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Sample records for oxalate co-precipitation method

  1. Co-precipitation of plutonium(IV) and americium(III) from nitric acid-oxalic acid solutions with bismuth oxalate

    International Nuclear Information System (INIS)

    Pius, I.C.; Noronha, D.M.; Chaudhury, Satyajeet

    2017-01-01

    Co-precipitation of plutonium and americium from nitric acid-oxalic acid solutions with bismuth oxalate has been investigated for the removal of these long lived α-active nuclides from waste solutions. Effect of concentration of bismuth and oxalic acid on the co-precipitation of Pu(IV) from 3 M HNO_3 has been investigated. Similar experiments were also carried out from 3.75 M HNO_3 on co-precipitation of Am(III) to optimize the conditions of precipitation. Strong co-precipitation of Pu(IV) and Am(III) with bismuth oxalate indicate feasibility of treatment of plutonium and americium bearing waste solutions. (author)

  2. A new method for the homogeneous precipitative separation of trace level lanthanides as oxalates: application to different types of geological samples

    International Nuclear Information System (INIS)

    Premadas, A.; Cyriac, Bincy; Kesavan, V.S.

    2013-01-01

    Oxalate precipitation of lanthanides in acidic medium is a widely used selective group separation method at percentage to trace level in different types of geological samples. Most of the procedures are based on the heterogeneous oxalate precipitation of lanthanides using calcium as carrier. In the heterogeneous precipitation, the co-precipitated impurities from the matrix elements are more, besides if the pH at the time of precipitation is not monitored carefully there is a chance of losing some of the lanthanides. In this report, we present a new homogeneous oxalate precipitation of trace level lanthanides from different types of geological samples using calcium as carrier. In the present method pH is getting adjusted (pH ∼1) on its own, after the hydrolysis of urea added to the sample solution. This acidic pH is essential for the complete precipitation of the lanthanides. Therefore, no critical parameter adjustment for the precipitation is involved in the proposed method. The oxalate precipitate obtained was in crystalline nature which facilitates the fast settlement, easy filtration; besides the co-precipitated matrix elements are very less as compared to normal heterogeneous oxalate precipitation of lanthanides. Another advantage is more quantity of the sample can be taken for the separation of lanthanides which is a limitation for other separation methods reported. Accuracy of the method was checked by analyzing nine international reference materials comprising different types of geological samples obtained from Canadian Certified Reference Project Materials such as syenite samples SY-2, SY-3 and SY-4; gabro sample MRG-1; soil samples SO-1 and SO-2; iron formation sample FeR-2; lake sediments LKSD-2 and LKSD-4. The values of the lanthanides obtained for these reference materials are comparable with recommended values, indicating that the method is accurate. The reproducibility is characterized by a relative standard deviation (RSD) of 1 to 6% (n=4). (author)

  3. Cerium oxalate precipitation

    International Nuclear Information System (INIS)

    Chang, T.P.

    1987-02-01

    Cerium, a nonradioactive, common stand-in for plutonium in development work, has been used to simulate several plutonium precipitation processes at the Savannah River Laboratory. There are similarities between the plutonium trifluoride and the cerium oxalate precipitations in particle size and extent of plating, but not particle morphology. The equilibrium solubility, precipitation kinetics, particle size, extent of plating, and dissolution characteristics of cerium oxalate have been investigated. Interpretations of particle size and plating based on precipitation kinetics (i.e., nucleation and crystal growth) are presented. 16 refs., 7 figs., 6 tabs

  4. Precipitation of plutonium oxalate from homogeneous solutions

    International Nuclear Information System (INIS)

    Rao, V.K.; Pius, I.C.; Subbarao, M.; Chinnusamy, A.; Natarajan, P.R.

    1986-01-01

    A method for the precipitation of plutonium(IV) oxalate from homogeneous solutions using diethyl oxalate is reported. The precipitate obtained is crystalline and easily filterable with yields in the range of 92-98% for precipitations involving a few mg to g quantities of plutonium. Decontamination factors for common impurities such as U(VI), Am(III) and Fe(III) were determined. TGA and chemical analysis of the compound indicate its composition as Pu(Csub(2)Osub(4))sub(2).6Hsub(2)O. Data are obtained on the solubility of the oxalate in nitric acid and in mixtures of nitric acid and oxalic acid of varying concentrations. Green PuOsub(2) obtained by calcination of the oxalate has specifications within the recommended values for trace foreign substances such as chlorine, fluorine, carbon and nitrogen. (author)

  5. Decomposition of oxalate precipitates by photochemical reaction

    International Nuclear Information System (INIS)

    Jae-Hyung Yoo; Eung-Ho Kim

    1999-01-01

    A photo-radiation method was applied to decompose oxalate precipitates so that it can be dissolved into dilute nitric acid. This work has been studied as a part of partitioning of minor actinides. Minor actinides can be recovered from high-level wastes as oxalate precipitates, but they tend to be coprecipitated together with lanthanide oxalates. This requires another partitioning step for mutual separation of actinide and lanthanide groups. In this study, therefore, some experimental work of photochemical decomposition of oxalate was carried out to prove its feasibility as a step of partitioning process. The decomposition of oxalic acid in the presence of nitric acid was performed in advance in order to understand the mechanistic behaviour of oxalate destruction, and then the decomposition of neodymium oxalate, which was chosen as a stand-in compound representing minor actinide and lanthanide oxalates, was examined. The decomposition rate of neodymium oxalate was found as 0.003 mole/hr at the conditions of 0.5 M HNO 3 and room temperature when a mercury lamp was used as a light source. (author)

  6. Optimization of precipitation conditions of thorium oxalate precipitate

    International Nuclear Information System (INIS)

    Pazukhin, Eh.M.; Smirnova, E.A.; Krivokhatskij, A.S.; Pazukhina, Yu.L.; Kiselev, P.P.

    1986-01-01

    Thorium precipitation in the form of difficultly soluble oxalate has been investigated. The equation binding the concentration of metal with the nitric acid in the initial solution and quantity of a precipitator necessary for minimization of desired product losses is derived. The graphical solution of this equation for a case, when the oxalic acid with 0.78 mol/l concentration is the precipitator, is presented

  7. Decomposition of oxalate precipitates by photochemical reaction

    International Nuclear Information System (INIS)

    Yoo, J.H.; Kim, E.H.

    1998-01-01

    A photo-radiation method was applied to decompose oxalate precipitates so that it can be dissolved into dilute nitric acid. This work has been studied as a part of partitioning of minor actinides. Minor actinides can be recovered from high-level wastes as oxalate precipitates, but they tend to be coprecipitated together with lanthanide oxalates. This requires another partitioning step for mutual separation of actinide and lanthanide groups. In this study, therefore, the photochemical decomposition mechanism of oxalates in the presence of nitric acid was elucidated by experimental work. The decomposition of oxalates was proved to be dominated by the reaction with hydroxyl radical generated from the nitric acid, rather than with nitrite ion also formed from nitrate ion. The decomposition rate of neodymium oxalate, which was chosen as a stand-in compound representing minor actinide and lanthanide oxalates, was found to be 0.003 M/hr at the conditions of 0.5 M HNO 3 and room temperature when a mercury lamp was used as a light source. (author)

  8. Two-stage precipitation of neptunium (IV) oxalate

    International Nuclear Information System (INIS)

    Luerkens, D.W.

    1983-07-01

    Neptunium (IV) oxalate was precipitated using a two-stage precipitation system. A series of precipitation experiments was used to identify the significant process variables affecting precipitate characteristics. Process variables tested were input concentrations, solubility conditions in the first stage precipitator, precipitation temperatures, and residence time in the first stage precipitator. A procedure has been demonstrated that produces neptunium (IV) oxalate particles that filter well and readily calcine to the oxide

  9. Organic oxalate as leachant and precipitant for the recovery of valuable metals from spent lithium-ion batteries

    International Nuclear Information System (INIS)

    Sun Liang; Qiu Keqiang

    2012-01-01

    Graphical abstract: Display Omitted Highlights: ► Vacuum pyrolysis as a pretreatment was used to separate cathode material from aluminum foils. ► Cobalt and lithium can be leached using oxalate while cobalt can be directly precipitated as cobalt oxalate. ► Cobalt and lithium can be separated efficiently from each other only in the oxalate leaching process. ► High reaction efficiency of LiCoO 2 was obtained with oxalate. - Abstract: Spent lithium-ion batteries containing lots of strategic resources such as cobalt and lithium are considered as an attractive secondary resource. In this work, an environmentally compatible process based on vacuum pyrolysis, oxalate leaching and precipitation is applied to recover cobalt and lithium from spent lithium-ion batteries. Oxalate is introduced as leaching reagent meanwhile as precipitant which leaches and precipitates cobalt from LiCoO 2 and CoO directly as CoC 2 O 4 ·2H 2 O with 1.0 M oxalate solution at 80 °C and solid/liquid ratio of 50 g L −1 for 120 min. The reaction efficiency of more than 98% of LiCoO 2 can be achieved and cobalt and lithium can also be separated efficiently during the hydrometallurgical process. The combined process is simple and adequate for the recovery of valuable metals from spent lithium-ion batteries.

  10. Precipitation stripping of neodymium from carboxylate extractant with aqueous oxalic acid solutions

    International Nuclear Information System (INIS)

    Konishi, Yasuhiro; Asai, Satoru; Murai, Tetuya

    1993-01-01

    This paper describes a precipitation stripping method in which neodymium ions are stripped from carboxylate extractant in organic solvent and simultaneously precipitated with aqueous oxalic acid solution. For the single-stage process, a quantitative criterion for precipitating oxalate powders was derived theoretically, and stripping experiments were done under the precipitation conditions. The resultant precipitates were neodymium oxalate, which is completely free from contamination by the carboxylate extractant and the organic solvent. The overall rate of stripping was controlled by the transfer of neodymium carboxylate in the organic solution, indicating that the presence of oxalic acid in the aqueous phase has no effect on the stripping rate. These findings demonstrate the feasibility of combining the conventional stripping and precipitation stages in a solvent extraction process for separation and purification of rare earths

  11. Modification the Oxalic Co-precipitation Method on a Novel Catalyst Cu/Zn/Al2O3/Cr2O3 for Autothermal Reforming Reaction of Methanol

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    Cheng- Hsin Kuo

    2013-12-01

    Full Text Available This study addresses the catalytic performance of Cu/ZnO/Al2O3/Cr2O3 in low-temperature of autothermal reforming (ATR reaction. Various operating conditions were used to decide the optimum reaction conditions: type of promoter (ZrO2, CeO2, and Cr2O3, precipitation temperature, precipitation pH, operation temperature, molar ratio of O2/CH3OH (O/C, and weight hourly space velocity (WHSV. The catalysts were prepared using the oxalic coprecipitation method. Characterization of the catalyst was conducted using a porosity analyzer, XRD, and SEM. The methanol conversion and volumetric percentage of hydrogen using the best catalyst (Cu/ZnO/Al2O3/Cr2O3 exceeded 93% and 43%, respectively. A catalyst prepared by precipitation at -5 oC and at pH of 1 converted methanol to 40% H2 and less than 3000 ppm CO at reaction temperature of 200 oC. The size and dispersion of copper and the degradation rate and turnover frequency of the catalyst was also calculated. Deactivation of the Cu catalyst at a reaction temperature of 200 oC occurred after 30 h. © 2013 BCREC UNDIP. All rights reservedReceived: 8th May 2013; Revised: 10th August 2013; Accepted: 18th August 2013[How to Cite: Cheng, H.K., Lesmana, D., Wu, H.S. (2013. Modification the Oxalic Co-precipitation Method on a Novel Catalyst Cu/Zn/Al2O3/Cr2O3 for Autothermal Reforming Reaction of Methanol. Bulletin of Chemical Reaction Engineering & Catalysis, 8 (2: 110-124. (doi:10.9767/bcrec.8.2.4844.110-124][Permalink/DOI: http://dx.doi.org/10.9767/bcrec.8.2.4844.110-124

  12. Dissolution of oxalate precipitate and destruction of oxalate ion by hydrogen peroxide in nitric acid solution

    International Nuclear Information System (INIS)

    Kim, Eung-Ho; Chung, Dong-Yong; Park, Jin-Ho; Yoo, Jae-Hyung

    2000-01-01

    This study aims at developing an oxalate precipitation process, which is applicable to a partitioning of long-lived radionuclides from the high-level radioactive liquid waste. In order to achieve this, a study for decomposition-reaction of oxalic acid by hydrogen peroxide was first carried out. The decomposition rates of H 2 O 2 and oxalic acid increased with an increase of nitric acid concentration, and especially those decomposition rates steeply increased at more than 2 M HNO 3 . Based on this result, the decomposition kinetics of H 2 O 2 and oxalic acid were suggested in this work. Then, the dissolution of oxalate precipitate and the destruction of oxalate ion in the solution were examined. Oxalate precipitates were prepared by adding oxalic acid into a simulated radioactive waste containing 8 metallic elements. The precipitates obtained thereby were dissolved in various nitric acid concentrations and reacted with H 2 O 2 at 90degC. When the oxalates were completely dissolved, most of the oxalates were decomposed by adding H 2 O 2 , but in a slurry state the decomposition yield of the oxalate decreased with an increase of the slurry density in the solution. Such phenomenon was considered to be due to a catalytic decomposition of H 2 O 2 on a solid surface of oxalate and the decomposition mechanism was explained by a charge transfer from a surface of oxalate solid to H 2 O 2 , producing OH radicals which can destruct H 2 O 2 explosively. Accordingly, the experimental condition for the decomposition of the oxalate precipitates was found to be most favorable at 3 M HNO 3 under the initial concentrations of 0.2 M oxalate and 1 M H 2 O 2 . At 3M HNO 3 , oxalate precipitates could be safely and completely dissolved, and almost decomposed. Additionally, it was observed that the presence of ferric ion in the solution largely affects the decomposition rate of H 2 O 2 . This could be explained by a chain reaction of hydrogen peroxide with ferric ion in the solution

  13. Precipitation of plutonium (III) oxalate and calcination to plutonium oxide

    International Nuclear Information System (INIS)

    Esteban, A.; Orosco, E.H.; Cassaniti, P.; Greco, L.; Adelfang, P.

    1989-01-01

    The plutonium based fuel fabrication requires the conversion of the plutonium nitrate solution from nuclear fuel reprocessing into pure PuO2. The conversion method based on the precipitation of plutonium (III) oxalate and subsequent calcination has been studied in detail. In this procedure, plutonium (III) oxalate is precipitated, at room temperature, by the slow addition of 1M oxalic acid to the feed solution, containing from 5-100 g/l of plutonium in 1M nitric acid. Before precipitation, the plutonium is adjusted to trivalent state by addition of 1M ascorbic acid in the presence of an oxidation inhibitor such as hydrazine. Finally, the precipitate is calcinated at 700 deg C to obtain PuO2. A flowsheet is proposed in this paper including: a) A study about the conditions to adjust the plutonium valence. b) Solubility data of plutonium (III) oxalate and measurements of plutonium losses to the filtrate and wash solution. c) Characterization of the obtained products. Plutonium (III) oxalate has several potential advantages over similar conversion processes. These include: 1) Formation of small particle sizes powder with good pellets fabrication characteristics. 2) The process is rather insensitive to most process variables, except nitric acid concentration. 3) Ambient temperature operations. 4) The losses of plutonium to the filtrate are less than in other conversion processes. (Author) [es

  14. Precipitation behavior of uranium in multicomponent solution by oxalic acid

    International Nuclear Information System (INIS)

    Shin, Y.J.; Kim, I.S.; Lee, W.K.; Shin, H.S.; Ro, S.G.

    1996-01-01

    A study on the precipitation of uranium by oxalic acid was carried out in a multicomponent solution. The precipitation method is usually applied to the treatment of radioactive waste and the recovery of uranium from a uranium-scrap contaminated with impurities. In these cases, the problem is how to increase the precipitation yield of target element and to prevent impurities from coprecipitation. The multicomponent solution in the present experiment was prepared by dissolving U, Nd, Cs and Sr in nitric acid. The effects of concentrations of oxalic acid and ascorbic acid on the precipitation yield and purity of uranium were observed. As results of the study, the maximum precipitation yield of uranium is revealed to be about 96.5% and the relative precipitation ratio of Nd, Cs and Sr versus uranium are discussed at the condition of the maximum precipitation yield of uranium, respectively. (author). 11 refs., 5 figs., 1 tab

  15. Study of lithium extraction from brine water, Bledug Kuwu, Indonesia by the precipitation series of oxalic acid and carbonate sodium

    Science.gov (United States)

    Sulistiyono, Eko; Lalasari, Latifa Hanum; Mayangsari, W.; Prasetyo, A. B.

    2018-05-01

    Lithium is one of the key elements in the development of batteries for electric car applications. Currently, the resources of the world's lithium are derived from brine water and lithium mineral based on spodumene rock. Indonesia which is located in the area of the ring of fire, has potential brine water resources in some area, such as brine water from Bledug Kuwu, Central Java that used in this research. The purposes of this research are to characterize brine water, Bledug Kuwu and to investigate the influence of chemical solvents on Li, Na, K, Ca, Mg, Al, B ion precipitation from brine water. This research was done with 2 times the process of chemical precipitation that runs series as follows: 5 liters of brine water were chemically precipitated using 400 ml of 12.43 N oxalic acid and followed by chemical precipitation using 400 mL of 7.07 N sodium carbonate solutions. Evaporation and filtration processes were also done twice in an effort to separate white precipitate and filtrate. The filtrate was analyzed by ICP-OES and white precipitates (salts) were analyzed by SEM, XRD, and XRF. The result shows that oxalate precipitation process extracted 32.24% Al, 23.42% B, 22.43% Ca, 14.26% Fe, 3.21 % K, 9.86% Na and 14.26% Li, the following process by carbonate precipitation process extracted 98.86% Mg, 73% Ca, 22.53% Li, 82.04% Al, 14.38% B, 12.50% K, 2.27% Na. There is 63.21% lithium is not extracted from the series process. The SEM analysis shows that the structure of granules on the precipitated salts by oxalic acid form gentle cubic-shaped solid. In the other hand, oxalate precipitation followed by sodium carbonate has various particle sizes and the shape of crystals is fragments, prism and cube look like magnesium carbonate, calcium chloride, and calcite's crystal respectively. This is in accordance with XRD analysis that phases of whewellite (CaC2O4.H2O), disodium oxalate (Na2C2O4), magnesite (MgCO3), calcium lithium aluminum (Al1.19 Ca1Li0.81), dolomite (CaCO3

  16. Study on the Key Technology of High Purity Strontium Titanate Powder Synthesized from Oxalic Acid Co-sediment Precipitation

    Science.gov (United States)

    Bi, Xiaoguo; Dong, Yingnan; Li, Yingjie; Niu, Wei; Tang, Jian; Ding, Shuang; Li, Meiyang

    2017-09-01

    Oxalate coprecipitation is applied in this paper, high purity titanium tetrachloride, and after the purification of strontium chloride, match with a certain concentration of solution, oxalate and strontium chloride and titanium tetrachloride in 1.005:1.000 make strontium titanium mixture ratio, slowly under 60°C to join in oxalic acid solution, aging around 4 h, get oxygen titanium strontium oxalate (SrTiO(C2O4)2 • 4H2 ) precipitation, after washing, drying and other process made oxygen titanium strontium oxalate powder.

  17. Studies on Pu(IV)/(III)-oxalate precipitation from nitric acid containing high concentration of calcium and fluoride ions

    International Nuclear Information System (INIS)

    Kalsi, P.K.; Pawar, S.M.; Ghadse, D.R.; Joshi, A.R.; Ramakrishna, V.V.; Vaidya, V.N.; Venugopal, V.

    2003-01-01

    Plutonium (IV)/(III) oxalate precipitation from nitric acid solution, containing large amount of calcium and fluoride ions was investigated. It was observed that direct precipitation of Pu (IV) oxalate from nitric acid containing large amount of calcium and fluoride ions did not give good decontamination of Pu from calcium and fluoride impurities. However, incorporation of hydroxide precipitation using ammonium hydroxide prior to Pu (IV) oxalate precipitation results into PuO 2 with much less calcium and fluoride impurities. Whereas, good decontamination from calcium and fluoride impurities could be obtained by employing Pu (III) oxalate precipitation directly from nitric acid containing large amount of calcium and fluoride ions. A method was also developed to recover Pu from the oxalate waste containing calcium and fluoride ions. (author)

  18. Continuous plutonium(IV) oxalate precipitation, filtration, and calcination process. [From product streams from Redox, Purex, or Recuplex solvent extraction plants

    Energy Technology Data Exchange (ETDEWEB)

    Beede, R L

    1956-09-27

    A continuous plutonium (IV) oxalate precipitation, filtration, and calcination process has been developed. Continuous and batch decomposition of the oxalate in the filtrates has been demonstrated. The processes have been demonstrated in prototype equipment. Plutonium (IV) oxalate was precipitated continuously at room temperature by the concurrent addition of plutonium (IV) nitrate feed and oxalic acid into the pan of a modified rotary drum filter. The plutonium (IV) oxalate was calcined to plutonium dioxide, which could be readily hydrofluorinated. Continuous decomposition of the oxalate in synthetic plutonium (IV) oxalate filtrates containing plutonium (IV) oxalate solids was demonstrated using co-current flow in a U-shaped reactor. Feeds containing from 10 to 100 g/1 Pu, as plutonium (IV) nitrate, and 1.0 to 6.5 M HNO/sub 3/, respectively, can be processed. One molar oxalic acid is used as the precipitant. Temperatures of 20 to 35/sup 0/C for the precipitation and filtration are satisfactory. Plutonium (IV) oxalate can be calcined at 300 to 400/sup 0/C in a screw-type drier-calciner to plutonium dioxide and hydrofluorinated at 450 to 550/sup 0/C. Plutonium dioxide exceeding purity requirements has been produced in the prototype equipment. Advantages of continuous precipitation and filtration are: uniform plutonium (IV) oxalate, improved filtration characteristics, elimination of heating and cooling facilities, and higher capacities through a single unit. Advantages of the screw-type drier-calciner are the continuous production of an oxide satisfactory for feed for the proposed plant vibrating tube hydrofluorinator, and ease of coupling continuous precipitation and filtration to this proposed hydrofluorinator. Continuous decomposition of oxalate in filtrates offers advantages in decreasing filtrate storage requirements when coupled to a filtrate concentrator. (JGB)

  19. Parametric study on co-precipitation of U/Th in MOX fuel of AHWR

    International Nuclear Information System (INIS)

    Tiwari, S.K.; Swaroopa Lakshmi, Y.; Nath, Baidurjya; Setty, D.S.; Kalyana Krishnan, G.; Saibaba, N.

    2015-01-01

    During manufacturing of Mixed Oxide Fuel (MOX) pellets for Advance Heavy Water Reactor (AHWR-LEU), around 30% rejected MOX pellets are generated in every cycle. These rejected MOX pellets are dissolved in nitric acid for recovery of U/Th. The recovered U/Th is recycled for production of MOX pellets. MOX pellets of varying compositions are used in AHWR fuel. Dissolution of MOX pellets in nitric acid is a challenging task because of its low surface area and longer dissolution times. High normal nitric acid is used in order to increase rate of dissolution, which in turn results in generation of high free acidity solution which influences the precipitation characteristics of Uranium (VI) by oxalic acid. Oxalic acid precipitation helps in generation of nitric acid which can be used for dissolution there by effectively facilitating nil effluent generation. Precipitation by oxalic acid unlike ammonia has advantage of zero liquid effluent discharge by complete recycle of oxalate filtrate to dissolution section. In the present work, the effect of various parameters like free acidity, residence time, concentration of oxalic acid, initial concentration of uranium and thorium etc. on the precipitation of U(VI) and Th(IV) in nitrate media by oxalic acid was carried out. The precipitated powder was subjected to various morphological evaluations like particle size etc. Study of various parameters on the co-precipitation of uranium and thorium by oxalic acid was carried out. It was observed that complete precipitation (> 99.9%) of thorium as oxalate does not depend on free acidity range (1- 6 N). Excess oxalic acid is not required for complete precipitation of thorium oxalate. The precipitation of uranyl oxalate varies with initial free acidity of solution. Uranyl oxalate precipitation does not take place at and above 5 N of free acidity

  20. Comparison of the method of classes and the quadrature of moment for the modelling of neodymium oxalate precipitation

    Energy Technology Data Exchange (ETDEWEB)

    Gaillard, J.P.; Lalleman, S.; Bertrand, M. [CEA, Centre de Marcoule, Nuclear Energy Division, RadioChemistry and Process Department, F-30207 Bagnols sur Ceze (France); Plasari, E. [Ecole Nationale Superieure des Industries Chimiques, Laboratoire Reactions et Genie des Procedes, Universite de Lorraine - CNRS,1 rue Grandville, BP 20451, 54001, Nancy Cedex (France)

    2016-07-01

    Oxalic precipitation is generally used in the nuclear industry to deal with radioactive waste and recover the actinides from a multicomponent solution. To facilitate the development of experimental methods and data acquisitions, actinides are often simulated using lanthanides, gaining experience more easily. The purpose of this article is to compare the results achieved by two methods for solving the population balance during neodymium oxalate precipitation in a continuous MSMPR (Mixed Suspension Mixed Product Removal). The method of classes, also called discretized population balance, used in this study is based on the method of Litster. Whereas, the Quadrature Method of Moment (QMOM) is written in terms of the transport equations of the moments of the number density function. All the integrals are solved through a quadrature approximation thanks to the product-difference algorithm or the Chebyshev algorithm. Primary nucleation, crystal growth and agglomeration are taken into account. Agglomeration phenomena have been found to be represented by a loose agglomerates model. Thermodynamic effects are modeled by activity coefficients which are calculated using the Bromley model. The sizes of particles predicted by the two methods are in good agreement with experimental measurements. (authors)

  1. Dynamic process model of a plutonium oxalate precipitator. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Miller, C.L.; Hammelman, J.E.; Borgonovi, G.M.

    1977-11-01

    In support of LLL material safeguards program, a dynamic process model was developed which simulates the performance of a plutonium (IV) oxalate precipitator. The plutonium oxalate precipitator is a component in the plutonium oxalate process for making plutonium oxide powder from plutonium nitrate. The model is based on state-of-the-art crystallization descriptive equations, the parameters of which are quantified through the use of batch experimental data. The dynamic model predicts performance very similar to general Hanford oxalate process experience. The utilization of such a process model in an actual plant operation could promote both process control and material safeguards control by serving as a baseline predictor which could give early warning of process upsets or material diversion. The model has been incorporated into a FORTRAN computer program and is also compatible with the DYNSYS 2 computer code which is being used at LLL for process modeling efforts.

  2. Dynamic process model of a plutonium oxalate precipitator. Final report

    International Nuclear Information System (INIS)

    Miller, C.L.; Hammelman, J.E.; Borgonovi, G.M.

    1977-11-01

    In support of LLL material safeguards program, a dynamic process model was developed which simulates the performance of a plutonium (IV) oxalate precipitator. The plutonium oxalate precipitator is a component in the plutonium oxalate process for making plutonium oxide powder from plutonium nitrate. The model is based on state-of-the-art crystallization descriptive equations, the parameters of which are quantified through the use of batch experimental data. The dynamic model predicts performance very similar to general Hanford oxalate process experience. The utilization of such a process model in an actual plant operation could promote both process control and material safeguards control by serving as a baseline predictor which could give early warning of process upsets or material diversion. The model has been incorporated into a FORTRAN computer program and is also compatible with the DYNSYS 2 computer code which is being used at LLL for process modeling efforts

  3. Physical simulation of precipitation of radioactive element oxalates by using the harmless neodymium oxalate for studying the agglomeration phenomena

    International Nuclear Information System (INIS)

    Lalleman, Sophie; Bertrand, Murielle; Plasari, Edouard

    2012-01-01

    Oxalic precipitation is usually applied in nuclear industry to process radioactive wastes or to recover actinides from a multicomponent solution.This paper deals with the development of methods adapted to a nuclear environment in order to study the agglomeration phenomena during actinide oxalic precipitation.These methods are previously set up with harmless elements that simulate the actinide behaviour: the lanthanides. A parametric study is carried out to quantify the influence of operating parameters on the agglomeration kernel and to determine a kinetic law for this mechanism. The experimental study is performed in a continuous-MSMPR precipitator at steady-state. The method is based on the resolution of two population balances using the moment approach, one for elementary crystals and the other for agglomerates. Provided that the kinetic rates of nucleation and growth are known, the agglomeration kernel can be obtained from a mathematical treatment of the experimental particle size distributions. Results point out that experimental crystal sizes are consistent with an independent kernel. It appears that the agglomeration kernel is directly proportional to supersaturation, increases with temperature but is limited by ionic strength and shear rate. (authors)

  4. Structural features and electrochemical properties of nanostructured ZnCo2O4 synthesized by an oxalate precursor method

    International Nuclear Information System (INIS)

    Kang, Wenpei; Feng, Fan; Zhang, Miaomiao; Liu, Shaojie; Shen, Qiang

    2013-01-01

    As a Li-ion battery anode, the active substance with a porous nanostructure can be endowed with a high electrochemical performance because of its porosity and remarkable surface area. In this paper, the thermal decomposition of zinc–cobalt binary oxalate precursors, precipitated from a solvothermal medium of ethanol and water (75/25, v/v) at 100 °C, has been performed to synthesize phase-pure ZnCo 2 O 4 spinels, thoroughly giving porous and rod-like configurations with an average length of a few micrometers. Interestingly, each of the as-obtained porous microrods has been well characterized to consist of ∼35.2-nm single-crystalline nanoparticles with polydisperse interspaces. More interestingly, porous ZnCo 2 O 4 microrods can deliver an initial specific discharge capacity of 1,293.7 mAh g −1 with the coulombic efficiency of 76.8 % at 0.2 A g −1 , reaching a value of 937.3 mAh g −1 over 100 discharge–charge cycles. Even at a high current density of 2.0 A g −1 , the porous ZnCo 2 O 4 nanostructures can still possess a reversible discharge capacity of ∼925.0 mAh g −1 , further assigned to the synergistic effect of Zn- and Co-based oxide components. Anyway, the facile oxalate precursor method can realize the controlling synthesis of porous and rod-like ZnCo 2 O 4 nanostructures with a high electrochemical performance

  5. Kinetic study of nucleation and crystal growth during oxalic precipitation in the nuclear industry

    International Nuclear Information System (INIS)

    Andrieu, Murielle

    1999-01-01

    In spite of an extensive use in chemical industry, most of precipitation processes are based on global and empirical knowledge. However, in the recent years, fundamental and phenomenological theories have been developed and they can be used to better understand the mechanisms of precipitation of plutonium IV oxalate, which is a significant stage of the irradiated fuel reprocessing. For this reason, appropriate methods were developed to study nucleation and crystal growth kinetics in a nuclear environment under a wide range of operating conditions. Each phenomena was studied individually in order to reduce the free parameters of the System. This study bears on the oxalates of plutonium and elements which simulate plutonium behaviour during the precipitation, neodymium III and uranium IV. A compact apparatus of a specific construction was used for nucleation measurements in accordance with the Nielsen's method. The state of the mixing was characterised at the reactor scale (macro-mixing) and at molecular scale (micro-mixing). The experimental results for the studied oxalates are in good agreement with the Volmer and Weber's theory. We propose primary nucleation kinetic laws over a wide range of operating conditions (temperature, non-stoichiometric conditions, acidity...). An original method, using a high seed charge, was developed for the determination of crystal growth kinetics, in a batch crystallizer. The crystal growth rate is first order with respect to the supersaturation and the kinetic constant follows an Arrhenius type relation with activation energies of 14, 29 and 36 kJ.mol -1 for respectively neodymium III, uranium IV and plutonium IV oxalates. The overall growth process is surface integration controlled, with a screw dislocation mechanism. [fr

  6. Nanoscale observations of the effect of citrate on calcium oxalate precipitation on calcite surfaces.

    Science.gov (United States)

    Burgos-Cara, Alejandro; Ruiz-Agudo, Encarnacion; Putnis, Christine V.

    2016-04-01

    Calcium oxalate (CaC2O4ṡxH2O) minerals are naturally occurring minerals found in fossils, plants, kidney stones and is a by-product in some processes such as paper, food and beverage production [1,2]. In particular, calcium oxalate monohydrate phase (COM) also known as whewellite (CaC2O4ṡH2O), is the most frequently reported mineral phase found in urinary and kidney stones together with phosphates. Organic additives are well known to play a key role in the formation of minerals in both biotic and abiotic systems, either facilitating their precipitation or hindering it. In this regard, recent studies have provided direct evidence demonstrating that citrate species could enhance dissolution of COM and inhibit their precipitation. [3,4] The present work aims at evauate the influence of pH, citrate and oxalic acid concentrations in calcium oxalate precipitation on calcite surfaces (Island Spar, Chihuahua, Mexico) through in-situ nanoscale observation using in situ atomic force microscopy (AFM, Multimode, Bruker) in flow-through experiments. Changes in calcium oxalate morphologies and precipitated phases were observed, as well as the inhibitory effect of citrate on calcium oxalate precipitation, which also lead to stabilization an the amorphous calcium oxalate phase. [1] K.D. Demadis, M. Öner, Inhibitory effects of "green"additives on the crystal growth of sparingly soluble salts, in: J.T. Pearlman (Ed.), Green Chemistry Research Trends, Nova Science Publishers Inc., New York, 2009, pp. 265-287. [2] M. Masár, M. Zuborová, D. Kaniansky, B. Stanislawski, Determination of oxalate in beer by zone electrophoresis on a chip with conductivity detection, J. Sep. Sci. 26 (2003) 647-652. [3] Chutipongtanate S, Chaiyarit S, Thongboonkerd V. Citrate, not phosphate, can dissolve calcium oxalate monohydrate crystals and detach these crystals from renal tubular cells. Eur J Pharmacol 2012;689:219-25. [4] Weaver ML, Qiu SR, Hoyer JR, Casey WH, Nancollas GH, De Yoreo JJ

  7. Study of Gel Growth Cobalt (II Oxalate Crystals as Precursor of Co3O4 Nano Particles

    Directory of Open Access Journals (Sweden)

    Yuniar Ponco Prananto

    2013-03-01

    Full Text Available Crystal growth of cobalt (II oxalate in silica gel at room temperature as precursor of Co3O4 nano particles has been studied. Specifically, this project is focusing on the use of two different reaction tube types toward crystallization of cobalt (II oxalate in gel. The gel was prepared at pH 5 by reacting sodium metasilicate solution with dilute nitric acid (for U-tube and oxalic acid (for straight tube, with gelling time of 4 days and crystal growth time of 8 (for straight tube and 12 (for U-tube weeks. Result shows that pink crystalline powder was directly formed using straight tube method. The use of different solvents in straight tube method affects crystallization and could delay direct precipitation of the product. In contrast, bigger and better shape of red block crystal was yielded from U-tube method; however, longer growth time was needed. FTIR studies suggest that both growth method produces identical compound of hydrated cobalt (II oxalate. © 2013 BCREC UNDIP. All rights reservedReceived: 25th October 2012; Revised: 30th November 2012; Accepted: 5th December 2012[How to Cite: Y.P. Prananto, M.M. Khunur, D.T. Wahyuni, R.A. Shobirin, Y.R. Nata, E. Riskah, (2013. Study of Gel Growth Cobalt (II Oxalate Crystals as Precursor of Co3O4 Nano Particles. Bulletin of Chemical Reaction Engineering & Catalysis, 7 (3: 198-204. (doi:10.9767/bcrec.7.3.4066.198-204][Permalink/DOI: http://dx.doi.org/10.9767/bcrec.7.3.4066.198-204 ] View in  |

  8. Preparation of cauliflower-like shaped Ba0.6Sr0.4TiO3 powders by modified oxalate co-precipitation method

    International Nuclear Information System (INIS)

    Li Mingli; Xu Mingxia

    2009-01-01

    The quantitative barium-strontium titanyl oxalate (Ba 0.6 Sr 0.4 TiO(C 2 O 4 ) 2 .4H 2 O, BSTO) precursor powders were prepared by the modified oxalate co-preparation method. It was based on the cation-exchange reaction between the stoichiometric solutions of oxalotitanic acid (H 2 TiO(C 2 O 4 ) 2 , HTO) and barium + strontium nitrate solution containing stoichiometric quantities of Ba and Sr ions. The pyrolysis of BSTO at 800 deg. C/4 h in air produced the homogeneous cauliflower-like shaped barium-strontium titanate (Ba 0.6 Sr 0.4 TiO 3 , BST) powders. The effect of polyethylene glycol (PEG) on morphology of BSTO and BST powders was also investigated. The characterization studies were carried on the as-dried BSTO and calcined BST powders by various physicochemical techniques, IR, X-ray diffraction (XRD), scanning electron microscopy (SEM), etc. The BSTO and BST powders obtained by aforementioned technique without PEG were homogeneous with spherical shape. The particles grew into spindle shape with the effect of PEG

  9. Optimisation of parameters for co-precipitation of uranium and plutonium - results of simulation studies

    International Nuclear Information System (INIS)

    Pandey, N.K.; Velvandan, P.V.; Murugesan, S.; Ahmed, M.K.; Koganti, S.B.

    1999-01-01

    Preparation of plutonium oxide from plutonium nitrate solution generally proceeds via oxalate precipitation route. In a nuclear fuel reprocessing scheme this step succeeds the partitioning step (separation of uranium and plutonium). Results of present studies confirm that it is possible to avoid partitioning step and recover plutonium and uranium as co-precipitated product. This also helps in minimising the risk of proliferation of fissile material. In this procedure, the solubility of uranium oxalate in nitric acid is effectively used. Co-precipitation parameters are optimised with simulated solutions of uranium nitrate and thorium nitrate (in place of plutonium). On the basis of obtained results a reconversion flow-sheet is designed and reported here. (author)

  10. Dynamic process model of a plutonium oxalate precipitator

    International Nuclear Information System (INIS)

    Borgonovi, G.M.; Hammelman, J.E.; Miller, C.L.

    1980-01-01

    A dynamic model of a plutonium oxalate precipitator is developed to provide a means of predicting plutonium inventory on a continuous basis. The model is based on state-of-the-art crystallization equations, which describe nucleation and growth phenomena. The model parameters were obtained through the use of batch experimental data. The model has been used to study the approach to steady state, to investigate the response to input transients, and to simulate the control of the precipitation process. 12 refs

  11. Morphological control of strontium oxalate particles by PSMA-mediated precipitation reaction

    Energy Technology Data Exchange (ETDEWEB)

    Yu Jiaguo [State Key Laboratory of Advanced Technology for Material Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China)]. E-mail: jiaguoyu@yahoo.com; Tang Hua [State Key Laboratory of Advanced Technology for Material Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Cheng Bei [State Key Laboratory of Advanced Technology for Material Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China)

    2005-05-15

    In this paper, strontium oxalate particles with different morphologies could be easily obtained by a precipitation reaction of sodium oxalate with strontium chloride in the absence and presence of poly-(styrene-alt-maleic acid) (PSMA). The as-prepared products were characterized with scanning electron microscopy and X-ray diffraction. The effects of pH, aging time and concentration of PSMA on the phase structures and morphologies of the as-prepared strontium oxalate particles were investigated and discussed. The results showed that strontium oxalate particles with various morphologies, such as, bi-pyramids, rods, peanuts, and spherical particles, etc., could be obtained by varying the experimental conditions. PSMA promoted the formation of strontium oxalate dihydrate (SOD) phase. Suitable pH values (pH 7 and 8) favor the formation of the peanut-shaped SrC{sub 2}O{sub 4} particles. This research may provide new insight into the control of morphologies and phase structures of strontium oxalate particles and the biomimetic synthesis of novel inorganic materials.

  12. Optimization of thorium oxalate precipitation conditions relative to thorium oxide sinterability

    International Nuclear Information System (INIS)

    White, G.D.; Bray, L.A.; Hart, P.E.

    1980-01-01

    The effect of thorium oxalate precipitation conditions on derived oxide sinterability was investigated with the objective of producing ThO 2 powder that could be sintered to high density without premilling. Precipitation conditions examined were temperature, digestion time and agitation method which were employed in a two-level factorial experimental design to delineate their effects. The two levels for each of the factors, respectively, were 10 0 C and 70 0 C, 15 min and 360 min, and mechanical stirrer and a homogenizer that imparted both mechanical and ultrasonic agitation. The ThO 2 derived from each of the precipitation trials was characterized with respect to morphology, surface area, and crystallite size as well as sinterability. Only precipitation temperature had a significant effect upon all the properties of the derived oxide powders

  13. Optimization of the conditions for the precipitation of thorium oxalate. II. Minimization of the product losses

    International Nuclear Information System (INIS)

    Pazukhin, E.M.; Smirnova, E.A.; Krivokhatskii, A.S.; Pazukhina, Yu.L.; Kiselev, P.P.

    1987-01-01

    The precipitation of thorium as a poorly soluble oxalate was investigated. An equation relating the concentrations of the metal and nitric acid in the initial solution and the amount of precipitant required to minimize the product losses was derived. A graphical solution of the equation is presented for the case where the precipitant is oxalic acid at a concentration of 0.78 M

  14. Laboratory-scale evaluations of alternative plutonium precipitation methods

    International Nuclear Information System (INIS)

    Martella, L.L.; Saba, M.T.; Campbell, G.K.

    1984-01-01

    Plutonium(III), (IV), and (VI) carbonate; plutonium(III) fluoride; plutonium(III) and (IV) oxalate; and plutonium(IV) and (VI) hydroxide precipitation methods were evaluated for conversion of plutonium nitrate anion-exchange eluate to a solid, and compared with the current plutonium peroxide precipitation method used at Rocky Flats. Plutonium(III) and (IV) oxalate, plutonium(III) fluoride, and plutonium(IV) hydroxide precipitations were the most effective of the alternative conversion methods tested because of the larger particle-size formation, faster filtration rates, and the low plutonium loss to the filtrate. These were found to be as efficient as, and in some cases more efficient than, the peroxide method. 18 references, 14 figures, 3 tables

  15. Analytical Study of Oxalates Coprecipitation

    Directory of Open Access Journals (Sweden)

    Liana MARTA

    2003-03-01

    Full Text Available The paper deals with the establishing of the oxalates coprecipitation conditions in view of the synthesis of superconducting systems. A systematic analytical study of the oxalates precipitation conditions has been performed, for obtaining superconducting materials, in the Bi Sr-Ca-Cu-O system. For this purpose, the formulae of the precipitates solubility as a function of pH and oxalate excess were established. The possible formation of hydroxo-complexes and soluble oxalato-complexes was taken into account. A BASIC program was used for tracing the precipitation curves. The curves of the solubility versus pH for different oxalate excess have plotted for the four oxalates, using a logaritmic scale. The optimal conditions for the quantitative oxalate coprecipitation have been deduced from the diagrams. The theoretical curves were confirmed by experimental results. From the precursors obtained by this method, the BSCCO superconducting phases were obtained by an appropriate thermal treatment. The formation of the superconducting phases was identified by X-ray diffraction analysis.

  16. Thorium oxalate solubility and morphology

    International Nuclear Information System (INIS)

    Monson, P.R. Jr.; Hall, R.

    1981-10-01

    Thorium was used as a stand-in for studying the solubility and precipitation of neptunium and plutonium oxalates. Thorium oxalate solubility was determined over a range of 0.001 to 10.0 in the concentration parameter [H 2 C 2 O 4 ]/[HNO 3 ] 2 . Morphology of thorium oxide made from the oxalate precipitates was characterized by scanning electron microscopy. The different morphologies found for oxalate-lean and oxalate-rich precipitations were in agreement with predictions based on precipitation theory

  17. LITERATURE REVIEW FOR OXALATE OXIDATION PROCESSES AND PLUTONIUM OXALATE SOLUBILITY

    Energy Technology Data Exchange (ETDEWEB)

    Nash, C.

    2012-02-03

    A literature review of oxalate oxidation processes finds that manganese(II)-catalyzed nitric acid oxidation of oxalate in precipitate filtrate is a viable and well-documented process. The process has been operated on the large scale at Savannah River in the past, including oxidation of 20 tons of oxalic acid in F-Canyon. Research data under a variety of conditions show the process to be robust. This process is recommended for oxalate destruction in H-Canyon in the upcoming program to produce feed for the MOX facility. Prevention of plutonium oxalate precipitation in filtrate can be achieved by concentrated nitric acid/ferric nitrate sequestration of oxalate. Organic complexants do not appear practical to sequester plutonium. Testing is proposed to confirm the literature and calculation findings of this review at projected operating conditions for the upcoming campaign. H Canyon plans to commence conversion of plutonium metal to low-fired plutonium oxide in 2012 for eventual use in the Mixed Oxide Fuel (MOX) Facility. The flowsheet includes sequential operations of metal dissolution, ion exchange, elution, oxalate precipitation, filtration, and calcination. All processes beyond dissolution will occur in HB-Line. The filtration step produces an aqueous filtrate that may have as much as 4 M nitric acid and 0.15 M oxalate. The oxalate needs to be removed from the stream to prevent possible downstream precipitation of residual plutonium when the solution is processed in H Canyon. In addition, sending the oxalate to the waste tank farm is undesirable. This report addresses the processing options for destroying the oxalate in existing H Canyon equipment.

  18. Liquid waste processing from plutonium (III) oxalate precipitation

    International Nuclear Information System (INIS)

    Esteban, A.; Cassaniti, P.; Orosco, E.H.

    1990-01-01

    Plutonium (III) oxalate filtrates contain about 0.2M oxalic acid, 0.09M ascorbic acid, 0.05M hydrazine, 1M nitric acid and 20-100 mg/l of plutonium. The developed treatment of liquid wastes consist in two main steps: a) Distillation to reduce up to 10% of the initial volume and refluxing to destroy organic material. Then, the treated solution is suitable to adjust the plutonium at the tetravalent state by addition of hydrogen peroxide and the nitric molarity up to 8.6M. b) Recovery and purification of plutonium by anion exchange using two columns in series containing Dowex 1-X4 resin. With the proposed process, it is possible to transform 38 litres of filtrates with 40mg/l of Pu into 0.1 l of purified solution with 15-20g/l of Pu. This solution is suitable to be recycled in the Pu (III) oxalate precipitation process. This process has several potential advantages over similar liquid waste treatments. These include: 1) It does not increase the liquid volume. 2) It consumes only few reagents. 3) The operations involved are simple, requiring limited handling and they are feasible to automatization. 4) The Pu recovery factor is about 99%. (Author) [es

  19. Anodic electrochemical performances of MgCo{sub 2}O{sub 4} synthesized by oxalate decomposition method and electrospinning technique for Li-ion battery application

    Energy Technology Data Exchange (ETDEWEB)

    Darbar, Devendrasinh [School of Mechanical and Building Science, Vellore Institute of Technology (VIT), Vellore 632014, Tamil Nadu (India); Department of Mechanical Engineering, National University of Singapore, 117576 (Singapore); Department of Physics, National University of Singapore, 117542 (Singapore); Reddy, M.V., E-mail: phymvvr@nus.edu.sg [Department of Physics, National University of Singapore, 117542 (Singapore); Department of Materials Science and Engineering, National University of Singapore, 117546 (Singapore); Sundarrajan, S. [Department of Mechanical Engineering, National University of Singapore, 117576 (Singapore); Pattabiraman, R. [School of Mechanical and Building Science, Vellore Institute of Technology (VIT), Vellore 632014, Tamil Nadu (India); Ramakrishna, S. [Department of Mechanical Engineering, National University of Singapore, 117576 (Singapore); Chowdari, B.V.R. [Department of Physics, National University of Singapore, 117542 (Singapore)

    2016-01-15

    Highlights: • MgCo{sub 2}O{sub 4} was prepared by oxalate decomposition method and electrospinning technique. • Electrospun MgCo{sub 2}O{sub 4} shows the reversible capacity of 795 and 227 mAh g{sup −1} oxalate decomposition MgCo{sub 2}O{sub 4} after 50 cycle. • Electrospun MgCo{sub 2}O{sub 4} show good cycling stability and electrochemical performance. - Abstract: Magnesium cobalt oxide, MgCo{sub 2}O{sub 4} was synthesized by oxalate decomposition method and electrospinning technique. The electrochemical performances, structures, phase formation and morphology of MgCo{sub 2}O{sub 4} synthesized by both the methods are compared. Scanning electron microscope (SEM) studies show spherical and fiber type morphology, respectively for the oxalate decomposition and electrospinning method. The electrospun nanofibers of MgCo{sub 2}O{sub 4} calcined at 650 °C, showed a very good reversible capacity of 795 mAh g{sup −1} after 50 cycles when compared to bulk material capacity of 227 mAh g{sup −1} at current rate of 60 mA g{sup −1}. MgCo{sub 2}O{sub 4} nanofiber showed a reversible capacity of 411 mAh g{sup −1} (at cycle) at current density of 240 mA g{sup −1}. Improved performance was due to improved conductivity of MgO, which may act as buffer layer leading to improved cycling stability. The cyclic voltammetry studies at scan rate of 0.058 mV/s show main cathodic at around 1.0 V and anodic peaks at 2.1 V vs. Li.

  20. Use of a pulsed column contactor as a continuous oxalate precipitation reactor

    International Nuclear Information System (INIS)

    Borda, Gilles; Brackx, Emmanuelle; Boisset, Laurence; Duhamet, Jean; Ode, Denis

    2011-01-01

    Research highlights: → A new type of continuous precipitating device was patented by CEA and tested with reaction between a surrogate nitrate cerium(III) or neodymium(III) and oxalate complexing agent. → Precipitate is confined in aqueous phase emulsion in tetrapropylene hydrogen and does not form deposit on the vessel walls. → Measure size of the precipitate ranges from 20 to 40 μm, it meets the process requirements to filter, and the precipitation reaction is complete. → The laboratory design can be extrapolated to an industrial uranium(IV) and minor actinide(III) coprecipitating column. - Abstract: The current objective of coprecipitating uranium, and minor actinides in order to fabricate a new nuclear fuel by direct (co)precipitation for further transmutation, requires to develop specific technology in order to meet the following requirements: nuclear maintenance, criticity, and potentially high flowrates due to global coprecipitation. A new type of device designed and patented by the CEA was then tested in 2007 under inactive conditions and with uranium. The patent is for organic confinement in a pulsed column (PC). Actually, pulsed columns have been working for a long time in a nuclear environment, as they allow high capacity, sub-critical design (annular geometry) and easy high activity maintenance. The precipitation reaction between the oxalate complexing agent and a surrogate nitrate - cerium(III) or neodymium(III) alone, or coprecipitated uranium(IV) and cerium(III) - occurs within an emulsion created in the device by these two phases flowing with a counter-current chemically inert organic phase (for example tetrapropylene hydrogen-TPH) produced by the stirring action of the column pulsator. The precipitate is confined and thus does not form deposits on the vessel walls (which are also water-repellent); it flows downward by gravity and exits the column continuously into a settling tank. The results obtained for precipitation of cerium or

  1. Turbulent precipitation of uranium oxalate in a vortex reactor - experimental study and modelling; Precipitation turbulente d'oxalate d'uranium en reacteur vortex - etude experimentale et modelisation

    Energy Technology Data Exchange (ETDEWEB)

    Sommer de Gelicourt, Y

    2004-03-15

    Industrial oxalic precipitation processed in an un-baffled magnetically stirred tank, the Vortex Reactor, has been studied with uranium simulating plutonium. Modelling precipitation requires a mixing model for the continuous liquid phase and the solution of population balance for the dispersed solid phase. Being chemical reaction influenced by the degree of mixing at molecular scale, that commercial CFD code does not resolve, a sub-grid scale model has been introduced: the finite mode probability density functions, and coupled with a model for the liquid energy spectrum. Evolution of the dispersed phase has been resolved by the quadrature method of moments, first used here with experimental nucleation and growth kinetics, and an aggregation kernel based on local shear rate. The promising abilities of this local approach, without any fitting constant, are strengthened by the similarity between experimental results and simulations. (author)

  2. Preparation of cauliflower-like shaped Ba{sub 0.6}Sr{sub 0.4}TiO{sub 3} powders by modified oxalate co-precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Li Mingli [School of Materials Science and Engineering, Key Laboratory for Advanced Ceramics and Machining Technology of Ministry of Education, Tianjin University, Tianjin 300072 (China)], E-mail: lml@tju.edu.cn; Xu Mingxia [School of Materials Science and Engineering, Key Laboratory for Advanced Ceramics and Machining Technology of Ministry of Education, Tianjin University, Tianjin 300072 (China)

    2009-04-17

    The quantitative barium-strontium titanyl oxalate (Ba{sub 0.6}Sr{sub 0.4}TiO(C{sub 2}O{sub 4}){sub 2}.4H{sub 2}O, BSTO) precursor powders were prepared by the modified oxalate co-preparation method. It was based on the cation-exchange reaction between the stoichiometric solutions of oxalotitanic acid (H{sub 2}TiO(C{sub 2}O{sub 4}){sub 2}, HTO) and barium + strontium nitrate solution containing stoichiometric quantities of Ba and Sr ions. The pyrolysis of BSTO at 800 deg. C/4 h in air produced the homogeneous cauliflower-like shaped barium-strontium titanate (Ba{sub 0.6}Sr{sub 0.4}TiO{sub 3}, BST) powders. The effect of polyethylene glycol (PEG) on morphology of BSTO and BST powders was also investigated. The characterization studies were carried on the as-dried BSTO and calcined BST powders by various physicochemical techniques, IR, X-ray diffraction (XRD), scanning electron microscopy (SEM), etc. The BSTO and BST powders obtained by aforementioned technique without PEG were homogeneous with spherical shape. The particles grew into spindle shape with the effect of PEG.

  3. Literature review for oxalate oxidation processes and plutonium oxalate solubility

    Energy Technology Data Exchange (ETDEWEB)

    Nash, C. A. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2015-10-01

    A literature review of oxalate oxidation processes finds that manganese(II)-catalyzed nitric acid oxidation of oxalate in precipitate filtrate is a viable and well-documented process. The process has been operated on the large scale at Savannah River in the past, including oxidation of 20 tons of oxalic acid in F-Canyon. Research data under a variety of conditions show the process to be robust. This process is recommended for oxalate destruction in H-Canyon in the upcoming program to produce feed for the MOX facility. Prevention of plutonium oxalate precipitation in filtrate can be achieved by concentrated nitric acid/ferric nitrate sequestration of oxalate. Organic complexants do not appear practical to sequester plutonium. Testing is proposed to confirm the literature and calculation findings of this review at projected operating conditions for the upcoming campaign.

  4. Turbulent precipitation of uranium oxalate in a vortex reactor - experimental study and modelling; Precipitation turbulente d'oxalate d'uranium en reacteur vortex - etude experimentale et modelisation

    Energy Technology Data Exchange (ETDEWEB)

    Sommer de Gelicourt, Y

    2004-03-15

    Industrial oxalic precipitation processed in an un-baffled magnetically stirred tank, the Vortex Reactor, has been studied with uranium simulating plutonium. Modelling precipitation requires a mixing model for the continuous liquid phase and the solution of population balance for the dispersed solid phase. Being chemical reaction influenced by the degree of mixing at molecular scale, that commercial CFD code does not resolve, a sub-grid scale model has been introduced: the finite mode probability density functions, and coupled with a model for the liquid energy spectrum. Evolution of the dispersed phase has been resolved by the quadrature method of moments, first used here with experimental nucleation and growth kinetics, and an aggregation kernel based on local shear rate. The promising abilities of this local approach, without any fitting constant, are strengthened by the similarity between experimental results and simulations. (author)

  5. Recovery of Am-Cm from high-activity waste concentrate by in-canyon-tank precipitation as oxalates

    International Nuclear Information System (INIS)

    Gray, L.W.; Burney, G.A.; Wilson, T.W.; McKibben, J.M.

    1980-01-01

    Savannah River Laboratory and Savannah River Plant have been separating actinides for more than 25 years. Work continues to upgrade processes and to initiate new processes. This report summarizes work on a precipitation process to separate kg amounts of Am and Cm from hundreds of kilograms of NaNO 3 and Al(NO 3 ) 3 . The developed process includes formic acid denitration of the Am-Cm bearing streams for acid adjustment; oxalate precipitation of the Am-Cm; and Mn +2 catalyzed oxidation of oxalate in both the decanted supernate and the precipitated actinides. The new process generates one fourth the radioactive waste as the solvent extraction process which it replaced, and produces a cleaner feed solution for downstream processing to separate the Am and Cm before conversion to their respective oxides

  6. Recovery Ce from Ce - TBP Used Oxalic Acid

    International Nuclear Information System (INIS)

    Purwani, MV; Subagiono, R.; Suyanti

    2007-01-01

    Recovery or stripping Ce from Ce - TBP product of monazite sand used oxalic acid. Ce - TBP as organic phase and oxalic acid as aqueous phase and as strong precipitant compound to precipitate metal element. The stripping product as Ce - oxalic precipitate. The influence parameter were percentage of oxalic acid, volume ratio of Ce-TBP with oxalic acid, time and rate of stripping. At stripping of 25 ml Ce - TBP used oxalic acid, the optimum condition were achieve at using 5% oxalic acid, volume ratio of Ce - TBP : 5% oxalic acid = 1 : 1, time of stripping 7.5 minute and rate of stripping 150 rpm. At the optimum condition was obtained the recovery efficiency was 100%. (author)

  7. Urinary oxalate excretion, as determined by isotope dilution and indirect colorimetry

    International Nuclear Information System (INIS)

    Prenen, J.A.C.; Boer, P.; Leersum, L. van; Oldenburg, S.J.; Endeman, H.J.

    1983-01-01

    A simple and reliable method for the determination of urinary oxalate excretion is described. Urinary oxalate is precipitated with calcium chloride, and the oxalate content of the precipitate is measured by an indirect colorimetric method developed by Neas and Guyon in 1972. For single urine samples, a correction is made for the incompleteness of the precipitation of calcium oxalate by isotope dilution. The range of normal values (5% limits) determined in 52 normal subjects was 0.121-0.325 mmol.24 h - 1 .m - 2 for a 1-day collection period and 0.145-0.301 mmol. 24 h - 1 .m - 2 for a 3-day collection period. The within-assay CV of a control urine with a low oxalate concentration was 9% (n=7) and the between-assay CV for the same control urine was 12% (n=6). When the values obtained for oxalate excretion were normalized to body surface area, there was no significant difference between males and females; the main source of variation was the intra-individual variation. (Auth.)

  8. Turbulent precipitation of uranium oxalate in a vortex reactor - experimental study and modelling

    International Nuclear Information System (INIS)

    Sommer de Gelicourt, Y.

    2004-03-01

    Industrial oxalic precipitation processed in an un-baffled magnetically stirred tank, the Vortex Reactor, has been studied with uranium simulating plutonium. Modelling precipitation requires a mixing model for the continuous liquid phase and the solution of population balance for the dispersed solid phase. Being chemical reaction influenced by the degree of mixing at molecular scale, that commercial CFD code does not resolve, a sub-grid scale model has been introduced: the finite mode probability density functions, and coupled with a model for the liquid energy spectrum. Evolution of the dispersed phase has been resolved by the quadrature method of moments, first used here with experimental nucleation and growth kinetics, and an aggregation kernel based on local shear rate. The promising abilities of this local approach, without any fitting constant, are strengthened by the similarity between experimental results and simulations. (author)

  9. Development of partitioning method

    International Nuclear Information System (INIS)

    Kobayashi, Tsutomu; Shirahashi, Koichi; Kubota, Masumitsu

    1989-11-01

    Precipitation behavior of elements in a high-level liquid waste (HLW) was studied by using the simulated liquid waste, when the transuranic elements group was precipitated and separated as oxalate from HLW generated from the reprocessing of spent nuclear fuel. The results showed that over 90 % of strontium and barium were precipitated when oxalic acid was directly added to HLW to precipitate the transuranic elements group, and the percentages of these elements precipitated were affected by molybdenum and or zirconium. Therefore, a method of adding oxalic acid into the filtrate was studied after removing previously molybdenum and zirconium as precipitate by denitrating HLW, and it was found that precipitated fractions of strontium and barium could be suppressed about 10 %. Adding oxalic acid under the co-existance of ascorbic acid is effective for quantitative precipitation of neptunium in HLW. In this case, it was found that adding ascorbic acid had little influence on precipitation behavior of the other elements except palladium. (author)

  10. De-agglomeration of thorium oxalate - a method for the synthesis of sinteractive thoria

    International Nuclear Information System (INIS)

    Ananthasivan, K.; Anthonysamy, S.; Singh, Alok; Vasudeva Rao, P.R.

    2002-01-01

    Thorium oxalate was obtained by precipitation in water and in non-aqueous solvents and de-agglomerated by ultrasonication in both aqueous as well as non-aqueous media. Sinteractive thoria (crystallite size 6-20 nm) obtained from the de-agglomerated thorium oxalate was characterised for residual carbon, crystallite size, specific surface area, particle size distribution and bulk density. Microstructure of the precursor and the product was studied using TEM and HRTEM. The morphology of the sintered pellets was studied using SEM. The reactivity of the calcined powders was determined by measuring the density of the sintered compacts. The solvent used for de-agglomeration was found to have significant influence on the microstructure of the powders. Thoria derived through aqueous precipitation route could be sintered to a density of 9.7 Mg m -3 at 1673 K. It was demonstrated that ultrasonic de-agglomeration could be a useful method for obtaining sinteractive thoria

  11. Optimization of air-sparged plutonium oxalate/hydroxide precipitators

    International Nuclear Information System (INIS)

    VanderHeyden, W.B.; Yarbro, S.L.; Fife, K.W.

    1997-04-01

    The high cost of waste management and experimental work makes numerical modeling an inexpensive and attractive tool for optimizing and understanding complex chemical processes. Multiphase open-quotes bubbleclose quotes columns are used extensively at the Los Alamos Plutonium Facility for a variety of different applications. No moving parts and efficient mixing characteristics allow them to be used in glovebox operations. Initially, a bubble column for oxalate precipitations is being modeled to identify the effect of various design parameters such as, draft tube location, air sparge rate and vessel geometry. Two-dimensional planar and axisymmetric models have been completed and successfully compared to literature data. Also, a preliminary three-dimensional model has been completed. These results are discussed in this report along with future work

  12. Method for rapid screening analysis of Sr-90 in edible plant samples collected near Fukushima, Japan

    International Nuclear Information System (INIS)

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

    2016-01-01

    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. - Highlights: • 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. • 90 Y-enriched eluate was analyzed by Cherenkov counting with a TDCR liquid scintillation counter. • 90 Sr ( 90 Y) concentration was determined in edible plant samples collected near the damaged Fukushima Daiichi NPPs with this method.

  13. Further Studies on Oxalic Acid Biosynthesis in Oxalate-accumulating Plants 1

    Science.gov (United States)

    Nuss, Richard F.; Loewus, Frank A.

    1978-01-01

    l-Ascorbic acid functions as a precursor of oxalic acid in several oxalate-accumulating plants. The present study extends this observation to include Rumex crispus L. (curly dock), Amaranthus retroflexus L. (red root pigweed), Chenopodium album L. (lamb's-quarters), Beta vulgaris L. (sugar beet), Halogeton glomeratus M. Bieb. (halogeton), and Rheum rhabarbarum L. (rhubarb). Several species with low oxalate content are also examined. When l-[1-14C]ascorbic acid is supplied to young seedlings of R. crispus or H. glomeratus, a major portion of the 14C is released over a 24-hour period as 14CO2 and only a small portion is recovered as [14C]oxalate, unlike cuttings from 2- or 4-month-old plants which retain a large part of the 14C as [14C]oxalic acid and release very little 14CO2. Support for an intermediate role of oxalate in the release of 14CO2 from l-[1-14C]ascorbic acid is seen in the rapid release of 14CO2 by R. crispus and H. glomeratus seedlings labeled with [14C]oxalic acid. The common origin of oxalic acid carbon in the C1 and C2 fragment from l-ascorbic acid is demonstrated by comparison of 14C content of oxalic acid in several oxalate-accumulators after cuttings or seedlings are supplied equal amounts of l-[1-14C]- or l-[UL-14C]ascorbic acid. Theoretically, l-[1-14C]ascorbic acid will produce labeled oxalic acid containing three times as much 14C as l-[UL-14C]ascorbic acid when equal amounts of label are provided. Experimentally, a ratio of 2.7 ± 0.5 is obtained in duplicate experiments with six different species. PMID:16660342

  14. Uranyl Oxalate Solubility

    Energy Technology Data Exchange (ETDEWEB)

    Leturcq, G.; Costenoble, S.; Grandjean, S. [CEA Marcoule DEN/DRCP/SCPS/LCA - BP17171 - 30207 Bagnols sur Ceze cedex (France)

    2008-07-01

    The solubility of uranyl oxalate was determined at ambient temperature by precipitation in oxalic-nitric solutions, using an initial uranyl concentration of 0.1 mol/L. Oxalic concentration varied from 0.075 to 0.3 mol/L while nitric concentration ranged between 0.75 and 3 mol/L. Dissolution tests, using complementary oxalic-nitric media, were carried out for 550 hours in order to study the kinetic to reach thermodynamic equilibrium. Similar solubility values were reached by dissolution and precipitation. Using the results, it was possible to draw the solubility surface versus oxalic and nitric concentrations and to determine both the apparent solubility constant of UO{sub 2}C{sub 2}O{sub 4}, 3H{sub 2}O (Ks) and the apparent formation constant of the first uranyl-oxalate complex UO{sub 2}C{sub 2}O{sub 4} (log {beta}1), for ionic strengths varying between 1 and 3 mol/L. Ks and log {beta}1 values were found to vary from 1.9 10{sup -8} to 9.2 10{sup -9} and from 5.95 to 6.06, respectively, when ionic strength varied from 1 to 3 mol/L. A second model may fit our data obtained at an ionic strength of 3 mol/L suggesting as reported by Moskvin et al. (1959) that no complexes are formed for [H{sup +}] at 3 M. The Ks value would then be 1.3 10{sup -8}. (authors)

  15. Separation of Am-Cm from NaNO3 waste solutions by in-canyon-tank precipitation as oxalates

    International Nuclear Information System (INIS)

    Gray, L.W.; Burney, G.A.; Wilson, T.W.; McKibben, J.M.

    1981-09-01

    A process for the purification of Am-Cm residues was developed specifically for application in Savannah River Plant (SRP) canyon tanks. These Am-Cm residues were collected from several campaigns to produce plutonium containing high isotopic concentrations of 240 Pu. An initial purification from Al 3+ had already been accomplished by a solvent extraction process. The product of this process was contaminated with NaNO 3 as a result of entrainment of the solvent extraction NaNO 3 scrub solution. To produce an acceptable feed solution for a later pressurized cation exchange chromatography separation and purification step, the bulk of the NaNO 3 must be removed. This purification process includes formic acid denitration, adjustment of contaminating cations by evaporation and water dilution, and oxalate precipitation of the actinides and lanthanides. After washing, the precipitate was dissolved in 8M nitric acid, and the oxalate was destroyed by nitric acid oxidation

  16. Influence of additives on the structure and microstructure of lanthanides and actinides oxalates

    International Nuclear Information System (INIS)

    Haidon, Blaise; Vitart, Anne-Lise; Rivenet, Murielle; Arab-Chapelet, Benedicte; Roussel, Pascal; Delahaye, Thibaud; Grandjean, Stephane; Abraham, Francis

    2015-07-01

    Oxalic conversion is a well-known process in the nuclear industry where it is used for precipitating plutonium as an oxalate thereafter calcinated into an oxide. As there is a strong relationship between the morphology of the oxalate precursor and that of the resulting oxide, it is of interest to control the oxalate structure and microstructure during the precipitation step. The influence of additives on the precipitation of neodymium (III) oxalates, non-radioactive analogs of actinides (III) oxalates, was explored. With the use of nitrilotri-methylphosphonic acid (NTMP), the structure and microstructure of the neodymium oxalates are different from that obtained without additive. (authors)

  17. Continuous precipitation process of plutonium salts; Procede continu de precipitation des sels de plutonium

    Energy Technology Data Exchange (ETDEWEB)

    Richard, P [Commissariat a l' Energie Atomique, Fontenay-aux-Roses (France). Centre d' Etudes Nucleaires

    1967-03-01

    This work concerns the continuous precipitation process of plutonium oxalate. Investigations about the solubility of different valence states in nitric-oxalic and in nitric-sulfuric-oxalic medium lead to select the precipitation process of tetravalent plutonium oxalate. Settling velocity and granulometry of tetravalent oxalate plutonium have been studied with variation of several precipitation parameters such as: temperature, acidity, excess of oxalic acid and aging time. Then are given test results of some laboratory continuous apparatus. Conditions of operation with adopted tubular apparatus are defined in conclusion. A flow-sheet is given for a process at industrial scale. (author) [French] Cette etude porte sur la precipitation continue de l'oxalate de plutonium. L'etude de la solubilite des differentes valences du plutonium dans des milieux acides nitrique-oxalique, puis nitrique-sulfurique-oxalique conduit a choisir la precipitation de l'oxalate de plutonium tetravalent. L'etude porte ensuite sur la sedimentation et la granulometrie de l'oxalate de Pu{sup 4+} obtenue en faisant varier differents parametres de la precipitation : la temperature, l'acidite, l'exces oxalique et le temps de murissement. La derniere partie traite des resultats obtenus avec plusieurs types d'appareils continus essayes au laboratoire. En conclusion sont donnees les conditions de marche de l'appareil tubulaire adopte, ainsi qu'une extrapolation a l'echelle industrielle sous forme d'un flow-sheet. (auteur)

  18. Structural variation study of cobalt nanoparticles synthesized by co-precipitation method using 59Co NMR

    Science.gov (United States)

    Manjunatha, M.; Kumar, Rajeev; B. M., Siddesh; Sahoo, Balaram; Damle, R.; Ramesh, K. P.

