separation, CD4+ cell separation and isolation of DNA of Hepatitis virus type B (HBV) and Epstein-Barr virus (EBV) are discussed. Finally, some promising perspectives will be pointed out. Invited talk at the 7th International Workshop on Advanced Materials Science and Nanotechnology IWAMSN2014, 2-6 November, 2014, Ha Long, Vietnam.
Synthesis, structural, magnetic and optical properties of Sr2CoSn based inverse Heusler alloy nanoparticles

NASA Astrophysics Data System (ADS)

Asvini, V.; Saravanan, G.; Kalaiezhily, R. K.; Ravichandran, K.

2018-05-01

The peculiar ternary full Heusler alloy Sr2CoSn nanoparticles are synthesized by co-precipitation method. X- ray diffraction pattern confirms the formation of XA or Xα structure of Sr2CoSn. Using Williamson-Hall plot (W-H plot), we are able to use the uniform deformation model and get low value of strain induced broadening. UV-Visible absorption spectrum shows sharp absorption peak at 210 nm and the estimated band gap energy of Sr2CoSn Heusler alloy nanoparticles is Eg = 4.6 eV (from Tauc plot). The presence of Sr2CoSn with the particle size of approximately 90 nm was observed using high resolution scanning electron microscopy. The magnetization measurements were carried out using VSM and studied M verses H hysteresis studies.
An Innovative Carbonate Coprecipitation Process For The Removal Of Zinc And Manganese From Mining Impacted Waters

EPA Science Inventory

Although mine drainage is usually thought of as acidic, there are many cases where the water is of neutral pH, but still contains metal species that can be harmful to human or aquatic animal health, such as manganese (Mn) and zinc (Zn). Typical treatment of mine drainage waters ...
Maghemite decorated with ultra-small palladium nanoparticles (γ-Fe2O3–Pd): applications in the Heck–Mizoroki olefination, Suzuki reaction and allylic oxidation of alkenes

EPA Science Inventory

A nanocatalyst comprising ultra-small Pd/PdO nanoparticles (<5 nm) supported on maghemite was prepared by a co-precipitation protocol using inexpensive raw materials and was deployed successfully in various significant synthetic transformations, namely the Heck–Mizoroki olefinati...
Influence of reaction medium during synthesis of Gantrez AN 119 nanoparticles for oral vaccination.

PubMed

Vandamme, Katrien; Melkebeek, Vesna; Cox, Eric; Deforce, Dieter; Lenoir, Joke; Adriaens, Els; Vervaet, Chris; Remon, Jean Paul

2010-02-01

Two synthesis methods of poly(methyl vinyl ether-co-maleic anhydride) (Gantrez AN 119) nanoparticles (NP) (used for oral vaccination) were compared. Wheat germ agglutinin (WGA) was used as ligand to enhance the bioadhesive properties of NP and beta-galactosidase as antigen. The first method encapsulated beta-galactosidase in NP by co-precipitation in an acetone/water mixture containing 44% acetone. In the second method, antigen addition occurred in 100% acetone. To improve stability, NP were crosslinked with 1,3-diaminopropane. The stability of WGA-conjugated NP with encapsulated antigen diminished at lower pH and when decreasing the amount of crosslinker. The binding type between WGA and polymer depended on the synthesis method: predominantly ionic bonds were formed using the 44% acetone method, whereas synthesis via the 100% acetone method resulted in covalent bonds. The biological activity of the WGA coating, evaluated via a pig gastric mucin binding test, was lower in NP prepared via the 100% acetone method. No release of native antigen was detected after hydrolysis of NP, due to the covalent antigen binding during antigen encapsulation and the high reactivity of the polymer. Moreover, the mucosal irritation capacity was evaluated upon nanoparticle hydrolysis using a slug mucosal irritation assay. Herein, hydrolysed NP of the 44% acetone method were classified as mild irritative. Copyright (c) 2009 Elsevier B.V. All rights reserved.
Effect of Co2+ and Y3+ ions insertion on the microstructure development and magnetic properties of Ni0.5Zn0.5Fe2O4 powders synthesized using Co-precipitation method

NASA Astrophysics Data System (ADS)

Rashad, M. M.; Rayan, D. A.; Turky, A. O.; Hessien, M. M.

2015-01-01

Nanocrystalline Ni0.5Zn0.5-xCoxFe2-zYzO4 powders (x=0-0.3 and z from 0 to 0.3) have been synthesized via a facile co-precipitation technique. X-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM) are utilized in order to study the effect of variation of cobalt and yttrium substitutions and its impact on crystalline size, lattice parameter, X-ray density, microstructure and magnetic properties of the formed powders. X-ray diffraction data indicated that, after doping, all samples consisted of the main spinel phase for the formed precursors precipitated at pH 10 annealed at 1000 oC for 2 h. The lattice parameter and the unit cell were decreased linearly with increasing Co content whereas they were increased with increasing the Y incorporation. Additionally, the porosity was increased with increasing Co concentration while it was decreased with increasing the Y insertion. The mean ionic radii and hopping and bond lengths was decreased with the value of Co2+ and they were increased with the value of Y3+ ion as well as both of Y3+ and Co2+ ions. The microstructures of the produced powders were found to be cubic like structure. The addition of Y3+ ion suppressed the grain size whereas addition of Co2+ ion enhanced the grain growth availably. An examination of the magnetic properties revealed an increase in saturation magnetization with increasing Co and Y concentrations incorporation up to x=0.3. Meanwhile, the formed powders exhibited superparamagnetic characteristics. A high saturation magnetization (77.0 emu/g) was achieved for Ni0.5Zn0.2Co0.3Fe2O4 sample annealed at 1000 oC for 2 h.
High carrier concentration ZnO nanowire arrays for binder-free conductive support of supercapacitors electrodes by Al doping.

PubMed

Zheng, Xin; Sun, Yihui; Yan, Xiaoqin; Sun, Xu; Zhang, Guangjie; Zhang, Qian; Jiang, Yaru; Gao, Wenchao; Zhang, Yue

2016-12-15

Doping semiconductor nanowires (NWs) for altering their electrical and optical properties is a critical strategy for tailoring the performance of nanodevices. Here, we prepared in situ Al-doped ZnO nanowire arrays by using continuous flow injection (CFI) hydrothermal method to promote the conductivity. This reasonable method offers highly stable precursor concentration for doping that effectively avoid the appearance of the low conductivity ZnO nanosheets. Benefit from this, three orders of magnitude rise of the carrier concentration from 10 16 cm -3 to 10 19 cm -3 can be achieved compared with the common hydrothermal (CH) mothed in Mott-Schottky measurement. Possible effect of Al-doping was discussed by first-principle theory. On this basis, Al-doped ZnO nanowire arrays was developed as a binder-free conductive support for supercapacitor electrodes and high capacitance was triggered. It is owing to the dramatically decreased transfer resistance induced by the growing free-moving electrons and holes. Our results have a profound significance not merely in the controlled synthesis of other doping nanomaterials by co-precipitation method but also in the application of binder-free energy materials or other materials. Copyright © 2016 Elsevier Inc. All rights reserved.
Facile synthesis of cobalt ferrite nanotubes using bacterial nanocellulose as template.