    2018-04-01

    We have synthesized cobalt nanoparticles using co-precipitation method. Further, the two phases of the cobalt is monitored by varying the synthesis parameters. 59Co NMR and XRD are used as characterization tools to study the phase variation in the cobalt samples. XRD and NMR results show a remarkable correlation in the two samples (Co-1 and Co-2). Co-2 has predominant fcc and hcp phases, whereas, Co-1 has fcc phase with lower amount of hcp. Both the samples show same saturation magnetization (Ms) but there is a remarkable difference in the phase composition. Thus, 59Co NMR appears to be a good tool to identify the phase purity of the ferromagnetic cobalt samples.

  19. Investigation of Neptunium Precipitator Cleanout Options

    International Nuclear Information System (INIS)

    Hill, B.C.

    2003-01-01

    Oxalate precipitation followed by filtration is used to prepare plutonium oxalate. Historically, plutonium oxalate has tended to accumulate in the precipitation tanks. These solids are periodically removed by flushing with concentrated (64 percent) nitric acid. The same precipitation tanks will now be used in the processing of neptunium. Literature values indicate that neptunium oxalate may not be as soluble as plutonium oxalate in nitric acid. Although a wide variety of options is available to improve neptunium oxalate solubility for precipitator flushing, most of these options are not practical for use. Many of these options require the use of incompatible or difficult to handle chemicals. Other options would require expensive equipment modifications or are likely to lead to product contamination. Based on review of literature and experimental results, the two best options for flushing the precipitator are (1) 64 percent nitric acid and (2) addition of sodium permanganate follow ed by sodium nitrite. Nitric acid is the easiest option to implement. It is already used in the facility and will not lead to product contamination. Experimental results indicate that neptunium oxalate can be dissolved in concentrated nitric acid (64 percent) at 60 degree C to a concentration of 2.6 to 5.6 grams of Np/liter after at least three hours of heating. A lower concentration (1.1 grams of Np/liter) was measured at 60 degree C after less than two hours of heating. These concentrations are acceptable for flushing if precipitator holdup is low (approximately 100-250 grams), but a second method is required for effective flushing if precipitator holdup is high (approximately 2 kilograms). The most effective method for obtaining higher neptunium concentrations is the use of sodium permanganate followed by the addition of sodium nitrite. There is concern that residual manganese from these flushes could impact product purity. Gas generation during permanganate addition is also a concern

  20. Morphology-controllable synthesis of cobalt oxalates and their conversion to mesoporous Co3O4 nanostructures for application in supercapacitors.

    Science.gov (United States)

    Wang, Dewei; Wang, Qihua; Wang, Tingmei

    2011-07-18

    In this work, one-dimensional and layered parallel folding of cobalt oxalate nanostructures have been selectively prepared by a one-step, template-free, water-controlled precipitation approach by simply altering the solvents used at ambient temperature and pressure. Encouragingly, the feeding order of solutions played an extraordinary role in the synthesis of nanorods and nanowires. After calcination in air, the as-prepared cobalt oxalate nanostructures were converted to mesoporous Co(3)O(4) nanostructures while their original frame structures were well maintained. The phase composition, morphology, and structure of the as-obtained products were studied in detail. Electrochemical properties of the Co(3)O(4) electrodes were carried out using cyclic voltammetry (CV) and galvanostatic charge-discharge measurements by a three-electrode system. The electrochemical experiments revealed that the layered parallel folding structure of mesoporous Co(3)O(4) exhibited higher capacitance compared to that of the nanorods and nanowires. A maximum specific capacitance of 202.5 F g (-1) has been obtained in 2 M KOH aqueous electrolyte at a current density of 1 A g(-1) with a voltage window from 0 to 0.40 V. Furthermore, the specific capacitance decay after 1000 continuous charge-discharge cycles was negligible, revealing the excellent stability of the electrode. These characteristics indicate that the mesoporous Co(3)O(4) nanostructures are promising electrode materials for supercapacitors.

  1. Continuous precipitation process of plutonium salts

    International Nuclear Information System (INIS)

    Richard, P.

    1967-03-01

    This work concerns the continuous precipitation process of plutonium oxalate. Investigations about the solubility of different valence states in nitric-oxalic and in nitric-sulfuric-oxalic medium lead to select the precipitation process of tetravalent plutonium oxalate. Settling velocity and granulometry of tetravalent oxalate plutonium have been studied with variation of several precipitation parameters such as: temperature, acidity, excess of oxalic acid and aging time. Then are given test results of some laboratory continuous apparatus. Conditions of operation with adopted tubular apparatus are defined in conclusion. A flow-sheet is given for a process at industrial scale. (author) [fr

  2. Characterization of oxalate-based 237NpO2 powder

    International Nuclear Information System (INIS)

    Rankin, D.T.; Burney, G.A.; Smith, P.K.; Sisson, R.D.

    1976-01-01

    238 Pu, a radioisotope heat source, is produced by irradiating reactor targets containing 237 NpO 2 . The neptunium oxide is obtained by precipitating and calcining 237 Np(IV) oxalate. The effects of oxalate precipitation parameters on particle morphology and size distribution of 237 NpO 2 powder were established to provide process controls for fabricating reactor targets

  3. Gas sensing properties of magnesium ferrite prepared by co-precipitation method

    International Nuclear Information System (INIS)

    Hankare, P.P.; Jadhav, S.D.; Sankpal, U.B.; Patil, R.P.; Sasikala, R.; Mulla, I.S.

    2009-01-01

    Polycrystalline magnesium ferrite (MgFe 2 O 4 ) was prepared by the co-precipitation method. The synthesized compound was characterized for their phase and morphology by X-ray diffraction and scanning electron microscopy, respectively. Conductance responses of the (MgFe 2 O 4 ) were measured towards gases like hydrogen sulfide (H 2 S), liquefied petroleum gas (LPG), ethanol vapors (C 2 H 5 OH), SO x , H 2 , NO x , NH 3, methanol, acetone and petrol. The gas sensing characterstics were obtained by measuring the sensitivity as a function of various controlling factors like operating temperatures and concentrations of gases. It was found that the sensor exhibited various responses towards these gases at different operating temperatures. Furthermore; the MgFe 2 O 4 based sensor exhibited a fast response and a good recovery towards petrol at temperature 250 deg. C. The results of the response towards petrol reveal that (MgFe 2 O 4 ) synthesized by a simple co-precipitation method, would be a suitable material for the fabrication of the petrol sensor.

  4. Reaction of hydrazine hydrate with oxalic acid: synthesis and crystal structure of dihydrazinium oxalate

    OpenAIRE

    Selvakumar, Rajendran; Premkumar, Thathan; Manivannan, Vadivelu; Saravanan, Kaliannan; Govindarajan, Subbiah

    2014-01-01

    The reaction of oxalic acid with hydrazine hydrate (in appropriate mole ratio) forms the dihydrazinium oxalate under specific experimental condition. The title compound is a molecular salt containing two discrete hydrazinium cations and an oxalate anion. The oxalate anion is perfectly planar and there is a crystallographic centre of symmetry in the middle of the C-C bond. The C-O bond distances are almost equal indicating the presence of resonance in the oxalate ion. The crystal packing is st...

  5. Separation of Am-Cm from Al(NO3)3 waste solutions by in-canyon-tank precipitation as oxalates

    International Nuclear Information System (INIS)

    Gray, L.W.; Burney, G.A.; Wilson, T.W.; McKibben, J.M.; Bibler, N.E.; Holtzscheiter, E.W.; Campbell, T.G.

    1982-04-01

    A process for recovery of Am-Cm residues from high-activity waste concentrates has been developed specifically for application in Savannah River Plant (SRP) canyon tanks. The Am-Cm residues were collected from a campaign to produce plutonium containing high isotopic concentrations of 242 Pu. The separation of Am-Cm from the high-activity waste stream, containing about 2M Al(NO 3 ) 3 , is necessary to produce an acceptable feed solution for a later pressurized cation exchange chromatography separation and purification step. The new process includes formic acid denitration, adjustment of contaminating cations by evaporation and water dilution, and oxalate precipitation of the actinides and lanthanides. After washing, the precipitate was dissolved in 8M nitric acid and the oxalate was destroyed by nitric acid oxidation that was catalyzed by manganous ions. This new process generates about one-fourth the waste of the californium solvent extraction process, which it replaced. The new process also produces a cleaner feed solution for the pressurized cation exchange chromatography separation and purification step

  6. Effects of solution concentration and capping agents on the properties of potassium titanyl phosphate noparticles synthesized using a co-precipitation method

    Science.gov (United States)

    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.

  7. Structural characterization of FeVO{sub 4} synthesized by co-precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Bera, Ganesh; Sinha, Sourav; Rambabu, P.; Das, P.; Gupta, A. K.; Turpu, G. R., E-mail: dr.tgreddy@gmail.com [Department of Pure and Applied Physics, Guru Ghasidas Vishwavidyalaya, Koni, Bilaspur 495 009 (India)

    2016-05-06

    A Low temperature method for synthesizing triclinic FeVO{sub 4} nanoparticles is manifested through co-precipitation method. Three precursor materials taken for the synthesis are Iron Nitrate, Ammonium Metavanadate and NaOH along with DI water. The attained precipitate was dried at 100°C for overnight and calcined at different temperatures ranging from 400°C - 650°C. The achieved powdered materials are studied through X-ray diffraction and found to be in pure single phase of P-1 space group symmetry. The crystallite size measured through Scherrer’s method is in found to be in the range of 40-60 nm. Raman spectroscopic studies were carried out at room temperature. Raman spectra is in agreement with the reported structural data of FeVO{sub 4}.

  8. Estimation of the oxalate content of foods and daily oxalate intake

    Science.gov (United States)

    Holmes, R. P.; Kennedy, M.

    2000-01-01

    BACKGROUND: The amount of oxalate ingested may be an important risk factor in the development of idiopathic calcium oxalate nephrolithiasis. Reliable food tables listing the oxalate content of foods are currently not available. The aim of this research was to develop an accurate and reliable method to measure the food content of oxalate. METHODS: Capillary electrophoresis (CE) and ion chromatography (IC) were compared as direct techniques for the estimation of the oxalate content of foods. Foods were thoroughly homogenized in acid, heat extracted, and clarified by centrifugation and filtration before dilution in water for analysis. Five individuals consuming self-selected diets maintained food records for three days to determine their mean daily oxalate intakes. RESULTS: Both techniques were capable of adequately measuring the oxalate in foods with a significant oxalate content. With foods of very low oxalate content (choice over IC for estimating the oxalate content of foods with a medium (>10 mg/100 g) to high oxalate content due to a faster analysis time and lower running costs, whereas IC may be better suited for the analysis of foods with a low oxalate content. Accurate estimates of the oxalate content of foods should permit the role of dietary oxalate in urinary oxalate excretion and stone formation to be clarified. Other factors, apart from the amount of oxalate ingested, appear to exert a major influence over the amount of oxalate excreted in the urine.

  9. Synthesis of highly sinterable YAG nanopowders by a modified co-precipitation method

    International Nuclear Information System (INIS)

    Chen, Zhi-Hui; Yang, Yun; Hu, Zhang-Gui; Li, Jiang-Tao; He, Shu-Li

    2007-01-01

    A hydrate precursor of yttrium aluminum garnet (YAG) was synthesized by a modified co-precipitation method, in which n-butanol was employed as a low-cost recyclable dehydration solvent. A mixed solution of ethanol and ammonia were used as precipitant. Pure YAG phase appeared after the as-prepared precursors being calcined at 850 o C for 2 h. The nanocrystalline YAG particles calcined at 1100 o C were well dispersed with average diameter of about 40 nm, which can be densified to transparency under vacuum sintering at 1700 o C for 5 h with TEOS as sintering additive

  10. Fungi, bacteria and soil pH: the oxalate-carbonate pathway as a model for metabolic interaction.

    Science.gov (United States)

    Martin, Gaëtan; Guggiari, Matteo; Bravo, Daniel; Zopfi, Jakob; Cailleau, Guillaume; Aragno, Michel; Job, Daniel; Verrecchia, Eric; Junier, Pilar

    2012-11-01

    The oxalate-carbonate pathway involves the oxidation of calcium oxalate to low-magnesium calcite and represents a potential long-term terrestrial sink for atmospheric CO(2). In this pathway, bacterial oxalate degradation is associated with a strong local alkalinization and subsequent carbonate precipitation. In order to test whether this process occurs in soil, the role of bacteria, fungi and calcium oxalate amendments was studied using microcosms. In a model system with sterile soil amended with laboratory cultures of oxalotrophic bacteria and fungi, the addition of calcium oxalate induced a distinct pH shift and led to the final precipitation of calcite. However, the simultaneous presence of bacteria and fungi was essential to drive this pH shift. Growth of both oxalotrophic bacteria and fungi was confirmed by qPCR on the frc (oxalotrophic bacteria) and 16S rRNA genes, and the quantification of ergosterol (active fungal biomass) respectively. The experiment was replicated in microcosms with non-sterilized soil. In this case, the bacterial and fungal contribution to oxalate degradation was evaluated by treatments with specific biocides (cycloheximide and bronopol). Results showed that the autochthonous microflora oxidized calcium oxalate and induced a significant soil alkalinization. Moreover, data confirmed the results from the model soil showing that bacteria are essentially responsible for the pH shift, but require the presence of fungi for their oxalotrophic activity. The combined results highlight that the interaction between bacteria and fungi is essential to drive metabolic processes in complex environments such as soil. © 2012 Society for Applied Microbiology and Blackwell Publishing Ltd.

  11. Surface analysis of transition metal oxalates: Damage aspects

    Energy Technology Data Exchange (ETDEWEB)

    Chenakin, S.P., E-mail: chenakin@imp.kiev.ua [Université Libre de Bruxelles (ULB), Chimie-Physique des Matériaux, B-1050 Bruxelles (Belgium); Institute of Metal Physics, Nat. Acad. Sci. of Ukraine, Akad. Vernadsky Blvd. 36, 03680 Kiev (Ukraine); Szukiewicz, R. [Université Libre de Bruxelles (ULB), Chimie-Physique des Matériaux, B-1050 Bruxelles (Belgium); Barbosa, R.; Kruse, N. [Université Libre de Bruxelles (ULB), Chimie-Physique des Matériaux, B-1050 Bruxelles (Belgium); Voiland School of Chemical Engineering and Bioengineering, Washington State University, 155 Wegner Hall, Pullman, WA 99164-6515 (United States)

    2016-05-15

    Highlights: • Gas evolution from the Mn, Co, Ni and Cu oxalate hydrates in vacuum, during exposure to X-rays and after termination of X-ray irradiation is studied. • A comparative study of the damage caused by X-rays in NiC{sub 2}O{sub 4} and CuC{sub 2}O{sub 4} is carried out. • Effect of Ar{sup +} bombardment on the structure and composition of CoC{sub 2}O{sub 4} is studied. - Abstract: The behavior of transition metal oxalates in vacuum, under X-ray irradiation and low-energy Ar{sup +} ion bombardment was studied. A comparative mass-spectrometric analysis was carried out of gas evolution from the surface of Mn, Co, Ni and Cu oxalate hydrates in vacuum, during exposure to X-rays and after termination of X-ray irradiation. The rates of H{sub 2}O and CO{sub 2} liberation from the oxalates were found to be in an inverse correlation with the temperatures of dehydration and decomposition, respectively. X-ray photoelectron spectroscopy (XPS) was employed to study the X-ray induced damage in NiC{sub 2}O{sub 4} and CuC{sub 2}O{sub 4} by measuring the various XP spectral characteristics and surface composition of the oxalates as a function of time of exposure to X-rays. It was shown that Cu oxalate underwent a significantly faster degradation than Ni oxalate and demonstrated a high degree of X-ray induced reduction from the Cu{sup 2+} to the Cu{sup 1+} chemical state. 500 eV Ar{sup +} sputter cleaning of CoC{sub 2}O{sub 4} for 10 min was found to cause a strong transformation of the oxalate structure which manifested itself in an appreciable alteration of the XP core-level and valence band spectra. The analysis of changes in stoichiometry and comparison of XP spectra of bombarded oxalate with respective spectra of a reference carbonate CoCO{sub 3} implied that the bombardment-induced decomposition of CoC{sub 2}O{sub 4} gave rise to the formation of CoO-like and disordered CoCO{sub 3}-like phases.

  12. Synthesis and structural characterization of actinide oxalate compounds

    International Nuclear Information System (INIS)

    Tamain, C.

    2011-01-01

    Oxalic acid is a well-known reagent to recover actinides thanks to the very low solubility of An(IV) and An(III) oxalate compounds in acidic solution. Therefore, considering mixed-oxide fuel or considering minor actinides incorporation in ceramic fuel materials for transmutation, oxalic co-conversion is convenient to synthesize mixed oxalate compounds, precursors of oxide solid solutions. As the existing oxalate single crystal syntheses are not adaptable to the actinide-oxalate chemistry or to their manipulation constrains in gloves box, several original crystal growth methods were developed. They were first validate and optimized on lanthanides and uranium before the application to transuranium elements. The advanced investigations allow to better understand the syntheses and to define optimized chemical conditions to promote crystal growth. These new crystal growth methods were then applied to a large number of mixed An1(IV)-An2(III) or An1(IV)-An2(IV) systems and lead to the formation of the first original mixed An1(IV)-An2(III) and An1(IV)-An2(IV) oxalate single crystals. Finally thanks to the first thorough structural characterizations of these compounds, single crystal X-ray diffraction, EXAFS or micro-RAMAN, the particularly weak oxalate-actinide compounds structural database is enriched, which is essential for future studied nuclear fuel cycles. (author) [fr

  13. Oxalic acid has an additional, detoxifying function in Sclerotinia sclerotiorum pathogenesis.

    Directory of Open Access Journals (Sweden)

    Annerose Heller

    Full Text Available The mechanism of the diseases caused by the necrotroph plant pathogen Sclerotinia sclerotiorum is not well understood. To investigate the role of oxalic acid during infection high resolution, light-, scanning-, transmission electron microscopy and various histochemical staining methods were used. Our inoculation method allowed us to follow degradation of host plant tissue around single hyphae and to observe the reaction of host cells in direct contact with single invading hyphae. After penetration the outer epidermal cell wall matrix appeared degraded around subcuticular hyphae (12-24 hpi. Calcium oxalate crystals were detected in advanced (36-48 hpi and late (72 hpi infection stages, but not in early stages. In early infection stages, surprisingly, no toxic effect of oxalic acid eventually secreted by S. sclerotiorum was observed. As oxalic acid is a common metabolite in plants, we propose that attacked host cells are able to metabolize oxalic acid in the early infection stage and translocate it to their vacuoles where it is stored as calcium oxalate. The effects, observed on healthy tissue upon external application of oxalic acid to non-infected, living tissue and cell wall degradation of dead host cells starting at the inner side of the walls support this idea. The results indicate that oxalic acid concentrations in the early stage of infection stay below the toxic level. In plant and fungi oxalic acid/calcium oxalate plays an important role in calcium regulation. Oxalic acid likely could quench calcium ions released during cell wall breakdown to protect growing hyphae from toxic calcium concentrations in the infection area. As calcium antimonate-precipitates were found in vesicles of young hyphae, we propose that calcium is translocated to the older parts of hyphae and detoxified by building non-toxic, stable oxalate crystals. We propose an infection model where oxalic acid plays a detoxifying role in late infection stages.

  14. Studies on gadolinium precipitation in moderator system of nuclear reactor

    International Nuclear Information System (INIS)

    Joshi, Akhilesh C.; Rajesh, Puspalata; Rufus, A.L.; Velmurugan, S.

    2015-01-01

    Gadolinium is used in the moderator system of many Pressurised Heavy Water Reactors (PHWRs) for start-up, shut-down and reactivity control during operation. It is very much essential to maintain gadolinium concentration in the system as desired. It has been reported that gadolinium gets precipitated in as oxalate in carbonated water under the influence of γ-radiation. Hence, studies were carried out to investigate the effect of dose, presence of other metal ions and metal surfaces on the precipitation of gadolinium. The results showed that the amount of carboxylic acids viz., formic acid and oxalic acid, formed due to radiolysis is dependent on the dose and that the curve passes though a maxima. Gadolinium is added in higher concentration in Advanced Heavy Water Reactor. So, experiments with high concentration of gadolinium were also carried out. Ultra pure water saturated with high purity CO 2 containing gadolinium and desired ion/surface was irradiated with γ-radiation from 60 Co source at 25°C to doses ranging from 2.5-16.6 Mrad. At lower doses, formation of carboxylic acids takes place but as the dose increases, decomposition of these acids starts and hence the concentration Vs dose passes through a maximum. It was found that precipitation of gadolinium as oxalate occurred at lower doses. At higher doses, it was seen that pH of the solution decreases and hence solubility of gadolinium oxalate increases. It was also observed that the amount of gadolinium precipitated varied linearly with the initial concentration of gadolinium varying from 2 ppm to 20 ppm. While for gadolinium concentration from 20 ppm to 400 ppm, gadolinium in particulate form was observed. The amount of carboxylic acids formed depends on the nature of cations present in solution. It was found that the amount of oxalic acid formed in the case of gadolinium was more than that formed in the case of sodium. Presence of metal oxides such as ZrO 2 formed over zircoloy surfaces was found to

  15. Acute oxalate nephropathy caused by ethylene glycol poisoning

    Directory of Open Access Journals (Sweden)

    Jung Woong Seo

    2012-12-01

    Full Text Available Ethylene glycol (EG is a sweet-tasting, odorless organic solvent found in many agents, such as anti-freeze. EG is composed of four organic acids: glycoaldehyde, glycolic acid, glyoxylic acid and oxalic acid in vivo. These metabolites are cellular toxins that can cause cardio-pulmonary failure, life-threatening metabolic acidosis, central nervous system depression, and kidney injury. Oxalic acid is the end product of EG, which can precipitate to crystals of calcium oxalate monohydrate in the tubular lumen and has been linked to acute kidney injury. We report a case of EG-induced oxalate nephropathy, with the diagnosis confirmed by kidney biopsy, which showed acute tubular injury of the kidneys with extensive intracellular and intraluminal calcium oxalate monohydrate crystal depositions.

  16. Studies in the solubility of Pu(III) oxalate

    Energy Technology Data Exchange (ETDEWEB)

    Hasilkar, S P; Khedekar, N B; Chander, K; Jadhav, V; Jain, H C [Bhabha Atomic Research Centre, Bombay (India). Fuel Reprocessing Div.

    1994-11-01

    Studies have been carried out on the solubility of Pu(III) oxalate by precipitation of Pu(III) oxalate from varying concentrations of HNO[sub 3]/HCl (0.5-2.0M) solutions and also by equilibrating freshly prepared Pu(III) oxalate with solutions containing varying concentrations of HNO[sub 3]/HCl, oxalic acid and ascorbic acid. Pu(III) solutions in HNO[sub 3] and HCl media were prepared by reduction of Pu(IV) with ascorbic acid. 0.01-0.10M ascorbic acid concentration in the aqueous solution was maintained as holding reductant. The solubility of Pu(III) oxalate was found to be a minimum in 0.5M-1M HNO[sub 3]/HCl solutions containing 0.05M ascorbic acid and 0.2M excess oxalic acid in the supernatant. (author) 6 refs.; 6 tabs.

  17. Removal of plutonium from nitric acid-oxalic acid solutions using anion exchange method

    International Nuclear Information System (INIS)

    Kasar, U.M.; Pawar, S.M.; Joshi, A.R.

    1999-01-01

    An anion exchange method using Amberlyst A-26 (MP) resin was developed for removal of Pu from nitric acid-oxalic acid solutions without destroying oxalate. The method consists of sorption of Pu(IV) on Amberlyst A-26, a macroporous anion exchange resin, from nitric acid-oxalic acid medium in the presence of Al(NO 3 ) 3 . Pu(IV) breakthrough capacity of Amberlyst A-26 using synthetic feed solution was determined. (author)

  18. Electrolytic destruction of oxalate ions in plutonium oxalate supernatant

    International Nuclear Information System (INIS)

    Michael, K.M.; Talnikar, S.G.; Jambunathan, U.; Kapoor, S.C.; Ramanujam, A.; Venkataraman, N.

    1996-01-01

    A simple and efficient electrolytic method is described for the destruction of the oxalate ions present in plutonium oxalate supernatant. Using platinum electrode and very little KMnO 4 , in situ generation of Mn 3+ ions is achieved which in turn destroys the oxalate. The use of lower current density helps in achieving maximum current efficiency. The end point is easily detectable by the pink colour of permanganate. By reversing the current, this slight excess of permanganate can be destroyed, thus avoiding the use of hydrogen peroxide. By this simple electrolytic method, the corrosive oxalate ion is completely destroyed and the salt content of the waste solution is considerably reduced. (author). 4 refs., 1 fig., 6 tabs

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

    Science.gov (United States)

    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.

  20. Microbial growth on oxalate by a route not involving glyoxylate carboligase

    Science.gov (United States)

    Blackmore, Maureen A.; Quayle, J. R.

    1970-01-01

    1. The metabolism of oxalate by the pink-pigmented organisms, Pseudomonas AM1, Pseudomonas AM2, Protaminobacter ruber and Pseudomonas extorquens has been compared with that of the non-pigmented Pseudomonas oxalaticus. 2. During growth on oxalate, all the organisms contain oxalyl-CoA decarboxylase, formate dehydrogenase and oxalyl-CoA reductase. This is consistent with oxidation of oxalate to carbon dioxide taking place via oxalyl-CoA, formyl-CoA and formate as intermediates, and also reduction of oxalate to glyoxylate taking place via oxalyl-CoA. 3. The pink-pigmented organisms, when grown on oxalate, contain l-serine–glyoxylate aminotransferase and hydroxypyruvate reductase but do not contain glyoxylate carboligase. The converse of this obtains in oxalate-grown Ps. oxalaticus. This indicates that, in contrast with Ps. oxalaticus, synthesis of C3 compounds from oxalate by the pink-pigmented organisms occurs by a variant of the `serine pathway' used by Pseudomonas AM1 during growth on C1 compounds. 4. Evidence in favour of this scheme is provided by the finding that a mutant of Pseudomonas AM1 that lacks hydroxypyruvate reductase is not able to grow on oxalate. PMID:5472155

  1. Variation in oxalate and oxalate decarboxylase production by six species of brown and white rot fungi

    DEFF Research Database (Denmark)

    Hastrup, Anne Christine Steenkjær; Oliver, Jason; Howell, Caitlin

      Oxalic acid (C2O4H2), the strongest of the organic acids is produced by both brown and white rot decay fungi and has been connected to various aspects of brown- and white rot decay including the Fenton reaction (Green and Highley, 1997; Munir et al.,2001). Oxalic acid is secreted into the wood...... cell lumen where it quickly dissociates into hydrogen ions and oxalate, resulting in a pH decrease of the environment, and oxalate-cation complexes. Generally, brown rot fungi accumulate larger quantities of oxalic acid in the wood than white rot fungi. The amount of oxalic acid has been shown to vary...... of formic acid and CO2 (Makela et al., 2002). So far only a few species of brown rot fungi have been shown to accumulate this enzyme (Micales, 1995, Howell and Jellison, 2006).   The purpose of this study was to investigate the variation in the levels of soluble oxalate and total oxalate, in correlation...

  2. Fe-based soft magnetic composites coated with NiZn ferrite prepared by a co-precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Peng, Yuandong; Yi, Yi; Li, Liya; Ai, Hengyu; Wang, Xiaoxu [State Key Laboratory of Powder Metallurgy, Central South University, Changsha 410083 (China); Chen, Lulu [Jiangsu Eagle-globe Group Co., Ltd., Nantong 226600 (China)

    2017-04-15

    Fe powder was coated with NiZn ferrite by a co-precipitation method using chlorate as the raw material. Soft magnetic composites were manufactured via compaction and heat treatment of the coated powder. The coated powder and heat treated powder were analysed using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD) and Raman spectroscopy. Their magnetic properties were determined using a Quantum Design-Vibrating Sample Magnetometer (QD-VSM). The composites were analysed with SEM and EDS. The permeability and magnetic loss of the composites were measured with a B-H curve analyzer. The results show that, using the co-precipitation method, the raw precipitate was successfully prepared and coated the pure Fe powder and turned into spinel NiZn ferrite treated at 600 ℃ for 1 h. After heat treatment at 500 ℃ under air, the insulation coating layer of soft magnetic composite (SMC) was not destroyed and containing Fe, Ni, Zn and oxygen. The permeabilities of the SMC are stable at edge of the 2–200 kHz frequency range and the total loss was lower. - Graphical abstract: Scanning electron microscopy (SEM) images of Fe/(NiZn)Fe{sub 2}O{sub 4} composite powder heated at 600 ℃ for 1 h. - Highlights: • Fe particles were coated with (NiZn)Fe{sub 2}O{sub 4} via a co-precipitation and calcined method. • Coating layers were uniform and dense. • The permeabilities of the SMC are stable at edge of the 2–200 kHz frequency range.

  3. Inhibition of calcium phosphate precipitation under environmentally-relevant conditions

    International Nuclear Information System (INIS)

    Cao Xinde; Harris, Willie G.; Josan, Manohardeep S.; Nair, Vimala D.

    2007-01-01

    Precipitation of Ca phosphates plays an important role in controlling P activity and availability in environmental systems. The purpose of this study was to determine inhibitory effects on Ca phosphate precipitation by Mg 2+ , SO 4 2- , CO 3 2- , humic acid, oxalic acid, biogenic Si, and Si-rich soil clay commonly found in soils, sediments, and waste streams. Precipitation rates were determined by measuring decrease of P concentration in solutions during the first 60 min; and precipitated solid phases identified using X-ray diffraction and electron microscopy. Poorly-crystalline hydroxyapatite (HAP: Ca 5 (PO 4 ) 3 OH) formed in control solutions over the experiment period of 24 h, following a second-order dependence on P concentration. Humic acid and Mg 2+ significantly inhibited formation of HAP, allowing formation of a more soluble amorphous Ca phosphate phase (ACP), and thus reducing the precipitation rate constants by 94-96%. Inhibition caused by Mg 2+ results from its incorporation into Ca phosphate precipitates, preventing formation of a well-crystalline phase. Humic acid likely suppressed Ca phosphate precipitation by adsorbing onto the newly-formed nuclei. Presence of oxalic acid resulted in almost complete inhibition of HAP precipitation due to preemptive Ca-oxalate formation. Carbonate substituted for phosphate, decreasing the crystallinity of HAP and thus reducing precipitation rate constant by 44%. Sulfate and Si-rich solids had less impact on formation of HAP; while they reduced precipitation in the early stage, they did not differ from the control after 24 h. Results indicate that components (e.g., Mg 2+ , humic acid) producing relatively soluble ACP are more likely to reduce P stability and precipitation rate of Ca phosphate in soils and sediments than are components (e.g., SO 4 2- , Si) that have less effect on the crystallinity

  4. Calcium extraction from brine water and seawater using oxalic acid

    Science.gov (United States)

    Natasha, Nadia Chrisayu; Lalasari, Latifa Hanum

    2017-01-01

    Calcium can be extracted not only from rocks but also from natural liquor such as seawater and brine water. In order to extract the calcium from seawater and brine water, oxalic acid was used in this research. Effect of variations of the volume of the oxalic acid at a constant concentration in seawater and brine water to produce calcium was investigated. The concentration of oxalic acid was 100 g/l and the variations of its volume were 2 ml, 4 ml, 6 ml, 8 ml, 10 ml, 20 ml, 30 ml, 40 ml, and 50 ml. The used seawater and brine water were firstly evaporated from 100 ml into 50 ml and then the oxalic acid was added into them with mixing to produce the calcium precipitates. The precipitates were analyzed by X-ray diffraction (XRD) and scanning electron microscope (SEM) and the filtrates were analyzed by inductively coupled plasma-optical emission spectrometry (ICP-OES). The SEM analysis showed that the precipitates from brine water were consisted of only calcium compound while from seawater sodium one was also found along with calcium compound. The XRD analysis showed that the calcium was present in the form of calcium oxalate for both seawater and brine water. The ICP-OES analysis of the filtrate from seawater precipitation showed that the its calcium content was decreased from 826.20 ppm to 0.04 ppm while from brine water, it decreased from 170.06 ppm to 1.96 ppm. These results showed that both seawater and brine water have the potential to be a raw material for calcium production.

  5. Novel approach to recover cobalt and lithium from spent lithium-ion battery using oxalic acid

    Energy Technology Data Exchange (ETDEWEB)

    Zeng, Xianlai; Li, Jinhui, E-mail: jinhui@tsinghua.edu.cn; Shen, Bingyu

    2015-09-15

    Highlights: • Short-cut recovery of cobalt and lithium was directly obtained using oxalic acid. • Short-cut recovery process was optimized for a high recovery rate. • Leaching process was controlled by chemical reaction. • Leaching order of the sampling LiCoO{sub 2} using oxalic acid was first proposed. - Abstract: With the booming of consumer electronics (CE) and electric vehicle (EV), a large number of spent lithium-ion battery (LIBs) have been generated worldwide. Resource depletion and environmental concern driven from the sustainable industry of CE and EV have motivated spent LIBs should be recovered urgently. However, the conventional process combined with leaching, precipitating, and filtering was quite complicated to recover cobalt and lithium from spent LIBs. In this work, we developed a novel recovery process, only combined with oxalic acid leaching and filtering. When the optimal parameters for leaching process is controlled at 150 min retention time, 95 °C heating temperature, 15 g L{sup −1} solid–liquid ratio, and 400 rpm rotation rate, the recovery rate of lithium and cobalt from spent LIBs can reach about 98% and 97%, respectively. Additionally, we also tentatively discovered the leaching mechanism of lithium cobalt oxide (LiCoO{sub 2}) using oxalic acid, and the leaching order of the sampling LiCoO{sub 2} of spent LIBs. All the obtained results can contribute to a short-cut and high-efficiency process of spent LIBs recycling toward a sound closed-loop cycle.

  6. Solubility of Plutonium (IV) Oxalate During Americium/Curium Pretreatment

    International Nuclear Information System (INIS)

    Rudisill, T.S.

    1999-01-01

    Approximately 15,000 L of solution containing isotopes of americium and curium (Am/Cm) will undergo stabilization by vitrification at the Savannah River Site (SRS). Prior to vitrification, an in-tank pretreatment will be used to remove metal impurities from the solution using an oxalate precipitation process. Material balance calculations for this process, based on solubility data in pure nitric acid, predict approximately 80 percent of the plutonium in the solution will be lost to waste. Due to the uncertainty associated with the plutonium losses during processing, solubility experiments were performed to measure the recovery of plutonium during pretreatment and a subsequent precipitation process to prepare a slurry feed for a batch melter. A good estimate of the plutonium content of the glass is required for planning the shipment of the vitrified Am/Cm product to Oak Ridge National Laboratory (ORNL).The plutonium solubility in the oxalate precipitation supernate during pretreatment was 10 mg/mL at 35 degrees C. In two subsequent washes with a 0.25M oxalic acid/0.5M nitric acid solution, the solubility dropped to less than 5 mg/mL. During the precipitation and washing steps, lanthanide fission products in the solution were mostly insoluble. Uranium, and alkali, alkaline earth, and transition metal impurities were soluble as expected. An elemental material balance for plutonium showed that greater than 94 percent of the plutonium was recovered in the dissolved precipitate. The recovery of the lanthanide elements was generally 94 percent or higher except for the more soluble lanthanum. The recovery of soluble metal impurities from the precipitate slurry ranged from 15 to 22 percent. Theoretically, 16 percent of the soluble oxalates should have been present in the dissolved slurry based on the dilution effects and volumes of supernate and wash solutions removed. A trace level material balance showed greater than 97 percent recovery of americium-241 (from the beta dec

  7. On preparation of nanocrystalline chromites by co-precipitation and autocombustion methods

    Energy Technology Data Exchange (ETDEWEB)

    Matulkova, Irena [Department of Inorganic Chemistry, Faculty of Science, Charles University in Prague, Hlavova 8, 128 43 Prague 2 (Czech Republic); Department of Radiation and Chemical Physics, Institute of Physics of the ASCR, v.v.i., Na Slovance 2, 182 21 Prague 8 (Czech Republic); Holec, Petr [Department of Inorganic Chemistry, Faculty of Science, Charles University in Prague, Hlavova 8, 128 43 Prague 2 (Czech Republic); Department of Materials Chemistry, Institute of Inorganic Chemistry of the ASCR, v.v i., Husinec-Rez 1001, 250 68 Rez (Czech Republic); Pacakova, Barbara; Kubickova, Simona; Mantlikova, Alice [Department of Magnetic Nanosystems, Institute of Physics of the ASCR, v.v.i., Na Slovance 2, 182 21 Prague 8 (Czech Republic); Plocek, Jiri [Department of Materials Chemistry, Institute of Inorganic Chemistry of the ASCR, v.v i., Husinec-Rez 1001, 250 68 Rez (Czech Republic); Nemec, Ivan; Niznansky, Daniel [Department of Inorganic Chemistry, Faculty of Science, Charles University in Prague, Hlavova 8, 128 43 Prague 2 (Czech Republic); Vejpravova, Jana, E-mail: vejpravo@fzu.cz [Department of Magnetic Nanosystems, Institute of Physics of the ASCR, v.v.i., Na Slovance 2, 182 21 Prague 8 (Czech Republic)

    2015-05-15

    Highlights: • ACr{sub 2}O{sub 4} nanopowders, A = Cu, Fe, Ni, Mn and Mg were obtained in high yield. • Co-precipitation and autocombustion routes were optimized for single-phase product. • The nanopowders were examined by X-ray diffraction and vibrational spectroscopy. • Formation of cubic or tetragonal phase in Jahn–Teller NiCr{sub 2}O{sub 4} can be controlled. - Abstract: We present a comprehensive study on optimization of wet preparation routes yielding well-crystalline spinel chromite, ACr{sub 2}O{sub 4} nanoparticles (A = Cu, Fe, Ni, Mn and Mg). The auto-combustion and co-precipitation methods in the presence of nitrate or chloride ions and under different atmospheres, followed by annealing of final products at different temperatures were tested. All samples were characterized by powder X-ray diffraction (PXRD) and vibrational spectroscopy in order to evaluate their phase composition, particle size and micro-strain. Selected samples were subjected to investigation by transmission electron microscopy (TEM). The degree of the particle crystallinity was estimated by relating the apparent crystallite size obtained from the PXRD analysis to the physical grain size observed by the TEM. Optimal conditions leading to single-phase and highly-crystalline chromite nanoparticles are proposed.

  8. Wet milling versus co-precipitation in magnetite ferrofluid preparation

    Directory of Open Access Journals (Sweden)

    Almásy László

    2015-01-01

    Full Text Available Various uses of ferrofluids for technical applications continuously raise the interest in improvement and optimization of preparation methods. This paper deals with preparation of finely granulated magnetite particles coated with oleic acid in hydrocarbon suspensions following either chemical co-precipitation from iron salt precursors or wet milling of micron size magnetite powder with the goal to compare the benefits and disadvantages of each method. Microstructural measurements showed that both methods gave similar magnetite particle size of 10-15 nm. Higher saturation magnetization was achieved for the wet-milled magnetite suspension compared to relatively rapid co-precipitation synthesis. Different efficacies of ferrophase incorporation into kerosene could be related to the different mechanisms of oleic acid bonding to nanoparticle surface. The comparative data show that wet milling represents a practicable alternative to the traditional co-precipitation since despite of longer processing time, chemicals impact on environment can be avoided as well as the remnant water in the final product.

  9. Synthesis of InGaZnO4 nanoparticles using low temperature multistep co-precipitation method

    International Nuclear Information System (INIS)

    Wu, Ming-Chung; Hsiao, Kai-Chi; Lu, Hsin-Chun

    2015-01-01

    Indium gallium zinc oxide (InGaZnO 4 , IGZO) has attracted explosive growth in investigations over the last decades as an important material in the thin-film transistor. In this study, the various nitrate precursors, including indium nitrate, gallium nitrate, and zinc nitrate, were prepared from the various metals dissolved in nitric acid. Then, we used these nitrate precursors to synthesize the IGZO precursor powder by the multistep co-precipitation method. The synthesis parameters of the co-precipitation method, such as reaction temperature, pH value and reaction time, were controlled precisely to prepare the high quality IGZO precursor powder. Finally, IGZO precursor powder was calcined at 900 °C. Then, the microstructure, the crystalline structure, the particle size distribution and specific surface area of calcined IGZO precursor powder were characterized by electron transmission microscopy, X-ray diffraction technique, dynamic light scattering method and the surface area and porosimetry analyzer, respectively. The relative density of IGZO tablet sintered at 1200 °C for 12 h is as high as 97.30%, and it showed highly InGaZnO 4 crystalline structure and the large grain size. The IGZO nanoparticles developed in our study has the potential for the high quality target materials used in the application of electronic devices. - Graphical abstract: Display Omitted - Highlights: • InGaZnO 4 (IGZO) nanoparticle was synthesized by multistep co-precipitation method. • The synthesis parameters were controlled precisely to prepare high quality powder. • The relative density of highly crystalline IGZO tablet is as high as 97.30%. • IGZO tablet exhibited highly crystalline structure and the large grain size

  10. Effect of Calcination at Synthesis of Mg-Al Hydrotalcite Using co-Precipitation Method

    Directory of Open Access Journals (Sweden)

    Niar Kurnia Julianti

    2017-01-01

    Full Text Available The use of hydrotalcite in catalysis has wide attention in academic research and industrial parties. Based on its utilization, hydrotalcite can be active catalyst or support. This research is focused on the investigation of characteristic like spesific surface area of Mg-Al hydrotalcite which is prepared with different temperature of calcination. Synthesis of Mg-Al hydrotalcites with Mg/Al molar ratio 3:1 were prepared by co-precipitation method. Mg(NO33.6H2O and Al(NO33.9H2O as precursors of Mg-Al hydrotalcite. Na2CO3 was used as precipitant agent and NaOH was used as buffer solution. The solution was mixed and aging for 5 hours at 650oC. The dried precipitate was calcined at 2500oC, 3500oC, 4500oC, 5500oC and 6500oC. The characterization of functional group was determined by Fourier Transform Infra Red (FT-IR. The Identical peaks diffractogram were analyzed by X-Ray Diffraction (XRD. The spesific surface area was determined by adsorption-desorption of nitrogen. The largest surface area that obtained from the calcination temperature of 650oC is 156.252 m2/g.

  11. Thermoluminescence and photoluminescence properties of NaCl:Mn, NaCL:Cu nano-particles produced using co-precipitation and sono-chemistry methods

    Energy Technology Data Exchange (ETDEWEB)

    Mehrabi, M. [Faculty of Physics, University of Kashan, Kashan (Iran, Islamic Republic of); Zahedifar, M. [Faculty of Physics, University of Kashan, Kashan (Iran, Islamic Republic of); Institute of Nanosince and Nanotechnology, University of Kashan, Kashan (Iran, Islamic Republic of); Saeidi-Sogh, Z. [Institute of Nanosince and Nanotechnology, University of Kashan, Kashan (Iran, Islamic Republic of); Ramazani-Moghaddam-Arani, A., E-mail: ramazmo@kashanu.ac.ir [Institute of Nanosince and Nanotechnology, University of Kashan, Kashan (Iran, Islamic Republic of); Sadeghi, E. [Faculty of Physics, University of Kashan, Kashan (Iran, Islamic Republic of); Institute of Nanosince and Nanotechnology, University of Kashan, Kashan (Iran, Islamic Republic of); Harooni, S. [Institute of Nanosince and Nanotechnology, University of Kashan, Kashan (Iran, Islamic Republic of)

    2017-02-21

    The NaCl: Cu and NaCl: Mn nanoparticles (NPs) were produced by co-precipitation and sono-chemistry methods and their thermoluminescence (TL) and photoluminescence (PL) properties were studied. By decreasing the particles size a considerable increase in sensitivity of the samples to high dose gamma radiation was observed. The NPs produced by sono-chemistry method have smaller size, homogeneous structure, more sensitivity to high gamma radiation and less fading than of those produced by co-precipitation method.

  12. PRECIPITATION BEHAVIOR OF Co PHASES IN B2-ORDERED(Ni,Co)Al COMPOUND

    Institute of Scientific and Technical Information of China (English)

    W.H. Tian; A.L. Fan; M. Nemoto

    2002-01-01

    The precipitation behavior of Co phases in B2-ordered (Ni, Co)Al has been investigatedin terms of transmission electron microscopy. Fine precipitation off cc-Co occurs in(Ni, Co)Al by aging at temperature over 973K. The orientation relationship betweenthe fcc-Co precipitates and the B2-(Ni, Co)Al matrix follows the Kurdjumow-Sachs(K-S) orientation relation. But when the aging temperature is under 873K the Coprecipitates have a hcp crystal structure. The orientation relationship between thehcp-Co precipitates and the B2-(Ni, Co)Al matrix follows the Burgers orientation re-lation. (Ni, Co)Al is hardened appreciably by the fine precipitation of both the fcc-Coand hcp-Co phases. The temperature dependence of the yield strength of precipitate-containing B2-ordered (Ni, Co)Al was investigated by compression tests over the rangeof 298-1273K. The fine precipitation of Co phases enhances greatly the low and in-termediate temperature yield strength. When the deformation temperature was over873K, the strength of precipitate-containing (Ni, Co)Al is comparable to ternary dual-phase (Ni, Co)Al+Ni3Al alloy.

  13. Concomitant carboxylate and oxalate formation from the activation of CO{sub 2} by a thorium(III) complex

    Energy Technology Data Exchange (ETDEWEB)

    Formanuik, Alasdair; Ortu, Fabrizio; Mills, David P. [School of Chemistry, The University of Manchester (United Kingdom); Inman, Christopher J. [Department of Chemistry and Biochemistry, School of Life Sciences, University of Sussex, Brighton (United Kingdom); Kerridge, Andrew [Department of Chemistry, Lancaster University (United Kingdom); Castro, Ludovic; Maron, Laurent [LPCNO, CNRA et INSA, Universite Paul Sabatier, Toulouse (France)

    2016-12-12

    Improving our comprehension of diverse CO{sub 2} activation pathways is of vital importance for the widespread future utilization of this abundant greenhouse gas. CO{sub 2} activation by uranium(III) complexes is now relatively well understood, with oxo/carbonate formation predominating as CO{sub 2} is readily reduced to CO, but isolated thorium(III) CO{sub 2} activation is unprecedented. We show that the thorium(III) complex, [Th(Cp''){sub 3}] (1, Cp''={C_5H_3(SiMe_3)_2-1,3}), reacts with CO{sub 2} to give the mixed oxalate-carboxylate thorium(IV) complex [{Th(Cp'')_2[κ"2-O_2C{C_5H_3-3,3'-(SiMe_3)_2}]}{sub 2}(μ-κ{sup 2}:κ{sup 2}-C{sub 2}O{sub 4})] (3). The concomitant formation of oxalate and carboxylate is unique for CO{sub 2} activation, as in previous examples either reduction or insertion is favored to yield a single product. Therefore, thorium(III) CO{sub 2} activation can differ from better understood uranium(III) chemistry. (copyright 2016 The Authors. Published by Wiley-VCH Verlag GmbH and Co. KGaA.)

  14. Characterization of ZnS nanoparticles synthesized by co-precipitation method

    International Nuclear Information System (INIS)

    Iranmanesh Parvaneh; Nourzpoor Mohsen; Saeednia Samira

    2015-01-01

    ZnS nanoparticles are prepared by homogeneous chemical co-precipitation method using EDTA as a stabilizer and capping agent. The structural, morphological, and optical properties of as-synthesized nanoparticles are investigated using x-ray diffraction, scanning electron microscopy, Fourier transform infrared spectroscopy, ultraviolet-visible (UV-Vis) absorption, and photoluminescence spectroscopy. The x-ray diffraction pattern exhibits a zinc-blended crystal structure at room temperature. The average particle size of the nanoparticles from the scanning electron microscopy image is about 50 nm. The ultraviolet absorption spectrum shows the blue shift in the band gap due to the quantum confinement effect. The photoluminescence spectrum of ZnS nanoparticles shows a blue visible spectrum. (paper)

  15. Update on probiotics for the treatment of calcium oxalate stones

    Directory of Open Access Journals (Sweden)

    Di ZHANG

    2016-09-01

    Full Text Available Urolithiasis is one of the common diseases in urinary system, among which calcium oxalate stone is the most common one with a high recurrence rate. An important pathological factor for the formation of calcium oxalate stone is the increased absorption of oxalate from intestine, which leads to a high urine oxalate concentration. Intestinal bacteria known to be able to degrade oxalate includes Oxalobacter formigenes, Enterococcus faecalis, Escherichia coli, Eubacterium lentum, Providencia rettgeri, Lactobacillus and Bifidobacterium species, etc. Among those, Oxalobacter formigenes is the first oxalate-degrading obligate anaerobe found in human, while the rest are just conditioned bacteria with the function to degrade intestinal oxalate. There are three kinds of enzymes in Oxalobacter formigenes involved in the metabolism of oxalate, namely oxalate-formate antiporter (OxlT, formyl-CoA transferase (Frc and oxalyl-CoA decarboxylase (Oxc. Animal experiments have verified that Oxalobacter formigenes could reduce intestinal oxalate absorption by promoting the secretion of oxalate and degradation as well, thus decrease the excretion of urine oxalate. The present review will focus on the research progress of probiotics treatment for the calcium oxalate stones so as to provide reference for further research and development. DOI: 10.11855/j.issn.0577-7402.2016.08.16

  16. Oxalic acid decreases calcium absorption in rats

    International Nuclear Information System (INIS)

    Weaver, C.M.; Martin, B.R.; Ebner, J.S.; Krueger, C.A.

    1987-01-01

    Calcium absorption from salts and foods intrinsically labeled with 45 Ca was determined in the rat model. Calcium bioavailability was nearly 10 times greater for low oxalate kale, CaCO 3 and CaCl 2 than from CaC 2 O 4 (calcium oxalate) and spinach (high in oxalates). Extrinsic and intrinsic labeling techniques gave a similar assessment of calcium bioavailability from kale but not from spinach

  17. Stability-indicating RP-HPLC method for the simultaneous determination of escitalopram oxalate and clonazepam.

    Science.gov (United States)

    Kakde, Rajendra B; Satone, Dinesh D; Gadapayale, Kamalesh K; Kakde, Megha G

    2013-07-01

    The objective of the current study was to develop a validated, specific stability-indicating reversed-phase liquid chromatographic (LC) method for the quantitative determination of escitalopram oxalate and clonazepam and their related substances in bulk drugs and pharmaceutical dosage forms in the presence of degradation products. Forced degradation studies were performed on the pure drugs of escitalopram oxalate and clonazepam, as per the stress conditions prescribed by the International Conference on Harmonization (ICH) using acid, base, oxidation, thermal stress and photolytic degradation to show the stability-indicating power of the method. Significant degradation was observed during acid and alkaline hydrolysis and no degradation was observed in other stress conditions. The chromatographic method was optimized using the samples generated from forced degradation studies. Good resolution between the peaks corresponded to the active pharmaceutical ingredients, escitalopram oxalate and clonazepam, and degradation products from the analyte were achieved on an ODS Hypersil C18 column (250 × 4.6 mm) using a mobile phase consisting of a mixture of acetonitrile-50 mM phosphate buffer + 10 mM triethylamine (70:30, v/v). The detection was conducted at 268 nm. The limit of detection and the limit of quantitation for escitalopram oxalate and clonazepam were established. The stress test solutions were assayed against the qualified working standards of escitalopram oxalate and clonazepam, which indicated that the developed LC method was stability-indicating. Validation of the developed LC method was conducted as per ICH requirements. The developed LC method was found to be suitable to check the quality of bulk samples of escitalopram oxalate and clonazepam.

  18. Development of Hydrotalcite Based Cobalt Catalyst by Hydrothermal and Co-precipitation Method for Fischer-Tropsch Synthesis

    Directory of Open Access Journals (Sweden)

    Muhammad Faizan Shareef

    2017-10-01

    Full Text Available This paper presents the effect of a synthesis method for cobalt catalyst supported on hydrotalcite material for Fischer-Tropsch synthesis. The hydrotalcite supported cobalt (HT-Co catalysts were synthesized by co-precipitation and hydrothermal method. The prepared catalysts were characterized by using various techniques like BET (Brunauer–Emmett–Teller, SEM (Scanning Electron Microscopy, TGA (Thermal Gravimetric Analysis, XRD (X-ray diffraction spectroscopy, and FTIR (Fourier Transform Infrared Spectroscopy. Fixed bed micro reactor was used to test the catalytic activity of prepared catalysts. The catalytic testing results demonstrated the performance of hydrotalcite based cobalt catalyst in Fischer-Tropsch synthesis with high selectivity for liquid products. The effect of synthesis method on the activity and selectivity of catalyst was also discussed. Copyright © 2017 BCREC Group. All rights reserved Received: 3rd November 2016; Revised: 26th February 2017; Accepted: 9th March 2017; Available online: 27th October 2017; Published regularly: December 2017 How to Cite: Sharif, M.S., Arslan, M., Iqbal, N., Ahmad, N., Noor, T. (2017. Development of Hydrotalcite Based Cobalt Catalyst by Hydrothermal and Co-precipitation Method for Fischer-Tropsch Synthesis. Bulletin of Chemical Reaction Engineering & Catalysis, 12(3: 357-363 (doi:10.9767/bcrec.12.3.762.357-363

  19. Study of calcium carbonate and sulfate co-precipitation

    KAUST Repository

    Zarga, Y.

    2013-06-01

    Co-precipitation of mineral based salts in scaling is still not well understood and/or thermodynamically well defined in the water industry. This study focuses on investigating calcium carbonate (CaCO3) and sulfate mixed precipitation in scaling which is commonly observed in industrial water treatment processes including seawater desalination either by thermal-based or membrane-based processes. Co-precipitation kinetics were studied carefully by monitoring several parameters simultaneously measured, including: pH, calcium and alkalinity concentrations as well as quartz microbalance responses. The CaCO3 germination in mixed precipitation was found to be different than that of simple precipitation. Indeed, the co-precipitation of CaCO3 germination time was not anymore related to supersaturation as in a simple homogenous precipitation, but was significantly reduced when the gypsum crystals appeared first. On the other hand, the calcium sulfate crystals appear to reduce the energetic barrier of CaCO3 nucleation and lead to its precipitation by activating heterogeneous germination. However, the presence of CaCO3 crystals does not seem to have any significant effect on gypsum precipitation. IR spectroscopy and the Scanning Electronic Microscopy (SEM) were used to identify the nature of scales structures. Gypsum was found to be the dominant precipitate while calcite and especially vaterite were found at lower proportions. These analyses showed also that gypsum crystals promote calcite crystallization to the detriment of other forms. © 2013 Elsevier Ltd.

  20. Synthesis of InGaZnO{sub 4} nanoparticles using low temperature multistep co-precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Ming-Chung, E-mail: mingchungwu@mail.cgu.edu.tw; Hsiao, Kai-Chi; Lu, Hsin-Chun

    2015-07-15

    Indium gallium zinc oxide (InGaZnO{sub 4}, IGZO) has attracted explosive growth in investigations over the last decades as an important material in the thin-film transistor. In this study, the various nitrate precursors, including indium nitrate, gallium nitrate, and zinc nitrate, were prepared from the various metals dissolved in nitric acid. Then, we used these nitrate precursors to synthesize the IGZO precursor powder by the multistep co-precipitation method. The synthesis parameters of the co-precipitation method, such as reaction temperature, pH value and reaction time, were controlled precisely to prepare the high quality IGZO precursor powder. Finally, IGZO precursor powder was calcined at 900 °C. Then, the microstructure, the crystalline structure, the particle size distribution and specific surface area of calcined IGZO precursor powder were characterized by electron transmission microscopy, X-ray diffraction technique, dynamic light scattering method and the surface area and porosimetry analyzer, respectively. The relative density of IGZO tablet sintered at 1200 °C for 12 h is as high as 97.30%, and it showed highly InGaZnO{sub 4} crystalline structure and the large grain size. The IGZO nanoparticles developed in our study has the potential for the high quality target materials used in the application of electronic devices. - Graphical abstract: Display Omitted - Highlights: • InGaZnO{sub 4} (IGZO) nanoparticle was synthesized by multistep co-precipitation method. • The synthesis parameters were controlled precisely to prepare high quality powder. • The relative density of highly crystalline IGZO tablet is as high as 97.30%. • IGZO tablet exhibited highly crystalline structure and the large grain size.

  1. The effects of copper proximity on oxalate production in Fibroporia radiculosa

    Science.gov (United States)

    Katie M. Jenkins; Carol A. Clausen; Frederick Green III

    2014-01-01

    Copper remains a key component used in wood preservatives available today. However, the observed tolerance of several critical wood rotting organisms continues to be problematic. Tolerance to copper has been linked to the production and accumulation of oxalate, which precipitates copper into insoluble copper-oxalate crystals, thus inactivating copper ions. The purpose...

  2. A new method for the analysis of soluble and insoluble oxalate in pulp and paper matrices

    CSIR Research Space (South Africa)

    Sithole, Bruce

    2013-11-01

    Full Text Available A novel method has been developed for determining soluble and insoluble forms of oxalate in pulp and paper samples by ion chromatography. Methanesulphonic acid is used to dissolve insoluble oxalate, and total oxalate is then determined by ion...

  3. Oxalate Acid-Base Cements as a Means of Carbon Storage

    Science.gov (United States)

    Erdogan, S. T.

    2017-12-01

    Emission of CO2 from industrial processes poses a myriad of environmental problems. One such polluter is the portland cement (PC) industry. PC is the main ingredient in concrete which is the ubiquitous binding material for construction works. Its production is responsible for 5-10 % of all anthropogenic CO2 emissions. Half of this emission arises from the calcination of calcareous raw materials and half from kiln fuel burning and cement clinker grinding. There have long been efforts to reduce the carbon footprint of concrete. Among the many ways, one is to bind CO2 to the phases in the cement-water paste, oxides, hydroxides, and silicates of calcium, during early hydration or while in service. The problem is that obtaining calcium oxide cheaply requires the decarbonation of limestone and the uptake of CO2 is slow and limited mainly to the surface of the concrete due to its low gas permeability. Hence, a faster method to bind more CO2 is needed. Acid-base (AB) cements are fast-setting, high-strength systems that have high durability in many environments in which PC concrete is vulnerable. They are made with a powder base such as MgO and an acid or acid salt, like phosphates. Despite certain advantages over PC cement systems, AB cements are not feasible, due to their high acid content. Also, the phosphoric acid used comes from non-renewable sources of phosphate. A potential way to reduce the drawbacks of using phosphates could be to use organic acids. Oxalic acid or its salts could react with the proper powder base to give concrete that could be used for infrastructure hence that would have very high demand. In addition, methods to produce oxalates from CO2, even atmospheric, are becoming widespread and more economical. The base can also be an industrial byproduct to further lower the environmental impact. This study describes the use of oxalic acid and industrial byproducts to obtain mortars with mechanical properties comparable to those of PC mortars. It is

  4. Cocrystal Screening of Ibuprofen with Oxalic Acid and Citric Acid via Grinding Method

    Science.gov (United States)

    Othman, M. F.; Anuar, N.; Rahman, S. Ad; Taifuddin, N. A. Ahmad

    2018-05-01

    Ibuprofen is a Class II Biological Safety Class (BSC) drugs used for relief of arthritis, as an analgesic and possesses the effect of antiplatelet. The major problem involves in ibuprofen is it has a low solubility and high permeability thus causes an unsatisfactory therapeutic effect to humans. Thus, in this work, alteration of ibuprofen’s physicochemical properties is conducted by means of cocrystallization technique. Co-crystallizations of ibuprofen were prepared with selected coformers using dry grinding and liquid assisted grinding (LAG) techniques in different molar ratios while ethanol and propanol were used as a solvent. The new crystalline forms were identified and characterized by differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD) and fourier transform infrared spectroscopy (FTIR). Analysis for Ibuprofen-Citric acid (IBP-CA) system, co-crystal was successfully formed in 1:2, 1:3, 2:1 and 3:1 molar ratios for neat grinding method although the co-crystal produced is unstable. Meanwhile, for Ibuprofen-Oxalic acid (IBP-OA) system, the co-crystal formation was identified only in 1:1, 1:2 and 1:3 molar ratios for the neat grinding method. LAG method shows that co-crystal formation was unsuccessful in both solvents for IBP-CA, while IBP-OA co-crystal was formed in the molar ratio 1:1, 2:1 and 3:1 in ethanol, and 2:1 and 3:1 in propanol.

  5. Oxalate molecule as the trap for gamma-irradiation energy in the amorphous aluminosilicate Al2(OH)6H4SiO4

    International Nuclear Information System (INIS)

    Nothig-Laslo, V.; Horvath, L.; Bilinski, H.

    1990-01-01

    Paramagnetic species which were the products of gamma irradiation at 77 K and at room temperature were studied by ESR spectroscopy in the amorphous aluminosilicate, Al2(OH)6H4SiO4, prepared in the presence and in the absence of oxalate ion. The aluminosilicate precipitated from the solution containing the oxalate ion in 10(-4) mol dm-3 concentration contained the oxalate only in trace amounts. When gamma-irradiated at 77 K and at room temperature, this compound gave the stable paramagnetic species represented by the single ESR line centered at g = 2.000. We ascribe this spectrum to the CO2- radical formed from the oxalate ion. The same aluminosilicate prepared in the absence of the oxalate either produced no stable paramagnetic product after gamma irradiation at room temperature or resulted in composite ESR spectra, indicating the presence of several paramagnetic species if irradiated at 77 K. Complex ESR spectra were transformed by heating to the stable paramagnetic centers which differed from the one obtained from oxalate ion. We conclude that in Al2(OH)6H4SiO4 oxalate acts as a trap for the gamma-radiation energy

  6. Destruction of oxalate by reaction with hydrogen peroxide. [Hydrazine oxalate

    Energy Technology Data Exchange (ETDEWEB)

    Mailen, J.C.; Tallent, O.K.; Arwood, P.C.

    1981-09-01

    The destruction of oxalate by oxidation to carbon dioxide using hydrogen peroxide was studied as an alternative method for the disposal of oxalate in connection with the possible use of an aqueous hydrazine oxalate solution as a scrubbing agent for solvent cleanup in processes for the recovery of uranium, plutonium, and thorium by solvent extraction. The rate of oxidation of oxalate by hydrogen peroxide in acid solution at the reflux temperature was adequate for process application; reaction half-times at 100/sup 0/C were less than one hour when the hydrogen peroxide concentration was greater than 0.5 M. The reaction was first order with respect to both the oxalate and hydrogen peroxide concentrations and had an activation energy of 58.7 kJ/g-mol. The rate increased with the hydrogen ion concentration as (H/sup +/)/sup 0/ /sup 3/ but was not significantly affected by the presence of 100 ppM of uranium or copper in solution. In the near-neutral hydrazine oxalate solutions, the reaction of either component with hydrogen peroxide was too slow for process application.

  7. The production of rare earth elements group via tributyl phosphate extraction and precipitation stripping using oxalic acid

    Directory of Open Access Journals (Sweden)

    Esmaeil Jorjani

    2016-11-01

    Full Text Available In this study, solvent extraction and precipitation stripping were used to produce rare earth elements (REEs. Tributyl phosphate (TBP was used to extract yttrium, lanthanum, cerium, and neodymium from an aqueous solution produced by nitric acid leaching of apatite concentrate. In the extraction stage, the effects of TBP concentration, pH, contact time, temperature, and phase ratio were investigated. The results show that about 95%, 90%, 87% and 80% of neodymium, cerium, lanthanum, and yttrium, respectively, can be extracted in optimum conditions of extraction. Hot, deionized water was used to scrub the impurities from the loaded organic phase. The results showed that three stages of scrubbing with a phase ratio (Va/Vo of five removed about 80%, 30%, 27%, and 15% of Ca, Mg, Fe, and P, respectively, from loaded TBP, while less than 9% of total REEs was lost. The effects on precipitation stripping of oxalic acid concentration, contact time, and phase ratio were investigated. The results showed that precipitation stripping is a viable alternative to traditional acid stripping in the REEs production process. Mixed REEs oxide with an assay of about 90% can be achieved as a final product.

  8. Synthesis and characterization of magnetite nanoparticles via the chemical co-precipitation method

    International Nuclear Information System (INIS)

    Petcharoen, K.; Sirivat, A.

    2012-01-01

    Highlights: ► Size-controlled magnetite nanoparticles were prepared via the chemical co-precipitation method in the range of 10–40 nm. ► The electrical conductivity of the smallest particle size is 1.3 × 10 −3 S/cm which belongs to the semiconductor material group. ► The surface modification of magnetite nanoparticles can provide the suspension stability over 1 week. - Abstract: Magnetite nanoparticles were synthesized via the chemical co-precipitation method using ammonium hydroxide as the precipitating agent. The size of the magnetite nanoparticles was carefully controlled by varying the reaction temperature and through the surface modification. Herein, the hexanoic acid and oleic acid were introduced as the coating agents during the initial crystallization phase of the magnetite. Their structure and morphology were characterized by the Fourier transform infrared spectroscopy (FTIR), the X-ray diffraction (XRD) and the field-emission scanning electron microscopy (FE-SEM). Moreover, the electrical and magnetic properties were studied by using a conductivity meter and a vibrating sample magnetometer (VSM), respectively. Both of the bare magnetite and the coated magnetite were of the cubic spinel structure and the spherical-shaped morphology. The reaction temperature and the surface modification critically affected the particle size, the electrical conductivity, and the magnetic properties of these particles. The particle size of the magnetite was increased through the surface modification and reaction temperature. In this study, the particle size of the magnetite nanoparticles was successfully controlled to be in the range of 10–40 nm, suitable for various biomedical applications. The electrical conductivity of the smallest particle size was 1.3 × 10 −3 S/cm, within the semi-conductive materials range, which was higher than that of the largest particle by about 5 times. All of the magnetite nanoparticles showed the superparamagnetic behavior with

  9. Heavy metal immobilization via microbially induced carbonate precipitation and co-precipitation

    Science.gov (United States)

    Lauchnor, E. G.; Stoick, E.