PubMed

Menchaca-Nal, S; Londoño-Calderón, C L; Cerrutti, P; Foresti, M L; Pampillo, L; Bilovol, V; Candal, R; Martínez-García, R

2016-02-10

A facile method for the preparation of cobalt ferrite nanotubes by use of bacterial cellulose nanoribbons as a template is described. The proposed method relays on a simple coprecipitation operation, which is a technique extensively used for the synthesis of nanoparticles (either isolated or as aggregates) but not for the synthesis of nanotubes. The precursors employed in the synthesis are chlorides, and the procedure is carried out at low temperature (90 °C). By the method proposed a homogeneous distribution of cobalt ferrite nanotubes with an average diameter of 217 nm in the bacterial nanocellulose (BC) aerogel (3%) was obtained. The obtained nanotubes are formed by 26-102 nm cobalt ferrite clusters of cobalt ferrite nanoparticles with diameters in the 9-13 nm interval. The nanoparticles that form the nanotubes showed to have a certain crystalline disorder, which could be attributed in a greater extent to the small crystallite size, and, in a lesser extent, to microstrains existing in the crystalline lattice. The BC-templated-CoFe2O4 nanotubes exhibited magnetic behavior at room temperature. The magnetic properties showed to be influenced by a fraction of nanoparticles in superparamagnetic state. Copyright © 2015 Elsevier Ltd. All rights reserved.
3-D dumbbell-like LiNi1/3Mn1/3Co1/3O2 cathode materials assembled with nano-building blocks for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Ryu, Won-Hee; Lim, Sung-Jin; Kim, Won-Keun; Kwon, HyukSang

2014-07-01

Dumbbell-like microsphere carbonate precursors including multi-transition metal components (Ni1/3Mn1/3Co1/3CO3) assembled with nano-building blocks were synthesized by urea-assisted solvo/hydrothermal method, and layered cathode materials (LiNi1/3Mn1/3Co1/3O2) were subsequently prepared using the similarly shaped carbonate precursors for Li-ion batteries. For the synthesis of hierarchical microsphere structures, the partial addition of viscous organic solvent (e.g. ethylene glycol) in aqueous solution played a crucial role, not only in suppressing the sudden particle growth but also in regulating the directional crystallization of carbonate particles on the surface. The dumbbell-like LiNi1/3Mn1/3Co1/3O2 assembled with nanocubes prepared via the urea-assisted solvo/hydrothermal method exhibited better electrochemical characteristics, such as initial discharge capacity, cyclic performance, and rate-capability as a cathode material of Li-ion batteries, compared with the LiNi1/3Mn1/3Co1/3O2 materials prepared via the conventional co-precipitation method.

Intelligent Processing of Ferroelectric Thin Films

DTIC Science & Technology

1993-09-03

the acetate precursors. The results from these experiments involving coprecipitation, hydrothermal , spray pyrolysis and freeze drying have shown that...Spray Pyrolysis (SP) D. Hydrothermal Processing (HP) The powder produced by each process was characterized by X-ray diffraction (XRD) and scanning...precursors were used as described above. Instead of ammonia solution, an oxalic acid solution was used as the3 precipitating agent. The precipitants
Surface immunoglobulin on cultured foetal mouse thymocytes

PubMed Central

Haustein, D.; Mandel, T. E.

1979-01-01

Organ cultures of 14–15 day foetal mouse thymus were used as a source of non-neoplastic differentiating T cells, free of contaminating B cells. Viable cells obtained from such cultured thymuses were radio-iodinated and immunoglobulins (Ig) were isolated by co-precipitation from the 125I-labelled cell-surface proteins released during 1 h of incubation at 37°. The precipitates, both reduced and unreduced, were then analysed by polyacrylamide gel electrophoresis. The unreduced material migrated in a 5% gel as a single peak with a mobility slightly faster than that of mouse IgG. After reduction, however, two peaks were obtained (in a 10% gel), one corresponding in migration to mouse light chain and the other which moved slightly faster than mouse μ chain. This pattern was identical with that previously seen for both surface Ig of normal mouse thymocytes and neoplastic T lymphoma cells. Uncultured, 15 day foetal thymocytes did not produce any detectable co-precipitated cell surface material. Ig detected in these experiments was therefore produced during in vitro culture by non-neoplastic T cells in a system free of contaminating B cells and mouse serum proteins. PMID:315364
[Effect of the interaction of microorganisms and iron oxides on arsenic releasing into groundwater in Chinese Loess].

PubMed

Xie, Yun-Yun; Chen, Tian-Hu; Zhou, Yue-Fei; Xie, Qiao-Qin

2013-10-01

A large part of groundwater in the Chinese Loess Plateau area is characterized by high arsenic concentration. Anaerobic bacteria have been considered to play key roles in promoting arsenic releasing from loess to groundwater. However, this hypothesis remains unconfirmed. Based on modeling experiments, this study investigated the speciation of arsenic in loess, and then determined the release rates and quantities of arsenic with the mediation of anaerobic bacteria. The results showed that arsenic contents in loess were between 23 mg.kg-1 and 30 mg.kg-1. No obvious arsenic content difference among loess samples was observed. The ratios for specific adsorbed, iron oxides co-precipitated and silicate co-precipitated arsenic were 37.76% , 36. 15% and 25. 69% , respectively. Indigenous microorganisms, dissimilatory iron reducing bacteria (DIRB) and sulfate reducing bacteria (SRB) could all promote the release of arsenic from loess. Organic matters highly affected the release rates. More than 100 mg.L-1 sodium lactate was required for all bacterial experiments to facilitate obvious arsenic release. Considering the redox condition in loess, the contribution of SRB to arsenic release in loess area was less feasible than that of DIRB and indigenous microorganisms.
Co-precipitated and collocated carbides and Cu-rich precipitates in a Fe-Cu steel characterized by atom-probe tomography.

PubMed

Kolli, R Prakash; Seidman, David N

2014-12-01

The composition of co-precipitated and collocated NbC carbide precipitates, Fe3C iron carbide (cementite), and Cu-rich precipitates are studied experimentally by atom-probe tomography (APT). The Cu-rich precipitates located at a grain boundary (GB) are also studied. The APT results for the carbides are supplemented with computational thermodynamics predictions of composition at thermodynamic equilibrium. Two types of NbC carbide precipitates are distinguished based on their stoichiometric ratio and size. The Cu-rich precipitates at the periphery of the iron carbide and at the GB are larger than those distributed in the α-Fe (body-centered cubic) matrix, which is attributed to short-circuit diffusion of Cu along the GB. Manganese segregation is not observed at the heterophase interfaces of the Cu-rich precipitates that are located at the periphery of the iron carbide or at the GB, which is unlike those located at the edge of the NbC carbide precipitates or distributed in the α-Fe matrix. This suggests the presence of two populations of NiAl-type (B2 structure) phases at the heterophase interfaces in multicomponent Fe-Cu steels.
Selective isolation of gold facilitated by second-sphere coordination with α-cyclodextrin

PubMed Central

Liu, Zhichang; Frasconi, Marco; Lei, Juying; Brown, Zachary J.; Zhu, Zhixue; Cao, Dennis; Iehl, Julien; Liu, Guoliang; Fahrenbach, Albert C.; Botros, Youssry Y.; Farha, Omar K.; Hupp, Joseph T.; Mirkin, Chad A.; Fraser Stoddart, J.

2013-01-01

Gold recovery using environmentally benign chemistry is imperative from an environmental perspective. Here we report the spontaneous assembly of a one-dimensional supramolecular complex with an extended {[K(OH2)6][AuBr4](α-cyclodextrin)2}n chain superstructure formed during the rapid co-precipitation of α-cyclodextrin and KAuBr4 in water. This phase change is selective for this gold salt, even in the presence of other square-planar palladium and platinum complexes. From single-crystal X-ray analyses of six inclusion complexes between α-, β- and γ-cyclodextrins with KAuBr4 and KAuCl4, we hypothesize that a perfect match in molecular recognition between α-cyclodextrin and [AuBr4]− leads to a near-axial orientation of the ion with respect to the α-cyclodextrin channel, which facilitates a highly specific second-sphere coordination involving [AuBr4]− and [K(OH2)6]+ and drives the co-precipitation of the 1:2 adduct. This discovery heralds a green host–guest procedure for gold recovery from gold-bearing raw materials making use of α-cyclodextrin—an inexpensive and environmentally benign carbohydrate. PMID:23673640
Uranium (III)-Plutonium (III) co-precipitation in molten chloride

NASA Astrophysics Data System (ADS)

Vigier, Jean-François; Laplace, Annabelle; Renard, Catherine; Miguirditchian, Manuel; Abraham, Francis

2018-02-01

Co-management of the actinides in an integrated closed fuel cycle by a pyrochemical process is studied at the laboratory scale in France in the CEA-ATALANTE facility. In this context the co-precipitation of U(III) and Pu(III) by wet argon sparging in LiCl-CaCl2 (30-70 mol%) molten salt at 705 °C is studied. Pu(III) is prepared in situ in the molten salt by carbochlorination of PuO2 and U(III) is then introduced as UCl3 after chlorine purge by argon to avoid any oxidation of uranium up to U(VI) by Cl2. The oxide conversion yield through wet argon sparging is quantitative. However, the preferential oxidation of U(III) in comparison to Pu(III) is responsible for a successive conversion of the two actinides, giving a mixture of UO2 and PuO2 oxides. Surprisingly, the conversion of sole Pu(III) in the same conditions leads to a mixture of PuO2 and PuOCl, characteristic of a partial oxidation of Pu(III) to Pu(IV). This is in contrast with coconversion of U(III)-Pu(III) mixtures but in agreement with the conversion of Ce(III).
HSP86 and HSP84 exhibit cellular specificity of expression and co-precipitate with an HSP70 family member in the murine testis

NASA Technical Reports Server (NTRS)

Gruppi, C. M.; Wolgemuth, D. J.

1993-01-01

This study extends to the protein level our previous observations, which had established the stage and cellular specificity of expression of hsp86 and hsp84 in the murine testis in the absence of exogenous stress. Immunoblot analysis was used to demonstrate that HSP86 protein was present throughout testicular development and that its levels increased with the appearance of differentiating germ cells. HSP86 was most abundant in the germ cell population and was present at significantly lower levels in the somatic cells. By contrast, the HSP84 protein was detected in the somatic cells of the testis rather than in germ cells. The steady-state levels of HSP86 and HSP84 paralleled the pattern of the expression of their respective mRNAs, suggesting that regulation at the level of translation was not a major mechanism controlling hsp90 gene expression in testicular cells. Immunoprecipitation analysis revealed that a 70-kDa protein coprecipitated with the HSP86/HSP84 proteins in testicular homogenates. This protein was identified as an HSP70 family member by immunoblot analysis, suggesting that HSP70 and HSP90 family members interact in testicular cells.
Functionalized magnetic iron oxide/alginate core-shell nanoparticles for targeting hyperthermia

PubMed Central

Liao, Shih-Hsiang; Liu, Chia-Hung; Bastakoti, Bishnu Prasad; Suzuki, Norihiro; Chang, Yung; Yamauchi, Yusuke; Lin, Feng-Huei; Wu, Kevin C-W

2015-01-01

Hyperthermia is one of the promising treatments for cancer therapy. However, the development of a magnetic fluid agent that can selectively target a tumor and efficiently elevate temperature while exhibiting excellent biocompatibility still remains challenging. Here a new core-shell nanostructure consisting of inorganic iron oxide (Fe3O4) nanoparticles as the core, organic alginate as the shell, and cell-targeting ligands (ie, D-galactosamine) decorated on the outer surface (denoted as Fe3O4@Alg-GA nanoparticles) was prepared using a combination of a pre-gel method and coprecipitation in aqueous solution. After treatment with an AC magnetic field, the results indicate that Fe3O4@Alg-GA nanoparticles had excellent hyperthermic efficacy in a human hepatocellular carcinoma cell line (HepG2) owing to enhanced cellular uptake, and show great potential as therapeutic agents for future in vivo drug delivery systems. PMID:26005343
Synthesis of Mn doped ZnS nanocrystals: Crystallographic and morphological study

NASA Astrophysics Data System (ADS)

Shaikh, Azharuddin Z.; Shirsath, Narendra B.; Sonawane, Prabhakar S.

2018-05-01

The influence of doping concentration on the physical properties of ZnS nanocrystals synthesized using coprecipitation method at room temperature is reported in this paper. In particular, we have studied the structural properties of Zn1-xMnxS where (x=0.01, 0.03, 0.05) by X-ray diffraction. X-ray peak broadening analysis used to calculate the crystalline sizes, lattice parameters, number of unit cell per particle and volume of unit cell. Crystalline ZnS with a cubic structure is confirmed by XRD results. The grain size of pure and Mn doped samples were found in the range of 7nm to 9nm. All the physical parameters of cubic ZnS nanocrystals were calculated are similar with standard values. The scanning electron microscope (SEM) which revealed that the synthesized nanocrystals are well-crystalline and possessing cubic phase.
Stability and cellular responses to fluorapatite-collagen composites.