    2017-12-01

    Microbially induced CaCO3 precipitation (MICP) has been successfully used in applications such as porous media consolidation and sealing of leakage pathways in the subsurface, and it has the potential to be used for remediation of metal and radionuclide contaminants in surface and groundwater. In this work, MICP is investigated for removal of dissolved heavy metals from contaminated mine discharge water via co-precipitation in CaCO3 or formation of other metal carbonates. The bacterially catalyzed hydrolysis of urea produces inorganic carbon and ammonium and increases pH and the saturation index of carbonate minerals to promote precipitation of CaCO3. Other heavy metal cations can be co-precipitated in CaCO3 as impurities or by replacing Ca2+ in the crystal lattice. We performed laboratory batch experiments of MICP in alkaline mine drainage sampled from an abandoned mine site in Montana and containing a mixture of heavy metals at near neutral pH. Both a model bacterium, Sporosarcina pasteurii, and a ureolytic bacterium isolated from sediments on the mine site were used to promote MICP. Removal of dissolved metals from the aqueous phase was determined via inductively coupled plasma mass spectrometry and resulting precipitates were analyzed via electron microscopy and energy dispersive x-ray spectroscopy (EDX). Both S. pasteurii and the native ureolytic isolate demonstrated ureolysis, increased the pH and promoted precipitation of CaCO3 in batch tests. MICP by the native bacterium reduced concentrations of the heavy metals zinc, copper, cadmium, nickel and manganese in the water. S. pasteurii was also able to promote MICP, but with less removal of dissolved metals. Analysis of precipitates revealed calcium carbonate and phosphate minerals were likely present. The native isolate is undergoing identification via 16S DNA sequencing. Ongoing work will evaluate biofilm formation and MICP by the isolate in continuous flow, gravel-filled laboratory columns. This research

  10. A review of plutonium oxalate decomposition reactions and effects of decomposition temperature on the surface area of the plutonium dioxide product

    International Nuclear Information System (INIS)

    Orr, R.M.; Sims, H.E.; Taylor, R.J.

    2015-01-01

    Plutonium (IV) and (III) ions in nitric acid solution readily form insoluble precipitates with oxalic acid. The plutonium oxalates are then easily thermally decomposed to form plutonium dioxide powder. This simple process forms the basis of current industrial conversion or ‘finishing’ processes that are used in commercial scale reprocessing plants. It is also widely used in analytical or laboratory scale operations and for waste residues treatment. However, the mechanisms of the thermal decompositions in both air and inert atmospheres have been the subject of various studies over several decades. The nature of intermediate phases is of fundamental interest whilst understanding the evolution of gases at different temperatures is relevant to process control. The thermal decomposition is also used to control a number of powder properties of the PuO_2 product that are important to either long term storage or mixed oxide fuel manufacturing. These properties are the surface area, residual carbon impurities and adsorbed volatile species whereas the morphology and particle size distribution are functions of the precipitation process. Available data and experience regarding the thermal and radiation-induced decompositions of plutonium oxalate to oxide are reviewed. The mechanisms of the thermal decompositions are considered with a particular focus on the likely redox chemistry involved. Also, whilst it is well known that the surface area is dependent on calcination temperature, there is a wide variation in the published data and so new correlations have been derived. Better understanding of plutonium (III) and (IV) oxalate decompositions will assist the development of more proliferation resistant actinide co-conversion processes that are needed for advanced reprocessing in future closed nuclear fuel cycles. - Highlights: • Critical review of plutonium oxalate decomposition reactions. • New analysis of relationship between SSA and calcination temperature. • New SEM

  11. Influencing the solubility of oxalates for the preparation of ceramic powders from mixed precipitates

    International Nuclear Information System (INIS)

    Krueger, C.; Fischer, S.; Fischer, St.; Chebani, M.Kh.

    1991-01-01

    Based on investigations of the solubility of oxalate with 140 Ba, 64 Cu and 59 Fe, techniques for quantitative oxalate coprecipitation were developed. Addition of organic solvents lowers the solubility and leads to a smaller particle size of products. (orig.) [de

  12. Self-aligned nanocrystalline ZnO hexagons by facile solid-state and co-precipitation route

    International Nuclear Information System (INIS)

    Thorat, J. H.; Kanade, K. G.; Nikam, L. K.; Chaudhari, P. D.; Panmand, R. P.; Kale, B. B.

    2012-01-01

    In this study, we report the synthesis of well-aligned nanocrystalline hexagonal zinc oxide (ZnO) nanoparticles by facile solid-state and co-precipitation method. The co-precipitation reactions were performed using aqueous and ethylene glycol (EG) medium using zinc acetate and adipic acid to obtain zinc adipate and further decomposition at 450 °C to confer nanocrystalline ZnO hexagons. XRD shows the hexagonal wurtzite structure of the ZnO. Thermal study reveals complete formation of ZnO at 430 °C in case of solid-state method, whereas in case of co-precipitation method complete formation was observed at 400 °C. Field emission scanning electron microscope shows spherical morphology for ZnO synthesized by solid-state method. The aqueous-mediated ZnO by co-precipitation method shows rod-like morphology. These rods are formed via self assembling of spherical nanoparticles, however, uniformly dispersed spherical crystallites were seen in EG-mediated ZnO. Transmission electron microscope (TEM) investigations clearly show well aligned and highly crystalline transparent and thin hexagonal ZnO. The particle size was measured using TEM and was observed to be 50–60 nm in case of solid-state method and aqueous-mediated co-precipitation method, while 25–50 nm in case of EG-mediated co-precipitation method. UV absorption spectra showed sharp absorption peaks with a blue shift for EG-mediated ZnO, which demonstrate the mono-dispersed lower particle size. The band gap of the ZnO was observed to be 3.4 eV which is higher than the bulk, implies nanocrystalline nature of the ZnO. The photoluminescence studies clearly indicate the strong violet and weak blue emission in ZnO nanoparticles which is quite unique. The process investigated may be useful to synthesize other oxide semiconductors and transition metal oxides.

  13. Self-aligned nanocrystalline ZnO hexagons by facile solid-state and co-precipitation route

    Energy Technology Data Exchange (ETDEWEB)

    Thorat, J. H. [Mahatma Phule College, Department of Chemistry (India); Kanade, K. G. [Annasaheb Awate College (India); Nikam, L. K. [B.G. College (India); Chaudhari, P. D.; Panmand, R. P.; Kale, B. B., E-mail: kbbb1@yahoo.com [Center for Materials for Electronics Technology (C-MET) (India)

    2012-02-15

    In this study, we report the synthesis of well-aligned nanocrystalline hexagonal zinc oxide (ZnO) nanoparticles by facile solid-state and co-precipitation method. The co-precipitation reactions were performed using aqueous and ethylene glycol (EG) medium using zinc acetate and adipic acid to obtain zinc adipate and further decomposition at 450 Degree-Sign C to confer nanocrystalline ZnO hexagons. XRD shows the hexagonal wurtzite structure of the ZnO. Thermal study reveals complete formation of ZnO at 430 Degree-Sign C in case of solid-state method, whereas in case of co-precipitation method complete formation was observed at 400 Degree-Sign C. Field emission scanning electron microscope shows spherical morphology for ZnO synthesized by solid-state method. The aqueous-mediated ZnO by co-precipitation method shows rod-like morphology. These rods are formed via self assembling of spherical nanoparticles, however, uniformly dispersed spherical crystallites were seen in EG-mediated ZnO. Transmission electron microscope (TEM) investigations clearly show well aligned and highly crystalline transparent and thin hexagonal ZnO. The particle size was measured using TEM and was observed to be 50-60 nm in case of solid-state method and aqueous-mediated co-precipitation method, while 25-50 nm in case of EG-mediated co-precipitation method. UV absorption spectra showed sharp absorption peaks with a blue shift for EG-mediated ZnO, which demonstrate the mono-dispersed lower particle size. The band gap of the ZnO was observed to be 3.4 eV which is higher than the bulk, implies nanocrystalline nature of the ZnO. The photoluminescence studies clearly indicate the strong violet and weak blue emission in ZnO nanoparticles which is quite unique. The process investigated may be useful to synthesize other oxide semiconductors and transition metal oxides.

  14. Substituting milk for apple juice does not increase kidney stone risk in most normocalciuric adults who form calcium oxalate stones.

    Science.gov (United States)

    Massey, L K; Kynast-Gales, S A

    1998-03-01

    Increasing intake of dietary calcium from less than 400 mg to 800 mg daily may decrease the absorption of dietary oxalate, which in turn would decrease urinary oxalate excretion. The effect of substituting milk for apple juice on urine composition and risk of calcium oxalate precipitability was studied. Twenty-one normocalciuric adults with a history of at least 1 calcium oxalate stone and urinary oxalate excretion exceeding 275 micromol/day on their self-selected diet. Randomized crossover trial. Each participant consumed two moderate-oxalate (2,011 micromol/day) study diets, which were identical except that one contained 360 mL milk and the other contained 540 mL apple juice as the beverage with meals. Four days free-living then 2 days in the metabolic unit of a university nutrition department. Tiselius risk index for calcium oxalate precipitability calculated from urine composition. Paired t tests. Twenty-four hour urinary oxalate excretion was 18% lower (Pjuice diet: 423 vs 514 micromol, respectively. Calcium excretion was 17% higher (Pjuice diet: 4.7 vs 3.9 mmol, respectively. Urinary magnesium and citrate excretion, volume, and Tiselius risk index did not differ between diets. Substituting 360 mL milk daily for apple juice with meals in a diet containing moderate amounts of dietary oxalate from whole grains, legumes, fruits, and vegetables does not increase the risk index of calcium oxalate precipitability in most normocalciuric adults who form stones.

  15. Synthesis of Nano-Structured La0.6Sr0.4Co0.2Fe0.8O3 Perovskite by Co-Precipitation Method

    Directory of Open Access Journals (Sweden)

    Ebrahim Mostafavi

    2015-06-01

    Full Text Available Nano-structured lanthanum strontium cobalt ferrite, La0.6Sr0.4Co0.2Fe0.8O3 (LSCF, was successfully synthesized via co-precipitation method using metal nitrates as starting materials. Effects of precipitating agent and calcination temperature on the phase composition and morphology of synthesized powders were systematically studied using X-ray diffraction (XRD and field emission scanning electron microscopy (FESEM, respectively. XRD analysis revealed that a single phase La0.6Sr0.4Co0.2Fe0.8O3 perovskite was obtained in the processed sample using ammonium carbonate as precipitating agent with a NH4+/NO3-molar ratio of 2 after calcination at 1000C for 1 h. The phase composition of products was also affected by changing pH values. Moreover, using sodium hydroxide as a precipitant resulted in a mixture of La0.6Sr0.4Co0.2Fe0.8O3 and cobalt ferrite (CoFe2O4 phases. Careless washing of the precursors can also led to the formation of mixed phase after calcination of final powders. Mean crystallite size of the obtained powders was not noticeably affected by varying calcination temperature from 900 to 1050C and remained almost the same at 10 nm, however increasing calcination temperature to 1100C resulted in sharp structural coarsening. FESEM studies demonstrate that relatively uniform particles with mean particle size of 90 nm were obtained in the sample processed with a NH4+/NO3- molar ratio of 2 after calcination at 1000C for 1 h.

  16. Development of a calcium phosphate co-precipitate/poly(lactide-co-glycolide) DNA delivery system: release kinetics and cellular transfection studies.

    Science.gov (United States)

    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.

  17. The effect of processing and preservation methods on the oxalate ...

    African Journals Online (AJOL)

    Dr. J. T. Ekanem

    vegetables and consequently the associated food safety problems. Keywords: .... vegetables prepared in slightly two different ... Table 2: Oxalate levels of selected leafy vegetables as a function of cooking method and the interplay of freezing.

  18. Evaluation of oxalate decarboxylase and oxalate oxidase for industrial applications.

    Science.gov (United States)

    Cassland, Pierre; Sjöde, Anders; Winestrand, Sandra; Jönsson, Leif J; Nilvebrant, Nils-Olof

    2010-05-01

    Increased recirculation of process water has given rise to problems with formation of calcium oxalate incrusts (scaling) in the pulp and paper industry and in forest biorefineries. The potential in using oxalate decarboxylase from Aspergillus niger for oxalic acid removal in industrial bleaching plant filtrates containing oxalic acid was examined and compared with barley oxalate oxidase. Ten different filtrates from chemical pulping were selected for the evaluation. Oxalate decarboxylase degraded oxalic acid faster than oxalate oxidase in eight of the filtrates, while oxalate oxidase performed better in one filtrate. One of the filtrates inhibited both enzymes. The potential inhibitory effect of selected compounds on the enzymatic activity was tested. Oxalate decarboxylase was more sensitive than oxalate oxidase to hydrogen peroxide. Oxalate decarboxylase was not as sensitive to chlorate and chlorite as oxalate oxidase. Up to 4 mM chlorate ions, the highest concentration tested, had no inhibitory effect on oxalate decarboxylase. Analysis of the filtrates suggests that high concentrations of chlorate present in some of the filtrates were responsible for the higher sensitivity of oxalate oxidase in these filtrates. Oxalate decarboxylase was thus a better choice than oxalate oxidase for treatment of filtrates from chlorine dioxide bleaching.

  19. Investigation of composition and properties of some neptunium (5) oxalate compounds

    International Nuclear Information System (INIS)

    Zubarev, V.G.; Krot, N.N.

    1981-01-01

    A simple way of neptunium (5) oxalate synthesis is described and its composition is determined: (NpO 2 ) 2 C 2 O 4 xH 2 O. The compound is precipitated from solution during pouring together stoichiometric quantities of neptunium (5) nitrate and ammonium, sodium or potassium oxalate at pH=4-5. An explanation to unusual effect of solubility change with time of neptunium (5) monooxalate complexes and alkali metal or ammonium ion is found taking into account the slow formation of precipitate and low solubility of the compound obtained (0.62 g/l as to metal). Thermal decomposition of the compound is studied. At 180 deg C a water molecule is split off and at 260 deg C decomposition of neptunium oxalate starts. IR spectra and interplane distances (dsub(hkl)) of the compound crystal lattice are determined. New data on the synthesis and properties of complex neptunium (5) oxalates and monovalent cation in second sphere with the ratio ligand: metal=2:1 and 3:1 are presented. On the basis of results of IR spectroscopy and X-ray phase analyses a supposition is made on the existence of such complex compounds [ru

  20. A new oxalate co-conversion technology based on liquid/liquid extraction columns

    International Nuclear Information System (INIS)

    Borda, Gilles; Ode, Denis; Duhamet, Jean; Allegri, Patrick

    2008-01-01

    The current objective of fabricating non proliferating nuclear fuel by 'direct' coprecipitation of uranium, plutonium and minor actinides requires a new process to replace the (co)precipitation step. The technological impact of an increased capacity on the work zone could require the development of a different concept for a continuous device capable of ensuring the proposed goal. A new type of device designed and patented by the Cea was tested in 2007. The patent is for organic confinement in a pulsed column. First, precipitation of cerium or neodymium alone has been carried out in this device, with satisfactory results. Moreover, a recent test campaign demonstrated that a uranium-cerium co-precipitate easily forms when the two nitrates are mixed in a pulsed column of the same size operating under very similar process conditions. Qualitatively, the co-precipitate meets the process requirements. (authors)

  1. Magnetic Properties of Copper Doped Nickel Ferrite Nanoparticles Synthesized by Co Precipitation Method

    Science.gov (United States)

    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.

  2. Supercritical antisolvent co-precipitation of rifampicin and ethyl cellulose.

    Science.gov (United States)

    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

  3. Separation and purification of uranium product from thorium in thorex process by precipitation technique

    International Nuclear Information System (INIS)

    Ramanujam, A.; Dhami, P.S.; Gopalakrishnan, V.; Mukherjee, A.; Dhumwad, R.K.

    1989-01-01

    A sequential precipitation technique is reported for the separation of uranium and thorium present in the uranium product stream of a single cycle 5 per cent TBP Thorex Process. It involves the precipitation of thorium as oxalate in 1M HNO 3 medium at 60-70degC and after filtration, precipitation of uranium as ammonium diuranate at 80-90degC from the oxalate supernatant. This technique has several advantages over the ion-exchange process normally used for treating these products. In order to meet the varying feed conditions, this method has been tested for feeds containing 10 g/1 uranium and 1-50 g/1 thorium in 1-6M HNO 3 . Various parameters like feed acidities, uranium and thorium concentrations, excess oxalic acid concentrations in the oxalate supernatant, precipitation temperatures, precipitate wash volumes etc. have been optimised to obtain more than 99 per cent recovery of thorium and uranium as their oxides with less than 50 ppm uranium losses to ammonium diuranate filtrate. The distribution patterns of different fission products and stainless steel corrosion products during various steps of this procedure have also been studied. For simulating the actual Thorex plant scale operation, experiments have been conducted with 25g and 100g lots of uranium per batch. (author). 6 tabs., 8 figs., 22 refs

  4. A new oxalate co-conversion technology based on liquid/liquid extraction columns

    Energy Technology Data Exchange (ETDEWEB)

    Borda, Gilles; Ode, Denis; Duhamet, Jean; Allegri, Patrick [CEA Nuclear Energy Division - Fuel Cycle Technology Division - System and Chemical Engineering Device Marcoule - 30207 Bagnols sur Ceze (France)

    2008-07-01

    The current objective of fabricating non proliferating nuclear fuel by 'direct' coprecipitation of uranium, plutonium and minor actinides requires a new process to replace the (co)precipitation step. The technological impact of an increased capacity on the work zone could require the development of a different concept for a continuous device capable of ensuring the proposed goal. A new type of device designed and patented by the Cea was tested in 2007. The patent is for organic confinement in a pulsed column. First, precipitation of cerium or neodymium alone has been carried out in this device, with satisfactory results. Moreover, a recent test campaign demonstrated that a uranium-cerium co-precipitate easily forms when the two nitrates are mixed in a pulsed column of the same size operating under very similar process conditions. Qualitatively, the co-precipitate meets the process requirements. (authors)

  5. Synthesis from zinc oxalate, growth mechanism and optical properties of ZnO nano/micro structures

    Energy Technology Data Exchange (ETDEWEB)

    Raj, C. Justin; Varma, K.B.R. [Materials Research Centre, Indian Institute of Science, Bangalore 560 012 (India); Joshi, R.K. [Special Center for Nano Sciences, Jawaharlal Nehru University, New Delhi 110067 (India)

    2011-11-15

    We report the synthesis of various morphological micro to nano structured zinc oxide crystals via simple precipitation technique. The growth mechanisms of the zinc oxide nanostructures such as snowflake, rose, platelets, porous pyramid and rectangular shapes were studied in detail under various growth conditions. The precursor powders were prepared using several zinc counter ions such as chloride, nitrate and sulphate along with oxalic acid as a precipitating agent. The precursors were decomposed by heating in air resulting in the formation of different shapes of zinc oxide crystals. Variations in ZnO nanostructural shapes were possibly due to the counter ion effect. Sulphate counter ion led to unusual rose-shape morphology. Strong ultrasonic treatment on ZnO rose shows that it was formed by irregular arrangement of micro to nano size hexagonal zinc oxide platelets. The X-ray diffraction studies confirmed the wurzite structure of all zinc oxide samples synthesized using different zinc counter ions. Functional groups of the zinc oxalate precursor and zinc oxide were identified using micro Raman studies. The blue light emission spectra of the various morphologies were recorded using luminescence spectrometer. (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  6. Influence of oxalate ligand functionalization on Co/ZSM-5 activity in Fischer Tropsch synthesis and hydrodeoxygenation of oleic acid into hydrocarbon fuels.

    Science.gov (United States)

    Ayodele, Olumide Bolarinwa

    2017-08-30

    Achieving high degree of active metal dispersions at the highest possible metal loading and high reducibility of the metal remains a challenge in Fischer Tropsch synthesis (FTS) as well as in hydrogeoxygenation (HDO).This study therefore reports the influence of oxalic acid (OxA) functionalization on the metal dispersion, reducibility and activity of Co supported ZSM-5 catalyst in FTS and HDO of oleic acid into paraffin biofuel. The Brunauer-Emmett-Teller (BET) results showed that cobalt oxalate supported ZSM-5 catalyst (CoOx/ZSM-5) synthesized from the incorporation of freshly prepared cobalt oxalate complex into ZSM-5 displayed increase in surface area, pore volume and average pore size while the nonfunctionalized cobalt supported on ZSM-5 (Co/ZSM-5) catalyst showed reduction in those properties. Furthermore, both XRD and XPS confirmed the presence of Co° formed from the decomposition of CoOx during calcination of CoOx/ZSM-5 under inert atmosphere. The HRTEM showed that Co species average particle sizes were smaller in CoOx/ZSM-5 than in Co/ZSM-5, and in addition, CoOx/ZSM-5 shows a clear higher degree of active metal dispersion. The FTS result showed that at CO conversion over Co/ZSM-5 and CoOx/ZSM-5 catalysts were 74.28% and 94.23% and their selectivity to C 5+ HC production were 63.15% and 75.4%, respectively at 4 h TOS. The HDO result also showed that the CoOx/ZSM-5 has higher OA conversion of 92% compared to 59% over Co/ZSM-5. In addition CoOx/ZSM-5 showed higher HDO and isomerization activities compared to Co/ZSM-5.

  7. Synthesis of LiNi0.8Co0.1Mn0.1O2 cathode material by chloride co-precipitation method

    Institute of Scientific and Technical Information of China (English)

    李灵均; 李新海; 王志兴; 伍凌; 郑俊超; 李金辉

    2010-01-01

    LiNi0.8Co0.1Mn0.1O2 was prepared by a chloride co-precipitation method and characterized by thermogravimetric analysis, X-ray diffractometry with Rietveld refinement,electron scanning microscopy and electrochemical measurements.Effects of lithium ion content and sintering temperature on physical and electrochemical performance of LiNi0.8Co0.1Mn0.1O2 were also investigated. The results show that the sample synthesized at 750℃with 105%lithium content has fine particle sizes around 200 nm and homogenous sizes distribution.The initial discharge capacity for the powder is 184 mA·h/g between 2.7 and 4.3 V at 0.1C and room temperature.

  8. OXALATE MASS BALANCE DURING CHEMICAL CLEANING IN TANK 6F

    Energy Technology Data Exchange (ETDEWEB)

    Poirier, M.; Fink, S.

    2011-07-22

    The Savannah River Remediation (SRR) is preparing Tank 6F for closure. The first step in preparing the tank for closure is mechanical sludge removal. Following mechanical sludge removal, SRS performed chemical cleaning with oxalic acid to remove the sludge heel. Personnel are currently assessing the effectiveness of the chemical cleaning to determine whether the tank is ready for closure. SRR personnel collected liquid samples during chemical cleaning and submitted them to Savannah River National Laboratory (SRNL) for analysis. Following chemical cleaning, they collected a solid sample (also known as 'process sample') and submitted it to SRNL for analysis. The authors analyzed these samples to assess the effectiveness of the chemical cleaning process. Analysis of the anions showed the measured oxalate removed from Tank 6F to be approximately 50% of the amount added in the oxalic acid. To close the oxalate mass balance, the author collected solid samples, leached them with nitric acid, and measured the concentration of cations and anions in the leachate. Some conclusions from this work are: (1) Approximately 65% of the oxalate added as oxalic acid was removed with the decanted liquid. (2) Approximately 1% of the oxalate (added to the tank as oxalic acid) formed precipitates with compounds such as nickel, manganese, sodium, and iron (II), and was dissolved with nitric acid. (3) As much as 30% of the oxalate may have decomposed forming carbon dioxide. The balance does not fully account for all the oxalate added. The offset represents the combined uncertainty in the analyses and sampling.

  9. Equilibrium aluminium hydroxo-oxalate phases during initial clay formation; H +-Al 3+-oxalic acid-Na + system

    Science.gov (United States)

    Bilinski, Halka; Horvath, Laszlo; Ingri, Nils; Sjöberg, Staffan

    1986-09-01

    The conditions necessary for initial clay formation have been studied in different model systems comprising different organic acids besides Si and Al. In the present paper the solid phases and the precipitation boundary characterizing the subsystem H +-Al 3+-oxalic acid (H 2L) are discussed. pH and tyndallometric measurements were performed in an ionic medium of 0.6 M Na(Cl) at 25 °C. The two phases Al 3(OH) 7(C 2O 4) · 3H 2O (phase I) and NaAl(OH) 2(C 2O 4) · 3H 2O (phase II) determine the precipitation boundary. The following formation constants for the two phases were deduced: lgβ1 = lg([ Al3+] -3[ H2C2O4] -1[ H+] 9 = -21.87 ± 0.08 and lgβ11 = lg([ Al3+] -1[ H2C2O4] -1[ H+] 4 = -5.61 ± 0.06. Phase I exists in the range [ Al] tot≥ 10 -4.4moldm-3,[ H2C2O4] tot ≥ 10 -4.9moldm-3 and at pH oxalic-rich natural waters. The more soluble sodium phase is unlikely to exist in natural waters. The two phases are metastable relative to crystalline gibbsite and may be considered as the first precipitation step in the transition from aqueous Al oxalates down to stable Al hydroxide. Model calculations illustrating these competing hydrolysis-complexation reactions are discussed in terms of predominance and speciation diagrams. The solid phases have been characterized by X-ray analysis of powders, TGA and IR spectra, and tentative structures are proposed. Phase I seems to be an octahedral layer structure, in which 3/5 of the octahedral sites between two close packed oxygen sheets are occupied by Al 3+ and the oxalate ion acts as a bridge ligand between two aluminium atoms. Phase II forms a more open sheet structure and has ion exchange properties. Powder data for a phase crystallized from the studied solution after a year are also presented. This phase, Na 4Al 2(OH) 2(C 2O 4) 4 · 10H 2O, supports the results from the equilibrium analysis of recent solution data by SJöBERG and ÖHMAN (1985), who have found the dinuclear complex Al 2(OH) 2(C 2O 4) 44- to exist in a

  10. The comparability of oxalate excretion and oxalate:creatinine ratio in the investigation of primary hyperoxaluria: review of data from a referral centre.

    Science.gov (United States)

    Clifford-Mobley, Oliver; Tims, Christopher; Rumsby, Gill

    2015-01-01

    Urine oxalate measurement is an important investigation in the evaluation of renal stone disease. Primary hyperoxaluria (PH) is a rare inherited metabolic disease characterised by persistently elevated urine oxalate, but the diagnosis may be missed in adults until renal failure has developed. Urine oxalate results were reviewed to compare oxalate:creatinine ratio and oxalate excretion, and to estimate the potential numbers of undiagnosed PH. Urine oxalate results from August 2011 to April 2013 were reviewed. Oxalate excretion and oxalate:creatinine ratio were evaluated for 24 h collections and ratio alone for spot urine samples. Oxalate:creatinine ratio and oxalate excretion were moderately correlated (R=0.63) in 24-h urine collections from patients aged 18 years and above. Sex-related differences were found requiring implementation of male and female reference ranges for oxalate:creatinine ratio. Of samples with both ratio and excretion above the reference range, 7% came from patients with confirmed PH. There were 24 patients with grossly elevated urine oxalate who had not been evaluated for PH. Oxalate:creatinine ratio and oxalate excretion were discordant in many patients, which is likely to be a result of intra-individual variation in creatinine output and imprecision in the collection itself. Some PH patients had urine oxalate within the reference range on occasion, and therefore it is not possible to exclude PH on the finding of a single normal result. A significant number of individuals had urine oxalate results well above the reference range who potentially have undiagnosed PH and are consequently at risk of renal failure. © The Author(s) 2014 Reprints and permissions: sagepub.co.uk/journalsPermissions.nav.

  11. Effect of Surface Precipitate on the Crevice Corrosion in HYBRID and Oxalic Acid Solution

    International Nuclear Information System (INIS)

    Park, S. Y.; Jung, J. Y.; Won, H. J.; Kim, S. B.; Choi, W. K.; Moon, J. K.; Park, S. J.

    2015-01-01

    In this study, we investigated the characteristics of the crevice corrosion for Inconel-600 and 304SS in OA solution according to the change in pH. The evaluation of the crevice corrosion with the chemical thermodynamic analysis identified the effect of the residual chemicals such as iron-oxalate and nickeloxalate to the crevice corrosion behavior. Test results were compared with those of HYBRID (HYdrizine Base Reductive metal Ion Decontamination). The crevice corrosion properties of 304 SS and Inconel-600 in HYBRID and oxalic acid solution were evaluated. In case of oxalic acid solution, the corrosion rate on 304SS was rapidly increased with a pH decrease of around 2, but there was no increase in the corrosion rate on Inconel-600

  12. Study of calcium carbonate and sulfate co-precipitation

    KAUST Repository

    Zarga, Y.; Ben Boubaker, H.; Ghaffour, NorEddine; Elfil, Hamza

    2013-01-01

    of CaCO3 nucleation and lead to its precipitation by activating heterogeneous germination. However, the presence of CaCO3 crystals does not seem to have any significant effect on gypsum precipitation. IR spectroscopy and the Scanning Electronic

  13. Multiscale structural characterizations of mixed U(iv)-An(iii) oxalates (An(iii) = Pu or Am) combining XAS and XRD measurements.

    Science.gov (United States)

    Arab-Chapelet, B; Martin, P M; Costenoble, S; Delahaye, T; Scheinost, A C; Grandjean, S; Abraham, F

    2016-04-28

    Mixed actinide(III,IV) oxalates of the general formula M2.2UAn(C2O4)5·nH2O (An = Pu or Am and M = H3O(+) and N2H5(+)) have been quantitatively precipitated by oxalic precipitation in nitric acid medium (yield >99%). Thorough multiscale structural characterization using XRD and XAS measurements confirmed the existence of mixed actinide oxalate solid solutions. The XANES analysis confirmed that the oxidation states of the metallic cations, tetravalent for uranium and trivalent for plutonium and americium, are maintained during the precipitation step. EXAFS measurements show that the local environments around U(+IV), Pu(+III) and Am(+III) are comparable, and the actinides are surrounded by ten oxygen atoms from five bidentate oxalate anions. The mean metal-oxygen distances obtained by XAS measurements are in agreement with those calculated from XRD lattice parameters.

  14. Electrochemical performance of multi-element doped α-nickel hydroxide prepared by supersonic co-precipitation method

    International Nuclear Information System (INIS)

    Zhang, Z.J.; Zhu, Y.J.; Bao, J.; Lin, X.R.; Zheng, H.Z.

    2011-01-01

    Highlights: → The α-nickel hydroxides doped with several elements were prepared by supersonic co-precipitation method. → Cyclic voltammetry and electrochemical impedance spectroscopy show sample C has the best electrochemical performance. → The charge/discharge tests show that the 0.5 C discharge capacity (346 mAh/g) of sample C is even larger than that (337 mAh/g) at 0.1 C rate, while the discharge capacity at 0.5 C rate is much lower than that at 0.1 C rate for samples A and B. - Abstract: The multi-element doped α-nickel hydroxides have been prepared by supersonic co-precipitation method. Three kinds of samples A, B, C were prepared by chemically coprecipitating Ni, Al, Co, Y, Zn. It was found that sample C produced better performance than the others. The cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) measurements indicated that sample C has better electrochemical performance, such as better reaction reversibility, higher proton diffusion coefficient and lower charge-transfer resistance, than those of samples A and B. The charge-discharge tests showed that the discharge capacity (346 mA h/g) of sample C is even larger at 0.5 C rate than that (337mAh/g) at 0.1 C rate, while the discharge capacity at 0.5 C rate is much lower than that at 0.1 C rate for samples A and B. It indicates that all doped elements can produce the synergic effect and further improve the electrochemical properties of the active materials.

  15. A Novel Method for Fabricating Double Layers Porous Anodic Alumina in Phosphoric/Oxalic Acid Solution and Oxalic Acid Solution

    Directory of Open Access Journals (Sweden)

    Yanfang Xu

    2016-01-01

    Full Text Available A novel method for fabricating ordered double layers porous anodic alumina (DL-PAA with controllable nanopore size was presented. Highly ordered large pore layer with interpore distance of 480 nm was fabricated in phosphoric acid solution with oxalic acid addition at the potential of 195 V and the small pore layer was fabricated in oxalic acid solution at the potential from 60 to 100 V. Experimental results show that the thickness of large pore layer is linearly correlative with anodizing time, and pore diameter is linearly correlative with pore widening time. When the anodizing potential in oxalic acid solution was adjusted from 60 to 100 V, the small pore layers with continuously tunable interpore distance from 142 to 241 nm and pore density from 1.94×109 to 4.89×109 cm−2 were obtained. And the interpore distance and the pore density of small pore layers are closely correlative with the anodizing potential. The fabricated DL-PAA templates can be widely utilized for fabrication of ordered nanomaterials, such as superhydrophobic or gecko-inspired adhesive materials and metal or semiconductor nanowires.

  16. A study of CO2 precipitation method considering an ionic CO2 and Ca(OH)2 slurry

    International Nuclear Information System (INIS)

    Park, Sangwon; Jo, Hoyong; Kang, Dongwoo; Park, Jinwon

    2014-01-01

    CCS (carbon capture and storage) is the most popular technology used for the reduction of CO 2 in the post-combustion stage. However, the CCS process has some disadvantages including uncertainty about the stability of the land that is used to store the separated CO 2 . Consequently, CCU (carbon capture and utilization) technologies have recently received increased attention as a possible replacement for CCS. In this study, we utilized CO 2 fixation methods by using the metal carbonate mechanism. We selected 5 and 30 wt% MEA (mono-ethanolamine) solutions to rapidly make a carbonate and Ca(OH) 2 slurry. In all of the experiments, normal temperature and pressure conditions were maintained (except during desorption to check for residual CO 2 in the MEA solution). Consequently, most of the CO 2 was converted to carbonate. The MEA converted CO 2 to ionic CO 2 and rapidly created calcium carbonate. Also the formed solids that were observed were determined to be CaCO 3 and Ca(OH) 2 by X-ray diffractometry. Also, the MEA solution could be reused to absorb CO 2 . Therefore, we have confirmed the development of our suggested CCS process. This process has the ability not only to reuse emitted CO 2 , but it can also be employed to reuse construction wastes that include heavy metals. - Highlights: • We propose novel CO 2 conversion technology by utilizing an amine solution. • In this study, alkaline solutions were used to produce CO 2 precipitate. • The MEA (mono-ethanolamine) solution has a sufficient potential to fix CO 2 with metal sources under moderate condition. • Also, the Ca(OH) 2 slurry yielded enough Ca 2+ ions to make carbonate

  17. Encapsulation of albumin in self-assembled layer-by-layer microcapsules: comparison of co-precipitation and adsorption techniques.

    Science.gov (United States)

    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.

  18. Role of cellular oxalate in oxalate clearance of patients with calcium oxalate monohydrate stone formation and normal controls.

    Science.gov (United States)

    Oehlschläger, Sven; Fuessel, Susanne; Meye, Axel; Herrmann, Jana; Froehner, Michael; Albrecht, Steffen; Wirth, Manfred P

    2009-03-01

    To examine the cellular, plasma, and urinary oxalate and erythrocyte oxalate flux in patients with calcium oxalate monohydrate (COM) stone formation vs normal controls. Pathologic oxalate clearance in humans is mostly integrated in calcium oxalate stone formation. An underlying cause of deficient oxalate clearance could be defective transmembrane oxalate transport, which, in many tissues, is regulated by an anion exchanger (SLC26). We studied 2 groups: 40 normal controls and 41 patients with COM stone formation. Red blood cells were divided for cellular oxalate measurement and for resuspension in a buffered solution (pH 7.40); 0.1 mmol/L oxalate was added. The supernatant was measured for oxalate immediately and 1 hour after incubation. The plasma and urinary oxalate were analyzed in parallel. The mean cellular oxalate concentrations were significantly greater in the normal controls (5.25 +/- 0.47 micromol/L) than in those with COM stone formation (2.36 +/- 0.28 micromol/L; P stone formation (0.31 +/- 0.02 mmol/L) than in the controls (0.24 +/- 0.02 mmol/L; P r = 0.49-0.63; P r = -0.29-0.41; P r = -0.30; P r = 0.25; P stone formation. Our data implicate the presence of a cellular oxalate buffer to stabilize plasma and urinary oxalate concentrations in normal controls.

  19. A review of plutonium oxalate decomposition reactions and effects of decomposition temperature on the surface area of the plutonium dioxide product

    Energy Technology Data Exchange (ETDEWEB)

    Orr, R.M.; Sims, H.E.; Taylor, R.J., E-mail: robin.j.taylor@nnl.co.uk

    2015-10-15

    Plutonium (IV) and (III) ions in nitric acid solution readily form insoluble precipitates with oxalic acid. The plutonium oxalates are then easily thermally decomposed to form plutonium dioxide powder. This simple process forms the basis of current industrial conversion or ‘finishing’ processes that are used in commercial scale reprocessing plants. It is also widely used in analytical or laboratory scale operations and for waste residues treatment. However, the mechanisms of the thermal decompositions in both air and inert atmospheres have been the subject of various studies over several decades. The nature of intermediate phases is of fundamental interest whilst understanding the evolution of gases at different temperatures is relevant to process control. The thermal decomposition is also used to control a number of powder properties of the PuO{sub 2} product that are important to either long term storage or mixed oxide fuel manufacturing. These properties are the surface area, residual carbon impurities and adsorbed volatile species whereas the morphology and particle size distribution are functions of the precipitation process. Available data and experience regarding the thermal and radiation-induced decompositions of plutonium oxalate to oxide are reviewed. The mechanisms of the thermal decompositions are considered with a particular focus on the likely redox chemistry involved. Also, whilst it is well known that the surface area is dependent on calcination temperature, there is a wide variation in the published data and so new correlations have been derived. Better understanding of plutonium (III) and (IV) oxalate decompositions will assist the development of more proliferation resistant actinide co-conversion processes that are needed for advanced reprocessing in future closed nuclear fuel cycles. - Highlights: • Critical review of plutonium oxalate decomposition reactions. • New analysis of relationship between SSA and calcination temperature.

  20. Synthesis of Zn{sub 0.95}Cr{sub 0.05}O DMS by co-precipitation and ceramic methods: Structural and magnetization studies

    Energy Technology Data Exchange (ETDEWEB)

    Paul Joseph, D. [Materials Science Centre, Department of Nuclear Physics, University of Madras, Guindy Campus, Chennai 600025 (India); Naveenkumar, S. [Materials Science Centre, Department of Nuclear Physics, University of Madras, Guindy Campus, Chennai 600025 (India); Sivakumar, N. [Materials Science Centre, Department of Nuclear Physics, University of Madras, Guindy Campus, Chennai 600025 (India); Venkateswaran, C. [Materials Science Centre, Department of Nuclear Physics, University of Madras, Guindy Campus, Chennai 600025 (India)]. E-mail: cvunom@hotmail.com

    2006-05-10

    Transitional metal ions-substituted ZnO are recently explored for SPINTRONICS applications. Synthesis of single-phase oxide 'diluted magnetic semiconductors' (DMS) is a must to explore the magnetic properties arising due to the strong sp-d exchange interaction. The synthesis route plays a vital role in this aspect. In this work, we have prepared Zn{sub 0.95}Cr{sub 0.05}O by using the co-precipitation method and also the standard ceramic method and optimized the conditions to obtain the single-phase compound. X-ray diffraction measurements were done on Zn{sub 0.95}Cr{sub 0.05}O annealed and sintered at various temperatures. Comparing these results, we conclude that the co-precipitation method is more convenient for obtaining single-phase compound by the relatively low temperature processing of the precipitated hydroxides. Pelleted sample examined for its magnetic property using a vibrating sample magnetometer (VSM) indicated ferromagnetic-like behavior at 300 K and a spin-glass state at 77 K.

  1. Plasma oxalic acid and calcium levels in oxalate poisoning

    Science.gov (United States)

    Zarembski, P. M.; Hodgkinson, A.

    1967-01-01

    Observations are reported on five cases of suicide or attempted suicide by poisoning with oxalic acid or ethylene glycol. Elevated oxalic acid levels were observed in the plasma, stomach contents, and a number of tissues. Raised oxalic acid levels in plasma were associated with reduced total and ultrafilterable calcium levels. It is suggested that the reduction in plasma total calcium level is due mainly to the deposition of calcium oxalate in the soft tissues, but inhibition of the parathyroid glands may be a contributory factor. Microscopic examination of various tissues indicated that oxalic acid is deposited in the tissues in two forms: (1) crystalline calcium oxalate dihydrate in the kidney and (2) a non-crystalline complex of calcium oxalate and lipid in liver and other tissues. PMID:5602563

  2. Preparation of LuAG Powders with Single Phase and Good Dispersion for Transparent Ceramics Using Co-Precipitation Method

    Science.gov (United States)

    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

  3. Preparation of LuAG Powders with Single Phase and Good Dispersion for Transparent Ceramics Using Co-Precipitation Method

    Directory of Open Access Journals (Sweden)

    Liangjie Pan

    2015-08-01

    Full Text Available 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.

  4. Advanced Oxidation: Oxalate Decomposition Testing With Ozone

    International Nuclear Information System (INIS)

    Ketusky, E.; Subramanian, K.

    2012-01-01

    At the Savannah River Site (SRS), oxalic acid is currently considered the preferred agent for chemically cleaning the large underground Liquid Radioactive Waste Tanks. It is applied only in the final stages of emptying a tank when generally less than 5,000 kg of waste solids remain, and slurrying based removal methods are no-longer effective. The use of oxalic acid is preferred because of its combined dissolution and chelating properties, as well as the fact that corrosion to the carbon steel tank walls can be controlled. Although oxalic acid is the preferred agent, there are significant potential downstream impacts. Impacts include: (1) Degraded evaporator operation; (2) Resultant oxalate precipitates taking away critically needed operating volume; and (3) Eventual creation of significant volumes of additional feed to salt processing. As an alternative to dealing with the downstream impacts, oxalate decomposition using variations of ozone based Advanced Oxidation Process (AOP) were investigated. In general AOPs use ozone or peroxide and a catalyst to create hydroxyl radicals. Hydroxyl radicals have among the highest oxidation potentials, and are commonly used to decompose organics. Although oxalate is considered among the most difficult organic to decompose, the ability of hydroxyl radicals to decompose oxalate is considered to be well demonstrated. In addition, as AOPs are considered to be 'green' their use enables any net chemical additions to the waste to be minimized. In order to test the ability to decompose the oxalate and determine the decomposition rates, a test rig was designed, where 10 vol% ozone would be educted into a spent oxalic acid decomposition loop, with the loop maintained at 70 C and recirculated at 40L/min. Each of the spent oxalic acid streams would be created from three oxalic acid strikes of an F-area simulant (i.e., Purex = high Fe/Al concentration) and H-area simulant (i.e., H area modified Purex = high Al/Fe concentration) after nearing

  5. ADVANCED OXIDATION: OXALATE DECOMPOSITION TESTING WITH OZONE

    Energy Technology Data Exchange (ETDEWEB)

    Ketusky, E.; Subramanian, K.

    2012-02-29

    At the Savannah River Site (SRS), oxalic acid is currently considered the preferred agent for chemically cleaning the large underground Liquid Radioactive Waste Tanks. It is applied only in the final stages of emptying a tank when generally less than 5,000 kg of waste solids remain, and slurrying based removal methods are no-longer effective. The use of oxalic acid is preferred because of its combined dissolution and chelating properties, as well as the fact that corrosion to the carbon steel tank walls can be controlled. Although oxalic acid is the preferred agent, there are significant potential downstream impacts. Impacts include: (1) Degraded evaporator operation; (2) Resultant oxalate precipitates taking away critically needed operating volume; and (3) Eventual creation of significant volumes of additional feed to salt processing. As an alternative to dealing with the downstream impacts, oxalate decomposition using variations of ozone based Advanced Oxidation Process (AOP) were investigated. In general AOPs use ozone or peroxide and a catalyst to create hydroxyl radicals. Hydroxyl radicals have among the highest oxidation potentials, and are commonly used to decompose organics. Although oxalate is considered among the most difficult organic to decompose, the ability of hydroxyl radicals to decompose oxalate is considered to be well demonstrated. In addition, as AOPs are considered to be 'green' their use enables any net chemical additions to the waste to be minimized. In order to test the ability to decompose the oxalate and determine the decomposition rates, a test rig was designed, where 10 vol% ozone would be educted into a spent oxalic acid decomposition loop, with the loop maintained at 70 C and recirculated at 40L/min. Each of the spent oxalic acid streams would be created from three oxalic acid strikes of an F-area simulant (i.e., Purex = high Fe/Al concentration) and H-area simulant (i.e., H area modified Purex = high Al/Fe concentration

  6. Novel approach to recover cobalt and lithium from spent lithium-ion battery using oxalic acid.

    Science.gov (United States)

    Zeng, Xianlai; Li, Jinhui; Shen, Bingyu

    2015-09-15

    With the booming of consumer electronics (CE) and electric vehicle (EV), a large number of spent lithium-ion battery (LIBs) have been generated worldwide. Resource depletion and environmental concern driven from the sustainable industry of CE and EV have motivated spent LIBs should be recovered urgently. However, the conventional process combined with leaching, precipitating, and filtering was quite complicated to recover cobalt and lithium from spent LIBs. In this work, we developed a novel recovery process, only combined with oxalic acid leaching and filtering. When the optimal parameters for leaching process is controlled at 150 min retention time, 95 °C heating temperature, 15 g L(-1) solid-liquid ratio, and 400 rpm rotation rate, the recovery rate of lithium and cobalt from spent LIBs can reach about 98% and 97%, respectively. Additionally, we also tentatively discovered the leaching mechanism of lithium cobalt oxide (LiCoO2) using oxalic acid, and the leaching order of the sampling LiCoO2 of spent LIBs. All the obtained results can contribute to a short-cut and high-efficiency process of spent LIBs recycling toward a sound closed-loop cycle. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Application of Carrier Element-Free Co-precipitation Method for Ni(II), Cu(II) and Zn(II) Ions Determination in Water Samples Using Chrysin

    International Nuclear Information System (INIS)

    Layth Imad Abd Ali; Wan Aini Wan Ibrahim; Azli Sulaiman; Mohd Marsin Sanagi

    2015-01-01

    A co-precipitation method was developed to separate and pre-concentrate Ni(II), Cu(II) and Zn(II) ions using an organic co precipitant, chrysin without adding any carrier element termed as carrier element-free co-precipitation (CEFC). Analytes were determined using flame atomic absorption spectrometry (FAAS). The influence of analytical conditions, such as pH of the solution, quantity of co-precipitant, standing time, centrifugation rate and time, sample volume, and interference of concomitant ions were investigated over the recovery yields of the trace metals. The limit of detection, the limit of quantification and linearity range obtained from the FAAS measurements were found to be in the range of 0.64 to 0.86 μg L -1 , 2.13 to 2.86 μg L -1 and 0.9972 to 0.9989 for Ni(II), Cu(III) and Zn(II) ions, respectively. The precision of the method, evaluated as the relative standard deviation (RSD) obtained after analyzing a series of 10 replicates, was between 2.6 % to 3.9 % for the trace metal ions. The proposed procedure was applied and validated by analyzing river water reference material for trace metals (SLRS-5) and spiking trace metal ions in some water samples. The recoveries of the analyte metal ions were between 94.7-101.2 %. (author)

  8. Superior sinterability of nano-crystalline gadolinium doped ceria powders synthesized by co-precipitation method

    International Nuclear Information System (INIS)

    Hari Prasad, D.; Kim, H.-R.; Park, J.-S.; Son, J.-W.; Kim, B.-K.; Lee, H.-W.; Lee, J.-H.

    2010-01-01

    Reduced sintering temperature of doped ceria can greatly simplify the fabrication process of solid oxide fuel cells (SOFCs) by utilizing the co-firing of all cell components with a single step. In the present study, nano-crystalline gadolinium doped ceria (GDC) powders of high sinterability at lower sintering temperature has been synthesized by co-precipitation at room temperature. The successful synthesis of nano-crystalline GDC was confirmed by XRD, TEM and Raman spectroscopy analysis. Dilatometry studies showed that GDC prepared by this method can be fully densified (97% relative density) at a sintering temperature of 950 o C which is fairly lower than ever before. It has also been found that the sintered samples have a higher ionic conductivity of 1.64 x 10 -2 S cm -1 at 600 o C which is suitable for the intermediate temperature SOFC application.

  9. Functional characterization of the oxaloacetase encoding gene and elimination of oxalate formation in the ?-lactam producer Penicillium chrysogenum

    NARCIS (Netherlands)

    Daran, J.M.; Pronk, J.T.; Driessen, A.J.M.; Nijland, J.G.; Lamboo, F.; Puig-Martinez, M.; Veiga, T.; Gombert, A.K.

    2011-01-01

    Penicillium chrysogenum is widely used as an industrial antibiotic producer, in particular in the synthesis of ß-lactam antibiotics such as penicillins and cephalosporins. In industrial processes, oxalic acid formation leads to reduced product yields. Moreover, precipitation of calcium oxalate

  10. Ultrastructural and biochemical studies on formation of calcium oxalate in plants

    International Nuclear Information System (INIS)

    Abdelmottaleb, A.M.

    1989-01-01

    Plant calcium oxalate crystals occur within cells called crystal idioblasts. Important aspects of this calcification phenomenon have not been characterized. This dissertation examines some of the aspects of this ubiquitous type of calcification including (1) characterization of ultrastructural features of developing crystal idioblasts, (2) determination of the relationship of specialized ultrastructural features of the idioblasts to transport of compounds and mechanisms of crystal deposition, and (3) the biochemical relationship between ascorbic acid metabolism and production of oxalic acid used for crystal formation. Structural and cytochemical studies revealed that crystal idioblasts have dense cytoplasm, modified plastids, enlarged nuclei, extensive endoplasmic reticulum, numerous dictyosomes and vesicles, and a bundle of raphide crystals in their vacuoles. A mechanism for Ca transport and crystal precipitation is proposed, based on these results. There is a strong and dynamic relationship between Ca concentration and oxalic acid produced for crystal formation, where increasing Ca level in the growth medium lead to increased total and insoluble oxalate in the plant. Calmodulin antagonists reduced oxalic acid production

  11. Turning sunlight into stone: the oxalate-carbonate pathway in a tropical tree ecosystem

    Directory of Open Access Journals (Sweden)

    G. Cailleau

    2011-07-01

    Full Text Available An African oxalogenic tree, the iroko tree (Milicia excelsa, has the property to enhance carbonate precipitation in tropical oxisols, where such accumulations are not expected due to the acidic conditions in these types of soils. This uncommon process is linked to the oxalate-carbonate pathway, which increases soil pH through oxalate oxidation. In order to investigate the oxalate-carbonate pathway in the iroko system, fluxes of matter have been identified, described, and evaluated from field to microscopic scales. In the first centimeters of the soil profile, decaying of the organic matter allows the release of whewellite crystals, mainly due to the action of termites and saprophytic fungi. In addition, a concomitant flux of carbonate formed in wood tissues contributes to the carbonate flux and is identified as a direct consequence of wood feeding by termites. Nevertheless, calcite biomineralization of the tree is not a consequence of in situ oxalate consumption, but rather related to the oxalate oxidation inside the upper part of the soil. The consequence of this oxidation is the presence of carbonate ions in the soil solution pumped through the roots, leading to preferential mineralization of the roots and the trunk base. An ideal scenario for the iroko biomineralization and soil carbonate accumulation starts with oxalatization: as the iroko tree grows, the organic matter flux to the soil constitutes the litter, and an oxalate pool is formed on the forest ground. Then, wood rotting agents (mainly termites, saprophytic fungi, and bacteria release significant amounts of oxalate crystals from decaying plant tissues. In addition, some of these agents are themselves producers of oxalate (e.g. fungi. Both processes contribute to a soil pool of "available" oxalate crystals. Oxalate consumption by oxalotrophic bacteria can then start. Carbonate and calcium ions present in the soil solution represent the end products of the oxalate

  12. Origin of Urinary Oxalate

    Science.gov (United States)

    Holmes, Ross P.; Knight, John; Assimos, Dean G.

    2007-04-01

    Urinary oxalate is mostly derived from the absorption of ingested oxalate and endogenous synthesis. The breakdown of vitamin C may also contribute small amounts to the urinary oxalate pool. The amount of oxalate absorbed is influenced by the oxalate content of the diet, the concentrations of divalent cations in the gut, the presence of oxalate-degrading organisms, transport characteristics of the intestinal epithelium, and other factors associated with the intestinal environment. Knowledge of pathways associated with endogenous oxalate synthesis is limited. Urinary oxalate excretion can be modified using strategies that limit dietary oxalate absorption and the ingestion of oxalogenic substrates such as hydroxyproline.

  13. Functional characterization of the oxaloacetase encoding gene and elimination of oxalate formation in the beta-lactam producer Penicillium chrysogenum

    NARCIS (Netherlands)

    Gombert, A. K.; Veiga, T.; Puig-Martinez, M.; Lamboo, F.; Nijland, J. G.; Driessen, A. J. M.; Pronk, J. T.; Daran, J. M.

    Penicillium chrysogenum is widely used as an industrial antibiotic producer, in particular in the synthesis of g-lactam antibiotics such as penicillins and cephalosporins. In industrial processes, oxalic acid formation leads to reduced product yields. Moreover, precipitation of calcium oxalate

  14. Effects of natural organic matter on calcium and phosphorus co-precipitation.

    Science.gov (United States)

    Sindelar, Hugo R; Brown, Mark T; Boyer, Treavor H

    2015-11-01

    Phosphorus (P), calcium (Ca) and natural organic matter (NOM) naturally occur in all aquatic ecosystems. However, excessive P loads can cause eutrophic or hyper-eutrophic conditions in these waters. As a result, P regulation is important for these impaired aquatic systems, and Ca-P co-precipitation is a vital mechanism of natural P removal in many alkaline systems, such as the Florida Everglades. The interaction of P, Ca, and NOM is also an important factor in lime softening and corrosion control, both critical processes of drinking water treatment. Determining the role of NOM in Ca-P co-precipitation is important for identifying mechanisms that may limit P removal in both natural and engineered systems. The main goal of this research is to assess the role of NOM in inhibiting Ca and P co-precipitation by: (1) measuring how Ca, NOM, and P concentrations affect NOM's potential inhibition of co-precipitation; (2) determining the effect of pH; and (3) evaluating the precipitated solids. Results showed that Ca-P co-precipitation occurs at pH 9.5 in the presence of high natural organic matter (NOM) (≈30 mg L(-1)). The supersaturation of calcite overcomes the inhibitory effect of NOM seen at lower pH values. Higher initial P concentrations lead to both higher P precipitation rates and densities of P on the calcite surface. The maximum surface density of co-precipitated P on the precipitated calcite surface increases with increasing NOM levels, suggesting that NOM does prevent the co-precipitation of Ca and P. Copyright © 2015 Elsevier Ltd. All rights reserved.

  15. Synthesis of well-dispersed magnetic CoFe2O4 nanoparticles in cellulose aerogels via a facile oxidative co-precipitation method.

    Science.gov (United States)

    Wan, Caichao; Li, Jian

    2015-12-10

    With the increasing emphasis on green chemistry, it is becoming more important to develop environmentally friendly matrix materials for the synthesis of nanocomposites. Cellulose aerogels with hierarchical micro/nano-scale three-dimensional network beneficial to control and guide the growth of nanoparticles, are suitable as a class of ideal green nanoparticles hosts to fabricate multifunctional nanocomposites. Herein, a facile oxidative co-precipitation method was carried out to disperse CoFe2O4 nanoparticles in the cellulose aerogels matrixes, and the cellulose aerogels were prepared from the native wheat straw based on a green NaOH/polyethylene glycol solution. The mean diameter of the well-dispersed CoFe2O4 nanoparticles in the hybrid aerogels is 98.5 nm. Besides, the hybrid aerogels exhibit strong magnetic responsiveness, which could be flexibly actuated by a small magnet. And this feature also makes this class of magnetic aerogels possibly useful as recyclable adsorbents and some magnetic devices. Meanwhile, the mild green preparation method could also be extended to fabricate other miscellaneous cellulose-based nanocomposites. Copyright © 2015 Elsevier Ltd. All rights reserved.

  16. and aluminum-substituted cobalt ferrite prepared by co-precipitation

    Indian Academy of Sciences (India)

    Structural and magnetic properties of zinc- and aluminum-substituted cobalt ferrite prepared by co-precipitation method. S T ALONE1,∗ and K M JADHAV2. 1Shiv Chhatrapati College, Aurangabad 431 004, India. 2Department of Physics, Dr. B. A. Marathwada University, Aurangabad 431 004, India. ∗Corresponding author.

  17. Lithium recycling and cathode material regeneration from acid leach liquor of spent lithium-ion battery via facile co-extraction and co-precipitation processes.

    Science.gov (United States)

    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.

  18. Formation of Silica-Lysozyme Composites Through Co-Precipitation and Adsorption

    Directory of Open Access Journals (Sweden)

    Daniela B. van den Heuvel

    2018-04-01

    Full Text Available 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 small-angle X-ray scattering, 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.

  19. Formation of Silica-Lysozyme Composites Through Co-Precipitation and Adsorption

    Science.gov (United States)

    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.

  20. Synthesis of YAG nanopowder by the co-precipitation method: Influence of pH and study of the reaction mechanisms

    Science.gov (United States)

    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.

  1. Synthesis and magnetic properties of bacterial cellulose—ferrite (MFe2O4, M  =  Mn, Co, Ni, Cu) nanocomposites prepared by co-precipitation method

    Science.gov (United States)

    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.

  2. Neptunium (IV) oxalate solubility

    International Nuclear Information System (INIS)

    Luerkens, D.W.

    1983-07-01

    The equilibrium solubility of neptunium (IV) oxalate in nitric/oxalic acid solutions was determined at 22 0 C, 45 0 C, and 60 0 C. The concentrations of nitric/oxalic acid solutions represented a wide range of free oxalate ion concentration. A mathematical solubility model was developed which is based on the formation of the known complexes of neptunium (IV) oxalate. the solubility model uses a simplified concentration parameter which is proportional to the free oxalate ion concentration. The solubility model can be used to estimate the equilibrium solubility of neptunium (IV) oxalate over a wide range of oxalic and nitric acid concentrations at each temperature

  3. Hygroscopic properties of oxalic acid and atmospherically relevant oxalates

    Science.gov (United States)

    Ma, Qingxin; He, Hong; Liu, Chang

    2013-04-01

    Oxalic acid and oxalates represent an important fraction of atmospheric organic aerosols, however, little knowledge about the hygroscopic behavior of these particles is known. In this study, the hygroscopic behavior of oxalic acid and atmospherically relevant oxalates (H2C2O4, (NH4)2C2O4, CaC2O4, and FeC2O4) were studied by Raman spectrometry and vapor sorption analyzer. Under ambient relative humidity (RH) of 10-90%, oxalic acid and these oxalates hardly deliquesce and exhibit low hygroscopicity, however, transformation between anhydrous and hydrated particles was observed during the humidifying and dehumidifying processes. During the water adsorption process, conversion of anhydrous H2C2O4, (NH4)2C2O4, CaC2O4, and FeC2O4 to their hydrated particles (i.e., H2C2O4·2H2O, (NH4)2C2O4·H2O, CaC2O4·H2O, and FeC2O4·2H2O) occurred at about 20% RH, 55% RH, 10% RH, and 75% RH, respectively. Uptake of water on hydrated Ca-oxalate and Fe-oxalate particles can be described by a multilayer adsorption isotherm. During the dehumidifying process, dehydration of H2C2O4·2H2O and (NH4)2C2O4·H2O occurred at 5% RH while CaC2O4·H2O and FeC2O4·2H2O did not undergo dehydration. These results implied that hydrated particles represent the most stable state of oxalic acid and oxalates in the atmosphere. In addition, the assignments of Raman shift bands in the range of 1610-1650 cm-1 were discussed according to the hygroscopic behavior measurement results.

  4. A review of plutonium oxalate decomposition reactions and effects of decomposition temperature on the surface area of the plutonium dioxide product

    Science.gov (United States)

    Orr, R. M.; Sims, H. E.; Taylor, R. J.

    2015-10-01

    Plutonium (IV) and (III) ions in nitric acid solution readily form insoluble precipitates with oxalic acid. The plutonium oxalates are then easily thermally decomposed to form plutonium dioxide powder. This simple process forms the basis of current industrial conversion or 'finishing' processes that are used in commercial scale reprocessing plants. It is also widely used in analytical or laboratory scale operations and for waste residues treatment. However, the mechanisms of the thermal decompositions in both air and inert atmospheres have been the subject of various studies over several decades. The nature of intermediate phases is of fundamental interest whilst understanding the evolution of gases at different temperatures is relevant to process control. The thermal decomposition is also used to control a number of powder properties of the PuO2 product that are important to either long term storage or mixed oxide fuel manufacturing. These properties are the surface area, residual carbon impurities and adsorbed volatile species whereas the morphology and particle size distribution are functions of the precipitation process. Available data and experience regarding the thermal and radiation-induced decompositions of plutonium oxalate to oxide are reviewed. The mechanisms of the thermal decompositions are considered with a particular focus on the likely redox chemistry involved. Also, whilst it is well known that the surface area is dependent on calcination temperature, there is a wide variation in the published data and so new correlations have been derived. Better understanding of plutonium (III) and (IV) oxalate decompositions will assist the development of more proliferation resistant actinide co-conversion processes that are needed for advanced reprocessing in future closed nuclear fuel cycles.

  5. PEG capped CaS nanoparticles synthesized by wet chemical co-precipitation method

    Science.gov (United States)

    Rekha, S.; Anila, E. I.

    2018-04-01

    Calcium sulfide (CaS) nanoparticles capped with polyethyleneglycol (PEG) were synthesized using wet chemical co-precipitation method. The structural and optical properties of the prepared sample were studied by X-ray diffractogram (XRD), transmission electron microscopy (TEM), diffuse reflectance spectrum (DRS) and photoluminescence (PL) spectrum. The structure of CaS nanoparticles is cubic as demonstrated by the X-ray powder diffraction (XRD) and selected area electron diffraction (SAED) analysis. TEMimage revealed the spherical morphology of the particles with diameter in the range 15-20 nm. The optical band gap of the prepared sample was determined from the DRS and its value was found to be 4.1 eV. The PL studies showed that the relative intensity of the PEG capped CaS nanoparticles was higher than that of uncapped CaS nanoparticles. The presence of various functional groups in the capped samples were examined by Fourier Transform Infrared (FTIR) spectroscopy.

  6. Effect of Gallium and Indium Co-Substituting on Upconversion Properties of Er/Yb:Yttrium Aluminum Garnet Powders Prepared by the Co-Precipitation Method.

    Science.gov (United States)

    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+.

  7. Evidence for a cytoplasmic pathway of oxalate biosynthesis in Aspergillus niger

    International Nuclear Information System (INIS)

    Kubicek, C.P.; Schreferl-Kunar, G.; Woehrer, W.; Roehr, M.

    1988-01-01

    Oxalate accumulation of up to 8 g/liter was induced in Aspergillus niger by shifting the pH from 6 to 8. This required the presence of P/sub i/ and a nitrogen source and was inhibited by the protein synthesis inhibitor cycloheximide. Exogenously added 14 CO 2 was not incorporated into oxalate, but was incorporated into acetate and malate, thus indicating the biosynthesis of oxalate by hydrolytic cleavage of oxaloacetate. Inhibition of mitochondrial citrate metabolism by fluorocitrate did not significantly decrease the oxalate yield. The putative enzyme that was responsible for this oxaloacetate hydrolase (EC 3.7.1.1), which was induced de novo during the pH shift. Subcellular fractionation of oxalic acid-forming mycelia of A. niger showed that this enzyme is located in the cytoplasm of A. niger. The results are consistent with a cytoplasmic pathway of oxalate formation which does not involve the tricarboxylic acid cycle

  8. Phase pure synthesis of BiFeO3 nanopowders using diverse precursor via co-precipitation method

    International Nuclear Information System (INIS)

    Shami, M. Yasin; Awan, M.S.; Anis-ur-Rehman, M.

    2011-01-01

    Highlights: → Synthesized phase pure BiFeO 3 using diverse precursor by co-precipitation method. → Optimized synthesis and processing parameters. → Thermal behavior, structure and microstructure were analyzed. → Resistivity vs temperature and dielectric constant vs frequency were measured. → Multiferroicity at room temperature was confirmed by M-H and P-E loops. - Abstract: Amorphous powder of BiFeO 3 (BFO) was synthesized at low-temperature (80 deg. C) by co-precipitation method. Optimal synthesis conditions for phase pure BFO were obtained. Powders were calcined in the temperature range from 400 to 600 deg. C for 1 h. Iso-statically pressed powder was sintered at 500 deg. C for 2 h. Differential scanning calorimetric thermo-gram guided for phase transition, crystallization and melting temperatures. X-ray diffraction confirmed the amorphous nature of as synthesized powder and phase formation of calcined powders. Calcination at temperature ≥400 deg. C resulted in nano crystalline powders with perovskite structure. Average crystallite size increased with the increase in calcination temperature. Scanning electron microscopic studies revealed dense granular microstructure of the sintered samples. The sintered samples exhibited high dc resistivity at room temperature which decreased with the increase in temperature. Dielectric constant, dielectric loss tangent and ac conductivity measurements were carried out in the frequency range (10 Hz to 2 MHz). The samples responded weak electric and magnetic polarization at room temperature with unsaturated and hysteresis free loops, respectively.

  9. Radiolysis of titanium potassium oxalate in aqueous solution. [. gamma. rays

    Energy Technology Data Exchange (ETDEWEB)

    Bundo, Y; Ono, I [Industrial Research Inst. of Kanagawa Prefecture, Yokohama (Japan); Ogawa, T

    1975-01-01

    The dissolution state of titanium potassium oxalate in aqueous solution is different according to the pH. The yellowish brown titanium complex produced by the reaction of titanium potassium oxalate and hydrogen peroxide seems to be different in its structure according to the pH. Considering these points, gamma-ray irradiation was carried out on the sample by dissolving titanium potassium oxalate in purified water under the conditions of oxygen saturation and nitrogen saturation, and the relation between irradiation dose and the production of titanium complex was determined. On the basis of the experimental result, the mechanism of forming hydrogen peroxide was presumed. The radiation source used was 2,000 Ci of /sup 60/Co. For photometric analysis, a 139 type photoelectric spectrophotometer of Hitachi Ltd. was used. From the experimental results, in neutral water, titanium potassium oxalate exists in the state that two oxalic acid ions are coordinated to titanyl ion, while in case of the pH lowered by the addition of sulfuric acid, it can exist in the state that one oxalic acid ion is coordinated to titanyl ion. The yield of hydrogen peroxide produced by irradiating titanium potassium oxalate aqueous solution with gamma-ray is the sum of the molecular product from water and the radiolysis product from titanium potassium oxalate.

  10. CO2-Free Power Generation on an Iron Group Nanoalloy Catalyst via Selective Oxidation of Ethylene Glycol to Oxalic Acid in Alkaline Media

    Science.gov (United States)

    Matsumoto, Takeshi; Sadakiyo, Masaaki; Ooi, Mei Lee; Kitano, Sho; Yamamoto, Tomokazu; Matsumura, Syo; Kato, Kenichi; Takeguchi, Tatsuya; Yamauchi, Miho

    2014-07-01

    An Fe group ternary nanoalloy (NA) catalyst enabled selective electrocatalysis towards CO2-free power generation from highly deliverable ethylene glycol (EG). A solid-solution-type FeCoNi NA catalyst supported on carbon was prepared by a two-step reduction method. High-resolution electron microscopy techniques identified atomic-level mixing of constituent elements in the nanoalloy. We examined the distribution of oxidised species, including CO2, produced on the FeCoNi nanoalloy catalyst in the EG electrooxidation under alkaline conditions. The FeCoNi nanoalloy catalyst exhibited the highest selectivities toward the formation of C2 products and to oxalic acid, i.e., 99 and 60%, respectively, at 0.4 V vs. the reversible hydrogen electrode (RHE), without CO2 generation. We successfully generated power by a direct EG alkaline fuel cell employing the FeCoNi nanoalloy catalyst and a solid-oxide electrolyte with oxygen reduction ability, i.e., a completely precious-metal-free system.

  11. Fabrication, spark plasma consolidation, and thermoelectric evaluation of nanostructured CoSb3

    DEFF Research Database (Denmark)

    Khan, A.; Saleemi, M.; Johnsson, M.

    2014-01-01

    Nanostructured powders of thermoelectric (TE) CoSb3 compounds were synthesized using a chemical alloying method. This method involved co-precipitation of oxalate precursors in aqueous solution with controlled pH, followed by thermochemical treatments including calcination and reduction to produce...... stoichiometric nanostructured CoSb3. Moreover, CoSb 3 nanoparticles were consolidated by spark plasma sintering (SPS) with a very brief processing time. Very high compaction densities (>95%) were achieved and the grain growth was almost negligible during consolidation. An iterative procedure was developed...... to minimize the grain growth while achieving sufficient densification. Grain sizes in the range of 500 nm to 1 μm, with compaction density of 95-98% were obtained. Preliminary measurements of thermal diffusivity and conductivity showed the dependence on grain size as well as on porosity. TE transport...