PubMed

Yoon, Byung-Ho; Kim, Hae-Won; Lee, Su-Hee; Bae, Chang-Jun; Koh, Young-Hag; Kong, Young-Min; Kim, Hyoun-Ee

2005-06-01

Fluorapatite (FA)-collagen composites were synthesized via a biomimetic coprecipitation method in order to improve the structural stability and cellular responses. Different amounts of ammonium fluoride (NH4F), acting as a fluorine source for FA, were added to the precipitation of the composites. The precipitated composites were freeze-dried and isostatically pressed in a dense body. The added fluorine was incorporated nearly fully into the apatite structure (fluoridation), and a near stoichiometric FA-collagen composite was obtained with complete fluoridation. The freeze-dried composites had a typical biomimetic network, consisting of collagen fibers and precipitates of nano-sized apatite crystals. The human osteoblast-like cells on the FA-collagen composites exhibited significantly higher proliferation and differentiation (according to alkaline phosphatase activity) than those on the hydroxyapatite-collagen composite. These enhanced osteoblastic cell responses were attributed to the fluorine release and the reduced dissolution rate.
Synthesis and characterization of CoFe2O4/polyaniline nanocomposites for electromagnetic interference applications.

PubMed

Praveena, K; Srinath, S

2014-06-01

The Cobalt ferrite (CoFe2O4) powders were synthesized by Co-precipitation method. The as prepared ferrite powders were incorporated into a polyaniline matrix at various volumetric ratios. The as prepared composites of ferrite and polyaniline powders were characterized using X-ray diffraction (XRD), transmission electron microscope (TEM). The particle size of CoFe2O4 is found to be 20 nm. The saturation magnetization (M(s)) of all the composites was found to be decreasing with decrease of ferrite content, while coercivity (H(c)) remained at the value corresponding to pure cobalt ferrite nanopowders. The complex permittivity (epsilon' and epsilon") and permeability (mu' and mu") of composite samples were measured in the range of 1 MHz to 1.1 GHz. The value of epsilon' and mu' found to be increased with ferrite volume concentration.
Superparamagnetic iron oxide nanoparticles incorporated into silica nanoparticles by inelastic collision via ultrasonic field: Role of colloidal stability

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sodipo, Bashiru Kayode; Azlan, Abdul Aziz; Innovation

2015-04-24

Superparamagnetic iron oxide nanoparticles (SPION)/Silica composite nanoparticles were prepared by ultrasonically irradiating colloidal suspension of silica and SPION mixture. Both silica and SPION were synthesized independently via co-precipitation and sol-gel method, respectively. Their mixtures were sonicated at different pH between 3 and 5. Electrophoresis measurement and other physicochemical analyses of the products demonstrate that at lower pH SPION was found incorporated into the silica. However, at pH greater than 4, SPION was unstable and unable to withstand the turbulence flow and shock wave from the ultrasonic field. Results suggest that the formation of the SPION/silica composite nanoparticles is strongly relatedmore » to the inelastic collision induced by ultrasonic irradiation. More so, the formation the composite nanoparticles via the ultrasonic field are dependent on the zeta potential and colloidal stability of the particles.« less
Characterization of Copper-Manganese-Aluminum-Magnesium Mixed Oxyhydroxide and Oxide Catalysts for Redox Reactions

NASA Astrophysics Data System (ADS)

Baksi, Arnab; Cocke, David L.; Gomes, Andrew; Gossage, John; Riggs, Mark; Beall, Gary; McWhinney, Hylton

Complex multi-metal catalysts require several stages in their preparation. These are: co-mixing, co-precipitation, milling and sol-gel, drying, dehydroxylation, and calcination and sometimes regeneration of the hydroxide by rehydration. These processes require thermal analysis (DTA, TGA, DSC) and accompanying off gas analysis, plus one or more of these: XRD, XPS, SEMEDS, FTIR and UV-VIS. In this study, hydrotalcite, hopcalite and mixed systems were prepared and guided by the above characterization techniques. The systems were initiated by mixing the chlorides or nitrates followed by hydrothermal treatments to produce the hydroxides which were further treated by washing, drying, and calcination. The thermal analysis was critical to guide the preparation through these stages and when combined with structural determination methods considerable understanding of their chemical and physical changes was obtained. The correlations between preparation and characterization will be discussed.
Effect of aluminum and yttrium doping on zinc sulphide nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sharma, Swati, E-mail: sharma.swati1507@gmail.com; Kashyap, Jyoti; Kapoor, A.

2016-05-06

In this work, pristine and doped Zinc Sulphide (ZnS) nanoparticles have been synthesized via chemical co-precipitation method. ZnS nanoparticles have been doped with Aluminium (Al) and Yttrium (Y) with doping concentration of 5wt% each. The structural and optical properties of the as prepared nanoparticles have been studied using X-Ray diffraction (XRD) technique and Photoluminescence spectroscopy. Average grain size of 2-3nm is observed through the XRD analysis. Effect of doping on stress, strain and lattice constant of the nanoparticles has also been analyzed. Photoluminescence spectra of the as prepared nanoparticles is enhanced due to Al doping and quenched due to Ymore » doping. EDAX studies confirm the relative doping percentage to be 3.47 % and 3.94% by wt. for Al and Y doped nanoparticles respectively. Morphology of the nanoparticles studied using TEM and SEM indicates uniform distribution of spherical nanoparticles.« less
Magnetite nanoparticles conjugated with lignin: A physicochemical and magnetic study

NASA Astrophysics Data System (ADS)

Klapiszewski, Łukasz; Zdarta, Jakub; Antecka, Katarzyna; Synoradzki, Karol; Siwińska-Stefańska, Katarzyna; Moszyński, Dariusz; Jesionowski, Teofil

2017-11-01

Using the by-product biopolymer lignin and nanoparticles of magnetite, well-known for its nontoxicity and magnetic properties, novel nanomagnetite-lignin hybrid materials were synthesized. In the first step, magnetite was produced via a co-precipitation method with hydrothermal treatment, and was found to have a particle size of around 20 nm. Nano-Fe3O4 was then combined with pre-activated lignin to obtain hybrids with various magnetite-lignin ratios, whose physicochemical and magnetic properties were thoroughly analyzed. Thermal analysis showed the hybrids to have higher thermal stability than pure lignin. Based on Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy it was demonstrated that the Fe3O4 and lignin are connected via Fesbnd Osbnd C bonds. Further measurements showed the nanomagnetite-lignin hybrid materials to have good magnetic properties. The results of this study suggest that the synthesized hybrids may find practical applications in many fields of science and industry.
Comparative Cytogenetic Study on the Toxicity of Magnetite and Zinc Ferrite Nanoparticles in Sunflower Root Cells

NASA Astrophysics Data System (ADS)