  12. Impact of Precipitants on the Structure and Properties of Fe-Co-Ce Composite Catalysts

    Directory of Open Access Journals (Sweden)

    Yongli Zhang

    2016-01-01

    Full Text Available Fe-Co-Ce composite catalysts were prepared by coprecipitation method using CO(NH22, NaOH, NH4HCO3, and NH3·H2O as precipitant agents. The effects of the precipitant agents on the physicochemical properties of the Fe-Co-Ce based catalysts were investigated by SEM, TEM, BET, TG-DTA, and XRD. It was found that the precipitant agents remarkably influenced the morphology and particle size of the catalysts and affected the COD removal efficiency, decolorization rate, and pH of methyl orange for catalytic wet air oxidation (CWAO. The specific surface area of the Fe-Co-Ce composite catalysts successively decreased in the order of NH3·H2O, NH4HCO3, NaOH, and CO(NH22, which correlated to an increasing particle size that increased for each catalyst. For the CWAO of a methyl orange aqueous solutions, the effects of precipitant agents NH3·H2O and NaOH were superior to those of CO(NH22 and NH4HCO3. The catalyst prepared using NH3·H2O as the precipitant agent was mostly composed of Fe2O3, CoO, and CeO2. The COD removal efficiency of methyl orange aqueous solution for NH3·H2O reached 92.9% in the catalytic wet air oxidation. Such a catalytic property was maintained for six runs.

  13. Effect of preparation conditions on Nickel Zinc Ferrite nanoparticles: A comparison between sol–gel auto combustion and co-precipitation methods

    Directory of Open Access Journals (Sweden)

    Manju Kurian

    2016-09-01

    Full Text Available The experimental conditions used in the preparation of nano crystalline mixed ferrite materials play an important role in the particle size of the product. In the present work a comparison is made on sol–gel auto combustion methods and co-precipitation methods by preparing Nickel Zinc Ferrite (Ni0.5Zn0.5Fe2O4 nano particles. The prepared ferrite samples were calcined at different temperatures and characterized by using standard methods. X-ray diffraction analysis indicated the formation of single phase ferrite nanoparticles for samples calcined at 500 °C. The lattice parameter range of 8.32–8.49 Å confirmed the cubic spinel structure. Average crystallite size estimated from X-ray diffractogram was found to be between 17 and 40 nm. The IR spectra showed two main absorption bands, the high frequency band ν1 around 600 cm−1 and the low frequency band ν2 around 400 cm−1 arising from tetrahedral (A and octahedral (B interstitial sites in the spinel lattice. TEM pictures showed particles in the nanometric range confirming the XRD data. The studies revealed that the sol–gel auto combustion method was superior to the co-precipitation method for producing single phase nano particles with smaller crystallite size.

  14. Evidence for a cytoplasmic pathway of oxalate biosynthesis in Aspergillus niger

    Energy Technology Data Exchange (ETDEWEB)

    Kubicek, C.P.; Schreferl-Kunar, G.; Woehrer, W.; Roehr, M.

    1988-03-01

    Oxalate accumulation of up to 8 g/liter was induced in Aspergillus niger by shifting the pH from 6 to 8. This required the presence of P/sub i/ and a nitrogen source and was inhibited by the protein synthesis inhibitor cycloheximide. Exogenously added /sup 14/CO/sub 2/ was not incorporated into oxalate, but was incorporated into acetate and malate, thus indicating the biosynthesis of oxalate by hydrolytic cleavage of oxaloacetate. Inhibition of mitochondrial citrate metabolism by fluorocitrate did not significantly decrease the oxalate yield. The putative enzyme that was responsible for this oxaloacetate hydrolase (EC 3.7.1.1), which was induced de novo during the pH shift. Subcellular fractionation of oxalic acid-forming mycelia of A. niger showed that this enzyme is located in the cytoplasm of A. niger. The results are consistent with a cytoplasmic pathway of oxalate formation which does not involve the tricarboxylic acid cycle.

  15. Oxalic acid overproduction by copper-tolerant brown-rot basidiomycetes on southern yellow pine treated with copper-based preservatives

    Science.gov (United States)

    Carol A. Clausen; Frederick Green

    2003-01-01

    Accumulation of oxalic acid (OA) by brown-rot fungi and precipitation of copper oxalate crystals in wood decayed by copper-tolerant decay fungi has implicated OA in the mechanism of copper tolerance. Understanding the role of OA in copper tolerance is important due to an increasing reliance on copper-based wood preservatives. In this study, four copper-tolerant brown-...

  16. Simplified method for the determination of strontium-90 in large amounts of bone-ash; Methode simplifiee de dosage du strontium 90 sur des quantites importantes de cendres d'os

    Energy Technology Data Exchange (ETDEWEB)

    Patti, F; Jeanmaire, L [Commissariat a l' Energie Atomique, Fontenay-aux-roses (France). Centre d' Etudes Nucleaires

    1966-06-01

    The principle of the determination is based on a 3-step process: 1) concentrating the strontium by attacking the ash with nitric acid; 2) elimination of residual phosphoric ions by a double precipitation of strontium oxalate; and 3) extraction of yttrium 90, counted in the oxalate form. The advantages of the method: -) using simple techniques it makes it possible to process 50 g of ash; -) the initial concentration of strontium considerably reduces the volume of the solutions as well as the size of precipitates handled. Fuming nitric acid is used in a specially designed burette. (authors) [French] Le principe du dosage repos sur un procede en 3 etapes: 1) Concentration du strontium par une attaque nitrique des cendres; 2) Elimination des ions phosphoriques restants par une double precipitation de l'oxalate de strontium. 3) Extraction de l'yttrium 90, compte sous forme d'oxalate. Interet de la methode: dans des conditions techniques simples, elle permet le traitement de 50 g de cendres d'os; la concentration initiale du strontium reduit notablement le volume des solutions ainsi que l'importance des precipites manipules. L'acide nitrique fumant est utilise par l'intermediaire d'une burette specialement concue a cet effet.

  17. Two New Families of Lanthanide Mixed-Ligand Complexes, Oxalate-Carbonate and Oxalate-Formate: Synthesis and Structure of [Ce(H 2O)] 2(C 2O 4) 2(CO 3)·2.5 H 2O and Ce(C 2O 4)(HCO 2)

    Science.gov (United States)

    Romero, S.; Mosset, A.; Trombe, J. C.

    1996-12-01

    Two new families of lanthanide complexes associating the ligands oxalate and carbonate or oxalate and formate have been prepared under autogenous pressure at 200°C using a pseudo-hydrothermal method. The two families have been extended to some lanthanides ( Ln): oxalate-carbonate Ln= Ce, Pr, Nd, and Eu; oxalate-formate Ln= La, Ce, and Sm. The starting suspension contains either oxalate or a mixture of oxalate and oxalic acid. The structures have been solved for the element cerium. In both cases, the structure is built up from cerium atoms sharing all their oxygen atoms with oxalate and carbonate or oxalate and formate ligands, thus forming a three-dimensional network. The cerium polyhedra share either faces or edges or corners. The coordination scheme of the oxalate ligands is variable: bischelating, bischelating and monodentate, or bischelating and bismonodentate. The carbonate group acts as a bischelating and bismonodentate ligand while the formate group is chelating and monodentate. The characterization of these two original families by infrared spectra and thermal behavior is presented for some pure phases. A tentative explanation of the synthesis of these two phases will be emphasized.

  18. The crystal structure of paramagnetic copper(ii) oxalate (CuC2O4):

    DEFF Research Database (Denmark)

    Christensen, Axel Nørlund; Lebech, Bente; Andersen, Niels Hessel

    2014-01-01

    Synthetic copper(ii) oxalate, CuC2O4, was obtained in a precipitation reaction between a copper(ii) solution and an aqueous solution of oxalic acid. The product was identified from its conventional X-ray powder patterns which match that of the copper mineral Moolooite reported to have...... the composition CuC2O4·0.44H2O. Time resolved in situ investigations of the thermal decomposition of copper(ii) oxalate using synchrotron X-ray powder diffraction showed that in air the compound converts to Cu2O at 215 °C and oxidizes to CuO at 345 °C. Thermo gravimetric analysis performed in an inert Ar....... The crystal structure consists of a random stacking of CuC2O4 micro-crystallites where half the Cu-atoms are placed at (2a) and the other half at (2b) positions with the corresponding oxalate molecules centred around the corresponding (2b) and (2a) site positions, respectively. The diffraction patterns...

  19. Synthesis, Characterization, and Atenolol Delivery Application of Functionalized Mesoporous Hydroxyapatite Nanoparticles Prepared by Microwave-Assisted Co-precipitation Method.

    Science.gov (United States)

    Mortazavi-Derazkola, Sobhan; Naimi-Jamal, Mohammad Reza; Ghoreishi, Seyedeh Masoumeh

    2016-01-01

    Atenolol has been used to treat angina and hypertension, either alone or with other antihypertensives. Despite its usefulness, it shows some side effects such as diarrhea and nausea in some patients. A method for slow release of atenolol in intestine is helpful to prevent such side effects. A facile co-precipitation microwave-assisted method was used to fabricate mesoporous hydroxyapatite nanoparticles (mHAp). It was then functionalized to have SO3H groups. The synthesized material was used for storage/slow release study of atenolol. Atenolol loaded mHAp shows immediate release of atenolol in pH 8, whileafter functionalizing shows up to ca. 30% release at the beginning. In pH 1, 50% of drug was released after 10 h from AT@mHAp and after 18h the drug was almost completely released.The drug release profiles of functionalized HAp at pH value 1 and 8reveals the complete release of atenolol in intestine pH, while no complete release is observed in stomach environment. The aims of this work were synthesis and characterization of mesoporous HAp through the microwave-assisted co-precipitation method and elucidate the underlying drug release capability of mesoporous HAp nanoparticles. The SO3H group was incorporated into the mesoporous HAp and then used as drug delivery carriers using atenolol as a model drug to investigate their drug storage/release properties in simulated body fluid (SBF). Increasing pH value to 8 causes increase in the drug release.

  20. Response of soil CO2 efflux to precipitation manipulation in a semiarid grassland.

    Science.gov (United States)

    Wei, Xiaorong; Zhang, Yanjiang; Liu, Jian; Gao, Hailong; Fan, Jun; Jia, Xiaoxu; Cheng, Jimin; Shao, Mingan; Zhang, Xingchang

    2016-07-01

    Soil CO2 efflux (SCE) is an important component of ecosystem CO2 exchange and is largely temperature and moisture dependent, providing feedback between C cycling and the climate system. We used a precipitation manipulation experiment to examine the effects of precipitation treatment on SCE and its dependences on soil temperature and moisture in a semiarid grassland. Precipitation manipulation included ambient precipitation, decreased precipitation (-43%), or increased precipitation (+17%). The SCE was measured from July 2013 to December 2014, and CO2 emission during the experimental period was assessed. The response curves of SCE to soil temperature and moisture were analyzed to determine whether the dependence of SCE on soil temperature or moisture varied with precipitation manipulation. The SCE significantly varied seasonally but was not affected by precipitation treatments regardless of season. Increasing precipitation resulted in an upward shift of SCE-temperature response curves and rightward shift of SCE-moisture response curves, while decreasing precipitation resulted in opposite shifts of such response curves. These shifts in the SCE response curves suggested that increasing precipitation strengthened the dependence of SCE on temperature or moisture, and decreasing precipitation weakened such dependences. Such shifts affected the predictions in soil CO2 emissions for different precipitation treatments. When considering such shifts, decreasing or increasing precipitation resulted in 43 or 75% less change, respectively, in CO2 emission compared with changes in emissions predicted without considering such shifts. Furthermore, the effects of shifts in SCE response curves on CO2 emission prediction were greater during the growing than the non-growing season. Copyright © 2016. Published by Elsevier B.V.

  1. Co-precipitation of loperamide hydrochloride and polyethylene glycol using aerosol solvent extraction system

    International Nuclear Information System (INIS)

    Widjojokusumo, Edward; Youn, Yong-Suk; Lee, Youn-Woo; Veriansyah, Bambang; Tjandrawinata, Raymond Rubianto

    2013-01-01

    The co-precipitation of loperamide hydrochloride (LPM) and polyethylene glycol (PEG) using aerosol solvent extraction system (ASES) was examined. Scanning electron microscopy - energy dispersive X-ray spectroscopy (SEM-EDS) analysis showed that the co-precipitation was achieved in various LPM-PEG mass ratios with changes in its morphology. In 10-50% PEG mass ratios, angular-shaped particles were formed, whereas in 65-90% PEG mass ratios, irregular-shaped particles were formed. X-ray diffraction (XRD) analysis of the co-precipitates revealed that the LPM retained amorphous structure, while, on the other hand, the PEG retained crystalline structure. Fourier transform infrared (FT-IR) spectra indicated carbonyl function group of LPM and ether function group of PEG appeared in the co-precipitates. Results of a dissolution test showed that the co-precipitates of LPM-PEG had higher dissolution rate compared to that of the raw material and processed LPM with ASES. Taken together, the co-precipitation of LPMPEG was achieved using ASES and higher in its dissolution rate

  2. Towards deriving Ni-rich cathode and oxide-based anode materials from hydroxides by sharing a facile co-precipitation method.

    Science.gov (United States)

    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.

  3. Hydroxyproline Metabolism and Oxalate Synthesis in Primary Hyperoxaluria.

    Science.gov (United States)

    Fargue, Sonia; Milliner, Dawn S; Knight, John; Olson, Julie B; Lowther, W Todd; Holmes, Ross P

    2018-06-01

    Background Endogenous oxalate synthesis contributes to calcium oxalate stone disease and is markedly increased in the inherited primary hyperoxaluria (PH) disorders. The incomplete knowledge regarding oxalate synthesis complicates discovery of new treatments. Hydroxyproline (Hyp) metabolism results in the formation of oxalate and glycolate. However, the relative contribution of Hyp metabolism to endogenous oxalate and glycolate synthesis is not known. Methods To define this contribution, we performed primed, continuous, intravenous infusions of the stable isotope [ 15 N, 13 C 5 ]-Hyp in nine healthy subjects and 19 individuals with PH and quantified the levels of urinary 13 C 2 -oxalate and 13 C 2 -glycolate formed using ion chromatography coupled to mass detection. Results The total urinary oxalate-to-creatinine ratio during the infusion was 73.1, 70.8, 47.0, and 10.6 mg oxalate/g creatinine in subjects with PH1, PH2, and PH3 and controls, respectively. Hyp metabolism accounted for 12.8, 32.9, and 14.8 mg oxalate/g creatinine in subjects with PH1, PH2, and PH3, respectively, compared with 1.6 mg oxalate/g creatinine in controls. The contribution of Hyp to urinary oxalate was 15% in controls and 18%, 47%, and 33% in subjects with PH1, PH2, and PH3, respectively. The contribution of Hyp to urinary glycolate was 57% in controls, 30% in subjects with PH1, and synthesis in individuals with PH2 and PH3. In patients with PH1, who have the highest urinary excretion of oxalate, the major sources of oxalate remain to be identified. Copyright © 2018 by the American Society of Nephrology.

  4. Protection of metal artefacts with the formation of metal-oxalates complexes by Beauveria bassiana.

    Directory of Open Access Journals (Sweden)

    Edith eJoseph

    2012-01-01

    Full Text Available Several fungi present high tolerance to toxic metals and some are able to transform metals into metal-oxalate complexes. In this study, the ability of Beauveria bassiana to produce copper oxalates was evaluated in vitro. Growth performance was tested on various copper-containing media. B. bassiana proved highly resistant to copper, tolerating concentrations of up to 20 g.L-1, and precipitating copper oxalates on all media tested. Chromatographic analyses showed that this species produced oxalic acid as sole metal chelator. The production of metal-oxalates can be used in the restoration and conservation of archaeological and modern metal artefacts. The production of copper-oxalates was confirmed directly using metallic pieces (both archaeological and modern. The conversion of corrosion products into copper oxalates was demonstrated as well. In order to assess whether the capability of B. bassiana to produce metal-oxalates could be applied to other metals, iron and silver were tested as well. Iron appears to be directly sequestered in the wall of the fungal hyphae forming oxalates and probably goethite. However, the formation of a homogeneous layer on the object is not yet optimal. Silver nitrate was extracellularly reduced into nanoparticles of elemental silver by an unknown mechanism. The production of copper oxalates is immediately applicable for the conservation of copper-based artefacts. For iron and silver this is not yet the case. However, the vast ability of B. bassiana to transform toxic metals using different immobilization mechanisms seems to offer considerable possibilities for industrial applications, such as the bioremediation of contaminated soils or the green synthesis of chemicals.

  5. 228Ra and 226Ra measurement on a BaSO4 co-precipitation source

    International Nuclear Information System (INIS)

    Medley, Peter; Martin, Paul; Bollhöfer, Andreas; Parry, David

    2015-01-01

    One of the most commonly-used methods for determination of 226 Ra, particularly in water samples, utilises co-precipitation of Ra with BaSO 4 , followed by microfiltration to produce a source for alpha counting. This paper describes two extensions to BaSO 4 co-precipitation methods which enable determination of 228 Ra using the same source. The adaptations presented here do not introduce any contaminants that will affect the separation of radium or alpha counting for 226 Ra, and can be used for re-analysis of already existing sources prepared by BaSO 4 co-precipitation. The first adaptation uses detection of 228 Ac on the source by gamma spectrometry. The detection efficiency is high, allowing analysis of water samples at sufficiently low activity to be suitable in testing for compliance with drinking water quality standards. As 228 Ac grows in quickly, taking less than 2 days to reach equilibrium with the 228 Ra parent, this can also be useful in radiological emergency response situations. The second adaptation incorporates a method for the digestion of BaSO 4 sources, allowing separation of thorium and subsequent determination of 228 Th activity. Although ingrowth periods for 228 Th can be lengthy, very low detection limits for 228 Ra can be achieved with this technique. - Highlights: • We developed two methods for 228 Ra measurement on Ba(Ra)SO 4 co-precipitation sources. • Measurement by gamma spectrometry using the daughter 228 Ac is rapid. • Detection limits are suitable for assessment of drinking water quality. • The second approach uses alpha spectrometry on a separated Th fraction. • This is more sensitive than gamma spectrometry after an ingrowth period greater than about 1 month

  6. Charge dynamics in conducting polyaniline–metal oxalate composites

    Indian Academy of Sciences (India)

    Unknown

    Polyaniline; metal oxalate composites; charge transport; mobile and fixed spins; VRH conduc- tion mechanism ... Al, Mn and Co on doping into Pani improve the poly- merization ... dopants on charge dynamics with EPR and other tech- niques.

  7. Characterization of γ- Al2O3 nanopowders synthesized by Co-precipitation method

    International Nuclear Information System (INIS)

    Jbara, Ahmed S.; Othaman, Zulkafli; Ati, Ali A.; Saeed, M.A.

    2017-01-01

    Co-precipitation technique has been used to synthesize gamma-Al 2 O 3 (γ-Al 2 O 3 ) nanopowders under annealing temperature effect. The crystalline phase and purity for the prepared powder were characterized by different spectroscopy techniques. XRD analysis confirms the gamma phase of alumina nanopowders with particle diameter ranging from 6 to 24 nm, which confirms the quantum dots formation, which is also supported by the BET measurement. The surface area of the prepared nanopowders is in the range of 109–367 m 2 /g. Morphology analysis indicates that γ-Al 2 O 3 nanopowders are consisted of grains almost spherical in shape. Some agglomeration of nanoparticles occurs, which become more regular hexagonal shaped with the increasing annealing temperature. The small nanoparticles size and the high surface area from a simple procedure for preparing γ-Al 2 O 3 may make it more suitable for use as an adsorbent for malachite green. - Highlights: • Co-precipitation technique is used to synthesize gamma- Al 2 O 3 nanopowders. • Pure gamma- Al 2 O 3 phase was obtained having maximum nanoparticle size is 24 nm. • The quantum dots were formed inside powder. • High surface area of nanopowders at the low annealing temperature. • Increasing annealing temperature causes the hexagonal agglomeration shape.

  8. Development, evaluation and optimization of superparamagnetite nanoparticles prepared by co-precipitation method.

    Science.gov (United States)

    Montaseri, Hashem; Alipour, Shohreh; Vakilinezhad, Molood Alsadat

    2017-08-01

    Magnetic nanoparticles (MNPs) are of high interest due to their application in medical fields, in particular for theranostics. Specific properties required for such particles include high magnetization, appropriate size and stability. Biocompatible magnetically soft magnetite particles (Fe 3 O 4 ) have been investigated for biological purposes. The intrinsic instability of these nanoparticles and their susceptibility to the oxidization in air, are limitations for their applications. Various methods have been described for synthesis of these nanoparticles among which co-precipitation method is widely experimented. In order to illustrate the synthesis of MNPs elaborately, the effect of different factors on particle formation were studied. The particles morphology, stability, paramagnetic effect, chemical structure and cytotoxicity were evaluated. Particles of 58 and 60 nm obtained by oleic acid coated (OMNPs) and citric acid coated (CMNPs) magnetite nanoparticles respectively. Transmission electron microscopy images exhibited the real sizes are 15 and 13 nm. Magnetic saturations of these nanoparticles were 72 and 68 emu/g which is suitable for medical applications. Both OMNPs and CMNPs were non-toxic to the SK-Br-3 and MCF-7 cells in the concentrations of <2.5 μg/mL. Since these particles exhibit relatively high magnetic saturation, low dose of such material would be required; therefore, these NPs seem to be suitable for theranostics.

  9. On the americium oxalate solubility

    International Nuclear Information System (INIS)

    Zakolupin, S.A.; Korablin, Eh.V.

    1977-01-01

    The americium oxalate solubility at different nitric (0.0-1 M) and oxalic (0.0-0.4 M) acid concentrations was investigated in the temperature range from 14 to 60 deg C. The dependence of americium oxalate solubility on the oxalic acid concentration was determined. Increasing oxalic acid concentration was found to reduce the americium oxalate solubility. The dependence of americium oxalate solubility on the oxalic acid concentration was noted to be a minimum at low acidity (0.1-0.3 M nitric acid). This is most likely due to Am(C 2 O 4 ) + , Am(C 2 O 4 ) 2 - and Am(C 2 O 4 ) 3 3- complex ion formation which have different unstability constants. On the basis of the data obtained, a preliminary estimate was carried out for the product of americium oxalate solubility in nitric acid medium (10 -29 -10 -31 ) and of the one in water (6.4x10 -20 )

  10. BaTiO3 thick fi lms obtained by tape casting from powders prepared by the oxalate route

    Directory of Open Access Journals (Sweden)

    Adelina Ianculescu

    2009-06-01

    Full Text Available BaTiO3 powders were prepared by co-precipitation via oxalate route. The size, morphology and particle size distribution of the oxalate powders have been optimized by the control of different synthesis parameters during the precipitation reaction (nature of salts, concentration of different solutions, aging time. The single phase BaTiO3 oxide particles were obtained after a thermal decomposition of the as-synthesized powders at 850°C for 4 hours under air atmosphere. Oxide powders with a suitable specifi c surface area were selected in order to obtain thick fi lms by the tape casting technique. The microstructure and dielectric properties of the thick films varied obviously depending on the deposition-calcination-sintering cycle used. A double depositioncalcination cycle followed by sintering, as well as a two step deposition-calcination-sintering procedure was used in order to improve the compactness and therefore, the dielectric behaviour. A higher dielectric constant value (~ 750 and lower dielectric losses (~ 2 % were achieved at room temperature and at 1 kHz frequency for the dense, double-deposited fi lm obtained after two deposition-calcination-sintering cycles. For this film, a superior value of the dielectric constant (~ 1100, almost frequency independent in the frequency range of 100 Hz – 10 kHz was gained also at the ferroelectric-paraelectric phase transition temperature of 130°C.

  11. Study of UO2-10WT%Gd2O3 fuel pellets obtained by seeding method using AUC co-precipitation and mechanical mixing processes

    International Nuclear Information System (INIS)

    Lima, M.M.F.; Ferraz, W.B.A.; Santos, M.M. dos; Pinto, L.C.M.; Santos, A.

    2008-01-01

    The use of gadolinium and uranium mixed oxide as a nuclear fuel aims to obtain a fuel with a performance better than that of UO 2 fuel. In this work, seeding method was used to improve ionic diffusivity during sintering to produce high density pellets containing coarse grains by co-precipitation and mechanical mixing processes. Sintered UO 2 -10 wt% Gd 2 O 3 pellets were obtained using the reference processes with 2 wt% and 5 wt% UO 2 seeds with two granulometries, less than 20 μm and between 20 and 38 μm. Characterisation was carried out by chemical analysis, surface area, X-ray diffraction, SEM, WDS, image analysis, and densitometry. The seeding method using mechanical mixing process was more effective than the co-precipitation method. Furthermore, mechanical mixing process resulted in an increase in density of UO 2 -10wt% Gd 2 O 3 with seeds in relation to that of UO 2 -10wt% Gd 2 O 3 without seeds. (author)

  12. Long-term sustainability of microbial-induced CaCO3 precipitation in aqueous media.

    Science.gov (United States)

    Gat, Daniella; Ronen, Zeev; Tsesarsky, Michael

    2017-10-01

    Microbially induced CaCO 3 precipitation (MICP) via urea hydrolysis is an emerging technique for soil amelioration, building materials rehabilitation and pollutants sequestration amongst other various environmental applications. The successful application of MICP requires the sustainability of the precipitated CaCO 3 ; to which the fate of ammonia, the main by-product of ureolysis, is potentially significante. Ammonia volatilization and biological ammonia oxidation both induce a pH decrease, which, in turn, might cause CaCO 3 dissolution. To examine the potential effect of accumulated ammonia on precipitated CaCO 3 , we conducted a long-term MICP batch experiment, using environmental enrichment cultures of ureolytic bacteria. Here we show that CaCO 3 precipitation was completed within 15-27 days, along with a rise in ammonium concentration. Following completion of ureolysis and precipitation, ammonium concentrations decreased, leading to a pH decrease. About 30 days after precipitation was completed, as much as 30% CaCO 3 dissolution, was observed. A two-step model, describing urea hydrolysis followed by the removal of ammonia from the precipitation solution, predicted CaCO 3 dissolution due to ammonia volatilization. We suggest that ureolytic MICP might result in ammonia volatilization, leading to significant CaCO 3 dissolution. These results provide basic insights into the sustainability of ureolytic MICP and should further encourage removal of the accumulated ammonia from the treated site. Copyright © 2017 Elsevier Ltd. All rights reserved.

  13. Effects of Calcium Source on Biochemical Properties of Microbial CaCO3 Precipitation.

    Science.gov (United States)

    Xu, Jing; Du, Yali; Jiang, Zhengwu; She, Anming

    2015-01-01

    The biochemical properties of CaCO3 precipitation induced by Sporosarcina pasteurii, an ureolytic type microorganism, were investigated. Effects of calcium source on the precipitation process were examined, since calcium source plays a key role in microbiologically induced mineralization. Regardless of the calcium source type, three distinct stages in the precipitation process were identified by Ca(2+), NH4 (+), pH and cell density monitoring. Compared with stage 1 and 3, stage 2 was considered as the most critical part since biotic CaCO3 precipitation occurs during this stage. Kinetics studies showed that the microbial CaCO3 precipitation rate for calcium lactate was over twice of that for calcium nitrate, indicating that calcium lactate is more beneficial for the cell activity, which in turn determines urease production and CaCO3 precipitation. X-ray diffraction analysis confirmed the CaCO3 crystal as calcite, although scanning electron microscopy revealed a difference in crystal size and morphology if calcium source was different. The findings of this paper further suggest a promising application of microbiologically induced CaCO3 precipitation in remediation of surface and cracks of porous media, e.g., cement-based composites, particularly by using organic source of calcium lactate.

  14. CO2 (carbon dioxide) fixation by applying new chemical absorption-precipitation methods

    International Nuclear Information System (INIS)

    Park, Sangwon; Lee, Min-Gu; Park, Jinwon

    2013-01-01

    CO 2 (carbon dioxide) is the most common greenhouse gas and most of it is emitted from human activities. The methods for CO 2 emission reduction can be divided into physical, chemical, and biochemical methods. Among the physical and chemical methods, CCS (carbon capture and storage) is a well-known reducing technology. However, this method has many disadvantages including the required storage area. In general, CCS requires capture and storage processes. In this study, we propose a method for reusing the absorbed CO 2 either in nature or in industry. The emitted CO 2 was converted into CO 3 2− using a conversion solution, and then made into a carbonate by combining the conversion solution with metal ions at normal temperature and pressure. The resulting carbonate was analyzed using FT-IR (Fourier transform infrared spectroscopy) and XRD (X-ray diffraction). We verified the formation of a solid consisting of calcite and vaterite. In addition, the conversion solution that was used could be reused in the same process of CCS technology. Our study demonstrates a successful method of reducing and reusing emitted CO 2 , thereby making CO 2 a potential future resource. - Highlights: • This study focused on a new CO 2 fixation process method. • In CCS technology, the desorption process requires high thermal energy consumption. • This new method does not require a desorption process because the CO 2 is accomplished through CaCO 3 crystallization. • A new absorption method is possible instead of the conventional absorption-desorption process. • This is not only a rapid reaction for fixing CO 2 , but also economically feasible

  15. Supercritical antisolvent co-precipitation of rifampicin and ethyl cellulose

    CSIR Research Space (South Africa)

    Djerafi, R

    2017-05-01

    Full Text Available . Using the solvent mixture, co-precipitates with particle sizes ranging between 190 and 230 nm 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...

  16. Structure and electrochemical properties of Mg2SnO4 nanoparticles synthesized by a facile co-precipitation method

    International Nuclear Information System (INIS)

    Tang, Hao; Cheng, Cuixia; Yu, Gaige; Liu, Haowen; Chen, Weiqing

    2015-01-01

    Nanosized Mg 2 SnO 4 has been synthesized by a facile co-precipitation method. The structure and morphology of the as-prepared samples are characterized by X-ray diffraction (XRD), X-ray photoelectron spectrometer (XPS), fourier Transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). It is found that Mg 2 SnO 4 sample is very sensitive to the aging time of the precursor. The single phase Mg 2 SnO 4 nanoparticles with ∼23 nm can be obtained at 900 °C using the aging 35 min percusor as source. The electrochemical properties of the powder obtained at 900 °C are investigated by galvanostatic discharge-charge tests and cyclic voltammograms (CVs). The initial specific discharge capacity reaches as high as 927.7 mAh g −1 at 0.2 mA cm −2 in 0.05–3.0 V, which indicates that Mg 2 SnO 4 nanoparticles could be a promising candidate of anode material for Li-ion batteries. - Highlights: • Nanosized Mg 2 SnO 4 has been synthesized by a facile co-precipitation method. • We find that Mg 2 SnO 4 sample is very sensitive to the ageing time of the precursor. • The single phase Mg 2 SnO 4 nanoparticles with about 23 nm can be obtained by calcining the ageing 35 min percusor at 900 °C. • The obtained powders show a better electrochemical performance

  17. The use of microemulsions for the synthesis of oxalate precursors of YBaCuO superconduction oxide

    International Nuclear Information System (INIS)

    Wang, L.; Zhang, Y.; Muhammed, M.

    1992-01-01

    Although emulsion technique has been used as an advanced separation method, little attention has been paid to the particular feature of emulsions as a powerful reaction media for synthesis of powders, e.g., precipitation of fine particles. In the present paper, the authors report the use of some microemulsion systems as a reaction media in a controlled coprecipitation of the oxalate precursors of superconducting YBa 2 Cu 3 O 7-δ ceramics. The phase diagram of the system: oil (hydrocarbon) - surfactant (Aerosol Orange T) - water, in the absence and presence of nitric/oxalic acids and nitrates, have been systematically investigated. Several hydrocarbons, n-hexane, n-haptene and n-octane have been tested. The different stability regions of microemulsions have been determined. The oxalate coprecipitation of Y, Ba and Cu from nitrate solution was studied under various operating conditions, pH, ratio of oil/surfactant/water and ratio of Y/Ba/Cu/.H 2 C 2 O 4 2 . The chemical and morphological properties of the oxalate powders obtained in the microemulsion systems have been examined by different techniques, e.g., ICP, TGA, XRD and SEM. By XRD, the optimum products are found to be amorphous oxalate composite with exact required stoichiometry and high homogeneity. The average size of the dispersed particles is 50-70 nm while the mean diameter of the agglomerates is around 300 nm. The best sinters bulk sample has T, (R = 0) at 92 K. These powders are used as fine precursors for the synthesis of high T c superconducting ceramics as bulk material and particularly thick films

  18. Gadolinium-doped ceria nanopowders synthesized by urea-based homogeneous co-precipitation (UBHP)

    Energy Technology Data Exchange (ETDEWEB)

    Accardo, G., E-mail: d16605@kist.re.kr [Fuel Cell Research Center, Korea Institute of Science and Technology, Hwarangno 14-gil, Seongbuk-gu, Seoul 136-791 (Korea, Republic of); Spiridigliozzi, L. [Department of Civil and Mechanical Engineering, INSTM Research Unit, University of Cassino and Southern Lazio, Via G. Di Biasio 43, 03043 Cassino, FR (Italy); Cioffi, R.; Ferone, C. [Department of Engineering, INSTM Research Unit, University Parthenope of Naples, Centro Direzionale, Is. C4, 80143 Napoli (Italy); Di Bartolomeo, E. [Department of Chemical Science and Technology, University of Rome “Tor Vergata”, Viale della Ricerca Scientifica, 00133 Rome (Italy); Yoon, Sung Pil [Fuel Cell Research Center, Korea Institute of Science and Technology, Hwarangno 14-gil, Seongbuk-gu, Seoul 136-791 (Korea, Republic of); Dell’Agli, G. [Department of Civil and Mechanical Engineering, INSTM Research Unit, University of Cassino and Southern Lazio, Via G. Di Biasio 43, 03043 Cassino, FR (Italy)

    2017-02-01

    Gadolinium (10%)-doped ceria was successfully synthesized by using an urea-based co-precipitation method (UBHP). A single fluorite phase was obtained after a low temperature (400 °C) calcination treatment. The resulting powders showed grains of nanometric size with some agglomerations and an overall good sinterability. Pellets were sintered at 1300 and 1500 °C for 3 h. The ionic conductivity was measured by electrochemical impedance spectroscopy measurements and a correlation between electrical properties and microstructure was revealed. The promising conductivity values showed that the synthesized powders are suitable for intermediate temperature solid oxide fuel cells (IT-SOFCs) applications. - Highlights: • Urea-based homogeneous co-precipitation is applied to synthesize nanocrystalline GDC. • Dense GDC samples at different sintering temperatures were characterized. • SEM and TEM revealed a well define microstructure and controlled composition. • Correlation between electrochemical properties by EIS and microstructure was discussed. • UBHP method can be used to prepare high performance GDC electrolytes.

  19. Enhanced luminescent properties of long-persistent Sr{sub 2}MgSi{sub 2}O{sub 7}:Eu{sup 2+}, Dy{sup 3+} phosphor prepared by the co-precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Pan Wen [State Key Laboratory of Fine Chemicals, Department of Materials Science and Chemical Engineering, School of Chemical Engineering, Dalian University of Technology, Zhongshan Road 158-43, Dalian Liaoning 116012 (China); Ning Guiling [State Key Laboratory of Fine Chemicals, Department of Materials Science and Chemical Engineering, School of Chemical Engineering, Dalian University of Technology, Zhongshan Road 158-43, Dalian Liaoning 116012 (China)], E-mail: ninggl@dlut.edu.cn; Zhang Xu; Wang Jing; Lin Yuan; Ye Junwei [State Key Laboratory of Fine Chemicals, Department of Materials Science and Chemical Engineering, School of Chemical Engineering, Dalian University of Technology, Zhongshan Road 158-43, Dalian Liaoning 116012 (China)

    2008-12-15

    Sr{sub 2}MgSi{sub 2}O{sub 7}:Eu{sup 2+}, Dy{sup 3+} phosphors were prepared by the (aminopropyl)-triethoxysilane (APTES) co-precipitation method. Effects of synthesis temperature on the crystal characteristics, luminescent properties and afterglow performance of Sr{sub 2}MgSi{sub 2}O{sub 7}:Eu{sup 2+}, Dy{sup 3+} phosphors have been discussed in detail and compared with the corresponding commercial product. The experimental results indicated that the sample could be synthesized at a relatively lower temperature and had better performance on the above-mentioned properties using the co-precipitation method.

  20. First estimates of the contribution of CaCO3 precipitation to the release of CO2 to the atmosphere during young sea ice growth

    Science.gov (United States)

    Geilfus, N.-X.; Carnat, G.; Dieckmann, G. S.; Halden, N.; Nehrke, G.; Papakyriakou, T.; Tison, J.-L.; Delille, B.

    2013-01-01

    report measurements of pH, total alkalinity, air-ice CO2 fluxes (chamber method), and CaCO3 content of frost flowers (FF) and thin landfast sea ice. As the temperature decreases, concentration of solutes in the brine skim increases. Along this gradual concentration process, some salts reach their solubility threshold and start precipitating. The precipitation of ikaite (CaCO3.6H2O) was confirmed in the FF and throughout the ice by Raman spectroscopy and X-ray analysis. The amount of ikaite precipitated was estimated to be 25 µmol kg-1 melted FF, in the FF and is shown to decrease from 19 to 15 µmol kg-1 melted ice in the upper part and at the bottom of the ice, respectively. CO2 release due to precipitation of CaCO3 is estimated to be 50 µmol kg-1 melted samples. The dissolved inorganic carbon (DIC) normalized to a salinity of 10 exhibits significant depletion in the upper layer of the ice and in the FF. This DIC loss is estimated to be 2069 µmol kg-1 melted sample and corresponds to a CO2 release from the ice to the atmosphere ranging from 20 to 40 mmol m-2 d-1. This estimate is consistent with flux measurements of air-ice CO2 exchange. Our measurements confirm previous laboratory findings that growing young sea ice acts as a source of CO2 to the atmosphere. CaCO3 precipitation during early ice growth appears to promote the release of CO2 to the atmosphere; however, its contribution to the overall release by newly formed ice is most likely minor.

  1. co-removal with nucleated Cu(II) precipitation in continuous-flow ...

    African Journals Online (AJOL)

    A compact nucleated precipitation technology using two fluidised sand columns in series was developed to pretreat model metal-plating wastewater containing high concentrations of Cu(II) and Cr(VI). Since either Cu(II) precipitation or Cr(VI) co-removal with Cu(II) precipitation was found to be highly pH dependent in batch ...

  2. Synthesis of cerium oxide (CeO{sub 2}) nanoparticles using simple CO-precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Farahmandjou, M.; Zarinkamar, M.; Firoozabadi, T. P., E-mail: farahamndjou@iauvaramin.ac.ir [Islamis Azad University, Varamin-Phisva Branch, Department of Physics, Varamin (Iran, Islamic Republic of)

    2016-11-01

    Synthesis of cerium oxide (CeO{sub 2}) nanoparticles was studied by new and simple co-precipitation method. The cerium oxide nanoparticles were synthesized using cerium nitrate and potassium carbonate precursors. Their physicochemical properties were characterized by high resolution transmission electron microscopy (HRTEM), scanning electron microscopy (Sem), X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (Ftir) and UV-Vis spectrophotometer. XRD pattern showed the cubic structure of the cerium oxide nanoparticles. The average particle size of CeO{sub 2} was around 20 nm as estimated by XRD technique and direct HRTEM observations. The surface morphological studies from Sem and Tem depicted spherical particles with formation of clusters. The sharp peaks in Ftir spectrum determined the existence of CeO{sub 2} stretching mode and the absorbance peak of UV-Vis spectrum showed the bandgap energy of 3.26 eV. (Author)

  3. Research on a pellet co-precipitation micro-filtration process for the treatment of liquid waste containing strontium

    International Nuclear Information System (INIS)

    Xin Luo; North China Institute of Science and Technology, Beijing; Guanghui Zhang; Xue Wang; Ping Gu

    2013-01-01

    The chemical precipitation method for radioactive wastewater treatment has the advantages of being simple and cost-effective. However, difficulties with the solid–liquid separation and sludge concentration restrict the application of this method. In this paper, a pellet co-precipitation micro-filtration (PCM) process was studied for treating strontium-containing wastewater on a laboratory scale. The seed was prepared by CaCO 3 powders. Sr 2+ and CO 3 2- were constantly crystallised on the seed surface, with Na 2 CO 3 as the precipitating agent in the pellet reactor. The following membrane separator with the addition of FeCl 3 enhanced the treatment effect. The average strontium concentrations in the raw water and in the effluent were 12.0 and 0.0220 mg/L, respectively. The strontium decontamination factor (DF) increased with the operation time, with an average value of 577. The precipitate particles formed gradually grew larger, with good sedimentation properties. When the experiment was complete, the formed precipitate was separated easily from the liquid phase and directly discharged. The concentration factor (CF) was 1,958. In the PCM process, crystallisation was the main mechanism for strontium removal, with the influent strontium level playing an important role. Membrane pore blockage and cake layer formation could help to further intercept the strontium crystallites. Furthermore, ferric chloride coagulation in the membrane separator also contributed to strontium removal. The PCM process has potential for wider application in the removal of strontium from wastewater. (author)

  4. Oxalate quantification in hemodialysate to assess dialysis adequacy for primary hyperoxaluria.

    Science.gov (United States)

    Tang, Xiaojing; Voskoboev, Nikolay V; Wannarka, Stacie L; Olson, Julie B; Milliner, Dawn S; Lieske, John C

    2014-01-01

    Patients with primary hyperoxaluria (PH) overproduce oxalate which is eliminated via the kidneys. If end-stage kidney disease develops they are at high risk for systemic oxalosis, unless adequate oxalate is removed during hemodialysis (HD) to equal or exceed ongoing oxalate production. The purpose of this study was to validate a method to measure oxalate removal in this unique group of dialysis patients. Fourteen stable patients with a confirmed diagnosis of PH on HD were included in the study. Oxalate was measured serially in hemodialysate and plasma samples in order to calculate rates of oxalate removal. HD regimens were adjusted according to a given patient's historical oxalate production, amount of oxalate removal at dialysis, residual renal clearance of oxalate, and plasma oxalate levels. After a typical session of HD, plasma oxalate was reduced by 78.4 ± 7.7%. Eight patients performed HD 6 times/week, 2 patients 5 times/week, and 3 patients 3 times/week. Combined oxalate removal by HD and the kidneys was sufficient to match or exceed endogenous oxalate production. After a median period of 9 months, pre-dialysis plasma oxalate was significantly lower than initially (75.1 ± 33.4 vs. 54.8 ± 46.6 mmol/l, p = 0.02). This methodology can be used to individualize the dialysis prescription of PH patients to prevent oxalosis during the time they are maintained on HD and to reduce risk of oxalate injury to a transplanted kidney.

  5. A neodymium(III)-ammonium complex involving oxalate and carbonate ligands: (NH4)2[Nd2(C2O4)3(CO3)(H2O)].H2O.

    Science.gov (United States)

    Trombe, Jean-Christian; Galy, Jean; Enjalbert, Renée

    2002-10-01

    The title compound, diammonium aqua-mu-carbonato-tri-mu-oxalato-dineodymium(III) hydrate, (NH(4))(2)[Nd(2)(CO(3))(C(2)O(4))(3)(H(2)O)].H(2)O, involving the two ligands oxalate and carbonate, has been prepared hydrothermally as single crystals. The Nd atoms form a tetranuclear unit across the inversion centre at (1/2, 1/2, 1/2). Starting from this tetranuclear unit, the oxalate ligands serve to develop a three-dimensional network. The carbonate group acts as a bis-chelating ligand to two Nd atoms, and is monodentate to a third Nd atom. The oxalate groups are all bis-chelating. The two independent Nd atoms are ninefold coordinated and the coordination polyhedron of these atoms is a distorted monocapped antiprism.

  6. Vibrational studies in aqueous solutions. Part II. The acid oxalate ion and oxalic acid

    Science.gov (United States)

    Shippey, T. A.

    1980-08-01

    Assignments for oxalic acid in solution are re-examined. A detailed assignment of the IR and Raman spectra of the acid oxalate ion is presented for the first time. Raman spectroscopy is used to study the first ionization of oxalic acid.

  7. Co-precipitation and solubility studies of cesium, potassium and sodium tetraphenylborate

    International Nuclear Information System (INIS)

    Peterson, R.A.

    1999-01-01

    This report contains the results from a study requested by High Level Waste Division on the co-precipitation and solubility of cesium, potassium, and sodium tetraphenylborate. Co-precipitation of cesium (Cs), potassium (K), and sodium (Na) tetraphenylborate (TPB) helps determine the efficiency of reagent usage in the Small Tank Precipitation Process. This process uses NaTPB to remove cesium from waste by means of precipitation. Previous studies by McCabe suggested that if the sodium ion concentration [Na+] increased the rate at which cesium tetraphenylborate (KTPB) in the presence of high [Na+] (∼5M) appears to produce a mixed solid phase composed of NaTPB and KTPB together in the crystal lattice

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

    Science.gov (United States)

    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.

  9. Membrane inlet mass spectrometry reveals that Ceriporiopsis subvermispora bicupin oxalate oxidase is inhibited by nitric oxide.

    Science.gov (United States)

    Moomaw, Ellen W; Uberto, Richard; Tu, Chingkuang

    2014-07-18

    Membrane inlet mass spectrometry (MIMS) uses a semipermeable membrane as an inlet to a mass spectrometer for the measurement of the concentration of small uncharged molecules in solution. We report the use of MIMS to characterize the catalytic properties of oxalate oxidase (E.C. 1.2.3.4) from Ceriporiopsis subvermispora (CsOxOx). Oxalate oxidase is a manganese dependent enzyme that catalyzes the oxygen-dependent oxidation of oxalate to carbon dioxide in a reaction that is coupled with the formation of hydrogen peroxide. CsOxOx is the first bicupin enzyme identified that catalyzes this reaction. The MIMS method of measuring OxOx activity involves continuous, real-time direct detection of oxygen consumption and carbon dioxide production from the ion currents of their respective mass peaks. (13)C2-oxalate was used to allow for accurate detection of (13)CO2 (m/z 45) despite the presence of adventitious (12)CO2. Steady-state kinetic constants determined by MIMS are comparable to those obtained by a continuous spectrophotometric assay in which H2O2 production is coupled to the horseradish peroxidase catalyzed oxidation of 2,2'-azinobis-(3-ethylbenzthiazoline-6-sulphonic acid). Furthermore, we used MIMS to determine that NO inhibits the activity of the CsOxOx with a KI of 0.58±0.06 μM. Copyright © 2014 The Authors. Published by Elsevier Inc. All rights reserved.

  10. Oxalate metal complexes in aerosol particles: implications for the hygroscopicity of oxalate-containing particles

    Directory of Open Access Journals (Sweden)

    T. Furukawa

    2011-05-01

    Full Text Available Atmospheric aerosols have both a direct and an indirect cooling effect that influences the radiative balance at the Earth's surface. It has been estimated that the degree of cooling is large enough to weaken the warming effect of carbon dioxide. Among the cooling factors, secondary organic aerosols (SOA play an important role in the solar radiation balance in the troposphere as SOA can act as cloud condensation nuclei (CCN and extend the lifespan of clouds because of their high hygroscopic and water soluble nature. Oxalic acid is an important component of SOA, and is produced via several formation pathways in the atmosphere. However, it is not certain whether oxalic acid exists as free oxalic acid or as metal oxalate complexes in aerosols, although there is a marked difference in their solubility in water and their hygroscopicity. We employed X-ray absorption fine structure spectroscopy to characterize the calcium (Ca and zinc (Zn in aerosols collected at Tsukuba in Japan. Size-fractionated aerosol samples were collected for this purpose using an impactor aerosol sampler. It was shown that 10–60% and 20–100% of the total Ca and Zn in the finer particles (<2.1 μm were present as Ca and Zn oxalate complexes, respectively. Oxalic acid is hygroscopic and can thus increase the CCN activity of aerosol particles, while complexes with various polyvalent metal ions such as Ca and Zn are not hygroscopic, which cannot contribute to the increase of the CCN activity of aerosols. Based on the concentrations of noncomplexed and metal-complexed oxalate species, we found that most of the oxalic acid is present as metal oxalate complexes in the aerosols, suggesting that oxalic acid does not always increase the hygroscopicity of aerosols in the atmosphere. Similar results are expected for other dicarboxylic acids, such as malonic and succinic acids. Thus, it is advisable that the cooling effect of organic aerosols should be estimated by including the

  11. Effects of freshwater Synechococcus sp. cyanobacteria pH buffering on CaCO3 precipitation: Implications for CO2 sequestration

    International Nuclear Information System (INIS)

    Martinez, Raul E.; Weber, Sebastian; Grimm, Christian

    2016-01-01

    In the present study, a mixed-flow steady-state bio-reactor was designed to biomineralize CO 2 as a consequence of photosynthesis from active Synechococcus sp. Dissolved CO 2 , generated by constant air bubbling of inorganic and cyanobacteria stock solutions, was the only source of inorganic carbon. The release of hydroxide ion by cyanobacteria from photosynthesis maintained highly alkaline pH conditions. In the presence of Ca 2+ and carbonate species, this led to calcite supersaturation under steady state conditions. Ca 2+ remained constant throughout the experiments showing the presence of steady state conditions. Similarly, the Synechococcus sp. biomass concentration remained stable within uncertainty. A gradual pH decrease was observed for the highest Ca 2+ condition coinciding with the formation of CaCO 3 . The high degree of supersaturation, under steady-state conditions, contributed to the stabilization of calcite and maintained a constant driving force for the mineral nucleation and growth. For the highest Ca 2+ condition a fast crystal growth rate was consistent with rapid calcite precipitation as suggested further by affinity calculations. Although saturation state based kinetic precipitation models cannot accurately reflect the controls on crystal growth kinetics or reliably predict growth mechanisms, the relatively reaction orders obtained from modeling of calcite precipitation rates as function of decreasing carbonate concentration suggest that the precipitation occurred via surface-controlled rate determining reactions. These high reaction orders support in addition the hypothesis that crystal growth proceeded through complex surface controlled mechanisms. In conclusion, the steady state supersaturated conditions generated by a constant cyanobacteria biomass and metabolic activity strongly suggest that these microorganisms could be used for the development of efficient CO 2 sequestration methods in a controlled large-scale environment. - Highlights:

  12. Comparison of the properties of simulated synroc synthesized by sol-gel and a novel co - precipitation method

    International Nuclear Information System (INIS)

    Potdar, H.S.; Vijayanand, S.; Khaja Mohaideen, K.; Joy, P.A.; Raja Madhavan, R.; Kutty, K.V.G.; Ambashta, R.D.; Wattal, P.K.

    2009-01-01

    Synroc is a multiphase dense titanate based ceramic designed for the incorporation of high-level waste (HLW) from the reprocessing of spent nuclear fuel. Synroc or synthetic rock consists of four main titanate phases - zirconolite (CaZrTi 2 O 7 ), hollandite (BaAlO 2 Ti 6 O 16 ), perovskite (CaTiO 3 ) and rutile (TiO 2 ), with the matrix composition as shown in Table 1. It is known that these phases have the capacity to incorporate most of the elements into their crystal structures which are present in the HLW derived from the reprocessing of spent nuclear fuel from power reactors. Synroc is considered as the most effective and durable means of immobilising various forms of high-level radioactive wastes for disposal. Synroc is also considered as a low-risk, tailored waste form, offering higher waste loading and over all cost savings. Simulated synroc precursor powders are typically produced by advanced wet chemical methods such as alkoxide hydrolysis and sol-gel routes. These routes were developed to produce powders with well defined physical and chemical characteristics such as correct chemical composition, high degree of homogeneity, reactivity and readily densifiable material to 99% of theoretical density during hot isostatic pressing. However, the reported alkoxide hydrolysis and hydroxide routes suffer from several disadvantages such as use of large quantities of organic solvents and their disposal as effluent, difficulty in maintaining exact chemical composition, use of costly alkoxide precursors which are moisture sensitive and require critical processing conditions to control their rate of hydrolysis, etc. In the present work we report a comparative study the characteristics of synroc-C (14% waste loading) powders and sintered pellets synthesized by the known alkoxide hydrolysis method and a simple chemical co-precipitation route developed by us. The advantages of the co-precipitation route are its simplicity, ease of handling and utilization of cheaper raw

  13. High variability of the heterogeneous ice nucleation potential of oxalic acid dihydrate and sodium oxalate

    Directory of Open Access Journals (Sweden)

    R. Wagner

    2010-08-01

    Full Text Available The heterogeneous ice nucleation potential of airborne oxalic acid dihydrate and sodium oxalate particles in the deposition and condensation mode has been investigated by controlled expansion cooling cycles in the AIDA aerosol and cloud chamber of the Karlsruhe Institute of Technology at temperatures between 244 and 228 K. Previous laboratory studies have highlighted the particular role of oxalic acid dihydrate as the only species amongst a variety of other investigated dicarboxylic acids to be capable of acting as a heterogeneous ice nucleus in both the deposition and immersion mode. We could confirm a high deposition mode ice activity for 0.03 to 0.8 μm sized oxalic acid dihydrate particles that were either formed by nucleation from a gaseous oxalic acid/air mixture or by rapid crystallisation of highly supersaturated aqueous oxalic acid solution droplets. The critical saturation ratio with respect to ice required for deposition nucleation was found to be less than 1.1 and the size-dependent ice-active fraction of the aerosol population was in the range from 0.1 to 22%. In contrast, oxalic acid dihydrate particles that had crystallised from less supersaturated solution droplets and had been allowed to slowly grow in a supersaturated environment from still unfrozen oxalic acid solution droplets over a time period of several hours were found to be much poorer heterogeneous ice nuclei. We speculate that under these conditions a crystal surface structure with less-active sites for the initiation of ice nucleation was generated. Such particles partially proved to be almost ice-inactive in both the deposition and condensation mode. At times, the heterogeneous ice nucleation ability of oxalic acid dihydrate significantly changed when the particles had been processed in preceding cloud droplet activation steps. Such behaviour was also observed for the second investigated species, namely sodium oxalate. Our experiments address the atmospheric scenario

  14. High variability of the heterogeneous ice nucleation potential of oxalic acid dihydrate and sodium oxalate

    Science.gov (United States)

    Wagner, R.; Möhler, O.; Saathoff, H.; Schnaiter, M.; Leisner, T.

    2010-08-01

    The heterogeneous ice nucleation potential of airborne oxalic acid dihydrate and sodium oxalate particles in the deposition and condensation mode has been investigated by controlled expansion cooling cycles in the AIDA aerosol and cloud chamber of the Karlsruhe Institute of Technology at temperatures between 244 and 228 K. Previous laboratory studies have highlighted the particular role of oxalic acid dihydrate as the only species amongst a variety of other investigated dicarboxylic acids to be capable of acting as a heterogeneous ice nucleus in both the deposition and immersion mode. We could confirm a high deposition mode ice activity for 0.03 to 0.8 μm sized oxalic acid dihydrate particles that were either formed by nucleation from a gaseous oxalic acid/air mixture or by rapid crystallisation of highly supersaturated aqueous oxalic acid solution droplets. The critical saturation ratio with respect to ice required for deposition nucleation was found to be less than 1.1 and the size-dependent ice-active fraction of the aerosol population was in the range from 0.1 to 22%. In contrast, oxalic acid dihydrate particles that had crystallised from less supersaturated solution droplets and had been allowed to slowly grow in a supersaturated environment from still unfrozen oxalic acid solution droplets over a time period of several hours were found to be much poorer heterogeneous ice nuclei. We speculate that under these conditions a crystal surface structure with less-active sites for the initiation of ice nucleation was generated. Such particles partially proved to be almost ice-inactive in both the deposition and condensation mode. At times, the heterogeneous ice nucleation ability of oxalic acid dihydrate significantly changed when the particles had been processed in preceding cloud droplet activation steps. Such behaviour was also observed for the second investigated species, namely sodium oxalate. Our experiments address the atmospheric scenario that coating layers

  15. Effects of Juice Processing on Oxalate Contents in Carambola Juice Products.

    Science.gov (United States)

    Huynh, Nha K; Nguyen, Ha V H

    2017-09-01

    Effects of processing methods including pressing, enzyme-assisted extraction, lactic acid fermentation by Lactobacillus acidophilus, and alcohol fermentation by Saccharomyces cerevisiae on total and soluble oxalate contents of carambola juices were studied. In comparison with pressing, the use of enzyme increased juice yields (15.89-17.29%), but resulted in higher total oxalate (1.60-1.73 times) and soluble oxalate contents (1.16-1.49 times). In addition, extension of enzyme incubation periods led to an increase in soluble oxalate contents in the products (p carambola juices. These results suggested that carambola juice products should only be consumed moderately, and that alcohol fermentation could be a potential method to reduce oxalate contents in foods in order to prevent the risks of forming kidney stones.

  16. Metabolic Conversion of l-Ascorbic Acid to Oxalic Acid in Oxalate-accumulating Plants 1

    Science.gov (United States)

    Yang, Joan C.; Loewus, Frank A.

    1975-01-01

    l-Ascorbic acid-1-14C and its oxidation product, dehydro-l-ascorbic acid, produced labeled oxalic acid in oxalate-accumulating plants such as spinach seedlings (Spinacia oleracea) and the detached leaves of woodsorrel (Oxalis stricta and O. oregana), shamrock (Oxalis adenopylla), and begonia (Begonia evansiana). In O. oregana, conversion occurred equally well in the presence or absence of light. This relationship between l-ascorbic acid metabolism and oxalic acid formation must be given careful consideration in attempts to explain oxalic accumulation in plants. PMID:16659288

  17. Precipitation kinetics of Mg-carbonates, influence of organic ligands and consequences for CO2 mineral sequestration

    International Nuclear Information System (INIS)

    Gautier, Q.

    2012-01-01

    Forming magnesium carbonate minerals through carbonation of magnesium silicates has been proposed as a safe and durable way to store carbon dioxide, with a possibly high potential to offset anthropogenic CO 2 emissions. To date however, chemical reactions involved in this process are facing strong kinetic limitations, which originate in the low reactivity of both Mg-silicates and Mg-carbonates. Numerous studies have focused on the dissolution of Mg-silicates, under the questionable hypothesis that this step limits the whole process. This thesis work focuses instead on the mechanisms and rates of formation of magnesium carbonates, which are the final products of carbonation reactions. The first part of the work is dedicated to studying the influence on magnesite precipitation kinetics of three organic ligands known to accelerate Mg-silicates dissolution rates: oxalate, citrate and EDTA. With help of mixed-flow reactor experiments performed between 100 and 150 C, we show that these ligands significantly reduce magnesite growth rates, through two combined mechanisms: (1) complexation of Mg 2+ cations in aqueous solution, which was rigorously estimated from a thermodynamic database established through a critical review of the literature, and (2) adsorption of ligands to a limited number of surface sites, leading to a decrease of the precipitation rate constant. The observed growth inhibition is maximal with citrate. We then used hydrothermal atomic force microscopy to probe the origin of the documented growth inhibition. Our observations show that citrate and oxalate interact with the crystal growth process on magnesite surface, modifying the shape of growth hillocks as well as the step generation frequency through spiral growth. We also show that the ligands adsorb preferentially on different kink-sites, which is probably related to their different structures and chemical properties. We propose that the stronger magnesite growth inhibition caused by citrate is related

  18. Upconversion emission study of Er3+/Yb3+ doped barium titanate phosphor prepared by co-precipitation method

    International Nuclear Information System (INIS)

    Mahata, M.K.; Dey, R.; Kumar, K.; Rai, V.K.; Rai, S.B.

    2012-01-01

    In the present work we have successfully synthesized the Er 3+ , Yb 3+ doped barium titanate phosphor via co-precipitation synthesis method. Under 980 nm excitation, tri-color upconversion fluorescence has been observed. The Fourier Transform Infrared measurement was done to check the presence of organic impurities. In order to find out how many photons are involved in each emission band, the variation of UC emission intensity of the codoped phosphor is studied with increase in excitation power. Upconversion emission spectra show that as the annealing temperature of the powder is increased, intensity of red emission decreases and intensity of green emission increases due to the decrease in maximum phonon frequency of the host material. (author)

  19. γ' Precipitation Study of a Co-Ni-Based Alloy

    Science.gov (United States)

    Locq, D.; Martin, M.; Ramusat, C.; Fossard, F.; Perrut, M.

    2018-05-01

    A Co-Ni-based alloy strengthened by γ'-(L12) precipitates was utilized to investigate the precipitation evolution after various cooling rates and several aging conditions. In this study, the precipitate size and volume fraction have been studied via scanning electron microscopy and transmission electron microscopy. The influence of the precipitation evolution was measured via microhardness tests. The cooling rate study shows a more sluggish γ' precipitation reaction compared to that observed in a Ni-based superalloy. Following a rapid cooling rate, the application of appropriate double aging treatments allows for the increase of the γ' volume fraction as well as the control of the size and distribution of the precipitates. The highest hardness values reach those measured on supersolvus cast and wrought Ni-based superalloys. The observed γ' precipitation behavior should have implications for the production, the heat treatment, the welding, or the additive manufacturing of this new class of high-temperature materials.

  20. Morphological control of calcium oxalate particles in the presence of poly-(styrene-alt-maleic acid)

    International Nuclear Information System (INIS)

    Yu Jiaguo; Tang Hua; Cheng Bei; Zhao Xiujian

    2004-01-01

    Calcium oxalate (CaOx) particles exhibiting different shapes and phase structures were fabricated by a simple precipitation reaction of sodium oxalate with calcium chloride in the absence and presence of poly-(styrene-alt-maleic acid) (PSMA) as a crystal modifier at room temperature. The as-obtained products were characterized with scanning electron microscopy (SEM) and X-ray diffraction (XRD). The effects of reaction conditions including pH, [Ca 2+ ]/[C 2 O 4 2- ] ratio and concentration of PSMA and CaC 2 O 4 on the crystal forms and morphologies of the as-obtained calcium oxalate were investigated. The results show that various crystal morphologies of calcium oxalate, such as parallelograms, plates, spheres, bipyramids etc. can be obtained depending on the experimental conditions. Higher polymer concentration favors formation of the metastable calcium oxalate dihydrate (COD) crystals. Lower pH is beneficial to the formation of plate-like CaOx crystals. Especially, the monodispersed parallelogram-like CaOx crystals can be produced by PSMA as an additive at pH 2. PSMA may act as a good inhibitor for urolithiasis since it induces the formation of COD and reduces the particle size of CaOx. This research may provide new insight into the morphological control of CaOx particles and the prevention of urolithiasis

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

    Science.gov (United States)

    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.

  2. Effect of Mineral Dissolution/Precipitation and CO2 Exsolution on CO2 transport in Geological Carbon Storage.

    Science.gov (United States)

    Xu, Ruina; Li, Rong; Ma, Jin; He, Di; Jiang, Peixue

    2017-09-19

    Geological carbon sequestration (GCS) in deep saline aquifers is an effective means for storing carbon dioxide to address global climate change. As the time after injection increases, the safety of storage increases as the CO 2 transforms from a separate phase to CO 2 (aq) and HCO 3 - by dissolution and then to carbonates by mineral dissolution. However, subsequent depressurization could lead to dissolved CO 2 (aq) escaping from the formation water and creating a new separate phase which may reduce the GCS system safety. The mineral dissolution and the CO 2 exsolution and mineral precipitation during depressurization change the morphology, porosity, and permeability of the porous rock medium, which then affects the two-phase flow of the CO 2 and formation water. A better understanding of these effects on the CO 2 -water two-phase flow will improve predictions of the long-term CO 2 storage reliability, especially the impact of depressurization on the long-term stability. In this Account, we summarize our recent work on the effect of CO 2 exsolution and mineral dissolution/precipitation on CO 2 transport in GCS reservoirs. We place emphasis on understanding the behavior and transformation of the carbon components in the reservoir, including CO 2 (sc/g), CO 2 (aq), HCO 3 - , and carbonate minerals (calcite and dolomite), highlight their transport and mobility by coupled geochemical and two-phase flow processes, and consider the implications of these transport mechanisms on estimates of the long-term safety of GCS. We describe experimental and numerical pore- and core-scale methods used in our lab in conjunction with industrial and international partners to investigate these effects. Experimental results show how mineral dissolution affects permeability, capillary pressure, and relative permeability, which are important phenomena affecting the input parameters for reservoir flow modeling. The porosity and the absolute permeability increase when CO 2 dissolved water is

  3. Nanoscale co-precipitation and mechanical properties of a high-strength low-carbon steel

    International Nuclear Information System (INIS)

    Mulholland, Michael D.; Seidman, David N.

    2011-01-01

    Nanoscale co-precipitation in a novel high-strength low-carbon steel is studied in detail after isothermal aging. Atom-probe tomography is utilized to quantify the co-precipitation of co-located Cu precipitates and M 2 C (M is any combination of Cr, Mo, Fe, or Ti) carbide strengthening precipitates. Coarsening of Cu precipitates is offset by the nucleation and growth of M 2 C carbide precipitate, resulting in the maintenance of a yield strength of 1047 ± 7 MPa (152 ± 1 ksi) for as long as 320 h of aging time at 450 deg. C. Impact energies of 153 J (113 ± 6 ft-lb) and 144 J (106 ± 2 ft-lb) are measured at -30 deg. C and -60 deg. C, respectively. The co-location of Cu and M 2 C carbide precipitates results in non-stationary-state coarsening of the Cu precipitates. Synchrotron-source X-ray diffraction studies reveal that the measured 33% increase in impact toughness after aging for 80 h at 450 deg. C is due to dissolution of cementite, Fe 3 C, which is the source of carbon for the nucleation and growth of M 2 C carbide precipitates. Less than 1 vol.% austenite is observed for aging treatments at temperatures less than 600 deg. C, suggesting that transformation-induced plasticity does not play a significant role in the toughness of specimens aged at temperatures less than 600 deg. C. Aging treatments at temperatures greater than 600 deg. C produce more austenite, in the range 2-7%, but at the expense of yield strength.

  4. NDA technique for the assay of wet plutonium oxalate

    International Nuclear Information System (INIS)

    Marshall, R.S.; Canada, T.R.

    1980-01-01

    A method has been developed to quantitatively measure batches of wet plutonium oxalate. The method is based on a count of coincidence neutrons to which a correction is applied for the effects of neutron moderation by water. A therma-neutron coincidence counter (TNC) with two concentric rings of 3 He detectors provides the signal needed for the water correction. The signal is the ratio of neutron counts between the detector rings that changes with the percent of water in plutonium oxalate. To evaluate the measurement technique, 26 batches of plutonium oxalate were measured in an in-line TNC. The evaluation showed the measurements to be essentially unbiased and precise to 2.2%

  5. A simple and rapid method of purification of impure plutonium oxide

    International Nuclear Information System (INIS)

    Michael, K.M.; Rakshe, P.R.; Dharmpurikar, G.R.; Thite, B.S.; Lokhande, Manisha; Sinalkar, Nitin; Dakshinamoorthy, A.; Munshi, S.K.; Dey, P.K.

    2007-01-01

    Impure plutonium oxides are conventionally purified by dissolution in HNO 3 in presence of HF followed by ion exchange separation and oxalate precipitation. The method is tedious and use of HF enhances corrosion of the plant equipment's. A simple and rapid method has been developed for the purification of the oxide by leaching with various reagents like DM water, NaOH and oxalic acid. A combination of DM water followed by hot leaching with 0.4 M oxalic acid could bring down the impurity levels in the oxide to the desired level required for fuel fabrication. (author)

  6. Oxalate: Effect on calcium absorbability

    International Nuclear Information System (INIS)

    Heaney, R.P.; Weaver, C.M.