Foca-nici, Ecaterina; Capraru, Gabriela; Creanga, Dorina

2010-12-01

In this experimental study the authors present their results regarding the cellular division rate and the percentage of chromosomal aberrations in the root meristematic cells of Helianthus annuus cultivated in the presence of different volume fractions of magnetic nanoparticle suspensions, ranging between 20 and 100 microl/l. The aqueous magnetic colloids were prepared from chemically co-precipitated ferrites coated in sodium oleate. Tissue samples from the root meristeme of 2-3 day old germinated seeds were taken to prepare microscope slides following Squash method combined with Fuelgen techniques. Microscope investigation (cytogenetic tests) has resulted in the evaluation of mitotic index and chromosomal aberration index that appeared diminished and respectively increased following the addition of magnetic nanoparticles in the culture medium of the young seedlings. Zinc ferrite toxic influence appeared to be higher than that of magnetite, according to both cytogenetic parameters.
Investigation of electrical and magnetic properties of ferro-nanofluid on transformers

PubMed Central

2011-01-01

This study investigated a simple model of transformers that have liquid magnetic cores with different concentrations of ferro-nanofluids. The simple model was built on a capillary by enamel-insulated wires and with ferro-nanofluid loaded in the capillary. The ferro-nanofluid was fabricated by a chemical co-precipitation method. The performances of the transformers with either air core or ferro-nanofluid at different concentrations of nanoparticles of 0.25, 0.5, 0.75, and 1 M were measured and simulated at frequencies ranging from 100 kHz to 100 MHz. The experimental results indicated that the inductance and coupling coefficient of coils grew with the increment of the ferro-nanofluid concentration. The presence of ferro-nanofluid increased resistance, yielding to the decrement of the quality factor, owing to the phase lag between the external magnetic field and the magnetization of the material. PMID:21711784
Investigation of electrical and magnetic properties of ferro-nanofluid on transformers.

PubMed

Tsai, Tsung-Han; Chen, Ping-Hei; Lee, Da-Sheng; Yang, Chin-Ting

2011-03-28

This study investigated a simple model of transformers that have liquid magnetic cores with different concentrations of ferro-nanofluids. The simple model was built on a capillary by enamel-insulated wires and with ferro-nanofluid loaded in the capillary. The ferro-nanofluid was fabricated by a chemical co-precipitation method. The performances of the transformers with either air core or ferro-nanofluid at different concentrations of nanoparticles of 0.25, 0.5, 0.75, and 1 M were measured and simulated at frequencies ranging from 100 kHz to 100 MHz. The experimental results indicated that the inductance and coupling coefficient of coils grew with the increment of the ferro-nanofluid concentration. The presence of ferro-nanofluid increased resistance, yielding to the decrement of the quality factor, owing to the phase lag between the external magnetic field and the magnetization of the material.
Takovite-aluminosilicate-Cr materials prepared by adsorption of Cr3+ from industrial effluents as catalysts for hydrocarbon oxidation reactions.

PubMed

Ciuffi, Katia J; de Faria, Emerson H; Marçal, Liziane; Rocha, Lucas A; Calefi, Paulo S; Nassar, Eduardo J; Pepe, Iuri; da Rocha, Zênis N; Vicente, Miguel A; Trujillano, Raquel; Gil, Antonio; Korili, Sophia A

2012-05-01

The catalytic efficiency of takovite-aluminosilicate-chromium catalysts obtained by adsorption of Cr(3+) ions from aqueous solutions by a takovite-aluminosilicate nanocomposite adsorbent is reported. The adsorbent was synthesized by the coprecipitation method. The catalytic activity of the final Cr-catalysts depended on the amount of adsorbed chromium. (Z)-cyclooctene conversion up to 90% with total selectivity for the epoxide was achieved when the oxidation was carried out with hydrogen peroxide, at room temperature. After five consecutive runs, the catalysts maintained high activity, although after the sixth reuse, the epoxide yields strongly decreased to 35%. The catalysts were also efficient for cyclohexane oxidation, reaching up to 18% conversion, with cyclohexanone/cyclohexanol selectivity close to 1.2. On the whole, their use as catalysts gives a very interesting application for the solids obtained by adsorption of a contaminant cation such as Cr(3+).
Investigation of structural, optical and electrical properties of Co3O4 nanoparticles

NASA Astrophysics Data System (ADS)

Bhargava, Richa; Khan, Shakeel; Ahmad, Naseem; Ansari, Mohd Mohsin Nizam

2018-05-01

In the current work, we report the synthesis of Cobalt oxide (Co3O4) NPs (NPs) by co-precipitation method. The structural analysis was confirmed by using X-ray diffractometer (XRD) which shows that the Co3O4 NPs have cubic phase. The average crystallite size and the lattice parameter were calculated for Co3O4 NPs. The functional groups of the as-synthesized sample were examined by Fourier transform infrared spectroscopy (FTIR). The optical band gap of Co3O4 NPs was estimated by using UV diffuse reflectance spectroscopy and the Band gap was evaluated by using Tauc relation. The temperature dependence of dielectric constant and dielectric loss were studied over a range of temperature 50-300 °C. The DC electrical resistivity of Co3O4 NPs shows a semiconducting behaviour and the value of activation energy was calculated by using Arrhenius equation.

Investigation of xFe2O4 (x = Mn, Co) doped hydroxylapatite ferromagnetic biomaterials for the treatment of damaged bone and magnetically targeted drug delivery systems

NASA Astrophysics Data System (ADS)

Anand, Vikas; Singh, K. J.; Kaur, Kulwinder; Bhatia, Gaurav

2016-05-01

Magnetically attracted MnFe2O4 and CoFe2O4 doped hydroxylapatite samples have been prepared by using co-precipitation method in the laboratory. Bioactive nature of samples has been confirmed from XRD spectra. Ferromagnetic behavior of samples has been studied by using vibration sample magnetometer. Human osteoblast cell line MG63 has been used to explore the cell viability of samples. Drug carrier ability of samples has been checked with gentamycin as an antibiotic and results show that samples can be used as excellent drug carriers. Drug loaded samples can be easily targeted to specific area due to their attractive nature towards external magnetic field. Our results indicate that prepared samples possess good bioactive as well as ferromagnetic behavior with drug carrier ability and hence, our samples can be potential candidates for the clinical applications.
A biosensor system using nickel ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Singh, Prachi; Rathore, Deepshikha