    1989-01-01

    Absorption of calcium from intrinsically labeled Ca oxalate was measured in 18 normal women and compared with absorption of Ca from milk in these same subjects, both when the test substances were ingested in separate meals and when ingested together. Fractional Ca absorption from oxalate averaged 0.100 +/- 0.043 when ingested alone and 0.140 +/- 0.063 when ingested together with milk. Absorption was, as expected, substantially lower than absorption from milk (0.358 +/- 0.113). Nevertheless Ca oxalate absorbability in these women was higher than we had previously found for spinach Ca. When milk and Ca oxalate were ingested together, there was no interference of oxalate in milk Ca absorption and no evidence of tracer exchange between the two labeled Ca species

  7. Studies on removal of plutonium from oxalic acid containing hydrochloric acid solutions

    Energy Technology Data Exchange (ETDEWEB)

    Ghadse, D R; Noronha, D M; Joshi, A R [Fuel Chemistry Division, Bhabha Atomic Research Centre, Mumbai (India)

    1994-06-01

    Solution containing hydrochloric acid, oxalic acid and considerable quantities of plutonium may be generated while recycling of scrap produced during the metallic fuel fabrication. Plutonium from such waste is normally recovered by anion exchange method after the destruction of oxalic acid using suitable oxidising agent. Solvent extraction and ion exchange methods are being explored in this laboratory for recovery of Pu from oxalic acid containing HCl solutions without prior destruction of oxalic acid. This paper describes the results on the determination of distribution ratios for extraction of Pu(IV) from hydrochloric acid using Aliquot-336 or HDEHP under varying experimental conditions. (author). 5 refs., 5 tabs.

  8. The bioavailability of oxalate from Oca (Oxalis tuberosa).

    Science.gov (United States)

    Albihn, P B; Savage, G P

    2001-08-01

    It is believed that soluble oxalate has higher bioavailability than insoluble oxalate. Oca (Oxalis tuberosa) is moderately high in oxalate and contains oxalate in soluble form only. We estimated the bioavailability of oxalate in oca based on the urinary excretion of oxalate after oxalate loading with oca to estimate the bioavailability of oxalate in oca. We also clarified whether bioavailability differs in various oxalate loads from the same food source and studied the effect of an additional calcium source on the bioavailability of oxalate from oca. Four men and 4 women ingested 50, 100 and 150 gm. oca as well as 100 gm. oca with 100 gm. sour cream. Oxalate was measured in a 6-hour urine sample from each volunteer. The mean bioavailability of oxalate from oca plus or minus standard deviation was 1.44% +/- 1.31% during the 6-hour period after intake. There was no significant difference in oxalate bioavailability among oxalate intake levels in this study, although oca consumption with sour cream significantly decreased the uptake of oxalate (p oca appears to be similar to that in spinach. However, bioavailability varies among individuals and depends on other constituents of a combined meal.

  9. The magnetic and colloidal properties of CoFe2O4 nanoparticles synthesized by co-precipitation.

    Science.gov (United States)

    Gyergyek, Sašo; Drofenik, Miha; Makovec, Darko

    2014-01-01

    Magnetic CoFe(2)O(4) nanoparticles were synthesized by co-precipitation at 80 °C. This co-precipitation was achieved by the rapid addition of a strong base to an aqueous solution of cations. The investigation of the samples that were quenched at different times after the addition of the base, using transmission electron microscopy (TEM) coupled with energy-dispersive X-ray spectroscopy (EDXS) and X-ray powder diffractometry, revealed the formation of a Co-deficient amorphous phase and Co(OH)(2), which rapidly reacted to form small CoFe(2)O(4) nanoparticles. The nanoparticles grew with the time of aging at elevated temperature. The colloidal suspensions of the nanoparticles were prepared in both an aqueous medium and in a non-polar organic medium, with the adsorption of citric acid and ricinoleic acid on the nanoparticles, respectively. The measurements of the room-temperature magnetization revealed the ferrimagnetic state of the CoFe(2)O(4) nanoparticles, while their suspensions displayed superparamagnetic behaviour.

  10. Oleic-acid-coated CoFe2O4 nanoparticles synthesized by co-precipitation and hydrothermal synthesis

    International Nuclear Information System (INIS)

    Gyergyek, Sašo; Drofenik, Miha; Makovec, Darko

    2012-01-01

    Highlights: ► Synthesis of oleic-acid-coated CoFe 2 O 4 nanoparticles from an aqueous solution. ► During the co-precipitation of Co 2+ /Fe 3+ single-phase spinel forms. ► During the co-precipitation of Co 2+ /Fe 2+ , feroxyhyte forms in addition to spinel. ► Oleic acid increases the spinel formation temperature and limits particle growth. ► Colloidal suspensions of ferrimagnetic CoFe 2 O 4 were prepared. - Abstract: Oleic-acid-coated CoFe 2 O 4 nanoparticles were synthesized by co-precipitation and hydrothermal synthesis. The coprecipitation of the nanoparticles was achieved by the rapid addition of a strong base to an aqueous solution of cations in the presence of the oleic acid surfactant, or without this additive. The nanoparticles were also synthesized by a hydrothermal treatment of suspensions of the precipitates, coprecipitated at room temperature in the presence of the oleic acid, or without it. The influence of the synthesis conditions, such as the valence state of the iron cation in the starting aqueous solution, the temperature of the treatment and the presence of oleic acid, on the particles size was systematically studied. X-ray powder diffractometry (XRD) and transmission electron microscopy (TEM) coupled with energy-dispersive X-ray spectroscopy (EDS) revealed that, although spinel forms at room temperature, a substantial amount of Co was incorporated within the secondary, feroxyhyte-like phase when the iron cation was in the 2+ state. In contrast, when iron was in the 3+ state, the spinel forms at elevated temperatures of approximately 60 °C. The presence of the oleic acid further increased the formation temperature for the stoichiometric spinel. Moreover, the oleic acid impeded the particles’ growth and enabled the preparation of colloidal suspensions of the nanoparticles in non-polar organic solvents. The nanoparticles’ size was successfully controlled by the temperature of the synthesis in the region where superparamagnetism

  11. Calcium oxalate stone and gout.

    Science.gov (United States)

    Marickar, Y M Fazil

    2009-12-01

    Gout is well known to be produced by increased uric acid level in blood. The objective of this paper is to assess the relationship between gout and calcium oxalate stone formation in the humans. 48 patients with combination of gout and calcium oxalate stone problem were included. The biochemical values of this group were compared with 38 randomly selected uric acid stone patients with gout, 43 stone patients with gout alone, 100 calcium oxalate stone patients without gout and 30 controls, making a total of 259 patients. Various biochemical parameters, namely serum calcium, phosphorus and uric acid and 24-h urine calcium, phosphorus, uric acid, oxalate, citrate and magnesium were analysed. ANOVA and Duncan's multiple-range tests were performed to assess statistical significance of the variations. The promoters of stone formation, namely serum calcium (P stone patients and gouty calcium oxalate stone patients compared to the non-gouty patients and controls. Urine oxalate (P stones patients. The inhibitor urine citrate (P stone gouty patients, followed by the gouty uric acid stone formers and gouty calcium oxalate stone patients. The high values of promoters, namely uric acid and calcium in the gouty stone patients indicate the tendency for urinary stone formation in the gouty stone patients. There is probably a correlation between gout and calcium oxalate urinary stone. We presume this mechanism is achieved through the uric acid metabolism. The findings point to the summation effect of metabolic changes in development of stone disease.

  12. Control of morphology and structure for β-Co nanoparticles from cobalt oxalate and research on its phase-change mechanism

    Energy Technology Data Exchange (ETDEWEB)

    Deng, Ying [State Key Laboratory of Powder Metallurgy, Central South University, Changsha 410083 (China); Chongqing University of Arts and Science, Chongqing 402160 (China); Xiong, Xiang, E-mail: xiangxiong88@qq.com [State Key Laboratory of Powder Metallurgy, Central South University, Changsha 410083 (China); Zou, J.P., E-mail: zoujp@csu.edu.cn [State Key Laboratory of Powder Metallurgy, Central South University, Changsha 410083 (China); Deng, Ling [Chengdu Chengliang Tool Group Co., Ltd., Chengdu 610056 (China); Tu, M.J. [Chongqing University of Arts and Science, Chongqing 402160 (China)

    2015-01-05

    Highlights: • Nanoscale precursor β-CoC{sub 2}O{sub 4}⋅2H{sub 2}O can be prepared by mechanical solid phase reaction. • Growth mechanism, morphology and crystal structure of β-CoC{sub 2}O{sub 4}⋅2H{sub 2}O have been studied. • Internal energy reserves of precursor making it directly generate β-Co in the thermal decomposition reaction. • Martensitic transformation of Co has been studied. • The Co powder will inherit the morphology of its precursor. - Abstract: The face-centered cubic crystal structure β-Co has excellent performance. As the main material to produce high toughness hard alloys and metal cermet, its morphology and structure will have an important impact on the performance of the alloy. This study, based on solid-phase reaction, starting from the crystal structure studied, discussed the effection of the mechanical solid-phase chemical reactions on the morphology of the cobalt precursor structure, researched the cobalt phase change mechanism, and presented a method to prepare nano β-Co. With H{sub 2}C{sub 2}O{sub 4}⋅2H{sub 2}O and Co(NO{sub 3}){sub 2}·6H{sub 2}O as raw materials, nano-crystalline cobalt oxalate powders with nearly spherical shape have been prepared by using solid-phase chemical reactions in high-speed ball milling, and then by decomposing at 400–450 °C, the target was prepared. The thermodynamical and IR analysis has been studied. The microstructure of the powders was characterized by XRD, SEM, TEM. It has been identified that a spherical, fcc structure, 100 nm β-Co powders was synthesized successfully, which confirmed the theoretical feasibility of this study.

  13. Impact of elevated CO_2 concentrations on carbonate mineral precipitation ability of sulfate-reducing bacteria and implications for CO_2 sequestration

    International Nuclear Information System (INIS)

    Paul, Varun G.; Wronkiewicz, David J.; Mormile, Melanie R.

    2017-01-01

    Interest in anthropogenic CO_2 release and associated global climatic change has prompted numerous laboratory-scale and commercial efforts focused on capturing, sequestering or utilizing CO_2 in the subsurface. Known carbonate mineral precipitating microorganisms, such as the anaerobic sulfate-reducing bacteria (SRB), could enhance the rate of conversion of CO_2 into solid minerals and thereby improve long-term storage of captured gasses. The ability of SRB to induce carbonate mineral precipitation, when exposed to atmospheric and elevated pCO_2, was investigated in laboratory scale tests with bacteria from organic-rich sediments collected from hypersaline Lake Estancia, New Mexico. The enriched SRB culture was inoculated in continuous gas flow and batch reactors under variable headspace pCO_2 (0.0059 psi to 20 psi). Solution pH, redox conditions, sulfide, calcium and magnesium concentrations were monitored in the reactors. Those reactors containing SRB that were exposed to pCO_2 of 14.7 psi or less showed Mg-calcite precipitation. Reactors exposed to 20 psi pCO_2 did not exhibit any carbonate mineralization, likely due to the inhibition of bacterial metabolism caused by the high levels of CO_2. Hydrogen, lactate and formate served as suitable electron donors for the SRB metabolism and related carbonate mineralization. Carbon isotopic studies confirmed that ∼53% of carbon in the precipitated carbonate minerals was derived from the CO_2 headspace, with the remaining carbon being derived from the organic electron donors, and the bicarbonate ions available in the liquid medium. The ability of halotolerant SRB to induce the precipitation of carbonate minerals can potentially be applied to the long-term storage of anthropogenic CO_2 in saline aquifers and other ideal subsurface rock units by converting the gas into solid immobile phases. - Highlights: • SRB under study are capable of precipitating calcite up to 14.7 psi pCO_2. • At 20 psi pCO_2, bacterial activity

  14. Determination method of radiostrontium

    International Nuclear Information System (INIS)

    1984-01-01

    This manual provides determination methods of strontium-90 and strontium-89 in the environment released from nuclear facilities, and it is a revised edition of the previous manual published in 1974. As for the preparation method of radiation counting sample, ion exchange method, oxalate separation method and solvent extraction method were adopted in addition to the method of fuming nitric acid separation adopted in the previous edition. Strontium-90 is determined by the separation and radioactivity determination of yttrium-90 in radioequilibrium with strontium-90. Strontium-89 is determined by subtraction of radioactivity of strontium-90 plus yttrium-90 from gross radioactivity of isolated strontium carbonate. Radioactivity determination should be carried out with a low-background 2 π-gas-flow counting system for the mounted sample on a filter having a chemical form of ferric hydroxide, yttrium oxalate or strontium carbonate. This manual describes sample preparation procedures as well as radioactivity counting procedures for environmental samples of precipitates as rain or snow, airborne dust, fresh water, sea water and soil, and also for ash sample made from biological or food samples such as grains, vegetables, tea leaves, pine needle, milk, marine organisms, and total diet, by employing a method of fuming nitric acid separation, ion exchange separation, oxalate precipitate separation or solvent extraction separation (only for an ash sample). Procedures for reagent chemicals preparation is also attached to this manual. (Takagi, S.)

  15. Apparatus and methods for regeneration of precipitating solvent

    Science.gov (United States)

    Liu, Guohai; Vimalchand, Pannalal; Peng, Wan Wang; Bonsu, Alexander

    2015-08-25

    A regenerator that can handle rich loaded chemical solvent containing precipitated absorption reaction products is disclosed. The invention is particularly suitable for separating CO.sub.2 from large gas streams that are typical of power plant processes. The internally circulating liquid stream in the regenerator (ICLS regenerator) rapidly heats-up the in-coming rich solvent stream in a downcomer standpipe as well as decreases the overall concentration of CO.sub.2 in the mixed stream. Both these actions lead to dissolution of precipitates. Any remaining precipitate further dissolves as heat is transferred to the mixed solution with an inverted bayonet tube heat exchanger in the riser portion of the regenerator. The evolving CO.sub.2 bubbles in the riser portion of the regenerator lead to substantial gas hold-up and the large density difference between the solutions in the downcomer standpipe and riser portions promotes internal circulation of the liquid stream in the regenerator. As minor amounts of solvent components present in the exit gas stream are condensed and returned back to the regenerator, pure CO.sub.2 gas stream exits the disclosed regenerator and condenser system.

  16. Precipitation of hydrated Mg carbonate with the aid of carbonic anhydrase for CO2 sequestration

    Science.gov (United States)

    Power, I. M.; Harrison, A. L.; Dipple, G. M.

    2011-12-01

    Strategies for sequestering CO2 directly from the atmosphere are likely required to achieve the desired reduction in CO2 concentration and avoid the most damaging effects of climate change [1]. Numerous studies have demonstrated the accelerated precipitation of calcium carbonate minerals with the aid of carbonic anhydrase (CA) as a means of sequestering CO2 in solid carbonate form; however, no study has examined precipitation of magnesium carbonate minerals using CA. Precipitation of magnesite (MgCO3) is kinetically inhibited [2]; therefore, Mg2+ must be precipitated as hydrated carbonate minerals. In laboratory experiments, the uptake of atmospheric CO2 into brine solutions (0.1 M Mg) was rate-limiting for the precipitation of dypingite [Mg5(CO3)4(OH)2-5H2O] with initial precipitation requiring 15 days [3]. It was also found that dypingite precipitation outpaced the uptake of CO2 gas into solution. CO2 uptake is limited by the hydration of CO2 to form carbonate ions [4]. Carbonic anhydrase (CA) enzymes are among the fastest known in nature and are able to catalyze the hydration of CO2, i.e., converting CO2(aq) to CO32- and HCO3- [5]. CA plays an important role in the carbon concentrating mechanism of photoautotrophic, chemoautotrophic, and heterotrophic prokaryotes and is involved in pH homeostasis, facilitated diffusion of CO2, ion transport, and the interconversion of CO2 and HCO3- [6]. Introducing CA into buffered Mg-rich solutions should allow for more rapid precipitation of hydrated magnesium carbonate minerals. Batch experiments were conducted using 125 mL flasks containing 100 mL of Millipore deionized water with 0.2 M of MgCl2-6H2O. To buffer pH, 1.0 g of pulverized brucite [Mg(OH)2] or 1.0 g of NaOH was added to the systems, which were amended with Bovine carbonic anhydrase (BCA) (Sigma-Aldrich). Solutions were stirred continuously and kept at room temperature (~22°C) with laboratory air introduced by bubbling. Temperature and pH were measured routinely

  17. Polymer-assisted co-precipitation route for the synthesis of Al 2 O 3

    Indian Academy of Sciences (India)

    It has been observed by field emission scanning electron microscopy analysis that the particle size reduced effectively (below 100 nm) when polymer-assisted co-precipitation route is used instead of the simple co-precipitation technique. A highly dense microstructure of sintered samples has been obtained, driven by ...

  18. The Synthesis of Calcium Salt from Brine Water by Partial Evaporation and Chemical Precipitation

    Science.gov (United States)

    Lalasari, L. H.; Widowati, M. K.; Natasha, N. C.; Sulistiyono, E.; Prasetyo, A. B.

    2017-02-01

    In this study would be investigated the effects of partial evaporation and chemical precipitation in the formation of calcium salt from brine water resources. The chemical reagents used in the study was oxalate acid (C2H2O4), ammonium carbonate (NH4)2CO3) and ammonium hydroxide (NH4OH) with reagent concentration of 2 N, respectively. The procedure was 10 liters brine water evaporated until 20% volume and continued with filtration process to separate brine water filtrate from residue (salt). Salt resulted from evaporation process was characterized by Scanning Electron Microscopy (SEM), X-Ray Fluorescence (XRF) and X-Ray Diffraction (XRD) techniques. Filtrate then was reacted with C2H2O4, (NH4)2CO3 and NH4OH reagents to get salt products in atmospheric condition and variation ratio volume brine water/chemicals (v/v) [10/1; 10/5; 10/10; 10/20; 10/30; 10:50; 20/1; 20/5; 20/10; 20/20; 20/30; 20:50]. The salt product than were filtered, dried, measured weights and finally characterized by SEM/EDS and XRD techniques. The result of experiment showed the chemical composition of brine water from Tirta Sanita, Bogor was 28.87% Na, 9.17% Mg, 2.94% Ca, 22.33% O, 0.71% Sr, 30.02% Cl, 1.51% Si, 1.23% K, 0.55% S, 1.31% Al. The chemical composition of salt resulted by partial evaporation was 53.02% Ca, 28.93%O, 9.50% Na, 2.10% Mg, 1.53% Sr, 1.20% Cl, 1.10% Si, 0.63% K, 0.40% S, 0.39% Al. The salt resulted by total evaporation was indicated namely as NaCl. Whereas salt resulted by partial evaporation was CaCO3 with a purity of 90 % from High Score Plus analysis. In the experiment by chemical precipitation was reported that the reagents of ammonium carbonate were more reactive for synthesizing calcium salt from brine water compared to reagents of oxalate acid and ammonium hydroxide. The salts precipitated by NH4OH, (NH4)2CO3, and H2C2O4 reagents were indicated as NaCl, CaCO3 and CaC2O4.H2O, respectively. The techniques of partial evaporation until 20% volume sample of brine water and

  19. Co-precipitation and solubility studies of cesium, potassium and sodium tetraphenylborate

    International Nuclear Information System (INIS)

    Peterson, R.A.

    2000-01-01

    This report contains the results from a study requested by High Level Waste on the co-precipitation and solubility of cesium, potassium, and sodium tetraphenylborate. Co-precipitation of cesium (Cs), potassium (K), and sodium (Na) tetraphenylborate (TPB) helps determine the efficiency of reagent usage in the Small Tank Precipitation Process. This process uses NaTPB to remove cesium from waste by means of precipitation. Previous studies by McCabe suggested that if the sodium ion concentration [Na + ] increased the rate at which cesium tetraphenylborate (CsTPB) precipitates also increases. Serkiz also demonstrated that the precipitation of potassium tetraphenylborate (KTPB) in the presence of high [Na + ] (∼5M) appears to produce a mixed solid phase composed of NaTPB and KTPB together in the crystal lattice. In the crystallographic structure of these three tetraphenylborate salts (Cs,K,NaTPB), the tetraphenylborate ion dominates the size of the crystals. Also, note that the three crystals have nearly identical structures with the exception of two additional peaks in the cesium pattern. Given these similarities, TPB precipitation in the presence of Na + , Cs + and K + likely produces an impure isomorphic crystalline mixture of CsTPB, KTPB and NaTPB. The authors speculate that the primary crystalline structure resembles that of KTPB with NaTPB and CsTPB mixed throughout the crystal structure. The precipitation of NaTPB makes some of the anticipated excess tetraphenylborate relatively unavailable for precipitation of cesium. Thus, the amount of excess tetraphenylborate required to completely precipitate all of the potassium and cesium may increase significantly

  20. High-performing mesoporous iron oxalate anodes for lithium-ion batteries.

    Science.gov (United States)

    Ang, Wei An; Gupta, Nutan; Prasanth, Raghavan; Madhavi, Srinivasan

    2012-12-01

    Mesoporous iron oxalate (FeC(2)O(4)) with two distinct morphologies, i.e., cocoon and rod, has been synthesized via a simple, scalable chimie douce precipitation method. The solvent plays a key role in determining the morphology and microstructure of iron oxalate, which are studied by field-emission scanning electron microscopy and high-resolution transmission electron microscopy. Crystallographic characterization of the materials has been carried out by X-ray diffraction and confirmed phase-pure FeC(2)O(4)·2H(2)O formation. The critical dehydration process of FeC(2)O(4)·2H(2)O resulted in anhydrous FeC(2)O(4), and its thermal properties are studied by thermogravimetric analysis. The electrochemical properties of anhydrous FeC(2)O(4) in Li/FeC(2)O(4) cells are evaluated by cyclic voltammetry, galvanostatic charge-discharge cycling, and electrochemical impedance spectroscopy. The studies showed that the initial discharge capacities of anhydrous FeC(2)O(4) cocoons and rods are 1288 and 1326 mA h g(-1), respectively, at 1C rate. Anhydrous FeC(2)O(4) cocoons exhibited stable capacity even at high C rates (11C). The electrochemical performance of anhydrous FeC(2)O(4) is found to be greatly influenced by the number of accessible reaction sites, morphology, and size effects.

  1. As cast precipitation microstructures in twin-roller melt-spun Cu{sub 90}Co{sub 10} alloys

    Energy Technology Data Exchange (ETDEWEB)

    Núñez-Coavas, H. [Facultad de Matemática, Astronomía y Física, Universidad Nacional de Córdoba, Ciudad Universitaria, 5000 Córdoba (Argentina); Pozo-López, G., E-mail: gpozo@famaf.unc.edu.ar [Facultad de Matemática, Astronomía y Física, Universidad Nacional de Córdoba, Ciudad Universitaria, 5000 Córdoba (Argentina); Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET) (Argentina); Instituto de Física Enrique Gaviola – CONICET (Argentina); Condó, A.M. [Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET) (Argentina); Centro Atómico Bariloche, Comisión Nacional de Energía Atómica, Instituto Balseiro, Universidad Nacional de Cuyo, Av. Bustillo 9500, 8400 San Carlos de Bariloche (Argentina); Urreta, S.E. [Facultad de Matemática, Astronomía y Física, Universidad Nacional de Córdoba, Ciudad Universitaria, 5000 Córdoba (Argentina); and others

    2016-12-15

    As cast Cu{sub 90}Co{sub 10} ribbons rapidly solidified by twin-roller melt spinning, exhibit special microstructure features. This processing method provides scenarios where a different phase selection takes place; coherent Co precipitates form directly from solidification, with neither a spinodal-like composition oscillation nor a discontinuously precipitated laminar phase. Samples are processed at tangential wheel speeds of 10 m/s (V10), 15 m/s (V15), 20 m/s (V20) and 30 m/s (V30). Microstructures resulting from this single step process are characterized and the hysteresis properties and the magnetoresistance effects evaluated. Samples V30 have a quite uniform density of coherent precipitates, with a narrow size distribution around 4 nm. On contrary, non-uniform precipitate distributions are found in samples cooled at lower rates; zones with a high density of coherent Co-rich precipitates are found forming colonies. These colonies are consistent with the extended compositional fluctuations occurring during very early stages in the cooling process. Samples may exhibit wide (V10) and even bimodal (V15) size distributions. Only samples V30 behave close to the ideal superparamagnetism. Samples V20 present relatively large coercivity and relative remanence and behave as an interacting superparamagnet, while the hysteresis loops of ribbons cooled at lower rates exhibit a ferromagnetic contribution in addition to the superparamagnetic-like one. This ferromagnetic component arises from blocked precipitates, larger than the upper bound size for superparamagnetic behavior at 300 K (12 nm). Room temperature magnetoresistance values associated to granular scattering units decrease as the mean precipitate size increases, but they remain below 2%, which is lower than that measured in samples annealed after rapid solidification, indicating that in this latter case contributions from the spinodally segregated matrix take place in addition to that of Co granules. - Highlights:

  2. PLZT (9/65/35) sintering and characterization through the Pechini and partial oxalate processes

    International Nuclear Information System (INIS)

    Cerqueira, Marinalva; Nasar, Ricardo Silveira; Leite, Edson Roberto; Longo, Elson; Varela, Jode Arana

    1996-01-01

    Zr Ti O 4 obtained by the Pechini method was used as precursor for obtaining PLZT. An aqueous solution of oxalic acid was prepared with ZT, Pb (NO 3 ) 2 and La 2 O 3 particles. After the Pb C 2 O 4 and La 2 O 3 precipitation on ZT, the material was calcined and x-ray diffraction (XRD) showed the cubic phase of PLZT. This material was sintered in two steps and density about 8.0 g/cm 3 were obtained. After second sintering XRD showed the occurrence of tetragonal and rhombohedral phases. This was caused by an estequiometric deviation, however the material showed a high optical transparency. (author)

  3. Growth and physico chemical characterization of lanthanum neodymium oxalate single crystals

    International Nuclear Information System (INIS)

    Raju, K.S.; John, Varughese; Ittyachen, M.A.

    1998-01-01

    Single crystals of lanthanum neodymium oxalate (LNO) are grown in sodium meta silicate gels, by the diffusion of a mixture of aqueous solutions of lanthanum nitrate and neodymium nitrate into the test tube having the set gel containing oxalic acid. The bluish pink coloured tabular crystals of LNO having well defined hexagonal basal planes appear either as foggy or clear, the latter at the greater depths inside the gel. The coloration of LNO visually observed is evidenced in UV-visible spectrum, by the revelation of well pronounced characteristic peaks in the visible region (500-900 nm). X-ray diffraction (XRD) of powdered LNO is ordered, meaning crystalline in nature, besides its isostructurality with similarly grown lanthanum samarium oxalate crystals. The single crystallinity of LNO is established by its oscillation XRD pattern. Thermogravimetric analysis (TGA) and differential scanning colorimetry (DSC) support that LNO loses water of crystallization around 120 degC and CO and CO 2 around 350-450 degC, while the infrared absorption (IR) spectrum of LNO establishes the presence of oxalate (C 2 O 4 ) 2- ions. Energy dispersive x-ray analysis (EDAX) confirms the presence of La and Nd in the sample. X-ray photoelectron spectroscopic (XPS) studies of LNO establish the presence of La and Nd in their respective oxide states. An empirical structure for LNO has been proposed on the basis of these findings. The smokiness in the foggy LNO crystal has been attributed due to the gel inclusion during the growth process. (author)

  4. Characterization of γ- Al{sub 2}O{sub 3} nanopowders synthesized by Co-precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Jbara, Ahmed S., E-mail: ahmedsbhe@yahoo.com [Center for Sustainable Nanomaterials, Universiti Teknologi Malaysia, Skudai - 81310, Johor Bahru (Malaysia); Physics Department, Science College, Al-Muthanna University, Samawah - 66001 (Iraq); Department of Physics, Faculty of Science, Universiti Teknologi Malaysia, Skudai - 81310, Johor Bahru (Malaysia); Othaman, Zulkafli [Center for Sustainable Nanomaterials, Universiti Teknologi Malaysia, Skudai - 81310, Johor Bahru (Malaysia); Department of Physics, Faculty of Science, Universiti Teknologi Malaysia, Skudai - 81310, Johor Bahru (Malaysia); Ati, Ali A. [Department of Physics, Faculty of Science, Universiti Teknologi Malaysia, Skudai - 81310, Johor Bahru (Malaysia); Saeed, M.A., E-mail: moalsd@gmail.com [Department of Physics, Faculty of Science, Universiti Teknologi Malaysia, Skudai - 81310, Johor Bahru (Malaysia); Division of Science and Technology, University of Education, Township, Lahore - 54770 (Pakistan)

    2017-02-15

    Co-precipitation technique has been used to synthesize gamma-Al{sub 2}O{sub 3} (γ-Al{sub 2}O{sub 3}) nanopowders under annealing temperature effect. The crystalline phase and purity for the prepared powder were characterized by different spectroscopy techniques. XRD analysis confirms the gamma phase of alumina nanopowders with particle diameter ranging from 6 to 24 nm, which confirms the quantum dots formation, which is also supported by the BET measurement. The surface area of the prepared nanopowders is in the range of 109–367 m{sup 2}/g. Morphology analysis indicates that γ-Al{sub 2}O{sub 3} nanopowders are consisted of grains almost spherical in shape. Some agglomeration of nanoparticles occurs, which become more regular hexagonal shaped with the increasing annealing temperature. The small nanoparticles size and the high surface area from a simple procedure for preparing γ-Al{sub 2}O{sub 3} may make it more suitable for use as an adsorbent for malachite green. - Highlights: • Co-precipitation technique is used to synthesize gamma- Al{sub 2}O{sub 3} nanopowders. • Pure gamma- Al{sub 2}O{sub 3} phase was obtained having maximum nanoparticle size is 24 nm. • The quantum dots were formed inside powder. • High surface area of nanopowders at the low annealing temperature. • Increasing annealing temperature causes the hexagonal agglomeration shape.

  5. Probable functions of calcium oxalate crystals in different tissues of ...

    African Journals Online (AJOL)

    Representatives of seven major edible aroid accessions were screened for calcium oxalate using standard histochemical methods. All the accessions were noted to contain calcium oxalate in the forms of raphide bundles and intra-amylar crystals. The crystals were widely present in all parts of the plants including spongy ...

  6. In vivo oxalate degradation by liposome encapsulated oxalate oxidase in rat model of hyperoxaluria

    Directory of Open Access Journals (Sweden)

    Tulika Dahiya

    2013-01-01

    Interpretation & conclusions: EMA-oxalate oxidase encapsulated liposome caused oxalate degradation in experimental hyperoxaluria indicating that the enzyme could be used as a therapeutic agent in hyperoxaluria leading to urinary stones.

  7. Enhanced nitrogen availability in karst ecosystems by oxalic acid release in the rhizosphere

    Directory of Open Access Journals (Sweden)

    Fujing ePan

    2016-05-01

    Full Text Available In karst ecosystems, a high level of CaCO3 enhances the stabilization of soil organic matter (SOM and causes nitrogen (N and/or phosphorus (P limitation in plants. Oxalic acid has been suggested to be involved in the nutrient-acquisition strategy of plants because its addition can temporarily relieve nutrient limitation. Therefore, understanding how oxalic acid drives N availability may help support successful vegetation restoration in the karst ecosystems of southwest China. We tested a model suggested by Clarholm et al. (2015 where oxalate reacts with Ca bridges in SOM, thus exposing previously protected areas to enzymatic attacks in a way that releases N for local uptake. We studied the effects of oxalic acid, microbial biomass C (MBC, and β-1,4-N-acetylglucosaminidase (NAG on potential N mineralization rates in rhizosphere soils of four plant species (two shrubs and two trees in karst areas. The results showed that rhizosphere soils of shrubs grown on formerly deforested land had significantly lower oxalic acid concentrations and NAG activity than that of trees in a 200-year-old forest. The levels of MBC in rhizosphere soils of shrubs were significantly lower than those of trees in the growing season, but the measure of shrubs and trees were similar in the non-growing season; the potential N mineralization rates showed a reverse pattern. Positive relationships were found among oxalic acid, MBC, NAG activity, and potential N mineralization rates for both shrubs and trees. This indicated that oxalic acid, microbes, and NAG may enhance N availability for acquisition by plants. Path analysis showed that oxalic acid enhanced potential N mineralization rates indirectly through inducing microbes and NAG activities. We found that the exudation of oxalic acid clearly provides an important mechanism that allows plants to enhance nutrient acquisition in karst ecosystems.

  8. Superior Photocatalytic Performance of CeO₂ Nanoparticles and Reduced Graphene Oxide Nanocomposite Prepared by Low Cost Co-Precipitation Method.

    Science.gov (United States)

    Jayanthi, Mani; Lavanya, Thirugnanam; Saradha, Nagarajan Anbil; Satheesh, Kaveri; Chenthamarai, SriRangarajan; Jayavel, Ramasamy

    2018-05-01

    In this article, cerium oxide nanoparticles (CeO2 NPs) and reduced graphene oxide nanocomposite have been fabricated through simple, easy and cost effective co-precipitation method. The structural, optical and morphological characterization provides the evidence of successful synthesis of CeO2 NPs and nanocomposite. X-ray photoelectron spectroscopic characterization provides useful information about the concentrations and proportions of Ce3+ and Ce4+ ions in nanoparticles as well as in nanocomposite. These studies provide an insight to understand enhanced photocatalytic activity of nanocomposite. The nanocomposite produces 81% photocatalytic degradation of methyl orange compared to only 45% degradation by CeO2 NPs alone.

  9. Design of Novel Precipitate-Strengthened Al-Co-Cr-Fe-Nb-Ni High-Entropy Superalloys

    Science.gov (United States)

    Antonov, Stoichko; Detrois, Martin; Tin, Sammy

    2018-01-01

    A series of non-equiatomic Al-Co-Cr-Fe-Nb-Ni high-entropy alloys, with varying levels of Co, Nb and Fe, were investigated in an effort to obtain microstructures similar to conventional Ni-based superalloys. Elevated levels of Co were observed to significantly decrease the solvus temperature of the γ' precipitates. Both Nb and Co in excessive concentrations promoted the formation of Laves and NiAl phases that formed either during solidification and remained undissolved during homogenization or upon high-temperature aging. Lowering the content of Nb, Co, or Fe prevented the formation of the eutectic type Laves. In addition, lowering the Co content resulted in a higher number density and volume fraction of the γ' precipitates, while increasing the Fe content led to the destabilization of the γ' precipitates. Various aging treatments were performed which led to different size distributions of the strengthening phase. Results from the microstructural characterization and hardness property assessments of these high-entropy alloys were compared to a commercial, high-strength Ni-based superalloy RR1000. Potentially, precipitation-strengthened high-entropy alloys could find applications replacing Ni-based superalloys as structural materials in power generation applications.

  10. Synthesis of unsymmetrical dimethylhydrazine oxalate from rejected liquid rocket propellant

    Science.gov (United States)

    Mu, Xiaogang; Yang, Jingjing; Zhang, Youzhi

    2018-02-01

    The rejected liquid propellant unsymmetrical dimethylhydrazine (UDMH) was converted to UDMH oxalate, which has commercial value. The UDMH oxalate structure and stability were investigated by the Fourier transform infrared spectroscopy, nuclear magnetic resonance spectroscopy, differential scanning calorimetry, and ultraviolet-visible spectrophotometric analysis. The results indicate that UDMH oxalate has good thermal and aqueous solution stability, a melting point of 144 °C, an initial decomposition temperature of 180 °C, and a peak wavelength of UV in aqueous solution at λ = 204 nm. This disposal method of rejected UDMH is highly efficient and environmentally safe.

  11. Synthesis and characterization of CaCO3 (calcite) nano particles from cockle shells (Anadara granosa Linn) by precipitation method

    Science.gov (United States)

    Widyastuti, Sri; Intan Ayu Kusuma, P.

    2017-06-01

    Calcium supplements can reduce the risk of osteoporosis, but they are not automatically absorbed in the gastrointestinal tract. Nanotechnology is presumed to have a capacity in resolving this problem. The preparation and characterization of calcium carbonate nano particle to improve the solubility was performed. Calcium carbonate nano particles were synthesized using precipitation method from cockle shells (Anadara granosa Linn). Samples of the cockle shells were dried in an oven at temperature of 50°C for 7 (seven) days and subsequently they were crushed and blended into fine powder that was sieved through 125-μm sieve. The synthesis of calcium carbonate nanocrystals was done by extracting using hydro chloride acid and various concentrations of sodium hydroxide were used to precipitate the calcium carbonate nano particles. The size of the nano particles was determined by SEM, XRD data, and Fourier transform infrared spectroscopy (FT-IR). The results of XRD indicated that the overall crystalline structure and phase purity of the typical calcite phase CaCO3 particles were approximately 300 nm in size. The method to find potential applications in industry to yield the large scale synthesis of aragonite nano particles by a low cost but abundant natural resource such as cockle shells is required.

  12. Preparation of Fe3O4/Bentonite Nanocomposite from Natural Iron Sand by Co-precipitation Method for Adsorbents Materials

    Science.gov (United States)

    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.

  13. CoCoRaHS: A Community Science Program Providing Valuable Precipitation Data to Guide Decision Making

    Science.gov (United States)

    Robinson, D. A.; Doesken, N.

    2017-12-01

    CoCoRaHS is an acronym for the Community Collaborative Rain, Hail and Snow Network. It is long-running, community-based network of volunteers working together to measure and map precipitation (rain, hail and snow). Precipitation is an ideal element for public engagement because it affects everyone, it is so variable in time and space and it impacts so many things. By using a standard precipitation gauge, stressing training and education, utilizing an interactive website, and having observations undergo quality assurance, the CoCoRaHS program provides high-quality data for natural resource, education and research applications. The program currently operates in all states, Canada and the Bahamas. It originated with the Colorado Climate Center at Colorado State University in 1998 due in part to the Fort Collins flood a year prior. Upwards of 12,000 observers submit observations each day. Observations meet federal guidelines and are archived at the U.S. National Centers for Environmental Information. Because of excellent spatial coverage, data quality, practical relevance, and accessibility, CoCoRaHS observations are used by a wide variety of organizations and individuals. The U.S. National Weather Service, hydrologists, emergency managers, city utilities (water supply, storm water), insurance adjusters, the U.S. Department of Agriculture, engineers, mosquito control commissions, ranchers and farmers, outdoor and recreation interests, teachers and students are just some examples of those who use CoCoRaHS data in making well-informed, meaningful decisions. Some examples of community applications and the science utility of CoCoRaHS observations include storm warnings, water supply and demand forecasts, disaster declarations (drought, winter storm, etc.), drought and food production assessments, calibration/validation of remote sensing, infrastructure evaluation and potential redesign (ice and snow loading, bridge, storm and sewer design), recreation planning, and

  14. Co-precipitation synthesis of YAG:Dy nanophosphor and its thermometric properties

    International Nuclear Information System (INIS)

    Chong, Joo-Yun; Zhang, Yuelan; Wagner, Brent K.; Kang, Zhitao

    2013-01-01

    Highlights: •YAG:Dy nanophosphors were synthesized with particle size of about 50 nm. •Optimized doping concentration of 6%Dy was determined. •Thermometric photoluminescence properties were studied between 20 and 350 °C. •Temperature-sensitive change in peak ratio of 496/457 nm emissions was demonstrated. •Suitable for potential thermographic applications when dispersed in a liquid media. -- Abstract: Dy 3+ doped yttrium aluminum garnet (YAG) nanophosphors were synthesized by a co-precipitation method for potential thermographic applications in a liquid media dispersed with fluorescent nanoparticles. The doping concentration and annealing temperature on the structural and optical properties of YAG:Dy were investigated. Pure phase YAG:Dy nanophosphors were obtained by annealing the co-precipitated hydroxide products at above 900 °C. Maximum photoluminescence intensity was observed from 6%Dy doped YAG samples. The effect of measuring temperature between 20 and 350 °C on the photoluminescence spectra of nano YAG:Dy was investigated. A temperature-sensitive change in the peak intensity ratio of 496/457 nm emission lines was demonstrated for such nanophosphors for the first time, suggesting potential applications in temperature monitoring of fuel spray

  15. Co-precipitation synthesis of YAG:Dy nanophosphor and its thermometric properties

    Energy Technology Data Exchange (ETDEWEB)

    Chong, Joo-Yun [School of Chemical and Biomolecular Engineering, Georgia Institute of Technology, Atlanta, GA 30332 (United States); Zhang, Yuelan [School of Materials Science and Engineering, Georgia Institute of Technology, Atlanta, GA 30332 (United States); Wagner, Brent K. [Georgia Tech Research Institute, Georgia Institute of Technology, Atlanta, GA 30332 (United States); Kang, Zhitao, E-mail: zhitao.kang@gtri.gatech.edu [Georgia Tech Research Institute, Georgia Institute of Technology, Atlanta, GA 30332 (United States); School of Materials Science and Engineering, Georgia Institute of Technology, Atlanta, GA 30332 (United States)

    2013-12-25

    Highlights: •YAG:Dy nanophosphors were synthesized with particle size of about 50 nm. •Optimized doping concentration of 6%Dy was determined. •Thermometric photoluminescence properties were studied between 20 and 350 °C. •Temperature-sensitive change in peak ratio of 496/457 nm emissions was demonstrated. •Suitable for potential thermographic applications when dispersed in a liquid media. -- Abstract: Dy{sup 3+} doped yttrium aluminum garnet (YAG) nanophosphors were synthesized by a co-precipitation method for potential thermographic applications in a liquid media dispersed with fluorescent nanoparticles. The doping concentration and annealing temperature on the structural and optical properties of YAG:Dy were investigated. Pure phase YAG:Dy nanophosphors were obtained by annealing the co-precipitated hydroxide products at above 900 °C. Maximum photoluminescence intensity was observed from 6%Dy doped YAG samples. The effect of measuring temperature between 20 and 350 °C on the photoluminescence spectra of nano YAG:Dy was investigated. A temperature-sensitive change in the peak intensity ratio of 496/457 nm emission lines was demonstrated for such nanophosphors for the first time, suggesting potential applications in temperature monitoring of fuel spray.

  16. Tuning size and catalytic activity of nano-clusters of cobalt oxide

    Indian Academy of Sciences (India)

    Unknown

    oxalic acid, (2) co-precipitating cobalt nitrate with sodium carbonate, and (3) using sodium dodecyl sul- .... Co(NO3)2 + Na2CO3 → CoCO3 + 2NaNO3,. CoCO3. ∆. → ∆ CoO + CO2,. CoO → (in air and heating) Co3O4. In method III, cobalt nitrate, sodium dodecyl sul- .... The conversion of cyclohexane on the current po-.

  17. Measurement of plutonium oxalate in thermal neutron coincidence counters

    International Nuclear Information System (INIS)

    Marshall, R.S.; Erkkila, B.H.

    1979-01-01

    A coincidence neutron counting method has been developed for assaying batches of plutonium oxalate. Using counting data from two concentric rings of 3 He detectors, corrections are made for the effects that water has on the coincidence neutron count rate. Batches of plutonium oxalate varying from 750 to 1000 g of plutonium and from 34 to 54% water are assayed with an average accuracy of +-3%

  18. High variability of the heterogeneous ice nucleation potential of oxalic acid dihydrate and sodium oxalate

    OpenAIRE

    R. Wagner; O. Möhler; H. Saathoff; M. Schnaiter; T. Leisner

    2010-01-01

    The heterogeneous ice nucleation potential of airborne oxalic acid dihydrate and sodium oxalate particles in the deposition and condensation mode has been investigated by controlled expansion cooling cycles in the AIDA aerosol and cloud chamber of the Karlsruhe Institute of Technology at temperatures between 244 and 228 K. Previous laboratory studies have highlighted the particular role of oxalic acid dihydrate as the only species amongst a variety of other investigated dicarboxylic acids to ...

  19. Sensitive indicators of Stipa bungeana response to precipitation under ambient and elevated CO2 concentration

    Science.gov (United States)

    Shi, Yaohui; Zhou, Guangsheng; Jiang, Yanling; Wang, Hui; Xu, Zhenzhu

    2018-02-01

    Precipitation is a primary environmental factor in the semiarid grasslands of northern China. With increased concentrations of atmospheric greenhouse gases, precipitation regimes will change, and high-impact weather events may be more common. Currently, many ecophysiological indicators are known to reflect drought conditions, but these indicators vary greatly among species, and few studies focus on the applicability of these drought indicators under high CO2 conditions. In this study, five precipitation levels (- 30%, - 15%, control, + 15%, and + 30%) were used to simulate the effects of precipitation change on 18 ecophysiological characteristics in Stipa bungeana, including leaf area, plant height, leaf nitrogen (N), and chlorophyll content, among others. Two levels of CO2 concentration (ambient, 390 ppm; 550 ppm) were used to simulate the effects of elevated CO2 on these drought indicators. Using gray relational analysis and phenotypic plasticity analysis, we found that total leaf area or leaf number (morphology), leaf water potential or leaf water content (physiology), and aboveground biomass better reflected the water status of S. bungeana under ambient and elevated CO2 than the 13 other analyzed variables. The sensitivity of drought indicators changed under the elevated CO2 condition. By quantifying the relationship between precipitation and the five most sensitive indicators, we found that the thresholds of precipitation decreased under elevated CO2 concentration. These results will be useful for objective monitoring and assessment of the occurrence and development of drought events in S. bungeana grasslands.

  20. Manganese oxalate nanorods as ballistic modifier for composite solid propellants

    Energy Technology Data Exchange (ETDEWEB)

    Singh, Supriya [Department of Chemistry, DDU Gorakhpur University, Gorakhpur 273009, U.P. (India); Chawla, Mohit [School of Basic Sciences, Indian Institute of Technology Mandi, Mandi 175005, H.P. (India); Siril, Prem Felix, E-mail: prem@iitmandi.ac.in [School of Basic Sciences, Indian Institute of Technology Mandi, Mandi 175005, H.P. (India); Singh, Gurdip [Department of Chemistry, DDU Gorakhpur University, Gorakhpur 273009, U.P. (India)

    2014-12-10

    Highlights: • Manganese oxalate nanorods were prepared using mild thermal precipitation and aging. • The nanorods were found to be efficient ballistic modifier for solid propellants. • The nanorods sensitized the thermolysis of ammonium perchlorate. • Controlled thermal decomposition of nanorods yielded manganese oxide nanoparticles. • MnO nanoparticles formed insitu in the condensed phase enhance the burning rates. - Abstract: Rod-shaped nanostructures of manganese oxalate (MnC{sub 2}O{sub 4}) were synthesized via mild thermal precipitation and aging process. Chemical composition of the MnC{sub 2}O{sub 4} nanorods was confirmed using Fourier transform infra-red (FTIR) spectroscopy and energy dispersive X-ray spectroscopy (EDS). X-ray diffraction (XRD) and selected area electron diffraction (SAED) studies revealed the crystal structure. Field emission scanning electron microscopy (FE-SEM) imaging and high resolution transmission electron microscopy (HR-TEM) were employed to study the structural features of the nanorods. The MnC{sub 2}O{sub 4} nanorods were found to be efficient ballistic modifier for the burning rate enhancement of composite solid propellants (CSPs). Thermal analysis using TGA-DSC showed that MnC{sub 2}O{sub 4} nanorods sensitized the thermal decomposition of ammonium perchlorate (AP) and the CSPs. Controlled thermal decomposition of the MnC{sub 2}O{sub 4} nanorods resulted in the formation of managanese oxide nanoparticles with mesoporosity. A plausible mechanism for the burning rate enhancement using MnC{sub 2}O{sub 4} nanorods was proposed.

  1. Non-invasive identification of metal-oxalate complexes on polychrome artwork surfaces by reflection mid-infrared spectroscopy.

    Science.gov (United States)

    Monico, Letizia; Rosi, Francesca; Miliani, Costanza; Daveri, Alessia; Brunetti, Brunetto G

    2013-12-01

    In this work a reflection mid-infrared spectroscopy study of twelve metal-oxalate complexes, of interest in art conservation science as alteration compounds, was performed. Spectra of the reference materials highlighted the presence of derivative-like and/or inverted features for the fundamental vibrational modes as result of the main contribution from the surface component of the reflected light. In order to provide insights in the interpretation of theses spectral distortions, reflection spectra were compared with conventional transmission ones. The Kramers-Kronig (KK) algorithm, employed to correct for the surface reflection distortions, worked properly only for the derivative-like bands. Therefore, to pay attention to the use of this algorithm when interpreting the reflection spectra is recommended. The outcome of this investigation was exploited to discriminate among different oxalates on thirteen polychrome artworks analyzed in situ by reflection mid-infrared spectroscopy. The visualization of the νs(CO) modes (1400-1200 cm(-1)) and low wavenumber bands (below 900 cm(-1)) in the raw reflection profiles allowed Ca, Cu and Zn oxalates to be identified. Further information about the speciation of different hydration forms of calcium oxalates were obtained by using the KK transform. The work proves reflection mid-infrared spectroscopy to be a reliable and sensitive spectro-analytical method for identifying and mapping different metal-oxalate alteration compounds on the surface of artworks, thus providing conservation scientists with a non-invasive tool to obtain information on the state of conservation and causes of alteration of artworks. Copyright © 2013 Elsevier B.V. All rights reserved.

  2. A kinetic and ESR investigation of iron(II) oxalate oxidation by hydrogen peroxide and dioxygen as a source of hydroxyl radicals

    DEFF Research Database (Denmark)

    Park, J S; Wood, P M; Davies, Michael Jonathan

    1997-01-01

    The reaction of Fe(II) oxalate with hydrogen peroxide and dioxygen was studied for oxalate concentrations up to 20 mM and pH 2-5, under which conditions mono- and bis-oxalate complexes (Fe[II](ox) and Fe[II](ox)2[2-]) and uncomplexed Fe2+ must be considered. The reaction of Fe(II) oxalate...... with hydrogen peroxide (Fe2+ + H2O2 --> Fe3+ + .OH + OH-) was monitored in continuous flow by ESR with t-butanol as a radical trap. The reaction is much faster than for uncomplexed Fe2+ and a rate constant, k = 1 x 10(4) M(-1) s(-1) is deduced for Fe(II)(ox). The reaction of Fe(II) oxalate with dioxygen...... by oxalate. Further ESR studies with DMPO as spin trap reveal that reaction of Fe(II) oxalate with hydrogen peroxide can also lead to formation of the carboxylate radical anion (CO2-), an assignment confirmed by photolysis of Fe(II) oxalate in the presence of DMPO....

  3. Production of mixed oxide fuel for fast reactor irradiation test by co-precipitation

    International Nuclear Information System (INIS)

    Todokoro, Akio; Masuda, Sumio; Naruki, Kaoru; Kaya, Akira; Koizumi, Masumichi

    1974-01-01

    Studies were made on the production of homogeneous mixed oxide by co-precipitation. Experiments were made on the effects of the addition rate of ammonia water, precipitation temperature, aging time of co-precipitate, and pH value. Plutonium refined by anion exchange was mixed with solution of uranium. The concentration of free acid in the mixed solution was adjusted to 1.5-2.0 M, and the total volume of the solution was made 3.01. The weight of Pu and U in the solution was 100g. The solution was kept at a definite temperature while being stirred. Concentrated ammonia solution was added to the solution at a definite rate. The precipitate thus formed was filtrated after aging, then dried for 24 hours at 100 +- 2 0 C. Dried co-precipitate was calcinated for 1 hr at 550 0 C. The reduction for 4 hours at 800 0 C gave the mixed powder of PuO 2 and UO 2 . After pressing, the powder was sintered for 2 hours at 1700 0 C. The shrinkage ratio decreased as the activity and tap density of the original powder increased. The activity determined by specific surface area increased as the rate of ammonia water addition increased, and as the precipitation temperature rose. Tap density was independent of the rate of addition of ammonia water. The activity of the powder increased and the tap density decreased as the aging time of precipitate increased. (Fukutomi, T.)

  4. Structural, Optical, Morphological and Microbial Studies on SnO₂ Nanoparticles Prepared by Co-Precipitation Method.

    Science.gov (United States)

    Arularasu, M V; Anbarasu, M; Poovaragan, S; Sundaram, R; Kanimozhi, K; Magdalane, C Maria; Kaviyarasu, K; Thema, F T; Letsholathebe, D; Mola, Genene T; Maaza, M

    2018-05-01

    Nanoparticles of tin oxide (SnO2) powders were prepared by co-precipitation method at 500 °C, 700 °C and 900 °C temperature. The sintered SnO2 nanoparticles, structural, optical, magnetic, morphological properties and microbial activity have been studied. XRD studies reveals that sintered powder which exhibits tetragonal crystal structure and both crystallinity as well as crystal size increase with increase in temperature. The morphological studies reveal randomly arranged grains with compact nature grain size increases with sintering temperature. The compositional analyses of SnO2 nanoparticles have been studied using X-ray photoelectron spectroscopy analysis. The optical band gap values of SnO2 nanoparticles were calculated to be about 4.3 eV in the temperature 500 °C, comparing with that of the bulk SnO2 3.78 eV, by optical absorption measurement. Room temperature M-H curve for pure SnO2 nanoparticles exhibits ferromagnetic behaviour. The tin oxide nanoparticles are acted as potential candidate material for bacterial and fungal activity.

  5. Acoustic Monitoring of Gravity-Driven Controls on CaCO3 Precipitates in a Fracture

    Science.gov (United States)

    Xu, Z.; Sheets, J.; Zhang, L.; Kim, D.; Kneafsey, T. J.; Cole, D. R.; Jun, Y. S.; Pyrak-Nolte, L. J.

    2017-12-01

    Sealing fractures by mineral precipitation is an important process for improving caprock integrity in subsurface reservoirs. In this study, the ability to monitor precipitate distribution in fractures with buoyant fluids was examined. Fractures with uniform aperture distributions of 0.5, 1.0 and 2.0 mm were created from acrylic plates to enable direct imaging of precipitate formation over time. CaCO3 precipitation was induced in a fracture from invasion of 1M CaCl2 and 0.3M Na2CO3 solutions. During chemical invasion, a fracture plane was oriented either parallel or perpendicular to gravity. Acoustic (P) wave transmission ( 1 MHz) and optical imaging were used to monitor the sample prior to, during and after fluid injection. Complementary X-ray computed tomography was performed throughout the experiments on vertical fractures and post injection for the horizontal fractures. Precipitate particle sizes during formation were determined using SAXS and WAXS. In both horizontal and vertical fractures, the density contrast between the two solutions affected the spatial distribution of precipitation. In vertical fractures, the denser CaCl2 solution almost completely displaced the NaCO3 solution, causing strong localization of precipitates. However, in the horizontal fractures, flow stratification occurred in the 2 mm aperture fractures, with the less dense Na2CO3 flowing over the CaCl2 solution, resulting in a more even distribution of precipitates cross the fracture plane. P-wave amplitudes increased up to 8% and the arrival time decreased with precipitate accumulation in the horizontal fracture. This is consistent with a three-layered approach as the seismic impedance inside the fracture increases. The initial contact between the two was observed as a decrease in the P-wave amplitude. As precipitates accumulated, the amplitude recovered and increased, with greater increases observed along the mixing flow path. Fractures in the subsurface may seal differently depending on

  6. Simplified method for the determination of strontium-90 in large amounts of bone-ash

    International Nuclear Information System (INIS)

    Patti, F.; Jeanmaire, L.

    1966-06-01

    The principle of the determination is based on a 3-step process: 1) concentrating the strontium by attacking the ash with nitric acid; 2) elimination of residual phosphoric ions by a double precipitation of strontium oxalate; and 3) extraction of yttrium 90, counted in the oxalate form. The advantages of the method: -) using simple techniques it makes it possible to process 50 g of ash; -) the initial concentration of strontium considerably reduces the volume of the solutions as well as the size of precipitates handled. Fuming nitric acid is used in a specially designed burette. (authors) [fr

  7. Fe(II)–Al(III) layered double hydroxides prepared by ultrasound-assisted co-precipitation method for the reduction of bromate

    International Nuclear Information System (INIS)

    Zhong, Yu; Yang, Qi; Luo, Kun; Wu, Xiuqiong; Li, Xiaoming; Liu, Yang; Tang, Wangwang; Zeng, Guangming; Peng, Bo

    2013-01-01

    Highlights: ► Fe(II)–Al(III) LDHs were synthesized by ultrasound-assisted co-precipitation method. ► The Fe–Al (30 min) exhibited highly reduction reactivity on bromate. ► Pseudo-first-order model described the experimental data well. ► The mechanisms of bromate removal were proposed. -- Abstract: Bromate is recognized as an oxyhalide disinfection byproduct in drinking water. In this paper, Fe(II)–Al(III) layered double hydroxides (Fe–Al LDHs) prepared by the ultrasound-assisted co-precipitation method were used for the reduction of bromate in solution. The Fe–Al LDHs particles were characterized by X-ray diffractometer, scanning electron microscopy and thermogravimetry–differential scanning calorimetry. It was found that ultrasound irradiation assistance promoted the formation of the hydrotalcite-like phase and then improved the removal efficiency of bromate. In addition, the effects of solid-to-solution ratio, contact time, initial bromate concentration, initial pH, coexisting anions on the bromate removal were investigated. The results showed the bromate with an initial concentration of 1.56 μmol/L could be completely removed from solution by Fe–Al LDHs within 120 min. When the initial bromate concentration was 7.81 μmol/L, the Fe–Al LDHs with irradiation time of 30 min exhibited the optimum removal efficiency and the bromate removal capacity (q e ) was 6.80 μmol/g. In addition, the appearance of sulfate and production of bromide were observed simultaneously in this process, which suggested that ion-exchange between sulfate and bromate, and the reduction of bromate to bromide by Fe 2+ were the main mechanisms responsible for the bromate removal by Fe–Al LDHs

  8. Magnetic Field Effects on CaCO3 Precipitation Process in Hard Water

    Directory of Open Access Journals (Sweden)

    Nelson Saksono

    2010-10-01

    Full Text Available Magnetic treatment is applied as physical water treatment for scale prevention especially CaCO3, from hard water in piping equipment by reducing its hardness.Na2CO3 and CaCl2 solution sample was used in to investigate the magnetic fields influence on the formation of particle of CaCO3. By changing the strength of magnetic fields, exposure time and concentration of samples solution, this study presents quantitative results of total scale deposit, total precipitated CaCO3 and morphology of the deposit. This research was run by comparing magnetically and non-magnetically treated  samples. The results showed an increase of deposits formation rate and total number of precipitated CaCO3 of magnetically treated samples. The increase of concentration solution sample will also raised the deposit under magnetic  field. Microscope images showed a greater number but smaller size of CaCO3 deposits form in magnetically treated samples, and aggregation during the processes. X-ray diffraction (XRD analysis showed that magnetically samples were dominated by calcite. But, there was a significant decrease of calcite’s peak intensities from magnetized  samples that indicated the decrease of the amount of calcite and an increase of total amorphous of deposits. This result  showed that magnetization of hard water leaded to the decreasing of ion Ca2+ due to the increasing of total CaCO3 precipitation process.

  9. Preparation and characterization of polyol assisted ultrafine Cu–Ni–Mg–Ca mixed ferrite via co-precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Boobalan, T. [Park College of Engineering and Technology, Coimbatore (India); Pavithradevi, S. [Department of Physics, Government College of Technology, Coimbatore (India); Suriyanarayanan, N., E-mail: nsuri22@gmail.com [Department of Physics, PSG Polytechnic College, Coimbatore (India); Manivel Raja, M. [Defence Metallurgical Research Laboratory, Ministry of Defence, Govt. of India, Hyderabad (India); Ranjith Kumar, E., E-mail: ranjueaswar@gmail.com [Dr. NGP Institute of Technology, Coimbatore (India)

    2017-04-15

    Nanocrystalline spinel ferrite of composition Cu{sub 0.2}Ni{sub 0.2}Mg{sub 0.2}Ca{sub 0.4}Fe{sub 2}O{sub 4} 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{sup −1} and 4000 cm{sup −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. - Highlights: • Polyol improves purity of the spinel ferrite. • TG curves confirm the single phase ferrite is obtained above 680 °C. • Super paramagnetic behavior is seen at lower annealing temperature. • Soft ferromagnetic behavior is obtained at 1050 °C.

  10. Improved CO sub 2 enhanced oil recovery -- Mobility control by in-situ chemical precipitation

    Energy Technology Data Exchange (ETDEWEB)

    Ameri, S.; Aminian, K.; Wasson, J.A.; Durham, D.L.

    1991-06-01

    The overall objective of this study has been to evaluate the feasibility of chemical precipitation to improve CO{sub 2} sweep efficiency and mobility control. The laboratory experiments have indicated that carbonate precipitation can alter the permeability of the core samples under reservoir conditions. Furthermore, the relative permeability measurements have revealed that precipitation reduces the gas permeability in favor of liquid permeability. This indicates that precipitation is occurring preferentially in the larger pores. Additional experimental work with a series of connected cores have indicated that the permeability profile can be successfully modified. However, Ph control plays a critical role in propagation of the chemical precipitation reaction. A numerical reservoir model has been utilized to evaluate the effects of permeability heterogeneity and permeability modification on the CO{sub 2} sweep efficiency. The computer simulation results indicate that the permeability profile modification can significantly enhance CO{sub 2} vertical and horizontal sweep efficiencies. The scoping studies with the model have further revealed that only a fraction of high permeability zones need to be altered to achieve sweep efficiency enhancement. 64 refs., 30 figs., 16 tabs.

  11. Structural and optical studies of Mg doped nanoparticles of chromium oxide (Cr2O3) synthesized by co-precipitation method

    Science.gov (United States)

    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).

  12. Synthesis and characterization of La(Cr,Fe,Mn)O{sub 3} nanoparticles obtained by co-precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Fabian, F.A., E-mail: fernandafabianro@gmail.com [Universidade Federal de Sergipe, Campus Prof. Aluísio Campos, Departamento de Física, 49100-000 São Cristóvão, SE (Brazil); Pedra, P.P.; Filho, J.L.S. [Universidade Federal de Sergipe, Campus Prof. Aluísio Campos, Departamento de Física, 49100-000 São Cristóvão, SE (Brazil); Duque, J.G.S.; Meneses, C.T. [Universidade Federal de Sergipe, Campus Prof. Alberto Carvalho, Departamento de Física, 49500-000 Itabaiana, SE (Brazil)

    2015-04-01

    Magnetic and structural properties have been investigated in La(Cr,Fe,Mn)O{sub 3} nanoparticles obtained by co-precipitation method. The X-ray diffraction measurements allied to Rietveld method confirm the formation of LaCrO{sub 3}, LaFeO{sub 3} and LaMnO{sub 3} nanoparticles with crystal structure orthorhombic (Pbnm), orthorhombic (Pnma) and rhombohedral (R-3c), respectively. We also verified an decreasing in the average crystallite size from 73 to 26 nm, depending of the transition metal. The magnetic measurements reveal an antiferromagnetic behavior for the LaCrO{sub 3} sample with T{sub N}~289 K, and a weak ferromagnetic ordering for the LaMnO{sub 3} sample with T{sub c}~200 K. - Highlights: • La(Cr,Fe,Mn)O{sub 3} nanoparticles were synthesized by coprecipitation method. • XRD results confirm the formation single phase in the compounds studied. • Magnetic property in the La(Fe,Cr,Mn)O{sub 3} nanoparticles dependent on the TM. • La(Cr,Fe)O{sub 3} nanoparticles presented behavior antiferromagnetic and LaMnO{sub 3} ferromagnetic.

  13. Oxalates in oca (New Zealand yam) (Oxalis tuberosa Mol.).

    Science.gov (United States)

    Ross, A B; Savage, G P; Martin, R J; Vanhanen, L

    1999-12-01

    Oca (Oxalis tuberosa Mol.) or New Zealand yam, in common with other members of this genus, contains oxalate, an antinutritive factor. Twelve South American and two New Zealand cultivars of oca were analyzed for total and soluble oxalate contents of the tubers. The range of total oxalate levels was 92-221 mg/100 g of fresh weight. Levels of soluble and total oxalate extracted from the tubers were not significantly different, suggesting that no calcium oxalate is formed in the tubers. The oxalate concentrations obtained in this study for oca suggest that previously reported values are too low and that oca is a moderately high oxalate-containing food. This is the first report of a tuber crop containing moderate to high levels of soluble oxalates in the tubers and no insoluble oxalates.

  14. One-step synthesis and characterizations of cerium oxide nanoparticles in an ambient temperature via Co-precipitation method

    Science.gov (United States)

    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.

  15. Preparation, characterization and catalytic effects of copper oxalate nanocrystals

    International Nuclear Information System (INIS)

    Singh, Gurdip; Kapoor, Inder Pal Singh; Dubey, Reena; Srivastava, Pratibha

    2012-01-01

    Graphical abstract: Prepared copper oxalate nanocrystals were characterized by FE-SEM and bright field TEM micrographs. Its catalytic activity was evaluated on the thermal decomposition of ammonium perchlorate using TG and TG-DSC techniques. Highlights: ► Preparation of nanocrystals (∼9.0 nm) of copper oxalate using Cu(NO 3 ) 2 ·2H 2 O, oxalic acid and acetone under thermal conditions. ► Method is simple and novel. ► Characterization using XRD, SEM, TEM, HRTEM and ED pattern. ► Catalytic activity of copper oxalate nanocrystals on AP thermal decomposition using thermal techniques (TG, TG-DSC and ignition delay). ► Kinetics of thermal decomposition of AP + CONs using isoconversional and model fitting kinetic approaches. - Abstract: Recent work has described the preparation and characterization of copper oxalate nanocrystals (CONs). It was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM) and electron diffraction pattern (ED). The catalytic activity of CONs on the thermal decomposition of ammonium perchlorate (AP) and composite solid propellants (CSPs) has been done by thermogravimetry (TG), differential scanning calorimetry (DSC) and ignition delay measurements. Burning rate of CSPs was also found to be enhanced in presence of copper oxalate nanocrystals. Kinetics of thermal decomposition of AP with and without CONs has also been investigated. The model free (isoconversional) and model-fitting kinetic approaches have been applied to data for isothermal TG decomposition.

  16. Isolation of oxalic acid tolerating fungi and decipherization of its potential to control Sclerotinia sclerotiorum through oxalate oxidase like protein.

    Science.gov (United States)

    Yadav, Shivani; Srivastava, Alok K; Singh, Dhanajay P; Arora, Dilip K

    2012-11-01

    Oxalic acid plays major role in the pathogenesis by Sclerotinia sclerotiorum; it lowers the pH of nearby environment and creates the favorable condition for the infection. In this study we examined the degradation of oxalic acid through oxalate oxidase and biocontrol of Sclerotinia sclerotiorum. A survey was conducted to collect the rhizospheric soil samples from Indo-Gangetic Plains of India to isolate the efficient fungal strains able to tolerate oxalic acid. A total of 120 fungal strains were isolated from root adhering soils of different vegetable crops. Out of 120 strains a total of 80 isolates were able to grow at 10 mM of oxalic acid whereas only 15 isolates were grow at 50 mM of oxalic acid concentration. Then we examined the antagonistic activity of the 15 isolates against Sclerotinia sclerotiorum. These strains potentially inhibit the growth of the test pathogen. A total of three potential strains and two standard cultures of fungi were tested for the oxalate oxidase activity. Strains S7 showed the maximum degradation of oxalic acid (23 %) after 60 min of incubation with fungal extract having oxalate oxidase activity. Microscopic observation and ITS (internally transcribed spacers) sequencing categorized the potential fungal strains into the Aspergillus, Fusarium and Trichoderma. Trichoderma sp. are well studied biocontrol agent and interestingly we also found the oxalate oxidase type activity in these strains which further strengthens the potentiality of these biocontrol agents.

  17. Biosynthesis of l-Ascorbic Acid and Conversion of Carbons 1 and 2 of l-Ascorbic Acid to Oxalic Acid Occurs within Individual Calcium Oxalate Crystal Idioblasts1

    Science.gov (United States)

    Kostman, Todd A.; Tarlyn, Nathan M.; Loewus, Frank A.; Franceschi, Vincent R.