2016-05-01

NiFe2O4 ferrite nanoparticles were synthesized by chemical co-precipitation method and the structural characteristics were investigated using X-ray diffraction technique, where single cubic phase formation of nanoparticles was confirmed. The average particle size of NiFe2O4 was found to be 4.9 nm. Nanoscale magnetic materials are an important source of labels for biosensing due to their strong magnetic properties which are not found in biological systems. This property of the material was exploited and the fabrication of the NiFe2O4 nanoparticle based biosensor was done in the form of a capacitor system, with NiFe2O4 as the dielectric material. The biosensor system was tested towards different biological materials with the help of electrochemical workstation and the same was analysed through Cole-Cole plot of NiFe2O4. The performance of the sensor was determined based on its sensitivity, response time and recovery time.
Embedding ultrafine ZnSnO3 nanoparticles into reduced graphene oxide composites as high-performance electrodes for lithium ion batteries

NASA Astrophysics Data System (ADS)

Ma, Yuhang; Jiang, Ranran; Li, Dan; Dong, Yutao; Liu, Yushan; Zhang, Jianmin

2018-05-01

Ultrafine ZnSnO3 nanoparticles, with an average diameter of 45 nm, homogeneously grown on reduced graphene oxide (rGO) have been successfully fabricated via methods of low temperature coprecipitation, colloid electrostatic self-assembly, and hydrothermal treatment. The uniformly distributed ZnSnO3 nanocrystals could inhibit the restacking of rGO sheets. In turn, the existence of rGO could hinder the growth and aggregation of ZnSnO3 nanoparticles in the synthesis process, increase the conductivity of the composite, and buffer the volume expansion of the ZnSnO3 nanocrystals upon lithium ion insertion and extraction. The obtained ZnSnO3/rGO exhibited superior cycling stability with a discharge/charge capacity of 718/696 mA h g-1 after 100 cycles at a current density of 0.1 A g-1.
Population and hierarchy of active species in gold iron oxide catalysts for carbon monoxide oxidation.

PubMed

He, Qian; Freakley, Simon J; Edwards, Jennifer K; Carley, Albert F; Borisevich, Albina Y; Mineo, Yuki; Haruta, Masatake; Hutchings, Graham J; Kiely, Christopher J

2016-09-27

The identity of active species in supported gold catalysts for low temperature carbon monoxide oxidation remains an unsettled debate. With large amounts of experimental evidence supporting theories of either gold nanoparticles or sub-nm gold species being active, it was recently proposed that a size-dependent activity hierarchy should exist. Here we study the diverging catalytic behaviours after heat treatment of Au/FeO x materials prepared via co-precipitation and deposition precipitation methods. After ruling out any support effects, the gold particle size distributions in different catalysts are quantitatively studied using aberration corrected scanning transmission electron microscopy (STEM). A counting protocol is developed to reveal the true particle size distribution from HAADF-STEM images, which reliably includes all the gold species present. Correlation of the populations of the various gold species present with catalysis results demonstrate that a size-dependent activity hierarchy must exist in the Au/FeO x catalyst.
Functionalized magnetic iron oxide/alginate core-shell nanoparticles for targeting hyperthermia.

PubMed

Liao, Shih-Hsiang; Liu, Chia-Hung; Bastakoti, Bishnu Prasad; Suzuki, Norihiro; Chang, Yung; Yamauchi, Yusuke; Lin, Feng-Huei; Wu, Kevin C-W

2015-01-01

Hyperthermia is one of the promising treatments for cancer therapy. However, the development of a magnetic fluid agent that can selectively target a tumor and efficiently elevate temperature while exhibiting excellent biocompatibility still remains challenging. Here a new core-shell nanostructure consisting of inorganic iron oxide (Fe3O4) nanoparticles as the core, organic alginate as the shell, and cell-targeting ligands (ie, D-galactosamine) decorated on the outer surface (denoted as Fe3O4@Alg-GA nanoparticles) was prepared using a combination of a pre-gel method and coprecipitation in aqueous solution. After treatment with an AC magnetic field, the results indicate that Fe3O4@Alg-GA nanoparticles had excellent hyperthermic efficacy in a human hepatocellular carcinoma cell line (HepG2) owing to enhanced cellular uptake, and show great potential as therapeutic agents for future in vivo drug delivery systems.
Development of magnetic octadecylsilane particles as solid-phase extraction adsorbent for the determination of fat-soluble vitamins in fruit juice-milk beverage by capillary liquid chromatography.

PubMed

Hu, Chaofan; Jia, Li; Liu, Qingqing; Zhang, Sheng

2010-07-01

A sensitive, fast and simple method based on magnetic octadecylsilane particles was developed for the extraction of three fat-soluble vitamins followed by capillary LC (CLC) analysis with UV detection. Magnetic octadecylsilane particles were prepared based on three-step reactions including co-precipitation, sol-gel polymerization and alkylation. The characterization of the prepared product was studied by scanning electron microscope and Fourier-transform infrared spectrometry. The particles were used as magnetic SPE adsorbent for the extraction of fat-soluble vitamins in fruit juice-milk beverage. The extraction condition and efficiency of the particles for fat-soluble vitamins were investigated. By coupling magnetic SPE with capillary LC with UV detection, low concentrations of fat-soluble vitamins in fruit juice-milk beverage can be detected without the interference from other substances in the sample matrix.
Protective effect of maghemite nanoparticles on ultraviolet-induced photo-damage in human skin fibroblasts

NASA Astrophysics Data System (ADS)

Lee, Kwon-Jai; An, Jeung-Hee; Shin, Jae-Soo; Kim, Dong-Hee; Kim, Changman; Ozaki, Hajime; Koh, Jae-Gui

2007-11-01

This study examined the optical properties of an oxidized form of maghemite (γ-Fe2O3) nanoparticles and their protective effects against the photoaging of human skin fibroblasts irradiated with ultraviolet (UV) light. Nanoparticles with diameters ranging from 8.7 to 12 nm were prepared using a chemical co-precipitation method. The nanoparticles were coated with two surfactants to obtain a water-based product. The onset of the absorption of the γ-Fe2O3 nanoparticles in the UV-visible absorption spectra increased with increasing particle size. The γ-Fe2O3 nanoparticles significantly inhibited the production of matrix metalloproteinase-1 in human skin fibroblast HS 68 cells by 60% compared with the UV-irradiated control. These results suggest that γ-Fe2O3 nanoparticles have photoprotective properties, and have potential use as an agent against photoaging.
ZnO supported CoFe2O4 nanophotocatalysts for the mineralization of Direct Blue 71 in aqueous environments.