    2001-01-01

    l-Ascorbic acid (AsA) and its metabolic precursors give rise to oxalic acid (OxA) found in calcium oxalate crystals in specialized crystal idioblast cells in plants; however, it is not known if AsA and OxA are synthesized within the crystal idioblast cell or transported in from surrounding mesophyll cells. Isolated developing crystal idioblasts from Pistia stratiotes were used to study the pathway of OxA biosynthesis and to determine if idioblasts contain the entire path and are essentially independent in OxA synthesis. Idioblasts were supplied with various 14C-labeled compounds and examined by micro-autoradiography for incorporation of 14C into calcium oxalate crystals. [14C]OxA gave heavy labeling of crystals, indicating the isolated idioblasts are functional in crystal formation. Incubation with [1-14C]AsA also gave heavy labeling of crystals, whereas [6-14C]AsA gave no labeling. Labeled precursors of AsA (l-[1-14C]galactose; d-[1-14C]mannose) also resulted in crystal labeling, as did the ascorbic acid analog, d-[1-14C]erythorbic acid. Intensity of labeling of isolated idioblasts followed the pattern OxA > AsA (erythorbic acid) > l-galactose > d-mannose. Our results demonstrate that P. stratiotes crystal idioblasts synthesize the OxA used for crystal formation, the OxA is derived from the number 1 and 2 carbons of AsA, and the proposed pathway of ascorbic acid synthesis via d-mannose and l-galactose is operational in individual P. stratiotes crystal idioblasts. These results are discussed with respect to fine control of calcium oxalate precipitation and the concept of crystal idioblasts as independent physiological compartments. PMID:11161021

  18. Hafnium(IV) complexation with oxalate at variable temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Friend, Mitchell T.; Wall, Nathalie A. [Washington State Univ., Pullmanm, WA (United States). Dept. of Chemistry

    2017-08-01

    Appropriate management of fission products in the reprocessing of spent nuclear fuel (SNF) is crucial in developing advanced reprocessing schemes. The addition of aqueous phase complexing agents can prevent the co-extraction of these fission products. A solvent extraction technique was used to study the complexation of Hf(IV) - an analog to fission product Zr(IV) - with oxalate at 15, 25, and 35 C in 1 M HClO{sub 4} utilizing a {sup 175+181}Hf radiotracer. The mechanism of the solvent extraction system of 10{sup -5} M Hf(IV) in 1 M HClO{sub 4} to thenoyltrifluoroacetone (TTA) in toluene demonstrated a 4{sup th}-power dependence in both TTA and H{sup +}, with Hf(TTA){sub 4} the only extractable species. The equilibrium constant for the extraction of Hf(TTA){sub 4} was determined to be log K{sub ex}=7.67±0.07 (25±1 C, 1 M HClO{sub 4}). The addition of oxalate to the aqueous phase decreased the distribution ratio, indicating aqueous Hf(IV)-oxalate complex formation. Polynomial fits to the distribution data identified the formation of Hf(ox){sup 2+} and Hf(ox){sub 2(aq)} and their stability constants were measured at 15, 25, and 35 C in 1 M HClO{sub 4}. van't Hoff analysis was used to calculate Δ{sub r}G, Δ{sub r}H, and Δ{sub r}S for these species. Stability constants were observed to increase at higher temperature, an indication that Hf(IV)-oxalate complexation is endothermic and driven by entropy.

  19. MRP-1 and BCRP Promote the Externalization of Phosphatidylserine in Oxalate-treated Renal Epithelial Cells: Implications for Calcium Oxalate Urolithiasis.

    Science.gov (United States)

    Li, YiFu; Yu, ShiLiang; Gan, XiuGuo; Zhang, Ze; Wang, Yan; Wang, YingWei; An, RuiHua

    2017-09-01

    To investigate the possible involvement of multidrug resistance-associated protein 1 (MRP-1) and breast cancer resistance protein (BCRP) in the oxalate-induced redistribution of phosphatidylserine (PS) in renal epithelial cell membranes. A western blot analysis was used to examine the MRP-1 and BCRP expression levels. Surface-expressed PS was detected by the annexin V-binding assay. The cell-permeable fluorogenic probe 2,7-dichlorofluorescein diacetate was used to measure the intracellular reactive oxygen species (ROS) level. A rat model of hyperoxaluria was obtained using 0.5% ethylene glycol and 1.0% ammonium chloride. In addition, certain animals received verapamil (50 mg/kg body weight), which is a common inhibitor of MRP-1 and BCRP. The degree of nephrolithiasis was assessed histomorphometrically using sections stained by Pizzolato method and by measuring the calcium oxalate crystal content in the renal tissue. Oxalate produced a concentration-dependent increase in the synthesis of MRP-1 and BCRP. Treatment with MK571 and Ko143 (MRP-1- and BCRP-specific inhibitors, respectively) significantly attenuated the oxalate-induced PS externalization. Adding the antioxidant N-acetyl-l-cysteine significantly reduced MRP-1 and BCRP expression. In vivo, markedly decreased nephrocalcinosis was observed compared with that in the rat model of hyperoxaluria without verapamil treatment. Oxalate induces the upregulation of MRP-1 and BCRP, which act as phospholipid floppases causing PS externalization in the renal epithelial cell membrane. The process is mediated by intracellular ROS production. The ROS-mediated increase in the synthesis of MRP-1 and BCRP can play an important role in hyperoxaluria-promoted calcium oxalate urolithiasis by facilitating phosphatidylserine redistribution in renal epithelial cells. Copyright © 2017 Elsevier Inc. All rights reserved.

  20. U{sub x}Th{sub 1-x}(C{sub 2}O{sub 4}){sub 2} solide characterisation studies

    Energy Technology Data Exchange (ETDEWEB)

    Carrigan, C.; Taylor, R.; Sarsfield, M. [National Nuclear Laboratory, Sellafield, Seascale, Cumbria, CA20 1PG (United Kingdom)

    2016-07-01

    Many advanced reprocessing schemes under development are aimed at co-processing and co-conversion of actinides, unlike current reprocessing plants that produce separate uranium and plutonium products. The most well developed option for the co-conversion stage is probably oxalate co-precipitation, followed by the thermal co-conversion to a mixed oxide product. It is thus envisaged that future processes will avoid separation of plutonium from uranium and instead allow part of the uranium to flow with the plutonium, resulting in co-precipitation as the oxalate, and finally co-conversion to a mixed uranium-plutonium oxide (MOX), which can be fabricated into recycled nuclear fuel for further energy generation. The co-crystallisation of uranium (IV) and plutonium (III) into a single oxalate structure ensures the homogenous distribution of the 2 actinides at the molecular scale. The joint conversion of uranium and plutonium to the oxide form makes it possible to remove the complicated step of blending and grinding the 2 distinct oxide powders, as currently employed for the purposes of MOX fuel fabrication. This concept can also be extended to other actinides, including minor actinides from partitioning processes such as SANEX (Selective Actinide Extraction) and GANEX (Grouped Actinide Extraction) processes or even a thorium containing product from recycle of thorium based fuels. A selection of U{sub x}Th{sub 1-x}(C{sub 2}O{sub 4}){sub 2} solids at varying concentrations of uranium and thorium were prepared by oxalate co-precipitation. Uranium (VI) was conditioned electrochemically at -0.7 V to uranium (IV), in the presence of hydrazine. The reduced uranium (IV) in nitric acid was mixed with thorium nitrate solutions at different concentration ratios with oxalic acid. The mixed tetravalent uranium-thorium oxalate solid products have been characterised by Raman and IR spectroscopies. The influence of thorium substituted into the uranium oxalate structure was evaluated

  1. U_xTh_1_-_x(C_2O_4)_2 solide characterisation studies

    International Nuclear Information System (INIS)

    Carrigan, C.; Taylor, R.; Sarsfield, M.

    2016-01-01

    Many advanced reprocessing schemes under development are aimed at co-processing and co-conversion of actinides, unlike current reprocessing plants that produce separate uranium and plutonium products. The most well developed option for the co-conversion stage is probably oxalate co-precipitation, followed by the thermal co-conversion to a mixed oxide product. It is thus envisaged that future processes will avoid separation of plutonium from uranium and instead allow part of the uranium to flow with the plutonium, resulting in co-precipitation as the oxalate, and finally co-conversion to a mixed uranium-plutonium oxide (MOX), which can be fabricated into recycled nuclear fuel for further energy generation. The co-crystallisation of uranium (IV) and plutonium (III) into a single oxalate structure ensures the homogenous distribution of the 2 actinides at the molecular scale. The joint conversion of uranium and plutonium to the oxide form makes it possible to remove the complicated step of blending and grinding the 2 distinct oxide powders, as currently employed for the purposes of MOX fuel fabrication. This concept can also be extended to other actinides, including minor actinides from partitioning processes such as SANEX (Selective Actinide Extraction) and GANEX (Grouped Actinide Extraction) processes or even a thorium containing product from recycle of thorium based fuels. A selection of U_xTh_1_-_x(C_2O_4)_2 solids at varying concentrations of uranium and thorium were prepared by oxalate co-precipitation. Uranium (VI) was conditioned electrochemically at -0.7 V to uranium (IV), in the presence of hydrazine. The reduced uranium (IV) in nitric acid was mixed with thorium nitrate solutions at different concentration ratios with oxalic acid. The mixed tetravalent uranium-thorium oxalate solid products have been characterised by Raman and IR spectroscopies. The influence of thorium substituted into the uranium oxalate structure was evaluated. Several vibrational modes

  2. Evaluation of Three Chitin Metal Silicate Co-Precipitates as a Potential Multifunctional Single Excipient in Tablet Formulations

    Directory of Open Access Journals (Sweden)

    Rana Al-Shaikh Hamid

    2010-05-01

    Full Text Available The performance of the novel chitin metal silicate (CMS co-precipitates as a single multifunctional excipient in tablet formulation using direct compression and wet granulation methods is evaluated. The neutral, acidic, and basic drugs Spironolactone (SPL, ibuprofen (IBU and metronidazole (MET, respectively, were used as model drugs. Commercial Aldactone®, Fleximex® and Dumazole® tablets containing SPL, IBU and MET, respectively, and tablets made using Avicel® 200, were used in the study for comparison purposes. Tablets of acceptable crushing strength (>40 N were obtained using CMS. The friability values for all tablets were well below the maximum 1% USP tolerance limit. CMS produced superdisintegrating tablets (disintegration time < 1 min with the three model drugs. Regarding the dissolution rate, the sequence was as follow: CMS > Fleximex® > Avicel® 200, CMS > Avicel® 200 > Dumazole® and Aldactone® > Avicel® 200 > CMS for IBU, MET and SPL, respectively. Compressional properties of formulations were analyzed using density measurements and the compression Kawakita equation as assessment parameters. On the basis of DSC results, CMS co precipitates were found to be compatible with the tested drugs. Conclusively, the CMS co-precipitates have the potential to be used as filler, binder, and superdisintegrant, all-in-one, in the design of tablets by the direct compression as well as wet granulation methods.

  3. Two novel metal-organic coordination polymers based on diphosphonate and oxalate: Synthesis, structures and properties

    Science.gov (United States)

    Niu, Qing-Jun; Zheng, Yue-Qing; Zhou, Lin-Xia; Zhu, Hong-Lin

    2015-07-01

    Two 2-(1-imidazole)-1-hydroxyl-1,1'-ethylidenediphosphonato and oxalic acid bridged coordination polymers (H2en)[Co3(H2zdn)2(ox)(H2O)2] (1) and Cd2(H2zdn)(ox)0.5(H2O) (2) (2-(1-imidazole)-1-hydroxyl-1,1'-ethylidenediphosphonic acid=H5zdn; oxalic acid=H2ox) were synthesized under hydrothermal conditions and characterized by the infrared (IR), thermogravimetric analyses (TGA), elemental analyses (EA) and X-ray diffraction (XRD). Compound 1 is bridged by phosphonate anions to 1D chain, and further linked by oxalate anions to 2D layer. Compound 2 is bridged by O-P-O units of H5zdn to the layer, and then pillared by oxalate anions to generate 3D frameworks. Compound 1 shows anti-ferromagnetic behaviors analyzed with the temperature-dependent zero-field ac magnetic susceptibilities, while compound 2 exhibits an influence on the luminescent property.

  4. Efficient electron-induced removal of oxalate ions and formation of copper nanoparticles from copper(II oxalate precursor layers

    Directory of Open Access Journals (Sweden)

    Kai Rückriem

    2016-06-01

    Full Text Available Copper(II oxalate grown on carboxy-terminated self-assembled monolayers (SAM using a step-by-step approach was used as precursor for the electron-induced synthesis of surface-supported copper nanoparticles. The precursor material was deposited by dipping the surfaces alternately in ethanolic solutions of copper(II acetate and oxalic acid with intermediate thorough rinsing steps. The deposition of copper(II oxalate and the efficient electron-induced removal of the oxalate ions was monitored by reflection absorption infrared spectroscopy (RAIRS. Helium ion microscopy (HIM reveals the formation of spherical nanoparticles with well-defined size and X-ray photoelectron spectroscopy (XPS confirms their metallic nature. Continued irradiation after depletion of oxalate does not lead to further particle growth giving evidence that nanoparticle formation is primarily controlled by the available amount of precursor.

  5. Effect of synthesis conditions on the preparation of YIG powders via co-precipitation method

    International Nuclear Information System (INIS)

    Rashad, M.M.; Hessien, M.M.; El-Midany, A.; Ibrahim, I.A.

    2009-01-01

    Yttrium iron garnet (YIG) (Y 3 Fe 5 O 12 ) powders have been synthesized through a co-precipitation method in the presence of sodium bis(2-ethylhexylsulfosuccinate), AOT as an anionic surfactant. The garnet precursors produced were obtained from aqueous iron and yttrium nitrates mixtures using 5 M sodium hydroxide at pH 10. A statistical Box-Behnken experimental design was used to investigate the effect of the main parameters (i.e. AOT surfactant concentration, annealing time and temperature) on YIG powder formation, crystallite size, morphology and magnetic properties. YIG particles were investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), and vibrating sample magnetometer. XRD revealed that the formation of single cubic phase of YIG was temperature dependent and increased by increasing the annealing temperature from 800 to 1200 o C. SEM micrographs showed that the addition of AOT surfactant promoted the microstructure of YIG in crystalline cubic-like structure. The magnetic properties were sensitive to the synthesis variables of annealing temperature, time and AOT surfactant concentration. The maximum saturation magnetization (28.13 emu/g), remanence magnetization (21.57 emu/g) and coercive force (703 Oe) were achieved at an annealing temperature of 1200 o C, time 2 h and 500 ppm of AOT surfactant concentration.

  6. A new fabrication route for SFR fuel using (U, Pu)O{sub 2} powder obtained by oxalic co-conversion

    Energy Technology Data Exchange (ETDEWEB)

    Vaudez, Stéphane, E-mail: stephane.vaudez@cea.fr [CEA, DEN, DEC, SPUA, Cadarache, F-13108 Saint-Paul-Lez-Durance (France); Belin, Renaud C.; Aufore, Laurence; Sornay, Philippe [CEA, DEN, DEC, SPUA, Cadarache, F-13108 Saint-Paul-Lez-Durance (France); Grandjean, Stéphane [CEA, DEN, DRCP, DIR, Marcoule, F-30207 Bagnols sur Cèze (France)

    2013-11-15

    The standard powder metallurgy preparation of SFR (Sodium Fast Reactor) oxide fuel involves UO{sub 2} and PuO{sub 2} co-milling. An alternative route, using a solid-solution of mixed oxide obtained by oxalic co-conversion as the starting material, is presented. It was used to manufacture nuclear fuels for the “COPIX” irradiation conducted in the Phenix SFR. Two processes using co-converted powders were tested to elaborate fuel pellets: (1) the Direct Process that consists in pressing and sintering the mixed oxide with the final Pu content and (2) the Dilution Process, which involves the dilution of a high Pu content mixed oxide with UO{sub 2}. After studying the structural and microstructural evolution with temperature of these innovative raw materials, the elaboration parameters were adjusted to obtain final pellets in accordance with the Phenix fuel specifications. This study demonstrates the feasibility of such new fabrication route at laboratory scale and, from a more fundamental prospect, allows a better understanding of the underlying phenomena involved during sintering.

  7. (Dimethylphosphorylmethanaminium hydrogen oxalate–oxalic acid (2/1

    Directory of Open Access Journals (Sweden)

    Sebastian Bialek

    2014-03-01

    Full Text Available The reaction of (dimethylphosphorylmethanamine (dpma with oxalic acid in ethanol yielded the title solvated salt, C3H11NOP+·C2HO4−·0.5C2H2O4. Its asymmetric unit consists of one dpmaH+ cation, one hydrogen oxalate anion and a half-molecule of oxalic acid located around a twofold rotation axis. The H atom of the hydrogen oxalate anion is statistically disordered over two positions that are trans to each other. The hydrogen oxalate monoanion is not planar (bend angle ∼16° whereas the oxalic acid molecule shows a significantly smaller bend angle (∼7°. In the crystal, the components are connected by strong O—H...O and much weaker N—H...O hydrogen bonds, leading to the formation of layers extending parallel to (001. The structure was refined from a racemically twinned crystal with twin components in an approximate 1:1 ratio.

  8. Mixing state of oxalic acid containing particles in the rural area of Pearl River Delta, China: implications for the formation mechanism of oxalic acid

    Directory of Open Access Journals (Sweden)

    C. Cheng

    2017-08-01

    Full Text Available The formation of oxalic acid and its mixing state in atmospheric particulate matter (PM were studied using a single-particle aerosol mass spectrometer (SPAMS in the summer and winter of 2014 in Heshan, a supersite in the rural area of the Pearl River Delta (PRD region in China. Oxalic-acid-containing particles accounted for 2.5 and 2.7 % in total detected ambient particles in summer and winter, respectively. Oxalic acid was measured in particles classified as elemental carbon (EC, organic carbon (OC, elemental and organic carbon (ECOC, biomass burning (BB, heavy metal (HM, secondary (Sec, sodium-potassium (NaK, and dust. Oxalic acid was found predominantly mixing with sulfate and nitrate during the whole sampling period, likely due to aqueous-phase reactions. In summer, oxalic-acid-containing particle number and ozone concentration followed a very similar trend, which may reflect the significant contribution of photochemical reactions to oxalic acid formation. The HM particles were the most abundant oxalic acid particles in summer and the diurnal variations in peak area of iron and oxalic acid show opposite trends, which suggests a possible loss of oxalic acid through the photolysis of iron oxalato-complexes during the strong photochemical activity period. In wintertime, carbonaceous particles contained a substantial amount of oxalic acid as well as abundant carbon clusters and BB markers. The general existence of nitric acid in oxalic-acid-containing particles indicates an acidic environment during the formation process of oxalic acid. The peak areas of nitrate, sulfate and oxalic had similar temporal change in the carbonaceous type oxalic acid particles, and the organosulfate-containing oxalic acid particles correlated well with total oxalic acid particles during the haze episode, which suggests that the formation of oxalic acid is closely associated with the oxidation of organic precursors in the aqueous phase.

  9. Dating oxalate minerals in rock surface deposits

    International Nuclear Information System (INIS)

    Watchman, A.

    2001-01-01

    Oxalate minerals are found associated with rocks, mineral coatings, micro-organisms, plants and animals. They are important in archaeology because they have been found intimately associated with organic binders in prehistoric paints. Oxalate minerals also accumulate in the coatings on rock shelter walls and fallen ceiling slabs where they form the natural backing supports for painting and opaque laminates covering engravings. Though the relationship between anthropogenic activity in a rock shelter and oxalate formation is often uncertain, the radiocarbon age of the oxalate may provide the only means for determining the antiquity of a rock painting or engraving. This paper examines the history of dating oxalate minerals at archaeological sites and provides insights into achieving reliable age estimates. (author). 37 refs., 1 fig., 2 tabs

  10. Pathology and Epidemiology of Oxalate Nephrosis in Cheetahs.

    Science.gov (United States)

    Mitchell, Emily P; Church, Molly E; Nemser, Sarah M; Yakes, Betsy Jean; Evans, Eric R; Reimschuessel, Renate; Lemberger, Karin; Thompson, Peter N; Terio, Karen A

    2017-11-01

    To investigate cases of acute oxalate nephrosis without evidence of ethylene glycol exposure, archived data and tissues from cheetahs ( Acinonyx jubatus) from North America ( n = 297), southern Africa ( n = 257), and France ( n = 40) were evaluated. Renal and gastrointestinal tract lesions were characterized in a subset of animals with ( n = 100) and without ( n = 165) oxalate crystals at death. Crystals were confirmed as calcium oxalate by Raman spectroscopy in 45 of 47 cheetahs tested. Crystals were present in cheetahs from 3.7 months to 15.9 years old. Cheetahs younger than 1.5 years were less likely to have oxalates than older cheetahs ( P = .034), but young cheetahs with oxalates had more oxalate crystals than older cheetahs ( P Cheetahs with oxalate crystals were more likely to have renal amyloidosis, interstitial nephritis, or colitis and less likely to have glomerular loop thickening or gastritis than those without oxalates. Crystal number was positively associated with renal tubular necrosis ( P ≤ .001), regeneration ( P = .015), and casts ( P ≤ .001) but inversely associated with glomerulosclerosis, renal amyloidosis, and interstitial nephritis. Crystal number was unrelated to the presence or absence of colitis and was lower in southern African than American and European animals ( P = .01). This study found no evidence that coexisting chronic renal disease (amyloidosis, interstitial nephritis, or glomerulosclerosis), veno-occlusive disease, gastritis, or enterocolitis contributed significantly to oxalate nephrosis. Oxalate-related renal disease should be considered as a potential cause of acute renal failure, especially in young captive cheetahs. The role of location, diet, stress, and genetic predisposition in the pathogenesis of oxalate nephrosis in cheetahs warrants further study.

  11. Study of structural phase transformation and hysteresis behavior of inverse-spinel α-ferrite nanoparticles synthesized by co-precipitation method

    Science.gov (United States)

    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.

  12. The promotion effect of coexisting hygroscopic composition on the reaction between oxalic acid and calcite during humidifying process

    Science.gov (United States)

    Ma, Q.; He, H.

    2012-12-01

    Internally mixed oxalic acid with mineral dust has been frequently detected in field measurements (Sullivan and Prather, 2007; Wang et al., 2012; Yang et al., 2009). Meanwhile, Furukawa and Takahashi (Furukawa and Takahashi, 2011) found that most of the oxalic acid in mineral mixture is present as metal oxalate complexes in the aerosols, however, the formation mechanism of these complexes is not well known. It was reported that cloud process of H2C2O4/CaCO3 mixture could lead to the formation of calcium oxalate (Gierlus et al., 2012). Recently, we used Raman spectroscopy to investigate the hygroscopic behavior of H2C2O4/CaCO3 mixture below saturation condition as well as the effect of coexisting hygroscopic compositions, e.g. Ca(NO3)2, NaCl, NH4NO3, and (NH4)2SO4. It was found that there was no interaction between H2C2O4 and calcite without third component during humidifying process under ambient condition. In contrast, the presence of coexisting Ca(NO)3, NaCl, or NH4NO3 could promote the reaction between H2C2O4 and calcite by providing an aqueous circumstance after deliquescence, resulting in the formation of calcium oxalate hydrates. Moreover, substitution of strong acid (HNO3) by medium acid (H2C2O4) occurred when water vapor was absorbed in Ca(NO3)2/H2C2O4 mixture (Ma and He, 2012). As for (NH4)2SO4, there existed a competition effect between (NH4)2SO4 and H2C2O4 for the reaction with CaCO3. CaCO3 was preferentially reacted with (NH4)2SO4 to form gypsum in the solution, while the residual NH4+ and C2O42- ions were bonded to (NH4)2C2O4 after efflorescence. These results implies a potential formation pathway of metal oxalate complexes in the atmosphere and also suggests that synergistic effect between different constituents in humidifying process of mixed particles should be considered in future hygroscopic behavior studies.

  13. Novel Inorganic Coordination Polymers Based on Cadmium Oxalates

    Science.gov (United States)

    Prasad, P. A.; Neeraj, S.; Vaidhyanathan, R.; Natarajan, Srinivasan

    2002-06-01

    Three new cadmium oxalate coordination polymers, I-III, with extended layered structures have been synthesized in the presence of imidazole. While I was prepared by the reaction between imidazolium oxalate and Cd, II and III were synthesized from their constituents using hydrothermal methods. [Cd(C2O4)(C3N2H4)]∞ (I): monoclinic, space group P21/c (no. 14), a=8.7093(1) Å, b=9.9477(3) Å, c=8.4352 Å, β=93.796(1)°, Z=4; [Cd(C2O4)2(C3N2H4)3(H2O)]∞ (II): monoclinic, space group P21/c (no. 14), a=7.8614(2) Å, b=14.9332(3) Å, c=15.9153(4) Å β=94.587(1)°, Z=4; [Cd(C2O4)2(C3N2H4)3(H2O)]∞ (III): monoclinic, space group P21/c (no. 14), a=11.844(2) Å, b=9.066(1) Å, c=18.583(2) Å, β=103.84(2)°, Z=4. While the structure of I is made from CdO5N distorted octahedra linked with oxalate, II and III are built-up from CdO6N, CdO5N2 distorted pentagonal bi-pyramids connected to oxalate units. The framework formulas of II and III are identical and their structures closely related. In all the cases, the networking between the Cd-O/N polyhedra and oxalates give rise to layered architectures with the amine molecules pointing in a direction perpendicular to the layers (in the inter-lamellar region). The difference in the linkages between the oxalates and the Cd atoms in I-III, produces unusual Cd-O-Cd one-dimensional chains, which have been observed for the first time.

  14. an oxalate-peroxide complex used in the preparation of doped barium titanate

    NARCIS (Netherlands)

    van der Gijp, S.; Winnubst, Aloysius J.A.; Verweij, H.

    1998-01-01

    A method is described for the preparation of homogeneously doped barium titanate, which can be applied in non-linear dielectric elements. Ba and Ti salts are dissolved, mixed with hydrogen peroxide and added to a solution of ammonium oxalate, resulting in the formation of an insoluble peroxo-oxalate

  15. Intercomparison of the measurements of oxalic acid in aerosols by gas chromatography and ion chromatography

    Science.gov (United States)

    Kawamura, Kimitaka; Barrie, Leonard A.; Toom-Sauntry, Desiree

    2010-12-01

    Oxalate, the anion of oxalic acid, is one of the most abundant measurable organic species in atmospheric aerosols. Traditionally, this bifunctional species has been measured by gas chromatography (GC) after derivatization to butyl ester and by ion chromatography (IC) without derivatization. However, there are few published comparisons of the two techniques. Here, we report the results of an intercomparison study for the measurement of oxalic acid in Arctic aerosols (oxalic acid by GC ranged from 6.5-59.1 ng m -3 (av. 26.0 ng m -3, median 26.2 ng m -3) whereas those by IC ranged from 6.6-52.1 ng m -3 (av. 26.6 ng m -3, median 25.4 ng m -3). They showed a good correlation ( r = 0.84) with a slope of 0.96. Thus, observations of oxalate obtained by GC employing dibutyl esters are almost equal to those by IC. Because the accuracy of oxalic acid by GC method largely depends on the method used, it is important to strictly examine the recovery in each study.

  16. Green and red luminescence in co-precipitation synthesized Pr:LuAG nanophosphor

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, S. Arun; Kumar, K. Ashok; Gunaseelan, M.; Senthilselvan, J., E-mail: jsselvan@hotmail.com [Department of Nuclear Physics, University of Madras, Guindy Campus, Chennai–600 025, Tamil Nadu (India); Asokan, K. [Materials Science Group, Inter University Accelerator Centre, New Delhi-110067 (India)

    2016-05-06

    Pr:LuAG nanophosphor is an effective candidate in magnetic resonance imaging coupled positron emission tomography (MRI-PET) for medical imaging and scintillator applications. LuAG:Pr (0.05, 0.15 mol%) nanoscale ceramic powders were synthesized by co-precipitation method using urea as precipitant. Effect of antisite defect on structure and luminescence behavior was investigated. Pr:LuAG nanoceramic powders are found crystallized in cubic structure by high temperature calcination at 1400 °C and it shows antisite defect. HR-SEM analysis revealed spherically shaped Pr:LuAG nanoceramic particulate powders with ∼100 nm size. By the excitation at 450 nm, Pr:LuAG nanophosphor exhibit green to red luminescence in the wavelength range of 520 to 680 nm, which is originated from multiplet transition of Pr{sup 3+} ions.

  17. About the role of physico-chemical properties and hydrodynamics on the progress of a precipitation reaction: the case of cerium oxalate particles produced during the coalescence of drops

    International Nuclear Information System (INIS)

    Jehannin, Marie

    2015-01-01

    The nucleation and growth of solid particles resulting from a precipitation process is an important topic both for fundamental science and industrial applications. In a precipitation process, different reactants, which are individually soluble in the same solvent, get in contact and react to form insoluble solid particles (the precipitate). The properties of the produced particles are the result of a strong coupling between the chemical reaction and the reactants feed and mixing rates. The latter are mainly provided by diffusive and convective transport through a reaction-diffusion-convection process. In the emulsion precipitation process considered here the reactants are enclosed into droplets. The local transport conditions can be modified in many ways by tuning the relevant parameters and thus be used to control the properties of the precipitated particles. The aim of this study is to investigate the impact of local flow and mixing conditions during the coalescence on the precipitates properties, mainly their size, morphology and distribution. The test system consists of two coalescing droplets: one drop contains oxalic acid dissolved in an aqueous solution, while the other one contains cerium nitrate. Upon contact of the two miscible solutions a precipitate of cerium oxalate is formed. Besides, by adding chosen amounts of diols into the droplets, their surface tensions can be adjusted. Differences in surface tension cause a surface tension gradient in the section where both drops get in contact. This can lead to a Marangoni flow directed from the low surface tension interface to the high surface tension interface. This local convective flow will modify the local mixing conditions of the two solutions. This study focuses on how, where, when, which precipitate forms as function of the initial stoichiometry of the reactants and of the process conditions (e.g. the mixing conditions affected by the Marangoni flow). For this purpose, two configurations of coalescing

  18. Magnetite nanoparticles prepared by co-precipitation method in different conditions

    Energy Technology Data Exchange (ETDEWEB)

    Aphesteguy, J.C., E-mail: caphestegu@fi.uba.ar [LAFMACEL-INTECIN, Facultad de Ingeniería, UBA, Paseo Colón 850, C1063EHA Buenos Aires (Argentina); Kurlyandskaya, G.V. [Universidad del País Vasco UPV-EHU, Dept. Electricidad y Electronica, 48940 Leioa (Spain); Ural Federal University, Dept. Magnetism and Magnetic Nanomaterials, 620000 Ekaterinburg (Russian Federation); Celis, J.P. de [National Technology University (UTN), Facultad Regional Avellaneda, Department of Chemistry (Argentina); Safronov, A.P. [Ural Federal University, Dept. Magnetism and Magnetic Nanomaterials, 620000 Ekaterinburg (Russian Federation); Institute of Electrophysics UD RAS, Ekaterinburg 620016 (Russian Federation); Schegoleva, N.N. [Institute of Metal Physics UD RAS, Ekaterinburg 620044 (Russian Federation)

    2015-07-01

    Magnetic nanoparticles (MNPs) of pure magnetite (Fe{sub 3}O{sub 4}) were prepared in an aqueous solution (sample M−I) and in a water-ethyl alcohol mixture (sample M−II) by the co-precipitation method. The structure and magnetic properties of both samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), magnetic (M−H) and microwave measurements (FMR). The mean average particle diameter and particle size distribution was evaluated by the Dynamic Light Scattering (DLS) and Brunauer- Emmett-Teller techniques (BET). The Quantitative chemical analysis of iron was performed by Inductively Coupled Plasma (ICP)- Atomic Emission Spectroscopy (AES) technique. The MNPs prepared in aqueous solution show a higher grain than those prepared in the water-ethyl alcohol mixture. The type of phase structure in both cases can be defined as “defective spinel”. The shape of the majority of M−I MNPs is octahedral. The shape of the majority of M−II MNPs is cubic. The specific surface area of MNPs was as high as 14.4 m{sup 2}/g for M−I sample and 77.8 m{sup 2}/g for sample M–II. The obtained saturation magnetization values of 75 emu/g (M−I) and 68 emu/g (M−II) are consistent with expected values for magnetite MNPs of observed sizes. Ferromagnetic resonance (FMR) measurements confirmed that MNPs of both types are magnetically homogeneous materials. FMR lines' position and line widths can be understood by invoking the local dipolar fields, deviations from sphericity, magnetocrystalline anisotropy and stresses. M−I sample shows sizeable zero field microwave absorption which is absent in the M−II case. The differences in microwave behaviour of M−I and M−II MNPs can be used in the design of microwave radiation absorbing multilayers. - Highlights: • Magnetite nanoparticles were prepared in two different conditions. • Specific surface area of sample prepared in water- ethanol mix is

  19. Selective removal of Cs and Re by precipitation in a Na2CO3-H2O2 solution

    International Nuclear Information System (INIS)

    Eil-Hee Lee; Jae-Gwan Lim; Dong-Yong Chung; Han-Beom Yang; Kwang-Wook Kim

    2010-01-01

    The removal of Cs and Re (as a surrogate for Tc) by selective precipitation from the simulated fission products which were co-dissolved with uranium during the oxidative dissolution of spent fuel in a Na 2 CO 3 -H 2 O 2 solution was investigated in this study. The precipitations of Cs and Re were examined by introducing sodium tetraphenylborate (NaTPB) and tetraphenylohosponium chloride (TPPCl), respectively. The precipitation of Cs by NaTPB and that of Re by TPPCl each took place within 5 min, and an increase in temperature up to 50 deg C and a stirring speed up to 1000 rpm hardly affected their precipitation rates. The most important factor in the precipitation with NaTPB and TPPCl was found to be a pH of the solution after precipitation. Since Mo tends to co-precipitate with Cs or Re at a lower pH, an effective precipitation with NaTPB and TPPCl was done at pH of above 9 without the co-precipitation of Mo. More than 99% of Cs and Re were precipitated when the initial concentration ratio of NaTPB to Cs was above 1 and when that of TPPCl to Re was above 1. The precipitation of Cs and Re was never affected by the concentration of Na 2 CO 3 and H 2 O 2 , even though they were raised up to 1.5 and 1.0 M, respectively. Precipitation yields of Cs and Re in a Na 2 CO 3 -H 2 O 2 solution were found to be dependent on the concentration ratios of [NaTBP]/[Cs] and [TPPCl]/[Re]. (author)

  20. Synthesis of Sr- and Mg- doped lanthanum gallate by carbonate co-precipitation

    International Nuclear Information System (INIS)

    Sunitha, Y.; Narasimham, K.V.N.S.V.P.L.; Raju, V.S.; Kumar, Sanjiv

    2010-01-01

    Sr- and Mg- doped lanthanum gallate (LSGM) are promising electrolytes for low temperature solid oxide fuel cells (SOFCs) in view of their high ionic conductivity and stability over a wide range of oxygen partial pressures. LSGM powders are usually prepared by solid-state reactions. However high sintering temperature (∼ 1500 deg C) required for densification and the formation of secondary phases are the major drawbacks of the method. Wet-chemical method is a suitable alternative to solid-state synthesis with the prospect of the realisation of phase pure material with good sinterability at comparatively lower temperatures. In this paper we present the results of our investigation on the synthesis of LaGaO 3 and LSGM by a wet-chemical method through carbonate co-precipitation using ammonium carbonate and ammonium bicarbonate as precipitants. Phase and microstructural evolution of the material have been studied by XRD and SEM respectively, while compositional analysis has been performed by ion beam analysis (IBA) techniques. In addition we have also investigated the incorporation of Sr and Mg in the lattice of LaGaO 3 by (a) solid-state reaction route and (b) wet-chemical approach

  1. 3.2.1. Synthesis, crystal and molecular structure of catena-(bis(µ1-oxalic acid-µ3-hydrogen oxalate-di-aqua-sodium(I.

    Directory of Open Access Journals (Sweden)

    Olga Kovalchukova*, Sergey Aldoshin, Andrey Utenyshev, Konstantin Bogenko, Valeriy Tkachev

    2015-07-01

    Full Text Available The crystal and molecular structure of catena-(bis(µ- oxalic acid-µ-hydrogen oxalate-di-aqua-sodium(I was detected by X-Ray analysis. The compound crystallizes in the triclinic space group P-1, with a(Å 6.2378(12; b(Å 7,1115(14; c(Å 10.489(2; α(° 94.65(3; β(° 100.12(3; γ(° 97.78(3. The sodium cation in the title compound is eight coordinated and forms a square antiprism. It is surrounded by two molecules of oxalic acid, one hydrogen oxalate anion and one water molecule. Both oxalic acid and hydrogen oxalate anion act as polydentate bridging ligands. Centrosymmetric sodium cations are bounded by hydrogen oxalate anions through a system of H bonds involving the molecules of oxalic acid. In the lattice, the 3D structure stabilized by H bonds is formed.

  2. Total and soluble oxalate content of some Indian spices.

    Science.gov (United States)

    Ghosh Das, Sumana; Savage, G P

    2012-06-01

    Spices, such as cinnamon, cloves, cardamom, garlic, ginger, cumin, coriander and turmeric are used all over the world as flavouring and colouring ingredients in Indian foods. Previous studies have shown that spices contain variable amounts of total oxalates but there are few reports of soluble oxalate contents. In this study, the total, soluble and insoluble oxalate contents of ten different spices commonly used in Indian cuisine were measured. Total oxalate content ranged from 194 (nutmeg) to 4,014 (green cardamom) mg/100 g DM, while the soluble oxalate contents ranged from 41 (nutmeg) to 3,977 (green cardamom) mg/100 g DM. Overall, the percentage of soluble oxalate content of the spices ranged from 4.7 to 99.1% of the total oxalate content which suggests that some spices present no risk to people liable to kidney stone formation, while other spices can supply significant amounts of soluble oxalates and therefore should be used in moderation.

  3. Atmospheric production of oxalic acid/oxalate and nitric acid/nitrate in the Tampa Bay airshed: Parallel pathways

    Science.gov (United States)

    Martinelango, P. Kalyani; Dasgupta, Purnendu K.; Al-Horr, Rida S.

    Oxalic acid is the dominant dicarboxylic acid (DCA), and it constitutes up to 50% of total atmospheric DCAs, especially in non-urban and marine atmospheres. A significant amount of particulate H 2Ox/oxalate (Ox) occurred in the coarse particle fraction of a dichotomous sampler, the ratio of oxalate concentrations in the PM 10 to PM 2.5 fractions ranged from 1 to 2, with mean±sd being 1.4±0.2. These results suggest that oxalate does not solely originate in the gas phase and condense into particles. Gaseous H 2Ox concentrations are much lower than particulate Ox concentrations and are well correlated with HNO 3, HCHO, and O 3, supporting a photochemical origin. Of special relevance to the Bay Region Atmospheric Chemistry Experiment (BRACE) is the extent of nitrogen deposition in the Tampa Bay estuary. Hydroxyl radical is primarily responsible for the conversion of NO 2 to HNO 3, the latter being much more easily deposited. Hydroxyl radical is also responsible for the aqueous phase formation of oxalic acid from alkenes. Hence, we propose that an estimate of rad OH can be obtained from H 2Ox/Ox production rate and we accordingly show that the product of total oxalate concentration and NO 2 concentration approximately predicts the total nitrate concentration during the same period.

  4. Recovery of plutonium from oxalate bearing solutions using a mixture of CMPO and TBP

    International Nuclear Information System (INIS)

    Mathur, J.N.; Murali, M.S.; Rizvi, G.H.; Iyer, R.H.; Badheka, L.P.; Banerji, A.; Michael, K.M.; Kapoor, S.C.; Dhumwad, R.K.

    1993-01-01

    A simple and efficient procedure has been developed to quantitatively recover Pu from oxalate bearing solutions using a mixture of octyl(phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide (CMPO) and TBP in dodecane. Pu(IV) in the range of 6.9 to 34.6 mg/1 was quantitatively extracted into 0.2 M CMPO+ 1.2 M TBP in dodecane from an aqueous solution containing 3.0 M HNO 3 and 0.1 M H 2 C 2 O 4 . At such low concentrations of Pu, the distribution ratio (D) did not change but the increase in oxalic acid concentration drastically reduced these values. The variation in HNO 3 concentration at a fixed concentration of 0.2 M CMPO + 1.2 M TBP has shown a dramatic increase in the D values, being 0.3 at 1.0 M and > 10 4 at 7.5 M. The extraction was almost quantitative even at the aqueous to organic ratio of 10:1. Plutonium could be quantitatively recovered (i) by stripping with 0.5 M acetic acid and (ii) by coprecipitating it directly from the organic phase with 0.3 M oxalic acid + 0.3 M calcium nitrate + sodium nitrite. ∼ 92% of the Pu was found in the precipitate and ∼7% in the supernatant. Using this procedure Pu, in a concentrated form (∼50 times), could be recovered from the oxalate bearing solutions without recourse to the destruction of oxalate ion. The slope of 2 from the nitrate ion as well as CMPO variation experiments suggest the species in the organic phase to be PuC 2 O 4 (NO 3 ) 2 .2CMPO. The absorption spectral study of Pu(IV) confirmed the above species in the organic phase. (author). 19 refs., 5 figs., 9 tabs

  5. Precipitation of calcium, magnesium, strontium and barium in tissues of four Acacia species (Leguminosae: Mimosoideae).

    Science.gov (United States)

    He, Honghua; Bleby, Timothy M; Veneklaas, Erik J; Lambers, Hans; Kuo, John

    2012-01-01

    Precipitation of calcium in plants is common. There are abundant studies on the uptake and content of magnesium, strontium and barium, which have similar chemical properties to calcium, in comparison with those of calcium in plants, but studies on co-precipitation of these elements with calcium in plants are rare. In this study, we compared morphologies, distributional patterns, and elemental compositions of crystals in tissues of four Acacia species grown in the field as well as in the glasshouse. A comparison was also made of field-grown plants and glasshouse-grown plants, and of phyllodes of different ages for each species. Crystals of various morphologies and distributional patterns were observed in the four Acacia species studied. Magnesium, strontium and barium were precipitated together with calcium, mainly in phyllodes of the four Acacia species, and sometimes in branchlets and primary roots. These elements were most likely precipitated in forms of oxalate and sulfate in various tissues, including epidermis, mesophyll, parenchyma, sclerenchyma (fibre cells), pith, pith ray and cortex. In most cases, precipitation of calcium, magnesium, strontium and barium was biologically induced, and elements precipitated differed between soil types, plant species, and tissues within an individual plant; the precipitation was also related to tissue age. Formation of crystals containing these elements might play a role in regulating and detoxifying these elements in plants, and protecting the plants against herbivory.

  6. Pseudomonas fluorescens ATCC 13525 Containing an Artificial Oxalate Operon and Vitreoscilla Hemoglobin Secretes Oxalic Acid and Solubilizes Rock Phosphate in Acidic Alfisols

    Science.gov (United States)

    Archana, G.; Naresh Kumar, G.

    2014-01-01

    Oxalate secretion was achieved in Pseudomonas fluorescens ATCC 13525 by incorporation of genes encoding Aspergillus niger oxaloacetate acetyl hydrolase (oah), Fomitopsis plaustris oxalate transporter (FpOAR) and Vitreoscilla hemoglobin (vgb) in various combinations. Pf (pKCN2) transformant containing oah alone accumulated 19 mM oxalic acid intracellularly but secreted 1.2 mM. However, in the presence of an artificial oxalate operon containing oah and FpOAR genes in plasmid pKCN4, Pf (pKCN4) secreted 13.6 mM oxalate in the medium while 3.6 mM remained inside. This transformant solubilized 509 μM of phosphorus from rock phosphate in alfisol which is 4.5 fold higher than the Pf (pKCN2) transformant. Genomic integrants of P. fluorescens (Pf int1 and Pf int2) containing artificial oxalate operon (plac-FpOAR-oah) and artificial oxalate gene cluster (plac-FpOAR-oah, vgb, egfp) secreted 4.8 mM and 5.4 mM oxalic acid, released 329 μM and 351 μM P, respectively, in alfisol. The integrants showed enhanced root colonization, improved growth and increased P content of Vigna radiata plants. This study demonstrates oxalic acid secretion in P. fluorescens by incorporation of an artificial operon constituted of genes for oxalate synthesis and transport, which imparts mineral phosphate solubilizing ability to the organism leading to enhanced growth and P content of V. radiata in alfisol soil. PMID:24705024

  7. Pseudomonas fluorescens ATCC 13525 containing an artificial oxalate operon and Vitreoscilla hemoglobin secretes oxalic acid and solubilizes rock phosphate in acidic alfisols.

    Directory of Open Access Journals (Sweden)

    Kavita Yadav

    Full Text Available Oxalate secretion was achieved in Pseudomonas fluorescens ATCC 13525 by incorporation of genes encoding Aspergillus niger oxaloacetate acetyl hydrolase (oah, Fomitopsis plaustris oxalate transporter (FpOAR and Vitreoscilla hemoglobin (vgb in various combinations. Pf (pKCN2 transformant containing oah alone accumulated 19 mM oxalic acid intracellularly but secreted 1.2 mM. However, in the presence of an artificial oxalate operon containing oah and FpOAR genes in plasmid pKCN4, Pf (pKCN4 secreted 13.6 mM oxalate in the medium while 3.6 mM remained inside. This transformant solubilized 509 μM of phosphorus from rock phosphate in alfisol which is 4.5 fold higher than the Pf (pKCN2 transformant. Genomic integrants of P. fluorescens (Pf int1 and Pf int2 containing artificial oxalate operon (plac-FpOAR-oah and artificial oxalate gene cluster (plac-FpOAR-oah, vgb, egfp secreted 4.8 mM and 5.4 mM oxalic acid, released 329 μM and 351 μM P, respectively, in alfisol. The integrants showed enhanced root colonization, improved growth and increased P content of Vigna radiata plants. This study demonstrates oxalic acid secretion in P. fluorescens by incorporation of an artificial operon constituted of genes for oxalate synthesis and transport, which imparts mineral phosphate solubilizing ability to the organism leading to enhanced growth and P content of V. radiata in alfisol soil.

  8. Remanence properties of Co-precipitated cobalt ferrite

    International Nuclear Information System (INIS)

    Bueno-Baques, D.; Medina-Boudri, Angela; Matutes-Aquino, J.

    2001-01-01

    Isothermal remanent magnetization (IRM) and DC demagnetization (DCD) curves of a co-precipitated cobalt ferrite sample were obtained. From the IRM and DCD data, the Henkel plot was obtained and analyzed in the Preisach model framework. The Henkel plot data are below the Wohlfarth line that indicates a dominant local disorder (demagnetizing-like effect). Forward and reverse switching field distribution curves were obtained from differentiation of the IRM and DCD curves. The peak values of these switching field distributions differ by a factor of about 2.7

  9. Synthesis, properties and space applications of chemically precipitated YBa/sub 2/Cu/sub 3/O/sub 7-x/ superconducting powders

    International Nuclear Information System (INIS)

    Trivedi, A.; Sundahl, R.C.; Olson, W.L.; Welsh, L.B.; Polak, A.J.; Dolgin, B.P.; Barder, T.J.; Karasek, K.R.; Parker, C.A.

    1988-01-01

    Processing properties of and chemically precipitated YBa/sub 2/Cu/sub 3/O/sub 7-x/ powders were evaluated. The authors have successfully developed a method for precipitating stoichiometric oxalate precursors for YBa/sub 2/Cu/sub 3/O/sub 7-x/ powders. Precipitation and calcination conditions were found to dramatically impact upon key powder characteristics such as particle size, morphology, phase composition and microscopic homogeneity. Four space applications were identified: a superconducting motor/generator, a magnetic bearing, an electromagnetic coupling, and a motor commutator. The primary device, a motor, would make use of superconducting windings and a superconducting flux bottle to improve efficiency

  10. Filterless pre-concentration by co-precipitation by formation of crystalline precipitate in the analysis of barium by FIA-FAES

    DEFF Research Database (Denmark)

    Plamboeck, C.; Westtoft, H.C.; Pedersen, S.A.

    2003-01-01

    A novel method based on flow injection analysis (FIA) and flame atomic emission spectrometry (FAES) is presented. It was developed for direct determination of barium in drinking water, in natural water, in digested samples of bone and liver, in saline water and in a standard reference material...... (NIST SRM 1640). It was found that digestion of bone by an incineration procedure was required, in order to extract most of the barium. In the FIA manifold, barium was pre-concentrated by co-precipitation with lead chromate leading to a crystalline deposit that adhered well to the inner walls of a nylon...

  11. ROLE OF THE MICROFLORA IN DISTAL INTESTINAL TRACT BY MAINTAINING OXALATE HOMEOSTASIS

    Directory of Open Access Journals (Sweden)

    Osolodchenko T.P.

    2015-05-01

    Full Text Available Human intestinal microflora is part of the human body and performs numerous function. Considerable research interest is in the field of probiotics for the prevention of kidney stones, which is one of the most common urological diseases.Urolithiasis is one of the most common urological diseases. This is polyetiological disease congenital and acquired character with complex physical and chemical processes that occur not only in the urinary system, but also the whole body. None of the treatments does not guarantee full recovery of the patient and often leads to relapse. The open methods of removal stones yield news minimally invasive the technologys. Development of stone formation depends on the presence of many factors, metabolic disorders, chronic urinary tract infections, genetic disorders and more. Most have the following metabolic disorders as hypercalciuria, hiperurikuria, hipotsytraturia , hyperoxaluria and hipomahniuria. Among all types of urolithiasis kaltsiyoksalatnyy ranked first in the prevalence rate - about 75.0 - 85.0 % of cases. Dietary restriction by oxalates іs the unreliable method of preventing disease. Although there is evidence for the growth inhibition normobiocenosis representatives, which in turn enhances the absorption of salts of oxalic acid oxalate in the application of sodium , magnesium and cobalt in their intragastric administration. Recently published many papers on the impact on the level of oxalate intestinal microflora. The first publications appeared on the influence of gram-negative obligate anaerobes O. formigenes the concentration of oxalate in the urine. This anaerobic bacteria living in the colon, its prevalence - 46.0 % - 77.0 % of the adult population. O. formigenes reveals the symbiotic interaction with the human body by reducing absorption of oxalate in the intestinal cavity with subsequent decrease in their concentration in plasma and urine. O. formigenes has two key enzymes - oksalyl

  12. Current Travertines Precipitation from CO2-rich Groundwaters as an alert of CO2 Leakages from a Natural CO2 Storage at Ganuelas-Mazarron Tertiary Basin (Murcia, Spain)

    International Nuclear Information System (INIS)

    Rodrigo-Naharro, J.; Delgado, A.; Herrero, M. J.; Granados, A.; Perez del Villar, L.

    2013-01-01

    Carbon capture and storage technologies represent the most suitable solutions related to the high anthropogenic CO 2 emissions to the atmosphere. As a consequence, monitoring of the possible CO 2 leakages from an artificial deep geological CO 2 storage is indispensable to guarantee its safety. Fast surficial travertine precipitation related to these CO 2 leakages can be used as an alert for these escapes. Since few studies exist focusing on the long-term behaviour of an artificial CO 2 DGS, natural CO 2 storage affected by natural or artificial escapes must be studied as natural analogues for predicting the long-term behaviour of an artificial CO 2 storage. In this context, a natural CO 2 reservoir affected by artificial CO 2 escapes has been studied in this work. This study has mainly focused on the current travertines precipitation associated with the upwelling CO 2 -rich waters from several hydrogeological wells drilled in the Ganuelas-Mazarron Tertiary basin (SE Spain), and consists of a comprehensive characterisation of parent-waters and their associated carbonates, including elemental and isotopic geochemistry, mineralogy and petrography. Geochemical characterisation of groundwaters has led to recognise 4 hydrofacies from 3 different aquifers. These groundwaters have very high salinity and electrical conductivity; are slightly acid; present high dissolved inorganic carbon (DIC) and free CO 2 ; are oversaturated in both aragonite and calcite; and dissolve, mobilize and transport low quantities of heavy and/or toxic elements. Isotopic values indicate that: i) the origin of parent-waters is related to rainfalls from clouds originated in the Mediterranean Sea or continental areas; ii) the origin of C is mainly inorganic; and iii) sulphate anions come mainly from the dissolution of the Messinian gypsum from the Tertiary Basin sediments. Current travertines precipitation seems to be controlled by a combination of several factors, such as: i) a fast decrease of the

  13. Magnetic and electrical properties of the La doped Mn-Zn ferrite nanoparticles synthesized by the co-precipitation method

    International Nuclear Information System (INIS)

    Chandel, Vipin; Vijeta; Thakur, Atul; Thakur, Preeti

    2013-01-01

    In the present study, nano crystalline Mn-Zn-La ferrite with chemical formula Mn 0.4 Zn 0.6 La 0.3 Fe 1.7 O 4 was successfully synthesized by a co-precipitation method. The prepared powders were presintered at 700℃. The pallets formed were finally sintered at 700℃, 800℃ and 900℃ for 3h reach. The structural and morphological behavior was investigated by the X-ray diffraction (XRD) and scanning electron microscopy (SEM). XRD confirms the formation of the expected spinel structure. Scanning Electron Microscopy (SEM) was used to characterize the microstructure of the ferrite samples i.e. grain morphology, grain size, grain size distribution and shape. Fourier transform infrared spectroscopy (FTIR) confirms the peaks of different molecules in the given sample. Electrical and magnetic properties were studied by using dc resistivity set up and vibrating sample magnetometer (VSM). (author)

  14. Spectra investigation on surface characteristics of graphene oxide nanosheets treated with tartaric, malic and oxalic acids.

    Science.gov (United States)

    Teng, Xiyao; Yan, Manqing; Bi, Hong

    2014-01-24

    The surface characteristics of graphene oxide nanosheets (GO) treated respectively with tartaric acid, malic acid and oxalic acid, have been investigated by mainly using optical spectroscopic methods including Fourier transform infrared spectroscopy (FT-IR), Ultraviolet-visible (UV-Vis) absorption and Raman spectroscopy. Additionally, the electrochemical property of the products has also been studied. The data revealed that oxygen-containing groups such as OH, COOH and CO on the GO surface have been almost removed and thus reduced graphene oxide nanosheets (RGN) were obtained. Interestingly, the number of sp(2) domains of RGN increases as treated by tartaric acidoxalic acid whereas the steric hindrance (SH) decreases and the ionization constant (IC) differs among these three acids. Furthermore, the specific capacitances (Cs) of GO have been greatly promoted from 2.4 F g(-1) to 100.8, 112.4, and 147 F g(-1) after treated with tartaric, malic and oxalic acids, respectively. This finding agrees well with the spectra result of the tendency of surface conjugated degree alteration. We claim that the difference in both SH and IC among these acids is the main reason for the diverse surface characteristics as well as the improved Cs of the RGN. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. METHOD OF RECOVERING TRANSURANIC ELEMENTS OF AN ATOMIC NUMBER BELOW 95

    Science.gov (United States)

    Seaborg, G.T.; James, R.A.

    1959-12-15

    The concentration of neptanium or plutonium by two carrier precipitation steps with identical carriers but using (after dissolution of the first carrier in nitric acid) a reduced quantity of carrier for the second precipitation is discussed. Carriers suitable are uranium(IV) hypophosphate, uranium(IV) pyrophosphate, uranium(IV) oxalate, thorium oxalate, thorium citrate, thorium tartrate, thorium sulfide, and uranium(IV) sulfide.

  16. Fabrication of ITO particles using a combination of a homogeneous precipitation method and a seeding technique and their electrical conductivity

    Directory of Open Access Journals (Sweden)

    Yoshio Kobayashi

    2015-09-01

    Full Text Available The present work proposes a method to fabricate indium tin oxide (ITO particles using precursor particles synthesized with a combination of a homogeneous precipitation method and a seeding technique, and it also describes their electronic conductivity properties. Seed nanoparticles were produced using a co-precipitation method with aqueous solutions of indium (III chloride, tin (IV chloride aqueous solution and sodium hydroxide. Three types of ITO nanoparticles were fabricated. The first type was fabricated using the co-precipitation method (c-ITO. The second and third types were fabricated using a homogeneous precipitation method with the seed nanoparticles (s-ITO and without seeds (n-ITO. The as-prepared precursor particles were annealed in air at 500 °C, and their crystal structures were cubic ITO. The c-ITO nanoparticles formed irregular-shaped agglomerates of nanoparticles. The n-ITO nanoparticles had a rectangular-parallelepiped or quasi-cubic structure. Most s-ITO nanoparticles had a quasi-cubic structure, and their size was larger than the n-ITO particles. The volume resistivities of the c-ITO, n-ITO and s-ITO powders decreased in that order because the regular-shaped particles were made to strongly contact with each other.

  17. Oxalate Content of Taro Leaves Grown in Central Vietnam

    Science.gov (United States)

    Du Thanh, Hang; Phan Vu, Hai; Vu Van, Hai; Le Duc, Ngoan; Le Minh, Tuan; Savage, Geoffrey

    2017-01-01

    Leaves were harvested from four different cultivars of Colocasia esculenta and three cultivars of Alocasia odora that were growing on nine different farms in central Vietnam. The total, soluble and insoluble oxalate contents of the leaves were extracted and measured using HPLC chromatography. Total calcium determinations were also carried out on the same samples. The total oxalate content of the leaves ranged from 433.8 to 856.1 mg/100 g wet matter (WM) while the soluble oxalate ranged from 147.8 to 339.7 mg/100 g WM. The proportion of soluble oxalate ranged from 28% to 41% (overall mean 35%) of the total oxalate content of the leaves. The equivalent insoluble oxalate proportion ranged from 59% to 72% of the total (overall mean 65%). There was little difference between the Colocasia esculenta and Alocasia odora taro cultivars, although the total oxalate content was significantly higher in Alocasia odora cultivars. The overall mean total calcium content was 279.5 mg/100 WM and the percentage of insoluble calcium bound as calcium oxalate ranged from 31.7% to 57.3% of the total calcium content (overall mean 47.1%). The oxalate content in taro leaves is a major factor to consider when different cultivars of taro are recommended for human or animal consumption. PMID:28231080

  18. Synthesis of composite nanoparticles using co-precipitation of a magnetic iron-oxide shell onto core nanoparticles

    International Nuclear Information System (INIS)

    Primc, Darinka; Belec, Blaž; Makovec, Darko

    2016-01-01

    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 Fe"3"+/Fe"2"+ 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 Fe"3"+ ions in a nitrate complex with urea ([Fe((CO(NH_2)_2)_6](NO_3)_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 Fe"3"+ ions into the suspension of the core nanoparticles. The key stage of the process is the thermal hydrolysis of the released Fe"3"+ 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 Fe"2"+ 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.Graphical abstract

  19. Preparation of (U, Gd)O2 by inverse co-precipitation in nitric solutions. Study of homogeneity and process optimization

    International Nuclear Information System (INIS)

    Marchi, Daniel E.; Menghini, Jorge E.; Trimarco, Viviana G.

    1999-01-01

    The inverse co-precipitation method has been used at the laboratory level to produce uranium - gadolinium mixed oxides. The formation of a mixed phase in the precipitates has been determined as well as the occurrence of only one phase in the sintered pellets, corresponding to a gadolinium - uranium solution. Moreover, a modification in the calcination-reduction stage was introduced that allows the elimination of the fissures previously detected in the sintered pellets

  20. Modelling the operation of precipitator with vortex effect

    International Nuclear Information System (INIS)

    Eysseric-Emile, C.

    1994-01-01

    In the Purex process which is implemented for the processing of irradiated fuels to eliminate fission products and to recover and valorise uranium and plutonium under the form of end products, a precipitation operation occurs to prepare the plutonium oxalate. This research thesis aims at analysing hydrodynamic characteristics of a specific apparatus used for this precipitation, the precipitator with vortex effect. In a first part, the author presents the problems associated with precipitation operations, their implementation in the processing of irradiated fuels, and compares the considered precipitator with other devices used for the precipitation of radioactive compounds. He proposes a review of literature on the vortex effect in agitated vessel, highlights the key parameter (the forced vortex radius), and reports some preliminary measurements performed on the precipitator. The author then reports the study of liquid phase flows in the precipitator, measurements of rate of suspension, and the study of micro-mixing with reactants. He finally reports attempts to validate trends noticed during flow analysis and a first simple modelling of the precipitator [fr

  1. Untitled

    Indian Academy of Sciences (India)

    Several media, it has been found that a saturated solution of starch and water could be employed to obtain acicular crystals. 2.3 Synthesis of mixed oxalates. The starting materials for the Synthesis of doped gamma ferric oxide were mixed oxalates of iron and the dopant (Mg/Co/Ni/Cu), which was co-precipitated from a.

  2. Short communication: Urinary oxalate and calcium excretion by dogs and cats diagnosed with calcium oxalate urolithiasis

    NARCIS (Netherlands)

    Dijcker, J.C.; Kummeling, A.; Hagen-Plantinga, E.A.; Hendriks, W.H.

    2012-01-01

    Introduction Urine concentrations of oxalate and calcium play an important role in calcium oxalate (CaOx) urolith formation in dogs and cats, with high excretions of both substances increasing the chance of CaOx urolithiasis. In 17 CaOx-forming dogs, urine calcium:creatinine ratio (Ca:Cr) was found

  3. Synthesis and characteristics of a novel 3-D organic amine oxalate: (enH2)1.5[Bi3(C2O4)6(CO2CONHCH2CH2NH3)].6.5H2O

    International Nuclear Information System (INIS)

    Yu Xiaohong; Zhang Hanhui; Cao Yanning; Chen Yiping; Wang Zhen

    2006-01-01

    A novel 3-D compound of (enH 2 ) 1.5 [Bi 3 (C 2 O 4 ) 6 (CO 2 CONHCH 2 CH 2 NH 3 )].6.5H 2 O has been hydrothermally synthesized and characterized by IR, ultraviolet-visible diffuse reflection integral spectrum (UV-Vis DRIS), fluorescence spectra, TGA and single crystal X-ray diffraction. It crystallizes in the monoclinic system, space group C2/c with a=31.110(8)A, b=11.544(3)A, c=22.583(6)A, β=112.419(3) o , V=7497(3)A 3 , Z=8, R 1 =0.0463 and wR 2 =0.1393 for unique 7686 reflections I>2σ(I). In the title compound, the Bi atoms have eight-fold and nine-fold coordination with respect to the oxygen atoms, with the Bi atoms in distorted dodecahedron and monocapped square antiprism, respectively. The 3-D framework of the title compound contains channels and is composed of linkages between Bi atoms and oxalate units, forming honeycomb-like layers with two kinds of 6+6 membered aperture, and pillared by oxalate ligands and monamide groups. The channels have N-ethylamine oxalate monamide group - CO 2 CONHCH 2 CH 2 NH 3 + , which is formed by the in situ reaction of en and oxalate acid. At room temperature, the complex exhibits intense blue luminescence with an emission peak at 445nm

  4. Oxalate Content of the Herb Good-King-Henry, Blitum Bonus-Henricus

    Directory of Open Access Journals (Sweden)

    Wanying Li

    2015-05-01

    Full Text Available The total, soluble and insoluble oxalate contents of the leaves, stems and buds of Good-King-Henry (Blitum Bonus-Henricus were extracted and measured using HPLC chromatography. The large, mature leaves contained 42% more total oxalate than in the small leaves and the soluble oxalate content of the large leaves was 33% higher than the smaller leaves. Cooking the mixed leaves, stems and buds in boiling water for two minutes significantly (p < 0.05 reduced the total oxalate when compared to the raw plant parts. Pesto sauce made from mixed leaves contained 257 mg total oxalate/100 g fresh weight; this was largely made up of insoluble oxalates (85% of the total oxalate content. Soup made from mixed leaves contained lower levels of total oxalates (44.26 ± 0.49 mg total oxalate/100 g fresh weight and insoluble oxalate made up 49% of the oxalate contents. The levels of oxalates in the Good-King-Henry leaves were high, suggesting that the leaves should be consumed occasionally as a delicacy because of their unique taste rather than as a significant part of the diet. However, the products made from Good-King-Henry leaves indicated that larger amounts could be consumed as the oxalate levels were reduced by dilution and processing.

  5. Oxalate Content of Taro Leaves Grown in Central Vietnam

    Directory of Open Access Journals (Sweden)

    Hang Du Thanh

    2017-01-01

    Full Text Available Leaves were harvested from four different cultivars of Colocasia esculenta and three cultivars of Alocasia odora that were growing on nine different farms in central Vietnam. The total, soluble and insoluble oxalate contents of the leaves were extracted and measured using HPLC chromatography. Total calcium determinations were also carried out on the same samples. The total oxalate content of the leaves ranged from 433.8 to 856.1 mg/100 g wet matter (WM while the soluble oxalate ranged from 147.8 to 339.7 mg/100 g WM. The proportion of soluble oxalate ranged from 28% to 41% (overall mean 35% of the total oxalate content of the leaves. The equivalent insoluble oxalate proportion ranged from 59% to 72% of the total (overall mean 65%. There was little difference between the Colocasia esculenta and Alocasia odora taro cultivars, although the total oxalate content was significantly higher in Alocasia odora cultivars. The overall mean total calcium content was 279.5 mg/100 WM and the percentage of insoluble calcium bound as calcium oxalate ranged from 31.7% to 57.3% of the total calcium content (overall mean 47.1%. The oxalate content in taro leaves is a major factor to consider when different cultivars of taro are recommended for human or animal consumption.

  6. Urinary oxalate to creatinine ratios in healthy Turkish schoolchildren.

    Science.gov (United States)

    Dursun, Ismail; Çelik, İlknur; Poyrazoglu, Hakan M; Köse, Kader; Tanrıkulu, Esen; Sahin, Habibe; Yılmaz, Kenan; Öztürk, Ahmet; Yel, Sibel; Gündüz, Zübeyde; Düşünsel, Ruhan

    2017-11-01

    we aimed to establish reference values for urinary oxalate to creatinine ratios in healthy children aged 6-15 years and to investigate the relationship between their nutritional habits and oxalate excretion. Random urine specimens from 953 healthy children aged 6-15 years were obtained and analyzed for oxalate and creatinine. Additionally, a 24-h dietary recall form was prepared and given to them. The ingredient composition of the diet was calculated. The children were divided into three groups according to age: Group I (69 years, n = 353), Group II (10-12 years, n = 335), and Group III (13-15 years, n = 265). The 95th percentile of the oxalate to creatinine ratio for subjects aged 6-9, 10-12, and 13-15 years were 0.048, 0.042, and 0.042 mg/mg, respectively. The oxalate to creatinine ratio was significantly higher in Group 1 than in Group 2 and Group 3. Urinary oxalate excretion was positively correlated with increased protein intake and negatively correlated with age. A significant positive correlation was determined between urinary oxalate excretion and the proline, serine, protein, and glycine content of diet. Dietary proline intake showed a positive correlation with the urine oxalate to creatinine ratio and was found to be an independent predictor for urinary oxalate. These data lend support to the idea that every country should have its own normal reference values to determine the underlying metabolic risk factor for kidney stone disease since regional variation in the dietary intake of proteins and other nutrients can affect normal urinary excretion of oxalate.

  7. Oxalate-metabolising genes of the white-rot fungus Dichomitus squalens are differentially induced on wood and at high proton concentration.

    Directory of Open Access Journals (Sweden)

    Miia R Mäkelä

    Full Text Available Oxalic acid is a prevalent fungal metabolite with versatile roles in growth and nutrition, including degradation of plant biomass. However, the toxicity of oxalic acid makes regulation of its intra- and extracellular concentration crucial. To increase the knowledge of fungal oxalate metabolism, a transcriptional level study on oxalate-catabolising genes was performed with an effective lignin-degrading white-rot fungus Dichomitus squalens, which has demonstrated particular abilities in production and degradation of oxalic acid. The expression of oxalic-acid decomposing oxalate decarboxylase (ODC and formic-acid decomposing formate dehydrogenase (FDH encoding genes was followed during the growth of D. squalens on its natural spruce wood substrate. The effect of high proton concentration on the regulation of the oxalate-catabolising genes was determined after addition of organic acid (oxalic acid and inorganic acid (hydrochloric acid to the liquid cultures of D. squalens. In order to evaluate the co-expression of oxalate-catabolising and manganese peroxidase (MnP encoding genes, the expression of one MnP encoding gene, mnp1, of D. squalens was also surveyed in the solid state and liquid cultures. Sequential action of ODC and FDH encoding genes was detected in the studied cultivations. The odc1, fdh2 and fdh3 genes of D. squalens showed constitutive expression, whereas ODC2 and FHD1 most likely are the main responsible enzymes for detoxification of high concentrations of oxalic and formic acids. The results also confirmed the central role of ODC1 when D. squalens grows on coniferous wood. Phylogenetic analysis revealed that fungal ODCs have evolved from at least two gene copies whereas FDHs have a single ancestral gene. As a conclusion, the multiplicity of oxalate-catabolising genes and their differential regulation on wood and in acid-amended cultures of D. squalens point to divergent physiological roles for the corresponding enzymes.

  8. Synthesis and structural characterisation of mixed An(IV)-An(III) actinide oxalates used as precursors for dedicated fuel or target

    International Nuclear Information System (INIS)

    Tamain, Christelle; Grandjean, Stephane; Arab Chapelet, Benedicte; Abraham, Francis

    2010-01-01

    Oxalic co-conversion process plays an important role by producing mixed-actinide compounds used as starting materials as they are particularly suitable precursors of actinide oxide solid solutions. In these oxalate compounds, a mixed crystallographic site which accommodates both elements in spite of their different oxidation states has been established. The charge compensation is ensured by monovalent cations present in the acidic solution. This communication reviews the various mixed-actinide oxalates obtained by crystallization from acidic solution. First, crystallographic structures determined by X-ray diffraction from single crystals are described. Then completing data obtained by powder X-ray diffraction are presented on various systems. The different supramolecular arrangements underline the complexity of An(IV)-An(III)/Ln(III) oxalate system and the need to pursue studies on single crystals. (authors)

  9. Synthesis and Characterization of Perovskite Type La1-xSrxAlO3-sigma(0<=X<=0.3) by Co-Precipitation Method

    International Nuclear Information System (INIS)

    Mahmoud, O.; Abderezak, G.

    2015-01-01

    This work shows the electrochemical activity of O/sub 2/ evolution reaction in KOH of perovskite type- aluminate oxide (La/sub 1-x/Sr/sub x/AlO/sub 3-sigma/ with x = 0, 0.1, 0.2, 0.3). La/sub 1-x/Sr/sub x/AlO/sub 3-sigma/ (0co-precipitation method. The white precipitates were then washed in distilled water by centrifugation, and calcined at 1000/degree C/ for 6h, the pure phase was characterized by X-ray diffraction (XRD), thermal gravimetric analysis and differential thermal (TG/DSC), Fourier transform infrared spectroscopy (FTIR), specific surface area (BET). The MEB micrographs are shown of the spherical grains and uniform agglomeration of the grains. The oxide powders were used as the films to form a support on Ni/oxides. Oxygen evolution on each oxide catalyst was signed in the cyclic voltammetry with +- 15 V range and the electrochemical impedance in the equivalent of 100 kHz. The results point out the electrode activity and stability of the x = 0.3 composition. (author)

  10. Recovery of Iron from Pyrolusite Leaching Slag by a Lab-Scale Circulation Process of Oxalic Acid Leaching and Ultraviolet Irradiation

    Directory of Open Access Journals (Sweden)

    Biao Deng

    2017-12-01

    Full Text Available Pyrolusite leaching slag is a Fe-containing slag generated from pyrolusite leaching process with SO2. Recovery of iron from the slag not only has economic benefit, but also prevents the secondary pollution to the environment. A novel lab-scale cyclic process for recovering iron from pyrolusite leaching slag was introduced. The process contains two steps: (1 iron was leached with oxalic acid and [Fe(C2O4n](3−2n+ solution was generated; (2 the [Fe(C2O4n](3−2n+ solution was irradiated by ultraviolet and ferrous oxalate precipitation were obtained. The effect of operation parameter on leaching and irradiation process were studied separately. In the leaching process, the optimal solid/liquid ratio, oxalic acid concentration, leaching temperature, stirring rate, and leaching time are 1:50, 0.40 mol/L, 95 °C, 300 r/min, and 3 h, respectively. In the irradiation process, the best irradiation wavelength, Fe/oxalic acid molar ratio and irradiation time are 254 nm, 1:4, and 30 min. Besides, a test of 9 continuous cycles was carried out and the performance and material balance of the combined process were investigated. The results showed that the cyclic process is entirely feasible and prove to be stable producing, and ferrous oxalate of 99.32% purity. Material balance indicated that 95.17% of iron was recovered in the form of FeC2O4·2H2O, and the recovery efficiency of oxalic acid was 58.52%.

  11. Two- and three-dimensional lanthanide-organic frameworks constructed using 1-hydro-6-oxopyridine-3-carboxylate and oxalate ligands.

    Science.gov (United States)

    Liu, Cai-Ming; Xiong, Ming; Zhang, De-Qing; Du, Miao; Zhu, Dao-Ben

    2009-08-07

    6-Hydroxypyridine-3-carboxylic acid (6-HOPy-3-CO(2)H) reacts with Ln(2)O(3) (Ln = Nd, Sm, Eu, Gd) and oxalic acid (H(2)OX) under hydrothermal conditions to generate four novel lanthanide-organic coordination polymeric networks [Ln(2)(1H-6-Opy-3-CO(2))(2)(OX)(2)(H(2)O)(3)] x 2.5 H(2)O (Ln = Nd, 1; Sm, 2; 1H-6-Opy-3-CO(2)(-) = 1-hydro-6-oxopyridine-3-carboxylate) and [Ln(1H-6-Opy-3-CO(2))(OX)(H(2)O)(2)] x H(2)O (Ln = Eu, 3; Gd, 4). The new co-ligand 1H-6-Opy-3-CO(2)(-) anion was generated by the autoisomerization of the single deprotonated 6-HOPy-3-CO(2)(-) anion (from the enol form into the ketone one). 1 and 2 are isomorphous, they possess a three-dimensional architecture constructed from Ln(3+) ions bridged by oxalate anions and two types of 1H-6-Opy-3-CO(2)(-) bridges, showing a three-nodal (4,5)-connected topology (3.4(2).5(2).6(3).7.8)(2)(3.5(3).6(2))(2)(3(2).6.7(2).8) or a simplified uninodal 6-connected topology (3(3).4(6).5(5).6), both topologies are completely new; while only one type of 1H-6-Opy-3-CO(2)(-) bridge is used to construct the two-dimensional layer networks of 3 and 4 besides oxalate bridges, both complexes 3 and 4 are isostructural, exhibiting the honeycomb topology 6(3). The lanthanide contraction effect is believed to play a key role in directing the formation of a particular structure. A magnetic study of 1-3 indicated that the coupling interaction between Ln(3+) ions is weak.

  12. Pseudomonas fluorescens ATCC 13525 Containing an Artificial Oxalate Operon and Vitreoscilla Hemoglobin Secretes Oxalic Acid and Solubilizes Rock Phosphate in Acidic Alfisols

    OpenAIRE

    Yadav, Kavita; Kumar, Chanchal; Archana, G.; Naresh Kumar, G.

    2014-01-01

    Oxalate secretion was achieved in Pseudomonas fluorescens ATCC 13525 by incorporation of genes encoding Aspergillus niger oxaloacetate acetyl hydrolase (oah), Fomitopsis plaustris oxalate transporter (FpOAR) and Vitreoscilla hemoglobin (vgb) in various combinations. Pf (pKCN2) transformant containing oah alone accumulated 19 mM oxalic acid intracellularly but secreted 1.2 mM. However, in the presence of an artificial oxalate operon containing oah and FpOAR genes in plasmid pKCN4, Pf (pKCN4) s...

  13. Synthesis and characterization of ZrO2-CuO co-doped ceria nanoparticles via chemical precipitation method.

    Science.gov (United States)

    Viruthagiri, G; Gopinathan, E; Shanmugam, N; Gobi, R

    2014-10-15

    In the present study, the fluorite cubic phase of bare and ZrO2-CuO co-doped ceria (CeO2) nanoparticles have been synthesized through a simple chemical precipitation method. X-ray diffraction results revealed that average grain sizes of the samples are within 5-6nm range. The functional groups present in the samples were identified by Fourier Transform Infrared Spectroscopy (FTIR) study. Surface area measurement was carried out for the ceria nanoparticles to characterize the surface properties of the synthesized samples. The direct optical cutoff wavelength from DRS analysis was blue-shifted evidently with respect to the bulk material and indicated quantum-size confinement effect in the nanocrystallites. PL spectra revealed the strong and sharp UV emission at 401nm. The surface morphology and the element constitution of the pure and doped nanoparticles were studied by scanning electron microscope fitted with energy dispersive X-ray spectrometer arrangement. The thermal decomposition course was followed using thermo gravimetric and differential thermal analyses (TG-DTA). Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Two novel metal–organic coordination polymers based on diphosphonate and oxalate: Synthesis, structures and properties

    International Nuclear Information System (INIS)

    Niu, Qing-Jun; Zheng, Yue-Qing; Zhou, Lin-Xia; Zhu, Hong-Lin

    2015-01-01

    Two 2-(1-imidazole)-1-hydroxyl-1,1'-ethylidenediphosphonato and oxalic acid bridged coordination polymers (H 2 en)[Co 3 (H 2 zdn) 2 (ox)(H 2 O) 2 ] (1) and Cd 2 (H 2 zdn)(ox) 0.5 (H 2 O) (2) (2-(1-imidazole)-1-hydroxyl-1,1'-ethylidenediphosphonic acid=H 5 zdn; oxalic acid=H 2 ox) were synthesized under hydrothermal conditions and characterized by the infrared (IR), thermogravimetric analyses (TGA), elemental analyses (EA) and X-ray diffraction (XRD). Compound 1 is bridged by phosphonate anions to 1D chain, and further linked by oxalate anions to 2D layer. Compound 2 is bridged by O–P–O units of H 5 zdn to the layer, and then pillared by oxalate anions to generate 3D frameworks. Compound 1 shows anti-ferromagnetic behaviors analyzed with the temperature-dependent zero-field ac magnetic susceptibilities, while compound 2 exhibits an influence on the luminescent property. - Graphical abstract: Linked by oxalate, two zoledronate-based metal–organic frameworks are synthesized, which exhibits the different frameworks. Magnetism and luminescent properties have been studied. The weak antiferromagnetic coupling is conducted in 1. - Highlights: • Compound 1 and 2 are first linked by oxalate anion based on zoledronic acid. • Compound 1 generates a classic “dia Diamond” (6 6 ) topology. • Compound 2 exhibits a (4 4 ·6 2 )(4 4 ·6 6 ) topology. • Magnetism and luminescent properties of 1 and 2 have been studied, respectively

  15. Effect of oxalic acid on the optical, thermal, dielectric and mechanical behaviour of ADP crystals

    International Nuclear Information System (INIS)

    Rajesh, P.; Ramasamy, P.

    2009-01-01

    The effect of the addition, over a concentration range from 1 to 5 mol%, of oxalic acid on the growth rate, optical transparency, hardness, dielectric behaviour, and SHG efficiency of ammonium dihydrogen phosphate single crystals grown by slow evaporation method has been investigated. UV-Vis studies show that the transparency of the oxalic acid added crystals decreased gradually. Thermal studies indicate that the decomposition temperatures of the crystal are decreased in oxalic acid added ADP crystals. It is observed from the dielectric measurements that the dielectric constant and dielectric loss increase with increase in temperature for all the crystals. Vicker's microhardness study reveals that the addition of higher concentration of oxalic acid decreases the hardness of the crystal. SHG efficiency of 1 mol% of oxalic acid is higher than the pure ADP.

  16. Novel methods for the synthesis of magnetite nanoparticles with special morphologies and textured assemblages

    Energy Technology Data Exchange (ETDEWEB)

    Nyiro-Kosa, Ilona, E-mail: kosaili@gmail.com [University of Pannonia, Department of Material Engineering (Hungary); Recnik, Aleksander [Jozef Stefan Institute, Department for Nanostructured Materials (Slovenia); Posfai, Mihaly [University of Pannonia, Department of Earth and Environmental Sciences (Hungary)

    2012-10-15

    There is an increasing technological demand for magnetic nanocrystals with special morphologies and controlled sizes. Several approaches are used for the synthesis of magnetite crystals with irregular or octahedral shapes; however, the room-temperature synthesis of nanocrystals with specific morphologies is not yet established. Here, we describe the synthesis of magnetite crystals (100-300 nm) at a relatively low temperature ({approx}70 Degree-Sign C) from organic precursors, including Fe(II) oxalate or Fe(II) sulfate, and study the effects of ethylene glycol and tetraethylene glycol on the final physical and chemical properties of the crystals. The magnetite crystals formed from different precursor materials (sulfate or oxalate green rust) show specific morphological and textural features. We show that octahedral magnetite crystals can be produced from Fe(II) oxalate via a simple co-precipitation process. Using different kinds and amounts of polyols, various types of particle morphologies and nanocrystal textures can be produced, including hexagonal-shaped clusters of elongated crystals and porous and solid, large, rounded polycrystalline aggregates.

  17. Novel methods for the synthesis of magnetite nanoparticles with special morphologies and textured assemblages

    International Nuclear Information System (INIS)

    Nyirő-Kósa, Ilona; Rečnik, Aleksander; Pósfai, Mihály

    2012-01-01

    There is an increasing technological demand for magnetic nanocrystals with special morphologies and controlled sizes. Several approaches are used for the synthesis of magnetite crystals with irregular or octahedral shapes; however, the room-temperature synthesis of nanocrystals with specific morphologies is not yet established. Here, we describe the synthesis of magnetite crystals (100–300 nm) at a relatively low temperature (∼70 °C) from organic precursors, including Fe(II) oxalate or Fe(II) sulfate, and study the effects of ethylene glycol and tetraethylene glycol on the final physical and chemical properties of the crystals. The magnetite crystals formed from different precursor materials (sulfate or oxalate green rust) show specific morphological and textural features. We show that octahedral magnetite crystals can be produced from Fe(II) oxalate via a simple co-precipitation process. Using different kinds and amounts of polyols, various types of particle morphologies and nanocrystal textures can be produced, including hexagonal-shaped clusters of elongated crystals and porous and solid, large, rounded polycrystalline aggregates.

  18. Recovery of vanadium (V) from used catalysts in sulfuric acid production units by oxalic acid

    International Nuclear Information System (INIS)

    Abdulbaki, M.; Shino, O.

    2009-07-01

    Vanadium penta oxide (V 2 O 5 ), is used, in large quantities as a catalyst for the oxidation of SO 2 to SO 3 in sulfuric acid production units, during the oxidation process the level of the oxidation declines with the time because of catalyst poisoning. So the spent catalyst is usually through out in a specified special places by General Fertilizer Company which causes a pollution of the land. The present paper, studies the recovery of vanadium from the spent catalyst by using the oxalic acid. The optimal conditions of spent catalyst leaching have been studied. It has been shown that 2%(w/w) of oxalic acid is the most suitable for leaching process at 70 degree centigrade. The precipitation of vanadium using some alkaline media NH 4 OH has been also studied, it has been shown that ammonium hydroxide was the best at 50 degree centigrade. (author)

  19. Inorganic-organic hybrid structure: Synthesis, structure and magnetic properties of a cobalt phosphite-oxalate, [C4N2H12][Co4(HPO3)2(C2O4)3

    International Nuclear Information System (INIS)

    Mandal, Sukhendu; Natarajan, Srinivasan

    2005-01-01

    A hydrothermal reaction of a mixture of cobalt (II) oxalate, phosphorous acid, piperazine and water at 150 o C for 96h followed by heating at 180 o C for 24h gave rise to a new inorganic-organic hybrid solid, [C 4 N 2 H 12 ][Co 4 (HPO 3 ) 2 (C 2 O 4 ) 3 ], I. The structure consists of edge-shared CoO 6 octahedra forming a [Co 2 O 10 ] dimers that are connected by HPO 3 and C 2 O 4 units forming a three-dimensional structure with one-dimensional channels. The amine molecules are positioned within these channels. The oxalate units have a dual role of connecting within the plane of the layer as well as out of the plane. Magnetic susceptibility measurement shows the compound orders antiferromagnetically at low temperature (T N =22K). Crystal data: I, monoclinic, space group=P2 1 /c (No. 14). a=7.614(15), b=7.514(14), c=17.750(3)A, β=97.351(3) o , V=1007.30(3)A 3 , Z=2, ρ calc =2.466g/cm 3 , μ (MoKα) =3.496mm -1 , R 1 =0.0310 and wR 2 =0.0807 data [I>2σ(I)

  20. Properties of Er{sub 2}O{sub 3} nanoparticles synthesized by a modified co-precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Castaneda C, J.; Maranon R, V. F.; Perez Ladron de G, H.; Rodriguez R, R. A.; Chiu Z, R. [Universidad de Guadalajara, Centro Universitario de los Lagos, Av. Enrique Diaz de Leon s/n, Lagos de Moreno 47460, Jalisco (Mexico); Meneses N, M. A., E-mail: jcc050769@yahoo.com.mx [Centro de Investigaciones en Optica, A. C., Apdo. Postal 1-948, Leon, Guanajuato (Mexico)

    2015-07-01

    Er{sub 2}O{sub 3} nanoparticles were synthesized by co-precipitation with the addition of ascorbate as stabilizing agent. The nanoparticles had spherical shapes with a mean diameter of 32 nm and were allocated in clusters, as determined by X-ray diffraction, atomic force microscopy and optical microscopy. Characteristic green and red emissions from Er{sup 3+} were recorded by pumping the nanoparticles at 525 nm, 805 nm and 975 nm. However, the luminescence spectra show an enhancement of red emission for Nir pump wavelengths. We proposed this behavior was due to phonon-assisted depopulation mechanisms and energy transfer processes related to the different excitation schemes. (Author)

  1. Method of grass samples preparation for strontium-90 and cesium-137 analysis with the exception of ashing

    International Nuclear Information System (INIS)

    Antonova, V.A.; Prokof'ev, O.N.; Khazina, M.A.; Bajkovskaya, L.V.

    1978-01-01

    A method is proposed for the preparation of grass samples in the analysis for 90 Sr and 137 Cs, in which radionuclides are removed into solution as a result of the thermal treatment of samples in 0.01N solution of hydrochloric acid. A grass sample 0.8 kg in weight is covered with 8-10 l of 0.01 N solution of hydrochloric acid and boiled for 30 min, while being constantly stirred. The solution is filtered through cheese cloth, carriers for 90 Y and 137 Cs are introduced, and then oxalates are precipitated at pH=4. After the oxalates have been separated from the filtrate the 137 Cs content is determined using the antimonium-iodide technique. The oxalate precipitate is calcined, dissolved in 2N hydrochloric acid, while boiling, and precipitated by ammonia. The precipitate of hydrooxides is filtered. The solution is acidified by 2N hydrochloric acid up to pH 2-3, and the carrier for 90 Y is introduced. The 90 Sr content is determined by a conventional technique. The percentage of the transition of radionuclides from the grass samples into solution ammounts to: 88+-6% for 90 Sr, and 81+-7% for 137 Cs

  2. Processing, structure and magnetic properties correlation in co-precipitated Ca-ferrite

    Energy Technology Data Exchange (ETDEWEB)

    Abasht, Behzad, E-mail: abasht@gmail.com [Space Thruster Research Institute, Iranian Space Research Center, Tabriz (Iran, Islamic Republic of); Department of Metallurgy and Materials Engineering, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of); Beitollahi, Ali; Mirkazemi, Seyyed Mohammad [Department of Metallurgy and Materials Engineering, Iran University of Science and Technology, Tehran (Iran, Islamic Republic of)

    2016-12-15

    La-substituted hexagonal calcium ferrite, Ca{sub 1−X}La{sub X}Fe{sub 12}O{sub 19} (x varies from 0 to 0.6 with the step of 0.2), was synthesized by applying co-precipitation method, in which the molar ratio of Fe{sup 3+}/(Ca{sup 2+}+La{sup 2+}) was 11. The ferrite precursors were prepared from aqueous solution of calcium nitrate, ferric nitrate and lanthanum nitrate by co-precipitation of calcium, iron and lanthanum ions by using an aqueous base of sodium hydroxide (1.5 M) at the pH of 14 and at room temperature. These precursors were calcinated with different amount of La at different temperature of 700, 1100 and 1200 °C for constant calcination time of 1 h in a static air atmosphere. Some tests such as simultaneous thermal analysis (STA), X-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM) were carried out to investigate the thermal behavior, crystallographic properties, morphology and magnetic properties of the precursor powders which were calcinated at different temperatures. The powder XRD patterns of samples which consisted of La as dopant and were calcinated at 1200 °C for 1 h, indicates the formation of calcium hexaferrite and also α-Fe{sub 2}O{sub 3} besides Magnetoplumbite-phase (M-phase). However, the results showed that CaFe{sub 4}O{sub 7} and α-Fe{sub 2}O{sub 3} phases were formed in the sample with the same condition but without using any dopant. The results of SEM showed that the calcium hexaferrite particle were regular hexagonal platelets with the size range of 1–2 µm. The magnetic properties such as maximum magnetization (M{sub Max}), remanent magnetization (M{sub r}) and coercivity (H{sub c}) were measured from the hysteresis loops. Low values of coercive field (16.3 kA m{sup −1}) and maximum magnetization (50.6 A m{sup 2} kg{sup −1}) were obtained from calcium hexaferrite particle in optimum amount of La (X=0.4) which calcinated at the temperature of 1200 °C. - Highlights: • In this

  3. Characterization of wheat germin (oxalate oxidase) expressed by Pichia pastoris

    International Nuclear Information System (INIS)

    Pan, Heng-Yen; Whittaker, Mei M.; Bouveret, Romaric; Berna, Anne; Bernier, Francois; Whittaker, James W.

    2007-01-01

    High-level secretory expression of wheat (Triticum aestivum) germin/oxalate oxidase was achieved in Pichia pastoris fermentation cultures as an α-mating factor signal peptide fusion, based on the native wheat cDNA coding sequence. The oxalate oxidase activity of the recombinant enzyme is substantially increased (7-fold) by treatment with sodium periodate, followed by ascorbate reduction. Using these methods, approximately 1 g (4 x 10 4 U) of purified, activated enzyme was obtained following eight days of induction of a high density Pichia fermentation culture, demonstrating suitability for large-scale production of oxalate oxidase for biotechnological applications. Characterization of the recombinant protein shows that it is glycosylated, with N-linked glycan attached at Asn47. For potential biomedical applications, a nonglycosylated (S49A) variant was also prepared which retains essentially full enzyme activity, but exhibits altered protein-protein interactions

  4. Application of the Alternative Traditional and Selective Precipitation Routes for Recovery of High Grade Thorium Concentrates from Egyptian Crude Monazite Sand

    International Nuclear Information System (INIS)

    Helaly, O.S.

    2017-01-01

    Process flow sheet selection for thorium separation in relatively high grade concentrate from Egyptian crude monazite sand was carried out. Traditional selective leaching and precipitation routes were applied after sulfuric acid digestion upon Egyptian crude monazite for this purpose. The resultant hot grey sulfate paste from monazite digestion was firstly cooled to ambient temperature then leached by normal water into two successive stages. The first leach solution contained most of the thorium which represents about 88% of the present thorium and its concentration in the liquor reached 4.5 g Th/l. This liquor also contains most of the free acids and major of impurities especially iron (more than 6.3 g Fe/l). Different routes were tested to evaluate the suitable conditions that verify maximum recovery of thorium from such monazite sulfate solution and producing relatively high grade concentrate. Two different possible traditional and selective methods were involved, namely; thorium initial precipitation with rare earth elements as double sulfate or its precipitation as phosphate through acidity control at ph 1.1 which seems to be the simple, brief and convenient route to accomplish this purpose. Further separation and/or upgrading of thorium from these precipitates (after conversion to hydroxides or without) were conducted through re-dissolution in hydrochloric acid and re-precipitation with different selective reagents in the form of hydroxide, oxalate or fluoride was also included. The target was accomplished through thorium co-precipitation with light rare earth elements as double sulfate, followed by its recovery from this fraction, where a concentrate of grade 68.3% was produced

  5. Colorimetric sensing of oxalate based on its inhibitory effect on the reaction of Fe (III) with curcumin nanoparticles

    Science.gov (United States)

    Pourreza, Nahid; Lotfizadeh, Neda; Golmohammadi, Hamed

    2018-03-01

    In this research, a new colorimetric method for the determination of oxalate using curcumin nanoparticles (CURNs) in the presence Fe (III) is introduced. The method is based on the inhibitory effect of oxalate ion on the reaction of (CURNs) with Fe (III) in acidic media. This reaction was monitored by measuring the increase in absorbance of CURNs-Fe3 + complex in the presence of oxalate ion at 427 nm. The effect of different parameters such as the pH of the sample solution, concentration of Fe (III), concentration of CURNs and the reaction time was examined and optimized. Under optimum experimental conditions, the absorption intensity was linear with the concentration of oxalate in the range of 0.15 to 1.70 μg mL- 1. The limit of detection (LOD) was 0.077 μg mL- 1 and the relative standard deviations (RSD) for 8 replicate measurements of 0.40 and 1.05 μg mL- 1 of oxalate were 4.20% and 2.74%, respectively. The developed method was successfully employed to the determination of oxalate in water, food and urine samples with satisfactory results.

  6. Addition of calcium compounds to reduce soluble oxalate in a high oxalate food system.

    Science.gov (United States)

    Bong, Wen-Chun; Vanhanen, Leo P; Savage, Geoffrey P

    2017-04-15

    Spinach (Spinacia oleracea L.) is often used as a base vegetable to make green juices that are promoted as healthy dietary alternatives. Spinach is known to contain significant amounts of oxalates, which are toxic and, if consumed regularly, can lead to the development of kidney stones. This research investigates adding 50-500mg increments of calcium carbonate, calcium chloride, calcium citrate and calcium sulphate to 100g of raw homogenates of spinach to determine whether calcium would combine with the soluble oxalate present in the spinach. Calcium chloride was the most effective additive while calcium carbonate was the least effective. The formation of insoluble oxalate after incubation at 25°C for 30min is a simple practical step that can be incorporated into the juicing process. This would make the juice considerably safer to consume on a regular basis. Copyright © 2016 Elsevier Ltd. All rights reserved.

  7. Structural, electrical, magnetic and dielectric properties of rare-earth substituted cobalt ferrites nanoparticles synthesized by the co-precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Nikumbh, A.K., E-mail: aknik@chem.unipune.ac.in; Pawar, R.A.; Nighot, D.V.; Gugale, G.S.; Sangale, M.D.; Khanvilkar, M.B.; Nagawade, A.V.

    2014-04-15

    Pure nanoparticles of the rare-earth substituted cobalt ferrites CoRE{sub x}Fe{sub 2−x}O{sub 4} (where RE=Nd, Sm and Gd and x=0.1 and 0.2) were prepared by the chemical co-precipitation method. X-ray diffraction, Transmission electron microscopy (TEM), d.c. electrical conductivity, Magnetic hysteresis and Thermal analysis are utilized in order to study the effect of variation in the rare-earth substitution and its impact on particle size, magnetic properties like M{sub S}, H{sub C} and Curie temperature. The phase identification of the materials by X-ray diffraction reveals the single-phase nature of the materials. The lattice parameter increased with rare-earth content for x≤0.2. The Transmission electron micrographs of Nd-, Sm- and Gd-substituted CoFe{sub 2}O{sub 4} exhibit the particle size 36.1 to 67.8 nm ranges. The data of temperature variation of the direct current electrical conductivity showed definite breaks, which corresponds to ferrimagnetic to paramagnetic transitions. The thermoelectric power for all compound are positive over the whole range of temperature. The dielectric constant decreases with frequency and rare-earth content for the prepared samples. The magnetic properties of rare-earth substituted cobalt ferrites showed a definite hysteresis loop at room temperature. The reduction of coercive force, saturation magnetization, ratio M{sub R}/M{sub S} and magnetic moments may be due to dilution of the magnetic interaction.

  8. Global Sensitivity Analysis to Assess Salt Precipitation for CO2 Geological Storage in Deep Saline Aquifers

    Directory of Open Access Journals (Sweden)

    Yuan Wang

    2017-01-01

    Full Text Available Salt precipitation is generated near the injection well when dry supercritical carbon dioxide (scCO2 is injected into saline aquifers, and it can seriously impair the CO2 injectivity of the well. We used solid saturation (Ss to map CO2 injectivity. Ss was used as the response variable for the sensitivity analysis, and the input variables included the CO2 injection rate (QCO2, salinity of the aquifer (XNaCl, empirical parameter m, air entry pressure (P0, maximum capillary pressure (Pmax, and liquid residual saturation (Splr and Sclr. Global sensitivity analysis methods, namely, the Morris method and Sobol method, were used. A significant increase in Ss was observed near the injection well, and the results of the two methods were similar: XNaCl had the greatest effect on Ss; the effect of P0 and Pmax on Ss was negligible. On the other hand, with these two methods, QCO2 had various effects on Ss: QCO2 had a large effect on Ss in the Morris method, but it had little effect on Ss in the Sobol method. We also found that a low QCO2 had a profound effect on Ss but that a high QCO2 had almost no effect on the Ss value.

  9. 4-Methoxybenzamidinium hydrogen oxalate monohydrate

    Directory of Open Access Journals (Sweden)

    Simona Irrera

    2012-12-01

    Full Text Available The title hydrated salt, C8H11N2O+·C2HO4−·H2O, was synthesized by a reaction of 4-methoxybenzamidine (4-amidinoanisole and oxalic acid in water solution. In the cation, the amidinium group forms a dihedral angle of 15.60 (6° with the mean plane of the benzene ring. In the crystal, each amidinium unit is bound to three acetate anions and one water molecule by six distinct N—H...O hydrogen bonds. The ion pairs of the asymmetric unit are joined by two N—H...O hydrogen bonds into ionic dimers in which the carbonyl O atom of the semi-oxalate anion acts as a bifurcated acceptor, thus generating an R12(6 motif. These subunits are then joined through the remaining N—H...O hydrogen bonds to adjacent semi-oxalate anions into linear tetrameric chains running approximately along the b axis. The structure is stabilized by N—H...O and O—H...O intermolecular hydrogen bonds. The water molecule plays an important role in the cohesion and the stability of the crystal structure being involved in three hydrogen bonds connecting two semi-oxalate anions as donor and a benzamidinium cation as acceptor.

  10. Co-precipitation synthesis and luminescence behavior of Ce-doped yttrium aluminum garnet (YAG:Ce) phosphor: The effect of precipitant

    International Nuclear Information System (INIS)

    Zhang Kai; Liu Hezhou; Wu Yating; Hu Wenbin

    2008-01-01

    YAG:Ce precursors were co-precipitated using ammonia water and ammonium hydrogen carbonate as precipitants, respectively. Phase transition of the precursors during sintering was compared between the two precipitants. The precursors synthesized with ammonia water transformed to YAG at about 1000 deg. C via YAlO 3 phase. The precursors synthesized with ammonium hydrogen carbonate directly converted to pure YAG at about 900 deg. C. Comparing the powders produced with the two precipitants, the powders produced with ammonia hydrogen carbonate showed good dispersity. When sintered at 1600 deg. C, aggregation of the powders synthesized with the two precipitants both became severe. With increase the sintering temperature, the maximum wavelength of excitation and emission spectra of the phosphors synthesized with ammonium water hardly varied. While the maximum wavelength of excitation spectra of the phosphors synthesized with ammonium hydrogen carbonate unchanged, and the emission spectra showed red shift. Because of size effect and higher loss of cerium content, the emission intensity of phosphors prepared with ammonium hydrogen carbonate was lower than the phosphors prepared with ammonium water, when sintered at the same temperature

  11. Acute oxalate nephropathy after ingestion of star fruit.

    Science.gov (United States)

    Chen, C L; Fang, H C; Chou, K J; Wang, J S; Chung, H M

    2001-02-01

    Acute oxalate nephropathy associated with ingestion of star fruit (carambola) has not been reported before. We report the first two cases. These patients developed nausea, vomiting, abdominal pain, and backache within hours of ingesting large quantities of sour carambola juice; then acute renal failure followed. Both patients needed hemodialysis for oliguric acute renal failure, and pathologic examinations showed typical changes of acute oxalate nephropathy. The renal function recovered 4 weeks later without specific treatment. Sour carambola juice is a popular beverage in Taiwan. The popularity of star fruit juice is not compatible with the rare discovery of star fruit-associated acute oxalate nephropathy. Commercial carambola juice usually is prepared by pickling and dilution processes that reduce oxalate content markedly, whereas pure fresh juice or mild diluted postpickled juice for traditional remedies, as used in our cases, contain high quantities of oxalate. An empty stomach and dehydrated state may pose an additional risk for development of renal injury. To avoid acute oxalate nephropathy, pure sour carambola juice or mild diluted postpickled juice should not be consumed in large amounts, especially on an empty stomach or in a dehydrated state.

  12. Growth mechanisms for spherical mixed hydroxide agglomerates prepared by co-precipitation method: A case of Ni1/3Co1/3Mn1/3(OH)2

    International Nuclear Information System (INIS)

    Yang, Yue; Xu, Shengming; Xie, Ming; He, Yinghe; Huang, Guoyong; Yang, Youcai

    2015-01-01

    Highlights: • Anisotropic growth of Ni 1/3 Co 1/3 Mn 1/3 (OH) 2 along the [0 0 1] direction was revealed. • DFT calculation results show crystal surface energies of (0 0 1) plane is highest. • A new model was proposed to explain the formation of spherical agglomerates. - Abstract: Spherical Ni 1/3 Co 1/3 Mn 1/3 (OH) 2 agglomerates were synthesized by the co-precipitation method in the presence of ammonia. The results show that the growth mechanism of spherical agglomerates follows three-stages, i.e. nucleation and anisotropic growth of single crystals; agglomeration of polycrystalline crystallites agglomerated by single crystal grains as primary particles to form embryonic agglomerates; formation, growth and consolidation of spherical agglomerates or particles by agglomeration of embryonic agglomerates, continued growth of individual crystals in the agglomerates and further attachment of primary particles. The first two stages are very fast while the last stage takes almost the entire process to complete. The main reason for the anisotropic growth of Ni 1/3 Co 1/3 Mn 1/3 (OH) 2 crystal is that crystal surface energy of E (001) , E (100) , E (101) and E (102) is different with E (001) being the highest. The morphology of the final spherical agglomerates is explained by partial re-crystallization of contacting primary particles. The growth process of spherical agglomerates was examined by X-ray diffraction, scanning electron microscope, transmission electron microscope and calculation of crystal surface energy using density function theory

  13. Removal of some Fission Products from Low Level Liquid Radioactive Waste by Chemical Precipitation liquid/Co-precipitation / Phosphate Coagulant

    International Nuclear Information System (INIS)

    Borai, E.H.; Attallah, M.F.; Hilal, M.A.; Abo-Aly, M.M.; Shehata, F.A.

    2008-01-01

    In Egypt radioactive waste has been generated from various uses of radioactive materials. Presence of cesium demonstrated a major problem from the removal point of view even by conventional and advanced technologies. Selective chemical precipitation has been oriented for removal of some fission products including 137 Cs from low level liquid radioactive waste (LLLRW). The aim of the present study was focused to investigate the effectiveness of various phosphate compounds that improved the precipitation process and hence the decontamination factor. The results showed that, maximum removal of 137 Cs reaching 46.4 % using di-sodium hydrogen phosphate as a selective coagulant. It was found that significant enhancement of co-precipitation of 137 Cs (62.5 %) was obtained due to presence of Nd 3+ in the LLLRW

  14. Application of a precipitation method for uranium recovery from abu-zaabal phosphoric acid plant, Egypt

    International Nuclear Information System (INIS)

    El-hazek, N.M.T.; Hussein, E.M.

    1995-01-01

    Current industrial recovery of uranium from 30% phosphoric acid-produced by the dihydrate process-is based on solvent extraction method. Uranium recovery from concentrated phosphoric acid (45-52% p o5 ) produced by evaporation of the 30% acid or directly produced by the hemihydrate process, by solvent extraction is difficult to apply in practice. In addition to possible contamination of the acid by the organic solvents and/or their deterioration. This paper investigates the possibility of applying a precipitation method (Weterings and Janssen, 1985) for uranium recovery from both low (28% P 2 O 5 ) and high (48% P 2 O 5 ) concentration phosphoric acids produced by abu-zaabal phosphoric acid plant (Abuzaabal fertilizers and chemicals Co., Egypt). The 28% acid produced by H 2 SO 4 dihydrate method and the 48% acid produced by evaporation of the 28% acid The applied precipitation method depends on using NH 4 F as a uranium precipitant from both low and high concentration phosphoric acids in presence of acetone as a dispersing agent. All the relevant factors have been studied

  15. Morphology and Kinetics of Growth of CaCO3 Precipitates Formed in Saline Water at 30°C

    Science.gov (United States)

    Sui, Xin; Wang, Baohui; Wu, Haiming

    2018-02-01

    The crystallization kinetics and morphology of CaCO3 crystals precipitated from the high salinity oilfield water were studied. The crystallization kinetics measurements show that nucleation and nuclei growth obey the first order reaction kinetics. The induction period of precipitation is extended in the high salinity solutions. Morphological studies show that impurity ions remain mostly in the solution phase instead of filling the CaCO3 crystal lattice. The morphology of CaCO3 precipitates can be changed from a smooth surface (calcite) to rough spheres (vaterite), and spindle rod bundles, or spherical, ellipsoid, flowers, plates and other shapes (aragonite).

  16. Structural stability and elastic properties of L12 Co3(Ga,W) precipitate from first-principle calculations

    International Nuclear Information System (INIS)

    Yao Qiang; Zhu Yuhong; Wang Yan

    2011-01-01

    Ultrasoft pseudopotential within a generalized gradient approximation was employed to study the structural stability, electronic structure, and elastic properties of ternary Co 3 (Ga,W) precipitate. The Young's and shear moduli of the polycrystals containing the Co 3 (Ga,W) precipitate were calculated using the Voigt-Reuss-Hill averaging scheme. Results show that the stable ternary Co 3 (Ga,W) compound has the L1 2 structure, and is ductile in nature. The structural stability of the Co 3 (Ga,W) compound is discussed together with the calculated electronic structure.

  17. Contrasting the co-variability of daytime cloud and precipitation over tropical land and ocean

    Science.gov (United States)

    Jin, Daeho; Oreopoulos, Lazaros; Lee, Dongmin; Cho, Nayeong; Tan, Jackson

    2018-03-01

    The co-variability of cloud and precipitation in the extended tropics (35° N-35° S) is investigated using contemporaneous data sets for a 13-year period. The goal is to quantify potential relationships between cloud type fractions and precipitation events of particular strength. Particular attention is paid to whether the relationships exhibit different characteristics over tropical land and ocean. A primary analysis metric is the correlation coefficient between fractions of individual cloud types and frequencies within precipitation histogram bins that have been matched in time and space. The cloud type fractions are derived from Moderate Resolution Imaging Spectroradiometer (MODIS) joint histograms of cloud top pressure and cloud optical thickness in 1° grid cells, and the precipitation frequencies come from the Tropical Rainfall Measuring Mission (TRMM) Multi-satellite Precipitation Analysis (TMPA) data set aggregated to the same grid.It is found that the strongest coupling (positive correlation) between clouds and precipitation occurs over ocean for cumulonimbus clouds and the heaviest rainfall. While the same cloud type and rainfall bin are also best correlated over land compared to other combinations, the correlation magnitude is weaker than over ocean. The difference is attributed to the greater size of convective systems over ocean. It is also found that both over ocean and land the anti-correlation of strong precipitation with weak (i.e., thin and/or low) cloud types is of greater absolute strength than positive correlations between weak cloud types and weak precipitation. Cloud type co-occurrence relationships explain some of the cloud-precipitation anti-correlations. Weak correlations between weaker rainfall and clouds indicate poor predictability for precipitation when cloud types are known, and this is even more true over land than over ocean.

  18. METHOD OF PROCESSING MONAZITE SAND

    Science.gov (United States)

    Welt, M.A.; Smutz, M.

    1958-08-26

    A process is described for recovering thorium, uranium, and rare earth values from monazite sand. The monazite sand is first digested with sulfuric acid and the resulting "monazite sulfate" solution is adjusted to a pH of between 0.4 and 3.0, and oxalate anions are added causing precipitation of the thorium and the rare earths as the oxalates. The oxalate precipitate is separated from the uranium containing supernatant solution, and is dried and calcined to the oxides. The thorium and rare earth oxides are then dissolved in nitric acid and the solution is contacted with tribntyl phosphate whereby an organic extract phase containing the cerium and thorium values is obtained, together with an aqueous raffinate containing the other rare earth values. The organic phase is then separated from the aqueous raffinate and the cerium and thorium are back extracted with an aqueous medium.

  19. Impact of location of CaCO3 precipitation on the development of intact anaerobic sludge

    NARCIS (Netherlands)

    Langerak, van E.P.A.; Ramaekers, H.; Wiechers, J.; Veeken, A.H.M.; Hamelers, H.V.M.; Lettinga, G.

    2000-01-01

    The development of intact anaerobic granular sludge was studied in UASB reactors under varying conditions of CaCO3 precipitation and biomass yield. Varying precipitating quantities were obtained using different calcium concentrations in the influent and different biomass yields were obtained by

  20. Current Travertines Precipitation from CO{sub 2}-rich Groundwaters as an alert of CO{sub 2} Leakages from a Natural CO{sub 2} Storage at Ganuelas-Mazarron Tertiary Basin (Murcia, Spain)

    Energy Technology Data Exchange (ETDEWEB)

    Rodrigo-Naharro, J.; Delgado, A.; Herrero, M. J.; Granados, A.; Perez del Villar, L.

    2013-02-01

    Carbon capture and storage technologies (CCS) represent the most suitable solutions related to the high anthropogenic CO{sub 2} emissions to the atmosphere. As a consequence, monitoring of the possible CO{sub 2} leakages from an artificial deep geological CO{sub 2} storage (DGS) is indispensable to guarantee its safety. Fast surficial travertine precipitation related to these CO{sub 2} leakages can be used as an alert for these escapes. Since few studies exist focusing on the long-term behaviour of an artificial CO{sub 2} DGS, natural CO{sub 2} storage affected by natural or artificial escapes must be studied as natural analogues for predicting the long-term behaviour of an artificial CO{sub 2} storage. In this context, a natural CO{sub 2} reservoir affected by artificial CO{sub 2} escapes has been studied in this work. This study has mainly focused on the current travertines precipitation associated with the upwelling CO{sub 2}-rich waters from several hydrogeological wells drilled in the Ganuelas-Mazarron Tertiary basin (SE Spain), and consists of a comprehensive characterisation of parent-waters and their associated carbonates, including elemental and isotopic geochemistry, mineralogy and petrography. Geochemical characterisation of groundwaters has led to recognise 4 hydrofacies from 3 different aquifers. These groundwaters have very high salinity and electrical conductivity; are slightly acid; present high dissolved inorganic carbon (DIC) and free CO{sub 2}; are oversaturated in both aragonite and calcite; and dissolve, mobilize and transport low quantities of heavy and/or toxic elements. Isotopic values indicate that: i) the origin of parent-waters is related to rainfalls from clouds originated in the Mediterranean Sea or continental areas; ii) the origin of C is mainly inorganic; and iii) sulphate anions come mainly from the dissolution of the Messinian gypsum from the Tertiary Basin sediments. Current travertines precipitation seems to be controlled by a

  1. Structural stability of (Pu1-xAmx)O2 (x=0.2;0.5;0.8) obtained by oxalate co-conversion

    International Nuclear Information System (INIS)

    Jankowiak, A.; Donnet, L.; Maillard, C.

    2008-01-01

    The EUROTRANS project investigates the transmutation of transuranium elements in dedicated reactors (ADS, FR). The study includes various subject areas: neutronics, physical properties, coolant type (sodium, lead, bismuth, helium), etc, and experimental work concerning the fabrication of minor actinide compounds for thermo-physical properties determination. For this program, the CEA was responsible for synthesizing three Pu 1-x Am x O 2 compounds with various Am and Pu content (x = 0.2, 0.5, 0.8). The selected synthesis route for the mixed Am and Pu oxide powder consists in actinides oxalates co-conversion. The purpose of the study was to determine by XRD the crystal structure and the lattice parameters change as a function of the time for each co-converted mixed oxides. After one year of experiment, although the lattice parameters significantly expanded, the compounds remained monophasic. The observations showed that the initial expansion rate and the a max stage value vary according to the Pu and Am content. (authors)

  2. Luminescent and morphological study of Sr2CeO4 blue phosphor prepared from oxalate precursors

    International Nuclear Information System (INIS)

    Ferrari, Jefferson L.; Pires, Ana M.; Serra, Osvaldo A.; Davolos, Marian R.

    2011-01-01

    Luminescent and morphological studies of Sr 2 CeO 4 blue phosphor prepared from cerium-doped strontium oxalate precursor are reported. Powder samples were prepared from 5 and 25 mol% Ce 3+ -doped strontium oxalate as well as from a mechanical mixture of strontium oxalate and cerium oxalate at a 4:1 ratio, respectively. All the samples were characterized by XRD, IR, PLS, and SEM. The luminescent and structural properties of the Sr 2 CeO 4 material are little affected by the SrCO 3 remaining from precursors. The Sr 2 CeO 4 material consists in one-dimensional chains of edge-sharing CeO 6 octahedra that are linked together by Sr 2+ ions. The carbonate ion might be associated with oxygen ions of the linear chain, and also with the oxygen atoms located in the equatorial position, which consequently affects the charge transfer bands between O 2- and Ce 4+ . As observed by SEM, the morphological changes are related to each kind of precursor and thermal treatment, along with irregular powder particles within the size range 0.5-2 μm.

  3. Growth of strontium oxalate crystals in agar–agar gel

    Indian Academy of Sciences (India)

    Growth of strontium oxalate crystals in agar–agar gel. P V DALAL. ∗ and K B SARAF. Postgraduate Department of Physics, Pratap College, Amalner 425 401, India. MS received 16 March 2008; revised 5 April 2010. Abstract. Single crystals of strontium oxalate have been grown by using strontium chloride and oxalic acid in.

  4. Effect of processing and cooking on total and soluble oxalate content in frozen root vegetables prepared for consumption

    Directory of Open Access Journals (Sweden)

    Z. LISIEWSKA

    2008-12-01

    Full Text Available The oxalate content of beetroot, carrot, celeriac and parsnip after freezing by traditional and modified methods (the latter resulting in a convenience food product, and after the preparation of frozen products for consumption was evaluated. The highest content of total and soluble oxalates (105 and 82 mg 100 g-1 fresh matter was found in beetroot. The lowest proportion (55% of soluble oxalates was noted in celeriac; this proportion was higher in the remaining vegetables, being broadly similar for each of them. Blanching brought about a significant decrease in total and soluble oxalates in fresh vegetables. Cooking resulted in a higher loss of oxalates. The level of oxalates in products prepared for consumption directly after freezing approximated that before freezing. Compared with the content before freezing, vegetables prepared for consumption by cooking after frozen storage contained less oxalates, except for total oxalates in parsnip and soluble oxalates in beetroot and celeriac. The highest ratio of oxalates to calcium was found in raw beetroot; it was two times lower in raw carrot; five times lower in raw celeriac; and eight times lower in raw parsnip. These ratios were lower after technological and culinary processing. The percentage of oxalate bound calcium depended on the species; this parameter was not significantly affected by the procedures applied. The true retention of oxalates according to Judprasong et al. (2006 was lower than retention calculated taking its content in 100 g fresh matter into account.;

  5. Synthesis and magnetic properties of (Eu–Ni) substituted Y-type hexaferrite by surfactant assisted co-precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Ali, Irshad, E-mail: irshadalibzu@gmail.com [Department of Physics, BahauddinZakariya University, Multan, P.O# 60800 (Pakistan); Islam, M.U. [Department of Physics, BahauddinZakariya University, Multan, P.O# 60800 (Pakistan); Sadiq, Imran [Department of Physics, BahauddinZakariya University, Multan, P.O# 60800 (Pakistan); Centre of Excellence in Solid State Physics, University of The Punjab, Lahore (Pakistan); Karamat, Nazia [Institute of Chemical Science, Bahauddin Zakariya University, Multan 60800 (Pakistan); Iftikhar, Aisha [Department of Physics, BahauddinZakariya University, Multan, P.O# 60800 (Pakistan); Khan, M. Azhar [Department of Physics, Islamia University of Bahawalpur, 63100 Pakistan (Pakistan); Shah, Afzal [Department of Chemistry, Quaid-i-Azam University, Islamabad 45320 (Pakistan); Athar, Muhammad [Institute of Chemical Science, Bahauddin Zakariya University, Multan 60800 (Pakistan); Shakir, Imran [Sustainable Energy Technologies (SET) Center, College of Engineering, King Saud University (Saudi Arabia); Ashiq, Muhammad Naeem, E-mail: naeemashiqqau@yahoo.com [Institute of Chemical Science, Bahauddin Zakariya University, Multan 60800 (Pakistan)

    2015-07-01

    A series of (Eu–Ni) substituted Y-type hexaferrite with composition Sr{sub 2}Co{sub (2−x)}Ni{sub x}Eu{sub y}Fe{sub (12−y)}O{sub 22} (x=0.0–1, Y=0.0–0.1) were prepared by the surfactant assisted co-precipitation method. The present samples were sintered at 1050 °C for 8 h. The shape of the particles is plate-like which is very advantageous for various applications and the grain size varies from 73 to 269 nm. The values of saturation magnetization (M{sub s}), remanent magnetization (M{sub r}) and magnetic moment (n{sub B}) were found to decrease which are attributed to the weakening of super exchange interactions. The values of in-plane Squareness ratios (M{sub r}/M{sub s}) ranging from 0.41 to 0.65 whereas in case of out of plane measurement it varies from 0.30 to 0.62.The investigated samples can be used in perpendicular recording media (PRM) due to high value of coercivity 2300 Oe which is analogous to the those of M-type and W-type hard magnetic. - Highlights: • The present samples sintered at 1050 °C for 8 h. • The grain size varies from 73 to 269 nm. • The magnetic moment varies from 15.27 to 6.07. • The shape of grains is plate like for microwave devices. • The present samples can be used in PRM due to high value of coercivity i.e. 2300 Oe.

  6. Enhanced Chemical Cleaning: Effectiveness Of The UV Lamp To Decompose Oxalates

    International Nuclear Information System (INIS)

    Ketusky, E.; Huff, T.; Sudduth, C.

    2010-01-01

    Enhanced Chemical Cleaning is a new process scheduled to begin cleaning Savannah River Site High Level Waste Tanks in 2012. It is an improvement over the current chemical cleaning method, in that it minimizes downstream impacts on the High Level Waste System. It is based on a state of the art scale removal process used on the secondary side of nuclear power plants, with modifications to accommodate the unique constraints created by the tanks. Both Enhanced Chemical Cleaning and the scale removal process are founded on dissolving metal oxides/hydroxides using oxalic acid, with subsequent oxalate decomposition via hydroxylation using ozone or peroxide, and UV light as a catalyst. A divergence Enhanced Chemical Cleaning has from nuclear power scale removal is the significantly increased solids concentration during oxalate decomposition. These solids can limit the ability of the UV light to create hydroxyl radicals, either by limiting the ability of the light to penetrate through the solution, or by increasing the fouling rate on the UV light. Both will decrease the overall catalytic effectiveness, thereby decreasing the concentration of formed hydroxyl radicals. The hydroxyl radicals are the driving force behind the oxalate decomposition. To understand the impact of increased solids, testing was performed using a medium pressure UV light inside an ozone supplied Oxalate Decomposition Reactor. Using a dissolved metal sludge simulant with an initial oxalate concentration greater than 12,000 ppm, and an initial pH of about 2.0, the spent acid solution was recirculated through the reactor, while the UV light was allowed to foul. For the first few hours, the oxalate decomposition rate was about 1,300 ppm/hour. After about 3 hours, enough time for the UV lamp to foul, the oxalate decomposition rate decreased to about 500 ppm/hour. The decomposition rate then remained roughly constant for the next 16 hours. Overall, testing showed that the oxalate destruction rate decreased

  7. Calcium oxalate contribution to calcium cycling in forests of contrasting nutrient status

    Science.gov (United States)

    Dauer, Jenny M.; Perakis, Steven S.

    2014-01-01

    Calcium oxalate (Ca oxalate) is an insoluble biomineral that forms in plants and fungi, and occurs in soils across many types of ecosystems. Assessing how Ca oxalate may shape ecosystem Ca cycling requires information on the distribution of Ca oxalate among plant biomass, detritus, and mineral soil, and how it varies with ecosystem Ca status. We compared two Douglas-fir forests of contrasting ecosystem Ca availability, and found that Ca oxalate was partitioned similarly among plant biomass, detritus and mineral soil major ecosystem compartments at both sites, and total pools of Ca oxalate were greater in the high-Ca forest. However, the proportional importance of Ca oxalate was greater in the low-Ca than high-Ca forest (18% versus 4% of actively cycling ecosystem Ca, respectively). And calcium oxalate in mineral soil, which is of particular interest as a potential long-term Ca reservoir, was a larger portion of total available Ca (exchangeable Ca plus Ca oxalate Ca) in the low-Ca site than the high-Ca site (9% versus 1% of available soil Ca, respectively). Calcium oxalate was the dominant form of Ca returned from plants to soil as leaf litterfall at the high-Ca site, yet calcium oxalate disappeared rapidly from decomposing litter (0.28 yr−1 or faster) at both sites. We conclude that accumulation of Ca oxalate in forest ecosystems appears most closely related to overall Ca supply for live biomass pools, and that the accumulation of Ca oxalate in forest floor and mineral soil is limited by rapid microbial degradation of putatively unavailable Ca oxalate.

  8. Magnetic and photocatalytic properties of nanocrystalline ZnMn2 O4

    Indian Academy of Sciences (India)

    Decomposition of oxalate precursors at low temperature (∼ 450°C) yielded phase pure ZnMn2O4 nanoparticles. The size of the nanoparticles of ZnMn2O4 obtained from reverse micellar method is relatively much smaller (20–30 nm) as compared to those made by the co-precipitation (40–50 nm) method. Magnetic studies ...

  9. Enhanced electrochemical performance of nano-sized LiFePO4/C synthesized by an ultrasonic-assisted co-precipitation method

    International Nuclear Information System (INIS)

    Liu Youyong; Cao Chuanbao

    2010-01-01

    A simple and effective method, the ultrasonic-assisted co-precipitation method, was employed to synthesize nano-sized LiFePO 4 /C. A glucose solution was used as the carbon source to produce in situ carbon to improve the conductivity of LiFePO 4 . Ultrasonic irradiation was adopted to control the size and homogenize the LiFePO 4 /C particles. The sample was characterized by X-ray powder diffraction, field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). FE-SEM and TEM show that the as-prepared sample has a reduced particle size with a uniform size distribution, which is around 50 nm. A uniform amorphous carbon layer with a thickness of about 4-6 nm on the particle surface was observed, as shown in the HRTEM image. The electrochemical performance was demonstrated by the charge-discharge test and electrochemical impedance spectra measurements. The results indicate that the nano-sized LiFePO 4 /C presents enhanced discharge capacities (159, 147 and 135 mAh g -1 at 0.1, 0.5 and 2 C-rate, respectively) and stable cycling performance. This study offers a simple method to design and synthesis nano-sized cathode materials for lithium-ion batteries.

  10. Raman spectral titration method: an informative technique for studying the complexation of uranyl with uranyl(vi)-DPA/oxalate systems as examples.

    Science.gov (United States)

    Liu, Qian; Zhang, Qianci; Yang, Suliang; Zhu, Haiqiao; Liu, Quanwei; Tian, Guoxin

    2017-10-10

    The Raman band at about 870 cm -1 originating from the symmetric stretch vibration (ν 1 ) of uranyl, UO 2 2+ , has proven to be very informative for investigating the complexation of uranyl using perchlorate or nitrate of known concentration as internal standards. The concentration of uranyl can be conveniently calculated by using the ratio of the directly read band intensities of uranyl and the added reference, ClO 4 - , with a factor of 1.72. While with NO 3 - of concentration lower than 1.8 M as the reference, a factor of 0.85 should be used. Furthermore, with added internal standards, the linear relationship between the Raman intensity and the concentration of the corresponding species is illustrated by the spectral titration of U(vi) with a very strong ligand, dipicolinic acid (DPA); and the application of a spectral titration method with Raman spectroscopy in studying the complexation of uranyl is demonstrated by the titration of U(vi) with oxalate. The stepwise changes in the Raman shift of 18, 17, and 6 cm -1 , corresponding to the three oxalate anions successively bonding to UO 2 2+ , imply that the coordination modes are different. In the 1 : 1 and 1 : 2 ratios of metal to ligand complexes, the oxalate anions bond to the uranyl ion in side-on bidentate mode, but in the 1 : 3 complex the third oxalate bonds in head-on mode, which is much weaker than the first two.

  11. Bioleaching of incineration fly ash by Aspergillus niger - precipitation of metallic salt crystals and morphological alteration of the fungus.

    Science.gov (United States)

    Xu, Tong-Jiang; Ramanathan, Thulasya; Ting, Yen-Peng

    2014-09-01

    This study examines the bioleaching of municipal solid waste incineration fly ash by Aspergillus niger , and its effect on the fungal morphology, the fate of the ash particles, and the precipitation of metallic salt crystals during bioleaching. The fungal morphology was significantly affected during one-step and two-step bioleaching; scanning electron microscopy revealed that bioleaching caused distortion of the fungal hyphae (with up to 10 μm hyphae diameter) and a swollen pellet structure. In the absence of the fly ash, the fungi showed a linear structure (with 2-4 μm hyphae diameter). Energy-dispersive X-ray spectroscopy and X-ray diffraction confirmed the precipitation of calcium oxalate hydrate crystals at the surface of hyphae in both one-step and two-step bioleaching. Calcium oxalate precipitation affects bioleaching via the weakening of the fly ash, thus facilitating the release of other tightly bound metals in the matrix.

  12. Determination of water-soluble forms of oxalic and formic acids in soils by ion chromatography

    Science.gov (United States)

    Karicheva, E.; Guseva, N.; Kambalina, M.

    2016-03-01

    Carboxylic acids (CA) play an important role in the chemical composition origin of soils and migration of elements. The content of these acids and their salts is one of the important characteristics for agrochemical, ecological, ameliorative and hygienic assessment of soils. The aim of the article is to determine water-soluble forms of same carboxylic acids — (oxalic and formic acids) in soils by ion chromatography with gradient elution. For the separation and determination of water-soluble carboxylic acids we used reagent-free gradient elution ion-exchange chromatography ICS-2000 (Dionex, USA), the model solutions of oxalate and formate ions, and leachates from soils of the Kola Peninsula. The optimal gradient program was established for separation and detection of oxalate and formate ions in water solutions by ion chromatography. A stability indicating method was developed for the simultaneous determination of water-soluble organic acids in soils. The method has shown high detection limits such as 0.03 mg/L for oxalate ion and 0.02 mg/L for formate ion. High signal reproducibility was achieved in wide range of intensities which correspond to the following ion concentrations: from 0.04 mg/g to 10 mg/L (formate), from 0.1 mg/g to 25 mg/L (oxalate). The concentration of formate and oxalate ions in soil samples is from 0.04 to 0.9 mg/L and 0.45 to 17 mg/L respectively.

  13. Effect of heat treatment on the structure of incorporated oxalate species and photoluminescent properties of porous alumina films formed in oxalic acid

    Science.gov (United States)

    Vrublevsky, I.; Jagminas, A.; Hemeltjen, S.; Goedel, W. A.

    2008-09-01

    The present work focuses on the use of IR spectroscopy and photoluminescence spectral measurements for studying the treatment temperature effect on the compositional and luminescent properties of oxalic acid alumina films. In line with the recent researches we have also found that heat treatment of porous alumina films formed in oxalic acid leads to considerable changes in their photoluminescence properties: upon annealing the intensity of photoluminescence (PL) increases reaching a maximum at the temperature of around 500 °C and then decreases. IR spectra of as-grown and heat-treated films have proved that PL emission in the anodic alumina films is related with the state of 'structural' oxalate species incorporated in the oxide lattice. These results allowed us to conclude that PL behavior of oxalic acid alumina films can be explained through the concept of variations in the bonding molecular orbitals of incorporated oxalate species including σ- and π-bonds.

  14. New indium selenite-oxalate and indium oxalate with two- and three-dimensional structures

    International Nuclear Information System (INIS)

    Cao Junjun; Li Guodong; Chen Jiesheng

    2009-01-01

    Two new indium(III) compounds with extended structures, [In 2 (SeO 3 ) 2 (C 2 O 4 )(H 2 O) 2 ].2H 2 O (I) and [NH 3 (CH 2 ) 2 NH 3 ][In(C 2 O 4 ) 2 ] 2 .5H 2 O (II), have been prepared under mild hydrothermal conditions and structurally characterized by single-crystal X-ray diffraction, thermogravimetric analysis and infrared spectroscopy. Compound I crystallizes in the triclinic system, space group P-1, with a=5.2596(11) A, b=6.8649(14) A, c=9.3289(19) A, α=101.78(3) o , β=102.03(3) o , γ=104.52(3) o , while compound II crystallizes in the orthorhombic system, space group Fdd2, with a=15.856(3) A, b=31.183(6) A, c=8.6688(17) A. In compound I, indium-selenite chains are bridged by oxalate units to form two-dimensional (2D) In 2 (SeO 3 ) 2 C 2 O 4 layers, separated by non-coordinating water molecules. In compound II, the indium atoms are connected through the oxalate units to generate a 3D open framework containing cross-linked 12- and 8-membered channels. - Graphical abstract: Two new indium(III) compounds have been hydrothermally synthesized and structurally characterized. In I, the indium-selenite chains are bridged by oxalate units to form 2D In 2 (SeO 3 ) 2 C 2 O 4 layers. In II, the indium atoms are connected through the oxalate units to generate a 3D open framework containing cross-linked 12- and 8-membered ring channels

  15. Synthesis of DME by CO2 hydrogenation over La2O3-modified CuO-ZnO-ZrO2/HZSM-5 catalysts

    Directory of Open Access Journals (Sweden)

    Zhang Yajing

    2017-01-01

    Full Text Available A series of La2O3-modified CuO-ZnO-ZrO2/HZSM-5 catalysts were prepared by an oxalate co-precipitation method. The catalysts were fully characterized by X-ray diffraction (XRD, N2 adsorption-desorption, hydrogen temperature pro-grammed reduction (H2-TPR, ammonia temperature programmed desorption (NH3-TPD, and X-ray photoelectron spectroscopy (XPS techniques. The effect of the La2O3 content on the structure and performance of the catalysts was thoroughly investigated. The catalysts were evaluated for the direct synthesis of dimethyl ether (DME from CO2 hydrogenation. The results displayed that La2O3 addition enhanced catalytic performance, and the maximal CO2 conversion (34.3% and DME selectivity (57.3% were obtained over the catalyst with 1% La2O3, which due to the smaller size of Cu species and a larger ratio of Cu+/Cu.

  16. Determination of alkaloids and oxalates in some selected food ...

    African Journals Online (AJOL)

    STORAGESEVER

    2009-01-05

    Jan 5, 2009 ... MATERIALS AND METHODS. Source of samples. Samples ... until the colour of solution changed from salmon pink colour to a faint yellow colour. .... Effect of cooking on the soluble and insoluble oxalate content of some New ...

  17. Photodegradation of Acid Black 1 and Removing Heavy Metals from the Water by an Inorganic Nanocomposite Synthesized via Simple Co-Precipitation Method

    Directory of Open Access Journals (Sweden)

    Marziyeh Mohammadi

    2016-07-01

    Full Text Available In this experimental work, PbS/ZnS/ZnO nanocomposite was synthesized via a simple co-precipitation method. The effect of Zn2+/Pb2+ mole ratio was investigated on the product size and morphology. The products were characterized via scanning electron microscopy to obtain product size and morphology. The optical properties of the nanocomposites were studied by ultra violet-visible spectroscopy. Photocatalytic activity of the product was examine by decomposition of acid black 1 as dye. To investigation of the effect of as synthesized nanocomposite on the water treatment, the influences of the nanocomposite to remove heavy ions was studied by atomic absorption spectroscopy. The results showed that the synthesized nanocomposite has well optical properties, photocatalytic and water treatment activities.

  18. Oxalate secretion by ectomycorrhizal Paxillus involutus is mineral-specific and controls calcium weathering from minerals

    Science.gov (United States)

    Schmalenberger, A.; Duran, A. L.; Bray, A. W.; Bridge, J.; Bonneville, S.; Benning, L. G.; Romero-Gonzalez, M. E.; Leake, J. R.; Banwart, S. A.

    2015-01-01

    Trees and their associated rhizosphere organisms play a major role in mineral weathering driving calcium fluxes from the continents to the oceans that ultimately control long-term atmospheric CO2 and climate through the geochemical carbon cycle. Photosynthate allocation to tree roots and their mycorrhizal fungi is hypothesized to fuel the active secretion of protons and organic chelators that enhance calcium dissolution at fungal-mineral interfaces. This was tested using 14CO2 supplied to shoots of Pinus sylvestris ectomycorrhizal with the widespread fungus Paxillus involutus in monoxenic microcosms, revealing preferential allocation by the fungus of plant photoassimilate to weather grains of limestone and silicates each with a combined calcium and magnesium content of over 10 wt.%. Hyphae had acidic surfaces and linear accumulation of weathered calcium with secreted oxalate, increasing significantly in sequence: quartz, granite mineral-specific oxalate exudation in ectomycorrhizal weathering to dissolve calcium bearing minerals, thus contributing to the geochemical carbon cycle. PMID:26197714

  19. Sintering behaviour of CeO2-Gd2O3 powders prepared by the oxalate coprecipitation method

    International Nuclear Information System (INIS)

    Duran, P.; Jurado, J.R.; Moure, C.

    1993-01-01

    The powder and compact characteristics as well as the sintering behaviour of two CeO 2 -Gd 2 O 3 compositions prepared by the oxalate coprecipitation method are studied as a function of the powder particle size and the pore-size distribution in the powder compacts. Shrinkage was measured at a constant heating rate and the results are compared with those obtained by isothermal sintering experiments. Grain growth and microstructural development on sintered samples were studied. (orig.)

  20. A study on the separation method of total rare earth oxides in Xenotime

    International Nuclear Information System (INIS)

    Shim, Sang Kwon; Park, Hea Kyung; Kim, Kyung Lim

    1990-01-01

    This study is concerned with the separation method of total rare earth oxides in Xenotime by acid digest method. Thioacetamide was used as a carrier, tartaric acid was used as a masking agent and oxalic acid was used as a precipitant. So the effects of three acid digest methods, pH of the solution, digesting time,tartaric acid, oxalic acid and aging time were oberved. The results showed that the best acid digest method was sulfuric acid leaching and mixed acid digest method, and that pH of the solution was 2, digesting time was 4 hours, tartaric acid was 100 ml of 2% solution, oxalic acid was 8 gr. and aging time was 1 hour. Through this experiment, it was confirmed by X-ray diffractometer that the separated total rare earth oxides consisted of the Yttrium and the other rare earth elements : Gadolinium, Dysprosium, Erbium, Ytterbium and trace rare earth elements. The pure rare earth oxides being separated by this method were dried and ignited at 900 deg C (Author)

  1. Neurotoxic effects of carambola in rats: the role of oxalate.

    Science.gov (United States)

    Chen, Chien-Liang; Chou, Kang-Ju; Wang, Jyh-Seng; Yeh, Jeng-Hsien; Fang, Hua-Chang; Chung, Hsiao-Min

    2002-05-01

    Carambola (star fruit) has been reported to contain neurotoxins that cause convulsions, hiccups, or death in uremic patients, and prolong barbiturate-induced sleeping time in rats. The constituent responsible for these effects remains uncertain. Carambola contains a large quantity of oxalate, which can induce depression of cerebral function and seizures. This study was conducted to investigate the role of oxalate in carambola toxicity in rats. The effects on barbiturate-induced sleeping time and death caused by intraperitoneal administration of carambola juice were observed in Sprague-Dawley rats. To obtain a dose-dependent response curve and evaluate the lethal dose, rats were treated with serial amounts of pure carambola juice diluted with normal saline in a volume of 1:1. To test the role of oxalate in the neurotoxic effect of carambola, either 5.33 g/kg carambola after oxalate removal or 5.33 g/kg of pure carambola juice diluted with normal saline were administered intraperitoneally, while the control group was given normal saline before pentobarbital injection. The effects of carambola and oxalate-removed carambola on barbiturate-induced sleeping time were compared with those of saline. To assess the lethal effect of oxalate in carambola, we gave rats chemical oxalate at comparable concentrations to the oxalate content of carambola. Carambola juice administration prolonged barbiturate-induced sleeping time in a dose-dependent manner. The sleeping time of rats that received normal saline and 1.33 g/kg, 2.67 g/kg, 5.33 g/kg, and 10.67 g/kg of carambola juice were 66 +/- 16.6, 93.7 +/- 13.4, 113.3 +/- 11.4, 117.5 +/- 29.0, and 172.5 +/- 38.8 minutes, respectively. The three higher-dose groups had longer sleeping times than controls (p carambola juice. Four of eight rats in the 10.67-g/kg group and all rats in the 21.33 g/kg and chemical oxalate groups died after seizure. Lethal doses of carambola juice were rendered harmless by the oxalate removal procedure

  2. 3.2.1. Synthesis, crystal and molecular structure of catena-(bis(µ1-oxalic acid)-µ3-hydrogen oxalate-di-aqua-sodium(I)).