PubMed

Sathishkumar, Panneerselvam; Pugazhenthiran, Nalenthiran; Mangalaraja, Ramalinga Viswanathan; Asiri, Abdullah M; Anandan, Sambandam

2013-05-15

In this study, an attempt was made to render both the magnetic and photocatalytic properties in a semiconductor material to enhance the efficiency of degradation and recycling possibility of magnetic nanophotocatalysts. CoFe2O4 and CoFe2O4 loaded ZnO nanoparticles were prepared by a simple co-precipitation method and characterized using various analytical tools and in addition to check its visible light assisted photocatalytic activity. CoFe2O4/ZnO nanocatalyst coupled with acceptor, peroxomonosulphate (PMS) showed 1.69-fold enhancement in Direct Blue 71 (triazo dye; DB71) mineralization within 5h. The accomplished enrichment in decolorization was due to the production of more number of non-selective and active free radicals at the catalyst surface. Copyright © 2013 Elsevier B.V. All rights reserved.
Gd3+ doped Mn-Zn soft ferrite nanoparticles: Superparamagnetism and its correlation with other physical properties

NASA Astrophysics Data System (ADS)

Thakur, Prashant; Sharma, Rohit; Sharma, Vineet; Barman, P. B.; Kumar, Manoj; Barman, Dipto; Katyal, S. C.; Sharma, Pankaj

2017-06-01

Superparamagnetic nanoparticles are very important in biomedicine due to their various applications like drug delivery, gene delivery in the body and also used for hyperthermia. In the present work, superparamagnetic nanoparticles of Mn0.5Zn0.5GdxFe2-xO4 (x = 0, 0.025, 0.050, 0.075, 0.1) ferrites have been prepared by co-precipitation method. Thorough characterizations (XRD, FTIR, FE-SEM, EDS, VSM and fluorescence spectroscopy) have proved the formation of cubical spinel superparamagnetic nanoparticles of soft ferrites. A cation distribution has been proposed for the determination of various important theoretical parameters for these samples. With the addition of Gd3+ nanoparticles have shown the superparamagnetism at room temperature confirmed by VSM analysis. Photoluminescence (PL) spectra shows a blue shift (for x = 0.025, 0.075) which may be due to quantum confinement.
Crystal structures and magnetic properties of magnetite (Fe{sub 3}O{sub 4})/Polyvinyl alcohol (PVA) ribbon

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ardiyanti, Harlina; Suharyadi, Edi, E-mail: esuharyadi@ugm.ac.id; Kato, Takeshi

2016-04-19

Ribbon of magnetite (Fe{sub 3}O{sub 4})/Polyvinyl Alcohol (PVA) nanoparticles have been successfully fabricated with various concentration of PVA synthesized by co-precipitation method. Particle size of nanoparticles Fe{sub 3}O{sub 4} sample and ribbon Fe{sub 3}O{sub 4}/PVA 25% sample is about 9.34 nm and 11.29 nm, respectively. The result of Vibrating Sample Magnetometer (VSM) showed that saturation magnetization value decreased from 76.99 emu/g to 15.01 emu/g and coercivity increased from 49.30 Oe to 158.35 Oe as increasing concentration of PVA. Atomic Force Microscopy (AFM) analysis showed that encapsulated PVA given decreasing agglomeration, controlled shape of nanoparticles Fe{sub 3}O{sub 4} more spherical and dispersed. Surfacemore » roughness decreased with increasing concentration of PVA.« less
Effect of Gold Nanoparticles Addition to CuO–ZnO/A₂O₃ Catalyst in Conversion of Carbon Dioxide to Methanol.

PubMed

Kim, Ki-Joong; Ahn, Ho-Geun

2017-04-01

Hydrogenation of carbon dioxide (CO₂) into methanol (CH₃OH) was carried out in the CuO–ZnO based supported gold catalyst prepared by the co-precipitation method. When gold nanoparticles were added to the CuO–ZnO/Al2O₃ catalysts (CuO–ZnO/Au/Al₂O₃), the CO₂ conversion and CH₃OH yield were increased (two times higher than that of CuO–ZnO/Al₂O₃ catalyst) with increasing reaction pressure, but selectivity of CH3OH was decreased. The main reason of this result could suggest the importance gold-oxides interface in CH₃OH formation through hydrogenation of CO₂. Maximum selectivity and yield to CH₃OH over CuO–ZnO/Au/Al₂O₃ were obtained at 250°C and under 15–20 bars.
Nanoscale zero-valent iron incorporated with nanomagnetic diatomite for catalytic degradation of methylene blue in heterogeneous Fenton system.

PubMed

Zha, Yiming; Zhou, Ziqing; He, Haibo; Wang, Tianlin; Luo, Liqiang

2016-01-01

Nanoscale zero-valent iron (nZVI) incorporated with nanomagnetic diatomite (DE) composite material was prepared for catalytic degradation of methylene blue (MB) in heterogeneous Fenton system. The material was constructed by two facile steps: Fe3O4 magnetic nanoparticles were supported on DE by chemical co-precipitation method, after which nZVI was incorporated into magnetic DE by liquid-phase chemical reduction strategy. The as-prepared catalyst was characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy, X-ray diffraction, magnetic properties measurement and nitrogen adsorption-desorption isotherm measurement. The novel nZVI@Fe3O4-diatomite nanocomposites showed a distinct catalytic activity and a desirable effect for degradation of MB. MB could be completely decolorized within 8 min and the removal efficiency of total organic carbon could reach to 90% after reaction for 1 h.
DOE Office of Scientific and Technical Information (OSTI.GOV)

Fu, Fang; Yao, Yuze; Wang, Haiyan

Rational and precise control of the structure and dimension of electrode materials is an efficient way to improve their electrochemical performance. In this work, solvothermal or co-precipitation method is used to synthesize lithium-rich layered oxide materials of Li1.2Mn0.56Co0.12Ni0.12O2 (LLO) with various morphologies and structures, including microspheres, microrods, nanoplates, and irregular nanoparticles. These materials exhibit strong structure- dependent electrochemical properties. The porous hierarchical structured LLO microrods exhibit the best performance, delivering a discharge capacity of 264.6 mAh g(-1) at 0.5 C with over 91% retention after 100 cycles. At a high rate of 5 C, a high discharge capacity of 173.6more » mAh g(-1) can be achieved. This work reveals the relationship between the morphologies and electrochemical properties of LLO cathode materials, and provides a feasible approach to fabricating robust and high-performance electrode materials for lithium-ion batteries.« less
A simple process to obtain anisotropic self-biased magnets constituted of stacked barium ferrite single domain particles

NASA Astrophysics Data System (ADS)

Mattei, Jean-Luc; Le, Cong Nha; Chevalier, Alexis; Maalouf, Azar; Noutehou, Nathan; Queffelec, Patrick; Laur, Vincent

2018-04-01

An efficient and inexpensive process is presented that produces highly oriented bulk compacts made of BaM particles. Barium hexaferrite particles (BaM, nominal composition BaFe11O19) were prepared by a chemical coprecipitation method, using different rates and types of precipitating agents (NaOH and Na2CO3). It was demonstrated that when a large excess of Na2CO3 is used, a noteworthy packing of hexagonal BaM platelets is obtained, after mechanical compaction and firing at moderate temperature (1140 °C), without including any more steps than those required for a conventional sintering process. The hysteresis loop displays a very competitive squareness of 0.88 (normalized remanent magnetization) and a coercivity of 215 kA/m, which make this BaM bulk ferrite suitable for self-biased applications.
Effect of Ce doping on structural, optical and photocatalytic properties of ZnO nano-structures.

PubMed

Selvam, N Clament Sagaya; Vijaya, J Judith; Kennedy, L John

2014-03-01

A novel self-assembled pure and Ce doped ZnO nano-particles (NPs) were successfully synthesized by a simple low temperature co-precipitation method. The prepared photocatalysts were characterized by X-ray diffraction (XRD), High resolution scanning electron microscopy (HR-SEM), High resolution transmission electron microscopy (HR-TEM), diffuse reflectance spectroscopy (DRS) and Photoluminescence (PL) spectroscopy. The results indicated that the prepared photocatalysts shows a novel morphology, high crystallinity, uniform size distribution, and more defects. Photocatalytic degradation (PCD) of nonylphenol, a potent endocrine disrupting chemical in aqueous medium was investigated. Higher amount of oxygen defects exhibits enhanced PCD of nonylphenol. In addition, the influence of the Ce contents on the structure, morphology, absorption, emission and photocatalytic activity of ZnO nanoparticles (NPs) were investigated systematically. The relative PCD efficiency of pure ZnO, Ce-doped ZnO NPs and commercial TiO2 (Degussa P-25) have also been discussed.
A moderate method for preparation DMSA coated Fe3O4 nanoparticles

NASA Astrophysics Data System (ADS)

Song, L. N.; Gu, N.; Zhang, Y.

2017-01-01

A moderate way to prepare water soluble magnetic Fe3O4 nanoparticles has been developed. Firstly, oleic acid coated Fe3O4 is prepared by coprecipitation. Second, oleic acid were replaced by 2,3-dimercaptosuccinnic acid (DMSA) to prepare DMSA/Fe3O4 in the mixed solution of n-hexane and acetone. After dialysis and filtration the DMSA/Fe3O4 can be transferred into distilled water to form stable Fe3O4 nanoparticle solutions. The TEM images indicated that the particles had spherical shape and the nanoparticles were found to be 12 nm with a relatively narrow size distribution with the hydrodynamic size of 30 nm. And the result of VSM shows that DMSA/Fe3O4 nanoparticles have a saturation magnetization of 31 emu/g. The IR spectra indicated that the iron oxide was located by carboxyl matrix.
Significant Improvement of Thermal Stability for CeZrPrNd Oxides Simply by Supercritical CO2 Drying

PubMed Central

Fan, Yunzhao; Wang, Zizi; Xin, Ying; Li, Qian; Zhang, Zhaoliang; Wang, Yingxia

2014-01-01

Pr and Nd co-doped Ce-Zr oxide solid solutions (CZPN) were prepared using co-precipitation and microemulsion methods. It is found that only using supercritical CO2 drying can result in a significant improvement of specific surface area and oxygen storage capacity at lower temperatures for CZPN after aging at 1000°C for 12 h in comparison with those using conventional air drying and even supercritical ethanol drying. Furthermore, the cubic structure was obtained in spite of the fact that the atomic ratio of Ce/(Ce+Zr+Pr+Nd) is as low as 29%. The high thermal stability can be attributed to the loosely aggregated morphology and the resultant Ce enrichment on the nanoparticle surface, which are caused by supercritical CO2 drying due to the elimination of surface tension effects on the gas-liquid interface. PMID:24516618
Rapid sequential determination of Pu, 90Sr and 241Am nuclides in environmental samples using an anion exchange and Sr-Spec resins.

PubMed

Lee, M H; Ahn, H J; Park, J H; Park, Y J; Song, K

2011-02-01

This paper presents a quantitative and rapid method of sequential separation of Pu, (90)Sr and (241)Am nuclides in environmental soil samples with an anion exchange resin and Sr Spec resin. After the sample solution was passed through an anion exchange column connected to a Sr Spec column, Pu isotopes were purified from the anion exchange column. Strontium-90 was separated from other interfering elements by the Sr Spec column. Americium-241 was purified from lanthanides by the anion exchange resin after oxalate co-precipitation. Measurement of Pu and Am isotopes was carried out using an α-spectrometer. Strontium-90 was measured by a low-level liquid scintillation counter. The radiochemical procedure of Pu, (90)Sr and (241)Am nuclides investigated in this study validated by application to IAEA reference materials and environmental soil samples. Copyright © 2010 Elsevier Ltd. All rights reserved.
Encapsulation of basic fibroblast growth factor by polyelectrolyte multilayer microcapsules and its controlled release for enhancing cell proliferation.

PubMed

She, Zhen; Wang, Chunxia; Li, Jun; Sukhorukov, Gleb B; Antipina, Maria N

2012-07-09

Basic fibroblast growth factor (FGF2) is an important protein for cellular activity and highly vulnerable to environmental conditions. FGF2 protected by heparin and bovine serum albumin was loaded into the microcapsules by a coprecipitation-based layer-by-layer encapsulation method. Low cytotoxic and biodegradable polyelectrolytes dextran sulfate and poly-L-arginine were used for capsule shell assembly. The shell thickness-dependent encapsulation efficiency was measured by enzyme-linked immunosorbent assay. A maximum encapsulation efficiency of 42% could be achieved by microcapsules with a shell thickness of 14 layers. The effects of microcapsule concentration and shell thickness on cytotoxicity, FGF2 release kinetics, and L929 cell proliferation were evaluated in vitro. The advantage of using microcapsules as the carrier for FGF2 controlled release for enhancing L929 cell proliferation was analyzed.
Polyaniline/Fe3O4-RGO Nanocomposites for Microwave Absorption

NASA Astrophysics Data System (ADS)

Mathew, Jithin; Sathishkumar, M.; Kothurkar, Nikhil K.; Senthilkumar, R.; Sabarish Narayanan, B.

2018-02-01

Fe3O4 nanoparticles were synthesized by co-precipitation of ferric chloride (FeCl3) and ferrous chloride (FeCl2). Reduced graphene oxide (RGO) was prepared by reducing the graphene oxide, which was synthesized by Hummer’s method, using hydrazine hydrate. Three nanocomposites based on sodium dodecyl benzene sulphonate (SDBS)-doped polyaniline were synthesized through in situ polymerization in the presence of the fillers (i) Fe3O4, (ii) reduced graphene oxide (RGO) and (iii) Fe3O4-decorated RGO respectively. The synthesized PANI and the composites were characterized by X-ray diffraction, Fourier transform infrared spectroscopy and transmission electron microscopy. Their microstructures, electrical conductivities, and EMI shielding effectiveness were studied. The nanocomposite containing 10 % RGO showed the maximum electrical conductivity and the one with 10 % RGO and 10 % Fe3O4 showed the maximum EMI shielding effectiveness of 7.5 dB for a 1 mm thick sample.

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