    OpenAIRE

    Olga Kovalchukova*, Sergey Aldoshin, Andrey Utenyshev, Konstantin Bogenko, Valeriy Tkachev

    2015-01-01

    The crystal and molecular structure of catena-(bis(µ- oxalic acid)-µ-hydrogen oxalate-di-aqua-sodium(I)) was detected by X-Ray analysis. The compound crystallizes in the triclinic space group P-1, with a(Å) 6.2378(12); b(Å) 7,1115(14); c(Å) 10.489(2); α(°) 94.65(3); β(°) 100.12(3); γ(°) 97.78(3). The sodium cation in the title compound is eight coordinated and forms a square antiprism. It is surrounded by two molecules of oxalic acid, one hydrogen oxalate anion and one water molecule. Both ox...

  3. Separation of Co(II) from dilute aqueous solutions by precipitate and adsorbing colloid flotation

    International Nuclear Information System (INIS)

    Aziz, M.; Benyamin, K.; Shakir, K.; Atomic Energy Establishment, Cairo

    1993-01-01

    Ion, precipitate and adsorbing colloid flotation of cobalt(II) have been investigated at different pH values, using N-dodecylpyridinium chloride (DPCl). A strong cationic surfactant, and sodium lauryl sulfate (NaLS), a strong anionic surfactant, as collectors. In case of adsorbing colloid flotation, hydrous manganese dioxide was used as an adsorbent. The precipitate flotation curves experimentally obtained with the two tested collectors were compared with the corresponding theoretical one calculated from the data published for Co(II) hydrolysis. The effects of the collector concentration, ageing of the water-MnO 2 -Co(II) system, bubbling time period, cobalt(II) concentration and foreign salts on the percent removal of Co(II) by adsorbing colloid flotation using DPCl as collector were determined. Removals approaching 100% could be achieved under the optimum conditions. (author) 44 refs.; 6 figs

  4. Carbamazepine-Fumaric Acid Co-Crystal Screening Using Solution Based Method

    Directory of Open Access Journals (Sweden)

    Abd Rahim Syarifah

    2016-01-01

    Full Text Available Co-crystals is a multi-component system which connected by non-covalent interactions, present physically as a solid form under ambient conditions. Nowadays, co-crystal has becoming as an alternative approach to improve the bioavailability of poor water soluble drugs especially for a weakly ionisable groups or neutral compounds. In this study the co-crystal screening was carried out for carbamazepine (CBZ and fumaric acid (FUM co-crystal former (CCF using non-stoichiometric method (addition of CBZ to CCF saturated solution and stoichiometric method (evaporation of 1:1 molar ratio of CBZ to CCF in acetonitrile, ethyl acetate, propanol, ethanol and formic acid solvent systems. The crystals produced from the screening were characterized using Powder X-ray Diffraction (PXRD, Differential Scanning Calorimetry (DSC and Fourier Transform Infrared (FT-IR. The PXRD analysis had confirmed that the co-crystal was successfully formed in both methods for all of the solvent system studied with an exception to formic acid in the stoichiometric method where no crystal was found precipitate. The findings from this study revealed that Form A and Form B of CBZ-FUM co-crystal had been successfully formed from different solvent systems.

  5. Isotopic fractionation of NBS oxalic acid and its influence in the calculated age of materials

    International Nuclear Information System (INIS)

    Nehmi, V.A.

    1979-10-01

    The intensity of the isotopic fractionation during the oxidation of NBS oxalic acid to carbon dioxide was checked. 30 reactions of oxidation of NBS oxalic acid with potassium permanganate were made. The resultant isotopic composition of CO 2 has been determined with a mass-spectrometer. A conclusion has been reached that the average of Δ 13 C is - 18.9% o with variation between - 17.7 and - 21.2%o. For values of Δ 13 C equal to - 22.0%o, the calculated age with isotopic correction shows the following deviations in relation to non-corrected age: 4% for materials of 1,000 years and 0.3% for 20,000 years.(Author) [pt

  6. Oxalic acid biosynthesis and oxalacetate acetylhydrolase activity in Streptomyces cattleya

    International Nuclear Information System (INIS)

    Houck, D.R.; Inamine, E.

    1987-01-01

    In addition to producing the antibiotic thienamycin, Streptomyces cattleya accumulates large amounts of oxalic acid during the course of a fermentation. Washed cell suspensions were utilized to determine the specific incorporation of carbon-14 into oxalate from a number of labeled organic and amino acids. L-[U- 14 C]aspartate proved to be the best precursor, whereas only a small percentage of label from [1,5- 14 C]citrate was found in oxalate. Cell-free extracts catalyzed the formation of [ 14 C]oxalate and [ 14 C]acetate from L-[U- 14 C]aspartate. When L-[4- 14 C]aspartate was the substrate only [ 14 C]acetate was formed. The cell-free extracts were found to contain oxalacetate acetylhydrolase, the enzyme that catalyzes the hydrolysis of oxalacetate to oxalate and acetate. The enzyme is constitutive and is analogous to enzymes in fungi that produce oxalate from oxalacetate. Properties of the crude enzyme were examined

  7. Choice of precipitant and calcination temperature of precursor for synthesis of NiCo2O4 for control of CO-CH4 emissions from CNG vehicles.

    Science.gov (United States)

    Trivedi, Suverna; Prasad, Ram

    2018-03-01

    Compressed natural gas (CNG) is most appropriate an alternative of conventional fuel for automobiles. However, emissions of carbon-monoxide and methane from such vehicles adversely affect human health and environment. Consequently, to abate emissions from CNG vehicles, development of highly efficient and inexpensive catalysts is necessary. Thus, the present work attempts to scan the effects of precipitants (Na 2 CO 3 , KOH and urea) for nickel cobaltite (NiCo 2 O 4 ) catalysts prepared by co-precipitation from nitrate solutions and calcined in a lean CO-air mixture at 400°C. The catalysts were used for oxidation of a mixture of CO and CH 4 (1:1). The catalysts were characterized by X-ray diffractometer, Brunauer-Emmett-Teller surface-area, X-ray photoelectron spectroscopy; temperature programmed reduction and Scanning electron microscopy coupled with Energy-Dispersive X-Ray Spectroscopy. The Na 2 CO 3 was adjudged as the best precipitant for production of catalyst, which completely oxidized CO-CH 4 mixture at the lowest temperature (T 100 =350°C). Whereas, for catalyst prepared using urea, T 100 =362°C. On the other hand the conversion of CO-CH 4 mixture over the catalyst synthesized by KOH limited to 97% even beyond 400°C. Further, the effect of higher calcination temperatures of 500 and 600°C was examined for the best catalyst. The total oxidation of the mixture was attained at higher temperatures of 375 and 410°C over catalysts calcined at 500 and 600°C respectively. Thus, the best precipitant established was Na 2 CO 3 and the optimum calcination temperature of 400°C was found to synthesize the NiCo 2 O 4 catalyst for the best performance in CO-CH 4 oxidation. Copyright © 2017. Published by Elsevier B.V.

  8. Some analytical methods used by the Marcoule Centre for the control of radioactive effluents; Quelques methodes analytiques, utilisees sur le centre de Marcoule pour le controle radioactif des effluents

    Energy Technology Data Exchange (ETDEWEB)

    Scheidhauer, J.; Messainguiral, L.; Drogue, N.; Meiranesio, A. M.

    1962-07-09

    After three years of operation, the authors propose a review of the various methods used to determine the radioactivity of wastewaters released by the Marcoule Centre Laboratory. They describe the three main steps of this control: firstly, measurements of the global alpha radioactivity and beta radioactivity (principle and measurement method), secondly, dosing of strontium 89 and strontium 90 (principle, used reactants, operation mode for nitric compound precipitation, ferric decontamination, separation of barium 140, oxalic precipitation, precipitate counting, exploitation of counting results), and thirdly, the possible dosing of other fission products present in the effluents: cerium 144, plutonium (by two different methods), natural uranium, caesium 137, zirconium 95, niobium 95, ruthenium 103 and 106, iodine 131. The principle, reactants, operational mode with different precipitations, measurement devices are indicated for each of these radio-elements.

  9. Isolation and some characteristics of anaerobic oxalate-degrading bacteria from the rumen.

    OpenAIRE

    Dawson, K A; Allison, M J; Hartman, P A

    1980-01-01

    Obligately anaerobic oxalate-degrading bacteria were isolated from an enriched population of rumen bacteria in an oxalate-containing medium that had been depleted of other readily metabolized substrates. These organisms, which are the first reported anaerobic oxalate degraders isolated from the rumen, were gram negative, nonmotile rods. They grew in a medium containing sodium oxalate, yeast extract, cysteine, and minerals. The only substrate that supported growth was oxalate. Growth was direc...

  10. ENHANCED CHEMICAL CLEANING: EFFECTIVENESS OF THE UV LAMP TO DECOMPOSE OXALATES

    Energy Technology Data Exchange (ETDEWEB)

    Ketusky, E.; Huff, T.; Sudduth, C.

    2010-01-19

    Enhanced Chemical Cleaning is a new process scheduled to begin cleaning Savannah River Site High Level Waste Tanks in 2012. It is an improvement over the current chemical cleaning method, in that it minimizes downstream impacts on the High Level Waste System. It is based on a state of the art scale removal process used on the secondary side of nuclear power plants, with modifications to accommodate the unique constraints created by the tanks. Both Enhanced Chemical Cleaning and the scale removal process are founded on dissolving metal oxides/hydroxides using oxalic acid, with subsequent oxalate decomposition via hydroxylation using ozone or peroxide, and UV light as a catalyst. A divergence Enhanced Chemical Cleaning has from nuclear power scale removal is the significantly increased solids concentration during oxalate decomposition. These solids can limit the ability of the UV light to create hydroxyl radicals, either by limiting the ability of the light to penetrate through the solution, or by increasing the fouling rate on the UV light. Both will decrease the overall catalytic effectiveness, thereby decreasing the concentration of formed hydroxyl radicals. The hydroxyl radicals are the driving force behind the oxalate decomposition. To understand the impact of increased solids, testing was performed using a medium pressure UV light inside an ozone supplied Oxalate Decomposition Reactor. Using a dissolved metal sludge simulant with an initial oxalate concentration greater than 12,000 ppm, and an initial pH of about 2.0, the spent acid solution was recirculated through the reactor, while the UV light was allowed to foul. For the first few hours, the oxalate decomposition rate was about 1,300 ppm/hour. After about 3 hours, enough time for the UV lamp to foul, the oxalate decomposition rate decreased to about 500 ppm/hour. The decomposition rate then remained roughly constant for the next 16 hours. Overall, testing showed that the oxalate destruction rate decreased

  11. Pore-Scale Study of Transverse Mixing Induced CaCO 3 Precipitation and Permeability Reduction in a Model Subsurface Sedimentary System

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Changyong; Dehoff, Karl; Hess, Nancy; Oostrom, Mart; Wietsma, Thomas W.; Valocchi, Albert J.; Fouke, Bruce W.; Werth, Charles J.

    2010-10-15

    A microfluidic pore structure etched into a silicon wafer was used as a two-dimensional model subsurface sedimentary system (i.e., a micromodel) to study mineral precipitation and permeability reduction relevant to groundwater remediation and geological carbon sequestration. Solutions containing CaCl2 and Na2CO3 at four different saturation states (Ω = [Ca2+] [CO32-] / KspCaCO3) were introduced through two separate inlets and they mixed by diffusion transverse to the main flow direction along the center of the micromodel resulting in CaCO3 precipitation. Precipitation rates increased and the total amount of precipitates decreased with increasing saturation state, and only vaterite and calcite crystals were formed (no aragonite). The relative amount of vaterite increased from 80% at the lowest saturation (Ωv = 2.8 for vaterite) state to 95% at the highest saturation state (Ωv = 4.5). Fluorescent tracer tests conducted before and after CaCO3 precipitation indicate that pore spaces were completely occluded by CaCO3 precipitates along the transverse mixing zone, thus significantly reducing porosity and permeability, and potentially limiting transformation from vaterite to the more stable calcite. The results suggest that mineral precipitation along plume margins can decrease both reactant mixing during groundwater remediation, and injection and storage efficiency during CO2 sequestration.

  12. Zirconium-carbon hybrid sorbent for removal of fluoride from water: oxalic acid mediated Zr(IV) assembly and adsorption mechanism

    Science.gov (United States)

    Halla, Velazquez-Jimenez Litza; Hurt Robert, H; Juan, Matos; Rene, Rangel-Mendez Jose

    2014-01-01

    When activated carbon (AC) is modified with zirconium(IV) by impregnation or precipitation, the fluoride adsorption capacity is typically improved. There is significant potential to improve these hybrid sorbent by controlling the impregnation conditions, which determine the assembly and dispersion of the Zr phases on carbon surfaces. Here, commercial activated carbon was modified with Zr(IV) together with oxalic acid (OA) used to maximize the zirconium dispersion and enhance fluoride adsorption. Adsorption experiments were carried out at pH 7 and 25 °C with a fluoride concentration of 40 mg L−1. The OA/Zr ratio was varied to determine the optimal conditions for subsequent fluoride adsorption. The data was analyzed using the Langmuir and Freundlich isotherm models. FTIR, XPS and the surface charge distribution were performed to elucidate the adsorption mechanism. Potentiometric titrations showed that the modified activated carbon (ZrOx-AC) possesses positive charge at pH lower than 7, and FTIR analysis demonstrated that zirconium ions interact mainly with carboxylic groups on the activated carbon surfaces. Moreover, XPS analysis demonstrated that Zr(IV) interacts with oxalate ions, and the fluoride adsorption mechanism is likely to involve –OH− exchange from zirconyl oxalate complexes. PMID:24359079

  13. Spectroscopic properties of Pr -doped erbium oxalate crystals

    Indian Academy of Sciences (India)

    Spectroscopic properties of praseodymium ions-doped erbium oxalate ... solution with specific gravity 1.04 g/cm3 was mixed homogeneously with 0.5 M oxalic ... of concentrated nitric acid were transferred carefully and gently through the wall ...

  14. High-temperature plastic flow of a precipitation-hardened FeCoNiCr high entropy alloy

    Energy Technology Data Exchange (ETDEWEB)

    He, J.Y.; Wang, H.; Wu, Y.; Liu, X.J. [State Key Laboratory for Advanced Metals and Materials, University of Science and Technology Beijing, Beijing 100083 (China); Nieh, T.G. [Department of Materials Science and Engineering, the University of Tennessee, Knoxville, TN 37996 (United States); Lu, Z.P., E-mail: luzhaoping@163.com [State Key Laboratory for Advanced Metals and Materials, University of Science and Technology Beijing, Beijing 100083 (China)

    2017-02-16

    In this work, we systematically investigated flow behavior of a high entropy alloy (HEA) strengthened by coherent γ′ precipitates in the temperature range of 1023–1173 K. In contrast to the single-phase FeCoNiCrMn HEA, this precipitate-hardened alloy, i.e., (FeCoNiCr){sub 94}Ti{sub 2}Al{sub 4}, exhibited large reduction of the steady-state strain rate (by ~2 orders of magnitude) or drastic enhancement in flow stress, indicating significant improvement in high-temperature properties. Our results showed that the deformation could be divided into two regimes. At temperatures below 1123 K, coherent γ′ precipitates effectively blocked the dislocation motion, thus resulted in a threshold stress effect. Above 1123 K, however, γ′ particles dissolved and the deformation was controlled by the ordinary dislocation climb mechanism. In addition, we conducted transmission electron microscopy to characterize dislocation-precipitate interaction to provide microstructural evidences to support our conclusion of the specific deformation mechanisms in the two temperature regimes.

  15. Investigation on clean-up of Zr and HDBP in PUREX process with UDMH oxalate

    International Nuclear Information System (INIS)

    Zhang Youzhi; Wang Xuanjun; Li Zhengli; Liu Xiangxuan

    2007-01-01

    It is generally accepted that the interracial crud formation is related to the complex formation of Zr with degradation products of TBP, such as DBP and MBP, in PUREX process, especially in the first cycle. The crud seriously deteriorates the operation of extraction column and therefore must be properly cleared up. Various clear up methods were studied and those with salt-free washing agents were recently focused. In this paper a new scrubbing agent 1,1- dimethylhydrazine (UDMH) oxalate was proposed, the optimized experimental conditions were described, and the possible mechanism was discussed. The influence of different factors, including reaction temperature, UDMH oxalate concentration, organic-to-aqueous phase ratio, and free UDMH concentration, on the decontamination factors were examined with simulated Zr- and/or DBP-loaded solvents. The optical experimental parameters are found as follows: temperature 40-60 degree C, phase ratio V (o) /V (a) =1, concentration of UDMH oxalate solution 0.4-0.6 mol/L. Especialy some UDMH was added into the UDMH oxalate queues solution to make the concentration of free UDMH 0.2-0.3 mol/L. Under these conditions, the decontaminator factor of Zr from the corresponding simulated solvent with UDMH oxalate is up to 143, slightly higher than that with sodium carbonate. The decontamination factor of HDBP from the corresponding simulated solvent with UDMH oxalate is up to 100, similar to sodium carbonate. (authors)

  16. Interaction of Celestine Concentrate and Reagent Grade SrSO4 with Oxalate Solutions

    Directory of Open Access Journals (Sweden)

    Abdullah Obut

    2012-12-01

    Full Text Available The interaction of reagent grade strontium sulphate and celestine concentrate with aqueous solutions of oxalic acid, sodiumoxalate and ammonium oxalate for the production of strontium carbonate were investigated for different oxalate compound:SrSO4 moleratios and reaction times using x-ray diffraction analysis and dissolution tests. Under the same experimental conditions, it was foundthat aqueous oxalic acid and sodium oxalate solutions had no or little effect on reagent grade strontium sulphate or celestineconcentrate, but aqueous ammonium oxalate solution converted them into strontium oxalate hydrate. Strontium carbonate was obtainedat conversion ratios of 74.7% for the celestine concentrate and 84.6 % for the reagent grade strontium sulphate by the decompositionof the obtained strontium oxalate hydrate at 600 °C under air atmosphere.

  17. Smad signaling pathway in pathogenesis of kidney injury induced by calcium oxalate stone in rats

    Directory of Open Access Journals (Sweden)

    Fan Zhang

    2016-10-01

    Full Text Available Objective: To investigate the involvement of Smad signaling pathway in the pathogenesis of kidney injury induced by calcium oxalate stone in rats to provide a reference for clinical treatment. Methods: Clean SD rats were randomly divided into 3 group, namely the control group, model group and pirfenidone group. Ethylene glycol + αhydroxy vitamin D3 was used as a stone-inducing agent to replicate the renal calcium oxalate stone model. Rats in the pirfenidone group were treated with pirfenidone intragastric administration. The serum Cr, BUN and 24-hour oxalate and calcium in renal tissues were assayed. The expressions of Bax/ Bcl2 protein, Caspase3 protein, TGFβ, Smad1, Smad2 and Smad3 proteins were detected by the fluorescent quantitation PCR method. Results: Compared with the rats of the control group, the results showed that the levels of serum BUN, Cr and 24-hour oxalate in rats of the model group were increased greatly, Bax and Caspase3 mRNA also increased while the level of Bcl2 decreased significantly, and the expressions of TGFβ, Smad1, Smad2 and Smad3 proteins increased distinctly as well (P<0.01. These abnormal parameters could be normalized effectively by pirfenidone. Conclusions: Activated TGFβ/Smad signaling pathway is involved in the pathogenesis of kidney injury induced by calcium oxalate stone in rats.

  18. Catalytic ozonation of oxalate with a cerium supported palladium oxide: An efficient degradation not relying on hydroxyl radical oxidation

    KAUST Repository

    Zhang, Tao; Li, Weiwei; Croue, Jean-Philippe

    2011-01-01

    The cerium supported palladium oxide (PdO/CeO 2) at a low palladium loading was found very effective in catalytic ozonation of oxalate, a probe compound that is difficult to be efficiently degraded in water with hydroxyl radical oxidation and one of the major byproducts in ozonation of organic matter. The oxalate was degraded into CO 2 during the catalytic ozonation. The molar ratio of oxalate degraded to ozone consumption increased with increasing catalyst dose and decreasing ozone dosage and pH under the conditions of this study. The maximum molar ratio reached around 1, meaning that the catalyst was highly active and selective for oxalate degradation in water. The catalytic ozonation, which showed relatively stable activity, does not promote hydroxyl radical generation from ozone. Analysis with ATR-FTIR and in situ Raman spectroscopy revealed that 1) oxalate was adsorbed on CeO 2 of the catalyst forming surface complexes, and 2) O 3 was adsorbed on PdO of the catalyst and further decomposed to surface atomic oxygen (*O), surface peroxide (*O 2), and O 2 gas in sequence. The results indicate that the high activity of the catalyst is related to the synergetic function of PdO and CeO 2 in that the surface atomic oxygen readily reacts with the surface cerium-oxalate complex. This kind of catalytic ozonation would be potentially effective for the degradation of polar refractory organic pollutants and hydrophilic natural organic matter. © 2011 American Chemical Society.

  19. Catalytic ozonation of oxalate with a cerium supported palladium oxide: An efficient degradation not relying on hydroxyl radical oxidation

    KAUST Repository

    Zhang, Tao

    2011-11-01

    The cerium supported palladium oxide (PdO/CeO 2) at a low palladium loading was found very effective in catalytic ozonation of oxalate, a probe compound that is difficult to be efficiently degraded in water with hydroxyl radical oxidation and one of the major byproducts in ozonation of organic matter. The oxalate was degraded into CO 2 during the catalytic ozonation. The molar ratio of oxalate degraded to ozone consumption increased with increasing catalyst dose and decreasing ozone dosage and pH under the conditions of this study. The maximum molar ratio reached around 1, meaning that the catalyst was highly active and selective for oxalate degradation in water. The catalytic ozonation, which showed relatively stable activity, does not promote hydroxyl radical generation from ozone. Analysis with ATR-FTIR and in situ Raman spectroscopy revealed that 1) oxalate was adsorbed on CeO 2 of the catalyst forming surface complexes, and 2) O 3 was adsorbed on PdO of the catalyst and further decomposed to surface atomic oxygen (*O), surface peroxide (*O 2), and O 2 gas in sequence. The results indicate that the high activity of the catalyst is related to the synergetic function of PdO and CeO 2 in that the surface atomic oxygen readily reacts with the surface cerium-oxalate complex. This kind of catalytic ozonation would be potentially effective for the degradation of polar refractory organic pollutants and hydrophilic natural organic matter. © 2011 American Chemical Society.

  20. Degradation of sulfated polysaccharide extracted from algal Laminaria japonica and its modulation on calcium oxalate crystallization

    Energy Technology Data Exchange (ETDEWEB)

    Ouyang Jianming, E-mail: toyjm@jnu.edu.cn [Department of Chemistry, Jinan University, Guangzhou 510632 (China); Institute of Biomineralization and Lithiasis Research, Jinan University, Guangzhou 510632 (China); Wang Miao; Lu Peng; Tan Jin [Department of Chemistry, Jinan University, Guangzhou 510632 (China); Institute of Biomineralization and Lithiasis Research, Jinan University, Guangzhou 510632 (China)

    2010-08-30

    Sulfated polysaccharide (LPS) extracted from alga Laminaria japonica was degraded by hydrogen peroxide (H{sub 2}O{sub 2}). The average molecular weight of LPS was apparently decreased from 172,000 to 9550 after degradation, while the proportion of sulfate groups (-OSO{sub 3}{sup -}) and carboxylic groups (-COO{sup -}) in the molecular chains of LPS were slightly decreased from 4.5% and 5.20% to 3.9% and 4.64%, respectively. The effects of degraded and natural LPS on formation of calcium oxalate (CaOxa) crystals were investigated in vitro using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), zeta-potential, and atomic absorption spectroscopy. LPS could increase the concentration of soluble Ca{sup 2+} ions in the solution, decrease the weight of precipitated CaOxa, and increase the negative value of zeta-potential of CaOxa crystals. LPS also inhibits the formation of thermodynamically stable calcium oxalate monohydrate (COM) crystals, while inducing and stabilizing metastable calcium oxalate dihydrate (COD) crystals. These results suggested that both degraded and natural LPS could decrease CaOxa crystallization, but the inhibition efficiency of the degraded LPS was clearly superior to that of the natural LPS. We expected this investigation would provide encouragement for further exploration into new drugs for the prevention and treatment of urolithiasis.

  1. Photocatalytic properties of BiVO4 prepared by the co-precipitation method: Degradation of rhodamine B and possible reaction mechanisms under visible irradiation

    International Nuclear Information System (INIS)

    Martinez-de la Cruz, A.; Perez, U.M. Garcia

    2010-01-01

    Bismuth vanadate (BiVO 4 ) was synthesized by the co-precipitation method at 200 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 4 photocatalyst (∼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 dissolved O 2 , and irradiation source was studied in order to know the details about the photodegradation mechanism.

  2. The enthalpies of interactions of Ca2+(aq) and C2O{4/2-} (aq) ions in complexon solutions: Competition between complexation and precipitation

    Science.gov (United States)

    Kustov, A. V.; Smirnova, N. L.; Berezin, B. D.; Trostin, V. N.

    2010-04-01

    The thermal effects of mixing of aqueous calcium chloride with sodium citrate and ethylenedi-aminetetraacetate in the absence and presence of sodium oxalate have been measured at 25°C. The thermal effects of dilution of aqueous calcium chloride solutions were determined. The thermal effects of calcium oxalate precipitation and formation of calcium complexes with citrate and ethylenediaminetetraacetate ions were calculated. The 1% solution of sodium citrate inhibited the formation of CaC2O4 (s); in a 1% solution of sodium ethylenediaminetetraacetate with [Ca2+][C2O{4/2-}] > 10-5, the endothermal formation of the [CaEdta]2- complex quickly changed to exothermal precipitation. The 3 and 5% solutions of complexons showed a pronounced inhibiting effect on the formation of urinary stones even when the concentration of calcium and oxalate ions in solution exceeded the product of solubility of CaC2O4 by four and more orders of magnitude.

  3. PTFE Additive and Re-annealing Effect on Thermoluminescence Response of CaSO4:Dy Derived from Co-precipitation Method

    Science.gov (United States)

    Nuraeni, Nunung; Dwi Septianto, Ricky; Iskandar, Ferry; Haryanto, Freddy; Waris, Abdul; Hiswara, Eri

    2017-07-01

    Effect of re-annealing treatment in thermoluminescence response of thermoluminescent dosimeter (TLD) CaSO4:Dy and CaSO4:Dy with PTFE (Polytetrafluoroethylene) addition was investigated. CaSO4:Dy was prepared by a co-precipitation method. The PTFE was added before re-annealing treatment which the mass ratio of CaSO4:Dy and PTFE was fixed to 2:3. The re-annealing treatments of the samples were done at temperature 700 °C for 1 hr. The obtained samples were characterized using a Fourier-transform infrared (FTIR) and X-ray diffraction (XRD) to observe the molecule bonding in sample and crystal properties, respectively. From the experimental results, it was observed that the thermoluminescence intensity of CaSO4:Dy, CaSO4:Dy re-annealed at 700 °C, and CaSO4:Dy + PTFE re-annealed at 700 °C are 57.03, 75.15, and 1191.11 nC, respectively. The intensity of 700 °C-re-annealed CaSO4:Dy increased significantly after PTFE addition.

  4. Structural and magnetic properties of nano-sized NiCuZn ferrites synthesized by co-precipitation method with ultrasound irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Harzali, Hassen, E-mail: harzali@mines-albi.fr [Laboratory of Applied Mineral Chemistry, Faculty of Sciences, University Tunis ElManar, Campus University, Farhat Hached El-Manar, 2092 Tunis (Tunisia); Saida, Fairouz; Marzouki, Arij; Megriche, Adel [Laboratory of Applied Mineral Chemistry, Faculty of Sciences, University Tunis ElManar, Campus University, Farhat Hached El-Manar, 2092 Tunis (Tunisia); Baillon, Fabien; Espitalier, Fabienne [Université de Toulouse, Mines Albi, CNRS, Centre RAPSODEE, Campus Jarlard, F-81013 Albi CT cedex 09 (France); Mgaidi, Arbi [Laboratory of Applied Mineral Chemistry, Faculty of Sciences, University Tunis ElManar, Campus University, Farhat Hached El-Manar, 2092 Tunis (Tunisia); Taibah University, Faculty of Sciences & art, Al Ula (Saudi Arabia)

    2016-12-01

    Sonochemically assisted co-precipitation has been used to prepare nano-sized Ni–Cu–Zn-ferrite powders. A suspension of constituent hydroxides was ultrasonically irradiated for various times at different temperatures with high intensity ultrasound radiation using a direct immersion titanium horn. Structural and magnetic properties were investigated using X-diffraction (XRD), FT-IR spectroscopy, transmission electron microscopy (TEM), Nitrogen adsorption at 77 K (BET) and Vibrating sample magnetometer (VSM). Preliminary experimental results relative to optimal parameters showed that reaction time t=2 h, temperature θ=90 °C and dissipated Power P{sub diss}=46.27 W. At these conditions, this work shows the formation of nanocrystalline single-phase structure with particle size 10–25 nm. Also, ours magnetic measurements proved that the sonochemistry method has a great influence on enhancing the magnetic properties of the ferrite. - Highlights: • Coprecipitation experiments were carried out with ultrasound. • The spinel ferrite NiCuZn was perfectly synthesized by ultrasound. • The saturation magnetization and crystals size are found to be correlated as the dissipated power was varied.

  5. Structural and magnetic properties of nano-sized NiCuZn ferrites synthesized by co-precipitation method with ultrasound irradiation

    International Nuclear Information System (INIS)

    Harzali, Hassen; Saida, Fairouz; Marzouki, Arij; Megriche, Adel; Baillon, Fabien; Espitalier, Fabienne; Mgaidi, Arbi

    2016-01-01

    Sonochemically assisted co-precipitation has been used to prepare nano-sized Ni–Cu–Zn-ferrite powders. A suspension of constituent hydroxides was ultrasonically irradiated for various times at different temperatures with high intensity ultrasound radiation using a direct immersion titanium horn. Structural and magnetic properties were investigated using X-diffraction (XRD), FT-IR spectroscopy, transmission electron microscopy (TEM), Nitrogen adsorption at 77 K (BET) and Vibrating sample magnetometer (VSM). Preliminary experimental results relative to optimal parameters showed that reaction time t=2 h, temperature θ=90 °C and dissipated Power P_d_i_s_s=46.27 W. At these conditions, this work shows the formation of nanocrystalline single-phase structure with particle size 10–25 nm. Also, ours magnetic measurements proved that the sonochemistry method has a great influence on enhancing the magnetic properties of the ferrite. - Highlights: • Coprecipitation experiments were carried out with ultrasound. • The spinel ferrite NiCuZn was perfectly synthesized by ultrasound. • The saturation magnetization and crystals size are found to be correlated as the dissipated power was varied.

  6. PREPARATION OF METAL OXIDE POWDERS FROM METAL LOADED VERSATIC ACID

    OpenAIRE

    KAKIHATA, Takayuki; USAMI, Kensuke; YAMAMOTO, Hideki; SHIBATA, Junji

    1998-01-01

    A production process for metal oxide powders was developed using a solvent extraction method. Versatic Acid 10 and D2EHPA solutions containing copper, zinc and nickel were used for a precipitation-stripping process, where oxalic acid was added to the solution as a precipitation reagent.Copper, zinc and nickel oxalates were easily formed in an aqueous phase, and 99.9% of precipitation was obtained for each metal during this process. These metal oxalates were easily converted to metal oxides by...

  7. Revisiting Pocos de Caldas. Application of the co-precipitation approach to establish realistic solubility limits for performance assessment

    International Nuclear Information System (INIS)

    Bruno, J.; Duro, L.; Jordana, S.; Cera, E.

    1996-02-01

    Solubility limits constitute a critical parameter for the determination of the mobility of radionuclides in the near field and the geosphere, and consequently for the performance assessment of nuclear waste repositories. Mounting evidence from natural system studies indicate that trace elements, and consequently radionuclides, are associated to the dynamic cycling of major geochemical components. We have recently developed a thermodynamic approach to take into consideration the co-precipitation and co-dissolution processes that mainly control this linkage. The approach has been tested in various natural system studies with encouraging results. The Pocos de Caldas natural analogue was one of the sites where a full testing of our predictive geochemical modelling capabilities were done during the analogue project. We have revisited the Pocos de Caldas data and expanded the trace element solubility calculations by considering the documented trace metal/major ion interactions. This has been done by using the co-precipitation/co-dissolution approach. The outcome is as follows: A satisfactory modelling of the behaviour of U, Zn and REEs is achieved by assuming co-precipitation with ferrihydrite. Strontium concentrations are apparently controlled by its co-dissolution from Sr-rich fluorites. From the performance assessment point of view, the present work indicates that calculated solubility limits using the co-precipitation approach are in close agreement with the actual trace element concentrations. Furthermore, the calculated radionuclide concentrations are 2-4 orders of magnitude lower than conservative solubility limits calculated by assuming equilibrium with individual trace element phases. 34 refs, 18 figs, 13 tabs

  8. Revisiting Pocos de Caldas. Application of the co-precipitation approach to establish realistic solubility limits for performance assessment

    Energy Technology Data Exchange (ETDEWEB)

    Bruno, J.; Duro, L.; Jordana, S.; Cera, E. [QuantiSci, Barcelona (Spain)

    1996-02-01

    Solubility limits constitute a critical parameter for the determination of the mobility of radionuclides in the near field and the geosphere, and consequently for the performance assessment of nuclear waste repositories. Mounting evidence from natural system studies indicate that trace elements, and consequently radionuclides, are associated to the dynamic cycling of major geochemical components. We have recently developed a thermodynamic approach to take into consideration the co-precipitation and co-dissolution processes that mainly control this linkage. The approach has been tested in various natural system studies with encouraging results. The Pocos de Caldas natural analogue was one of the sites where a full testing of our predictive geochemical modelling capabilities were done during the analogue project. We have revisited the Pocos de Caldas data and expanded the trace element solubility calculations by considering the documented trace metal/major ion interactions. This has been done by using the co-precipitation/co-dissolution approach. The outcome is as follows: A satisfactory modelling of the behaviour of U, Zn and REEs is achieved by assuming co-precipitation with ferrihydrite. Strontium concentrations are apparently controlled by its co-dissolution from Sr-rich fluorites. From the performance assessment point of view, the present work indicates that calculated solubility limits using the co-precipitation approach are in close agreement with the actual trace element concentrations. Furthermore, the calculated radionuclide concentrations are 2-4 orders of magnitude lower than conservative solubility limits calculated by assuming equilibrium with individual trace element phases. 34 refs, 18 figs, 13 tabs.

  9. Bioleaching of incineration fly ash by Aspergillus niger – precipitation of metallic salt crystals and morphological alteration of the fungus

    Directory of Open Access Journals (Sweden)

    Tong-Jiang Xu

    2014-09-01

    Full Text Available This study examines the bioleaching of municipal solid waste incineration fly ash by Aspergillus niger, and its effect on the fungal morphology, the fate of the ash particles, and the precipitation of metallic salt crystals during bioleaching. The fungal morphology was significantly affected during one-step and two-step bioleaching; scanning electron microscopy revealed that bioleaching caused distortion of the fungal hyphae (with up to 10 μm hyphae diameter and a swollen pellet structure. In the absence of the fly ash, the fungi showed a linear structure (with 2–4 μm hyphae diameter. Energy-dispersive X-ray spectroscopy and X-ray diffraction confirmed the precipitation of calcium oxalate hydrate crystals at the surface of hyphae in both one-step and two-step bioleaching. Calcium oxalate precipitation affects bioleaching via the weakening of the fly ash, thus facilitating the release of other tightly bound metals in the matrix.

  10. Nephroprotective effect of Corn Silk extract on oxalic acid-induced nephrocalcinosis in rabbit model

    OpenAIRE

    Faruk Hassan Al-Jawad; Rafi Abdul Majeed Al-Razzuqi; Zainab Awaen Al-Ebady; Thulfuqar Abdul Majeed Al-Razzuqi

    2012-01-01

    ABSTRACT Background : Nephrocalcinosis is a state of deposition of calcium phosphate or oxalate in the renal parenchyma. It may occur in patients with renal tubular acidosis, vitamin D intoxication, and hyperparathyroidism. Corn silk was used in traditional Chinese medicine to relieve renal pains. Aim: To evaluate the effect of Corn silk aqueous extract in reducing calcium deposits from renal parenchyma in oxalic acid-induced nephrocalcinosis model. Materials and methods: Fourteen healthy...

  11. Oxaloacetate hydrolase, the C-C bond lyase of oxalate secreting fungi

    NARCIS (Netherlands)

    Han, Y.; Joosten, H.J.; Niu, W.; Zhao, Z.; Mariano, P.S.; McCalman, M.; Kan, van J.; Schaap, P.J.; Dunaway-Mariano, D.

    2007-01-01

    Oxalate secretion by fungi is known to be associated with fungal pathogenesis. In addition, oxalate toxicity is a concern for the commercial application of fungi in the food and drug industries. Although oxalate is generated through several different biochemical pathways, oxaloacetate

  12. Adaptable coordination of U(IV) in the 2D-(4,4) uranium oxalate network: From 8 to 10 coordinations in the uranium (IV) oxalate hydrates

    International Nuclear Information System (INIS)

    Duvieubourg-Garela, L.; Vigier, N.; Abraham, F.; Grandjean, S.

    2008-01-01

    Crystals of uranium (IV) oxalate hydrates, U(C 2 O 4 ) 2 .6H 2 O (1) and U(C 2 O 4 ) 2 .2H 2 O (2), were obtained by hydrothermal methods using two different U(IV) precursors, U 3 O 8 oxide and nitric U(IV) solution in presence of hydrazine to avoid oxidation of U(IV) into uranyl ion. Growth of crystals of solvated monohydrated uranium (IV) oxalate, U(C 2 O 4 ) 2 .H 2 O.(dma) (3), dma=dimethylamine, was achieved by slow diffusion of U(IV) into a gel containing oxalate ions. The three structures are built on a bi-dimensional complex polymer of U(IV) atoms connected through bis-bidentate oxalate ions forming [U(C 2 O 4 )] 4 pseudo-squares. The flexibility of this supramolecular arrangement allows modifications of the coordination number of the U(IV) atom which, starting from 8 in 1 increases to 9 in 3 and, finally increases, to 10 in 2. The coordination polyhedron changes from a distorted cube, formed by eight oxygen atoms of four oxalate ions, in 1, to a mono-capped square anti-prism in 3 and, finally, to a di-capped square anti-prism in 2, resulting from rotation of the oxalate ions and addition of one and two water oxygen atoms in the coordination of U(IV). In 1, the space between the ∞ 2 [U(C 2 O 4 ) 2 ] planar layers is occupied by non-coordinated water molecules; in 2, the space between the staggered ∞ 2 [U(C 2 O 4 ) 2 .2H 2 O] layers is empty, finally in 3, the solvate molecules occupy the interlayer space between corrugated ∞ 2 [U(C 2 O 4 ) 2 .H 2 O] sheets. The thermal decomposition of U(C 2 O 4 ) 2 .6H 2 O under air and argon atmospheres gives U 3 O 8 and UO 2 , respectively. - Graphical abstract: The adaptable environment of U(IV) in U(IV) oxalates: from eight cubic coordination in U(C 2 O 4 ) 2 .6H 2 O (a) completed by water oxygens to nine in [U(C 2 O 4 ) 2 .H 2 O](C 2 NH 5 ) (b) and ten coordination in U(C 2 O 4 ) 2 .2H 2 O (c)

  13. Strontium isotope fractionation during strontianite (SrCO3) dissolution, precipitation and at equilibrium

    Science.gov (United States)

    Mavromatis, Vasileios; Harrison, Anna L.; Eisenhauer, Anton; Dietzel, Martin

    2017-12-01

    In this study we examine the behavior of stable Sr isotopes between strontianite [SrCO3] and reactive fluid during mineral dissolution, precipitation, and at chemical equilibrium. Experiments were performed in batch reactors at 25 °C in 0.01 M NaCl solutions wherein the pH was adjusted by bubbling of a water saturated gas phase of pure CO2 or atmospheric air. The equilibrium Sr isotope fractionation between strontianite and fluid after dissolution of the solid under 1 atm CO2 atmosphere was estimated as Δ88/86SrSrCO3-fluid = δ88/86Sr SrCO3 - δ88/86Srfluid = -0.05 ± 0.01‰. On the other hand, during strontianite precipitation, an enrichment of the fluid phase in 88Sr, the heavy isotopomer, was observed. The evolution of the δ88/86Srfluid during strontianite precipitation can be modeled using a Rayleigh distillation approach and the estimated, kinetically driven, fractionation factor αSrCO3-fluid between solid and fluid is calculated to be 0.99985 ± 0.00003 corresponding to Δ88/86SrSrCO3-fluid = -0.15‰. The obtained results further support that under chemical equilibrium conditions between solid and fluid a continuous exchange of isotopes occurs until the system approaches isotopic equilibrium. This isotopic exchange is not limited to the outer surface layer of the strontianite crystal, but extends to ∼7-8 unit cells below the crystal surface. The behavior of Sr isotopes in this study is in excellent agreement with the concept of dynamic equilibrium and it suggests that the time needed for achievement of chemical equilibrium is generally shorter compared to that for isotopic equilibrium. Thus it is suggested that in natural Sr-bearing carbonates an isotopic change may still occur close to thermodynamic equilibrium, despite no observable change in aqueous elemental concentrations. As such, a secondary and ongoing change of Sr isotope signals in carbonate minerals caused by isotopic re-equilibration with fluids has to be considered in order to use Sr

  14. Uranyl oxalate hydrates: structures and IR spectra

    International Nuclear Information System (INIS)

    Giesting, P.A.; Porter, N.J.; Burns, P.C.

    2006-01-01

    The novel compound (UO 2 ) 2 C 2 O 4 (OH) 2 (H 2 O) 2 (UrOx2A) and the previously studied compound UO 2 C 2 O 4 (H 2 O) 3 (UrOx3) have been synthesized by mild hydrothermal methods. Single crystal diffraction data collected at 125 K using MoK α radiation and a CCD-based area detector were used to solve and refine the crystal structures by full-matrix least-squares techniques to agreement indices (UrOx2A, UrOx3) wR 2 = 0.037, 0.049 for all data, and R1 0.015, 0.024 calculated for 1285, 2194 unique reflections respectively. The compound UrOx2A is triclinic, space group P1, Z = 1, a = 5.5353(4), b 6.0866(4), c = 7.7686(6) Aa, α = 85.6410(10) , β = 89.7740(10) , γ = 82.5090(10) , V = 258.74(3) Aa 3 . The compound UrOx3 is monoclinic, space group P2 1 /c, Z = 4, a = 5.5921(4), b = 16.9931(13), c = 9.3594(7) Aa, β = 99.5330(10) , V = 877.11(11) Aa 3 . The structures consist of chains of uranyl pentagonal bipyramids connected by oxalate groups and, in UrOx2A, hydroxyl groups; UrOx2A is also notable for its high (2:1) ratio of uranyl to oxalate groups, higher than any observed in other published structures of uranyl oxalates. The structure determined for UrOx3, previously studied by Jayadevan and Chackraburtty (1972); Mikhailov et al. (1999) is in agreement with the previous results; however, the increased precision of the present low-temperature structure refinement allows for the assignment of H atom positions based on the difference Fourier map of electron density. The infrared spectra of these two materials collected at room temperature are also presented and compared with previous work on uranyl oxalate systems. (orig.)

  15. Structural, magnetic and optical characterization of Ni{sub 0.8}Zn{sub 0.2}Fe{sub 2}O{sub 4} nano particles prepared by co-precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Kannan, Y.B., E-mail: ybkans@gmail.com [Department of Physics, Arumugam Pillai Seethai Ammal College, Tiruppattur 630211 (India); Saravanan, R. [Research Centre & PG Department of Physics, The Madura College, Madurai 625011 (India); Srinivasan, N. [Research Centre & PG Department of Physics, Thiagarajar College, Madurai 625009 (India); Praveena, K. [School of Physics, Univeristy of Hyderabad, Hyderabad 500046 (India); Sadhana, K. [Material Research Center, Indian Institute of Science, Bangalore 560012 (India)

    2016-12-01

    Bond strength values, between tetrahedral sites and octahedral sites atoms in the unit cell, are evaluated using maximum entropy method (MEM) for the Ni{sub 0.8}Zn{sub 0.2}Fe{sub 2}O{sub 4} nano ferrite particles, prepared by co-precipitation method and sintered at 900 °C. The spinel structure is confirmed from the XRD analysis done using the Rietveld method. Substitution of zinc ion causes increase in lattice parameter value. Thermal behavior, morphology, magnetic properties and optical band gap energy values of the sample are determined by using thermogravimetric analysis and differential thermal analysis, scanning electron microscope, vibrating sample magnetometer and UV–VIS–NIR techniques respectively. Low value of saturation magnetization is attributed to the disorder in cation distribution.

  16. Preparation of magnetic albumin nanoparticles via a simple and one-pot desolvation and co-precipitation method for medical and pharmaceutical applications.

    Science.gov (United States)

    Nosrati, Hamed; Salehiabar, Marziyeh; Manjili, Hamidreza Kheiri; Danafar, Hossein; Davaran, Soodabeh

    2018-03-01

    In this study, iron oxide magnetic bovine serum albumin core-shell nanoparticles (BSA coated IONPs) with narrow particle size distribution were synthesized under one-pot reaction via the desolvation and chemical co-precipitation method. Functionalized IONPs were characterized by X-ray diffraction (XRD), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), fourier transform infrared spectroscopy (FTIR), and transmission electron microscopy (TEM) techniques. Furthermore, vibrating sample magnetometer (VSM) analysis show these nanoparticles (NPs) have an excellent magnetic properties. Cellular toxicity of IONPs was also investigated on HFF2 cell lines. Additionally, a hemolysis test of as prepared core-shell NPs were performed. The presence of albumin as a biomolecule coating on the surface of IONPs showed an improving effect to reduce the cytotoxicity. The properties of the designed NPs propose the BSA coated IONPs as a promising candidate for multifunctional biomedical applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Zirconia-mullite obtained from co-precipitated zirconia-mullite composite powders by SPS

    Energy Technology Data Exchange (ETDEWEB)

    Li, H.Z.; Li, Z.J.; Luo, X.D. [Univ. of Science and Technology Liaoning, Anshan (China). School of High Temperature Materials and Magnesium Resource Engineering; Gui, J.Y.; Xie, Z.P. [Tsinghua Univ., Beijing (China). School of Materials Science and Engineering

    2016-07-01

    The co-precipitation method is used to fabricate precursor powder. This powder is densified by means of the spark plasma sintering (SPS) technique at 1500 C with a holding time of 7 min to prepare zirconia-mullite samples. Their density measures up to 97 % of the theoretical density, and the sintered mullite compacts exhibit better strength properties (289 ± 12 MPa) and H{sub v} (9.99 GPa). The mode of fracture is changed with the addition of ZrO{sub 2} and extensive fine cleavages are observed on the grain surface. These cleavages join together to form steps, which can absorb more energy. The flexural strength of the samples is almost double that of pure mullite, which is related to the formation of cleavages.

  18. Advances on reverse strike co-precipitation method of uranium-plutonium mixed solutions

    International Nuclear Information System (INIS)

    Menghini, Jorge E.; Marchi, Daniel E.; Orosco, Edgardo H.; Greco, Luis

    2000-01-01

    The reverse strike coprecipitation of uranium-plutonium mixed solutions, is an alternative way to obtain MOX fuel pellets. Previous tests, carried out in the Alpha Laboratory, included a stabilization step for transforming 100 % of plutonium into Pu +4 . Therefore, the plutonium precipitated as Pu(OH) 4 . In this second step, the stabilization process was suppressed. In this way, besides Pu(OH) 4 , a part of the precipitated is composed of a mixed salt: AD(U,Pu). Then, a homogeneous solid solution is formed in the early steps of the process. The powders showed higher tap density, better performance during the pressing and lower sinterability than the powders obtained in previous tests. The advantageous and disadvantageous effects of the stabilization step are analyzed in this paper. (author)

  19. Synthesis of alumina/YAG 20 vol% composite by co-precipitation

    Directory of Open Access Journals (Sweden)

    Radosław Lach

    2011-12-01

    Full Text Available Co-precipitation of alumina/YAG precursor from aluminum and yttrium nitrate solution with ammonium carbonate results in dawsonite. Its crystallographic parameters differ from the compound precipitated with no yttrium additive. It suggests that yttrium ions become incorporated into the dawsonite structure. The DSC/TG and X-ray diffraction measurements show decomposition of dawsonite at elevated temperatures resulting in γ-Al2O3 and then δ- and θ-alumina modifications. Full transformation to α-Al2O3 and YAG occurs at temperatures higher than 1230°C. Starting powder for the sintering experiments was prepared using the coprecipitated precursor calcined at 600°C. Seeding of such powder with 5 wt.% α-Al2O3 results in material of 98% density at 1500°C. Much lower densification show compacts of unseeded powder.

  20. Decontamination effectiveness of mixtures of citric acid, oxalic acid and EDTA

    International Nuclear Information System (INIS)

    Speranzini, R.A.

    1990-01-01

    An experimental study of the decontamination effectiveness of citric acid, oxalic acid and EDTA mixtures was conducted to assess whether oxalic acid could be removed from decontamination solutions to minimize corrosion. In loop experiments, radioactive specimens from two boiling water reactors and one pressurized water reactor were suspended in solutions of single acids or in mixtures of reagents at total reagent concentrations of less than 0.1 wt% under conditions similar to those used to decontaminate reactor systems. Rate constants for dissolution of oxides and decontamination factors were measured. Based on the results, it was concluded that under certain conditions, oxalic acid was the most effective reagent for the dissolution of oxides. It was also found, however, that conditions under which effective dissolution occurred in solutions of oxalic acid and/or citric acid were difficult to define and control. EDTA was found to be an effective reagent for dissolution of oxides such that rates of dissolution in EDTA containing solutions at 117 degrees Celsius were comparable to rates in oxalic acid containing solutions. At 90 degrees Celsius, EDTA acted synergistically with oxalic acid such that the rate of dissolution of oxides in citric-acid/oxalic-acid/EDTA solutions was higher than in citric-acid/EDTA solutions. The rates of dissolution of oxides were significantly reduced when 60 mg/kg of ferric ion was added to the citric-acid/oxalic-acid, citric-acid/EDTA and citric-acid/oxalic-acid/EDTA solutions. It was concluded that effective decontaminations of BWR and PWR systems could be achieved with mixtures of citric acid and EDTA

  1. Synthesis and characterization of superparamagnetic nanoparticles obtained by precipitation in inverse microemulsion for biomedical applications

    International Nuclear Information System (INIS)

    Puca Pacheco, Mercedes; Guerrero Aquino, Marco; Tacuri Calanchi, Enrique; Lopez Campos, Raul G.

    2013-01-01

    In this work the preparation of nanoparticles of magnetite by methods of precipitation in inverse microemulsions and the conventional method 'Chemical Co-precipitation' is reported. Magnetite nanoparticles were characterized by X-ray diffraction, Moessbauer spectroscopy and vibrating sample magnetometer (VSM). The results showed that the nanoparticles obtained by the method of precipitation in inverse microemulsion showed a superparamagnetic behavior and had a particle average diameter of 9 nm, while by the conventional method 'Chemical Co-precipitation' were 17 nm. In addition, other benefits observed in the application of the method of precipitation in inverse microemulsion with regard to the conventional method is that it allowed obtaining spheroidal magnetite nanoparticles, monodisperse and with magnetic and chemical properties which might have better results in medical applications. (author)

  2. Co-precipitation of oppositely charged nanoparticles: the case of mixed ligand nanoparticles

    International Nuclear Information System (INIS)

    Moglianetti, Mauro; Ponomarev, Evgeniy; Szybowski, Maxime; Stellacci, Francesco; Reguera, Javier

    2015-01-01

    Colloid stability is of high importance in a multitude of fields ranging from food science to biotechnology. There is strong interest in studying the stability of small particles (of a size of a few nanometres) with complex surface structures, that make them resemble the complexity of proteins and other natural biomolecules, in the presence of oppositely charged nanoparticles. While for nanoparticles with homogeneously charged surfaces an abrupt precipitation has been observed at the neutrality of charges, data are missing about the stability of nanoparticles when they have more complex surface structures, like the presence of hydrophobic patches. To study the role of these hydrophobic patches in the stability of nanoparticles a series of negatively charged nanoparticles has been synthesized with different ratios of hydrophobic content and with control on the structural distribution of the hydrophobic moiety, and then titrated with positively charged nanoparticles. For nanoparticles with patchy nanodomains, the influence of hydrophobic content was observed together with the influence of the size of the nanoparticles. By contrast, for nanoparticles with a uniform distribution of hydrophobic ligands, size changes and hydrophobic content did not play any role in co-precipitation behaviour. A comparison of these two sets of nanoparticles suggests that nanodomains present at the surfaces of nanoparticles are playing an important role in stability against co-precipitation. (paper)

  3. Putative Aspergillus niger-induced oxalate nephrosis in sheep : clinical communication

    Directory of Open Access Journals (Sweden)

    C.J. Botha

    2009-05-01

    Full Text Available A sheep farmer provided a maize-based brewer's grain (mieliemaroek and bales of Eragrostis curvula hay to ewes and their lambs, kept on zero-grazing in pens. The 'mieliemaroek' was visibly mouldy. After 14 days in the feedlot, clinical signs, including generalised weakness, ataxia of the hind limbs, tremors and recumbency, were noticed. Six ewes died within a period of 7 days. A post mortem examination was performed on 1 ewe. The carcass appeared to be cachectic with mild effusions into the body cavities; mild lung congestion and pallor of the kidneys were observed. Microscopical evaluation revealed nephrosis and birefringent oxalate crystals in the renal tubules when viewed under polarised light. A provisional diagnosis of oxalate nephrosis with subsequent kidney failure was made. Amongst other fungi, Aspergillus niger was isolated from 'mieliemaroek' samples submitted for fungal culture and identification. As A. niger is known to synthesise oxalates, a qualitative screen to detect oxalic acid in the mieliemaroek and purified A. niger isolates was performed using high-performance liquid chromatography (HPLC. Oxalic acid was detected, which supported a diagnosis of soluble oxalate-induced nephropathy.

  4. Conceptual design of a novel CO2 capture process based on precipitating amino acid solvents

    NARCIS (Netherlands)

    Sanchez Fernandez, E.; Heffernan, K.; Ham, L.V. van der; Linders, M.J.G.; Eggink, E.; Schrama, F.N.H.; Brilman, D.W.F.; Goetheer, E.L.V.; Vlugt, T.J.H.

    2013-01-01

    Amino acid salt based solvents can be used for CO2 removal from flue gas in a conventional absorption-thermal desorption process. Recently, new process concepts have been developed based on the precipitation of the amino acid zwitterion species during the absorption of CO2. In this work, a new

  5. Effect of pH variation on the stability and structural properties of In(OH){sub 3} nanoparticles synthesized by co-precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Goh, Kian Wei; Wong, Yew Hoong [University of Malaya, Department of Mechanical Engineering, Faculty of Engineering, Kuala Lumpur (Malaysia); Johan, Mohd Rafie [University of Malaya, Department of Mechanical Engineering, Faculty of Engineering, Kuala Lumpur (Malaysia); University of Malaya, Nanotechnology and Catalysis Research Centre, Kuala Lumpur (Malaysia)

    2016-10-15

    Indium hydroxide (In(OH){sub 3}) nanoparticles were synthesized at various pH values (8-11) by co-precipitation method. Its properties were characterized by X-ray diffractometer, Fourier transform infrared spectroscopy, Raman spectroscopy and transmission electron microscope. The electrostatic stability of nanoparticles is carried out through zeta potential measurement. The crystallite size of nanoparticles calculated by Scherrer equation has similar trend with the values obtained from William-Hall plot. TEM images show that the particles size is within the range of 11.76-20.76 nm. The maximum zeta potential is 3.68 mV associated with the smallest particle size distribution of 92.6 nm occurred at pH 10. Our work clearly confirms the crystallite size, stability and the morphology of In(OH){sub 3} NPs are strongly depending on the pH of precursor solution. (orig.)

  6. The metabolic and ecological interactions of oxalate-degrading bacteria in the Mammalian gut.

    Science.gov (United States)

    Miller, Aaron W; Dearing, Denise

    2013-12-06

    Oxalate-degrading bacteria comprise a functional group of microorganisms, commonly found in the gastrointestinal tract of mammals. Oxalate is a plant secondary compound (PSC) widely produced by all major taxa of plants and as a terminal metabolite by the mammalian liver. As a toxin, oxalate can have a significant impact on the health of mammals, including humans. Mammals do not have the enzymes required to metabolize oxalate and rely on their gut microbiota for this function. Thus, significant metabolic interactions between the mammalian host and a complex gut microbiota maintain the balance of oxalate in the body. Over a dozen species of gut bacteria are now known to degrade oxalate. This review focuses on the host-microbe and microbe-microbe interactions that regulate the degradation of oxalate by the gut microbiota. We discuss the pathways of oxalate throughout the body and the mammalian gut as a series of differentiated ecosystems that facilitate oxalate degradation. We also explore the mechanisms and functions of microbial oxalate degradation along with the implications for the ecological and evolutionary interactions within the microbiota and for mammalian hosts. Throughout, we consider questions that remain, as well as recent technological advances that can be employed to answer them.

  7. Development of long-lived radionuclide partitioning technology

    Energy Technology Data Exchange (ETDEWEB)

    Yoo, Jae Hyung; Lee, Eil Hee; Kim, Kwang Wook; Yang, Han Beom; Chung, Dong Yong; Lim, Jae Kwan; Shin, Young Jun; Kim, Heung Ho; Kown, Sun Gil; Kim, Young Hwan; Hwang, Doo Seung

    1996-07-01

    This study has been focused on the development of unit processes for partitioning in the 1st stage, and experimentally carried out to examine the separation characteristics and operation conditions on the following unit processes. (1) Removal of a small amount of uranium by extraction with TBP, (2) Removal of Zr and Mo and destruction of nitric acid by uranium by denitration with formic acid, (3) Co-precipitation of Am, Np and RE oxalic acid, (4) Dissolution and destruction of oxalate by hydrogen peroxide, (5) Co-extraction of Am, Np and RE by nitric acid, (8) Back-extraction of Np by oxalic acid, (9) Adsorption and elution of Cs and Sr by zeolite, and (10) Advanced separation of radionuclide by electrochemical REDOX method. The results obtained from each unit process will be use as the basic materials for the establishment of optimal partitioning and design of process equipment. (author). 46 refs., 54 tabs., 222 figs.

  8. Precipitation behaviors of Cs and Re(/Tc) by NaTPB and TPPCl from a simulated fission products-(Na2CO3-NaHCO3)-H2O2 solution

    International Nuclear Information System (INIS)

    Lee, Eil Hee; Lim, Jae Gwan; Chung, Dong Yong; Yang, Han Beum; Kim, Kwang Wook

    2010-01-01

    In this study, the removal of Cs and Tc from a simulated fission products (FP) solution which were co-dissolved with U during the oxidative-dissolution of spent fuel in a mixed carbonate solution of (Na 2 CO 3 -NaHCO 3 )-H 2 O 2 was investigated by using a selective precipitation method. As Cs and Tc might cause an unstable behavior due to the high decay heat emission of Cs as well as the fast migration of Tc when disposed of underground, it is one of the important issues to removal them in views of the increase of disposal safety. The precipitation of Cs and Re (as a surrogate for Tc) was examined by introducing sodium tetraphenylborate (NaTPB) and tetraphenylphosponium chloride (TPPCl), respectively. Precipitation of Cs by NaTPB and that of Re by TPPCl were completed within 5 minutes. Their precipitation rates were not influenced so much by the temperature and stirring speed even if they were increased by up to 50 .deg. C and 1,000 rpm. However, the pH of the solution was found to have a great influence on the precipitation with NaTPB and TPPCl. Since Mo tends to co-precipitate with Re at a lower pH, especially, it was effective that a selective precipitation of Re by TPPCl was carried out at pH of above 9 without co-precipitation of Mo and Re. Over 99% of Cs was precipitated when the ratio of [NaTPB]/[Cs]>1 and more than 99% of Re, likewise, was precipitated when the ratio of [TPPCl]/[Re]>1.

  9. Iron doped SnO{sub 2}/Co{sub 3}O{sub 4} nanocomposites synthesized by sol-gel and precipitation method for metronidazole antibiotic degradation

    Energy Technology Data Exchange (ETDEWEB)

    Agarwal, Shilpi [Department of Applied Chemistry, University of Johannesburg, Johannesburg (South Africa); Tyagi, Inderjeet [Department of Chemistry, Indian Institute of Technology Roorkee, 247667 (India); Gupta, Vinod Kumar, E-mail: vinodg@uj.ac.za [Department of Applied Chemistry, University of Johannesburg, Johannesburg (South Africa); Sohrabi, Maryam; Mohammadi, Sanaz [Department of Chemistry, Shahr-e-Qods Branch, Islamic Azad University, Tehran (Iran, Islamic Republic of); Golikand, Ahmad Nozad, E-mail: anozad@aeoi.org.ir [Department of Chemistry, Shahr-e-Qods Branch, Islamic Azad University, Tehran (Iran, Islamic Republic of); Jaber Research Laboratory, NSTRI, P.O. Box: 14395-836, Tehran (Iran, Islamic Republic of); Fakhri, Ali, E-mail: ali.fakhri88@yahoo.com [Young Researchers and Elites Club, Science and Research Branch, Islamic Azad University, Tehran (Iran, Islamic Republic of)

    2017-01-01

    Sol-gel and precipitation reaction methods were used to synthesize Un-doped and Fe-doped SnO{sub 2}/Co{sub 3}O{sub 4} nanocomposites under UV light; the synthesized nanocomposites were applied for the photocatalytic degradation of metronidazole antibiotic. The developed photo catalyst was well characterized using energy dispersive X-ray spectrometer (EDX), X-ray diffraction (XRD), vibrating sample magnetometer (VSM), field emission scanning electron microscopy (FE-SEM), UV–Visible and photoluminescence (PL) spectroscopy. Effective parameters such as pH, photocatalyst dose and contact time was optimized and well investigated. From the obtained facts it is clear that the 98.3% of MTZ was degraded with in 15 min, pH 6 and 0.1 g catalyst when the Fe molar ratio was 1:1 at %. As compared to results obtained from un-doped SnO{sub 2}/Co{sub 3}O{sub 4} nanocomposites Fe doped SnO{sub 2}/Co{sub 3}O{sub 4} nanocomposites possess greater photocatalytic efficiency. - Graphical abstract: Surface textural and morphological presentation. - Highlights: • Un-doped and Fe-doped SnO{sub 2}/Co{sub 3}O{sub 4} nanocomposites were applied as photocatalyst. • The nanocomposites exhibited photocatalytic property under UV light. • The maximum degradation was observed for Fe-doped SnO{sub 2}/Co{sub 3}O{sub 4} (1:1) photocatalyst. • 0.1 g photocatalyst is sufficient to carry out 98.3% degradation of MTZ.

  10. Solubility Determination of Uranium (IV) Oxalates U(C2O4)2.6H2O and M2U2(C2O4)5.nH2O (M = mono-charged cation)

    International Nuclear Information System (INIS)

    Costenoble, Sylvain; Grandjean, Stephane; Arab-Chapelet, Benedicte; Abraham, Francis

    2008-01-01

    The solubility of uranium (IV) oxalate compounds was studied in order to have a precise insight of the behaviour of An(IV)-An(III) (An(IV) = U, Np or Pu and An(III) = Pu or Am) mixed oxalate in the context of oxalic co-conversion for actinide co-management. Concepts of thermodynamics of aqueous-solid solution are reviewed by introducing LIPPMANN theory and THORSTENSON and PLUMMER 'stoichiometric saturation' model in a way to understand and model the system of interest. Different analytical techniques have been developed in order to titrate uranium and/or other actinides at trace levels in solution. This thorough investigation is the basis of further experiments on the solubility of mixed U(IV)- An(III) oxalate solid solutions as a function of the nature of the trivalent actinide and the An(III)/U(IV) ratio. (authors)

  11. Gently reduced graphene oxide incorporated into cobalt oxalate rods as bifunctional oxygen electrocatalyst

    International Nuclear Information System (INIS)

    Phihusut, Doungkamon; Ocon, Joey D.; Jeong, Beomgyun; Kim, Jin Won; Lee, Jae Kwang; Lee, Jaeyoung

    2014-01-01

    Graphical abstract: - Abstract: Water-oxygen electrochemistry is at the heart of key renewable energy technologies (fuel cells, electrolyzers, and metal-air batteries) due to the sluggish kinetics of oxygen reduction reaction (ORR) and oxygen evolution reaction (OER). Although much effort has been devoted to the development of improved bifunctional electrocatalysts, an inexpensive, highly active oxygen electrocatalyst, however, remains to be a challenge. In this paper, we present a facile and robust method to create gently reduced graphene oxide incorporated into cobalt oxalate microstructures (CoC 2 O 4 /gRGO) and demonstrate its excellent and stable electrocatalytic activity in both OER and ORR, arising from the inherent properties of the components and their physicochemical interaction. Our synthesis technique also explores a single pot method to partially reduce graphene oxide and form CoC 2 O 4 structures while maintaining the solution processability of reduced graphene oxide. While the OER activity of CoC 2 O 4 /gRGO is exclusively due to CoC 2 O 4 , which transformed into OER-active Co species, the combination with gRGO significantly improves OER stability. On the other hand, CoC 2 O 4 /gRGO exhibits synergistic effect towards ORR, via a quasi-four-electron pathway, leading to a slightly higher ORR limiting current than Pt/C. Remarkably, gRGO offers dual functionality, contributing to ORR activity via the N-functional groups and also enhancing OER stability through the gRGO coating around CoC 2 O 4 structures. Our results suggest a new class of metal-carbon composite that has the potential to be alternative bifunctional catalysts for regenerative fuel cells and metal-air batteries

  12. Seasonal variations of ochreous precipitates in mine effluents in Finland

    International Nuclear Information System (INIS)

    Kumpulainen, Sirpa; Carlson, Liisa; Raeisaenen, Marja-Liisa

    2007-01-01

    Ochreous precipitate and water samples were collected from the surroundings of seven closed sulphide mines in Finland. In the Hammaslahti Zn-Cu-Au mine, Otravaara pyrite mine and Paroistenjaervi Cu-W-As mine, the collection was repeated in different seasons to study mineralogical and geochemical variations of precipitates. The sampling was done in 1999-2002 from the ditches and drainage ponds of the tailings and waste rock piles that are susceptible to seasonal changes. Mineralogy of the precipitates was evaluated by X-ray diffraction (XRD) and infrared spectroscopy (IR), and precipitate geochemistry was examined by selective extractions. Schwertmannite (Fe 8 O 8 (OH) 6 SO 4 ) was the most typical Fe hydroxide mineral found. Goethite was almost as common as schwertmannite, was often poorly ordered, and contained up to 10 wt.% of SO 4 . Goethite and schwertmannite were commonly found as mixtures, and they occurred in similar pH and SO 4 concentrations. Ferrihydrite (nominally Fe 5 HO 8 . 4H 2 O) was typically found in areas not influenced by acid mine drainage, and also in acid mine waters with high organic matter or As content. Jarosite (KFe 3 (SO 4 ) 2 (OH) 6 ) was found only in one site. In addition, some gypsum (CaSO 4 . 2H 2 O) and aluminous sulphate precipitates (presumably basaluminite, Al 4 (SO 4 )(OH) 10 . 5H 2 O) were identified. Selective extractions showed that acid extracts Fe tot /S tot -ratios of schwertmannite and goethite samples were similar, but the ratio of oxalate-extractable to total Fe, Fe ox /Fe tot , of goethite samples were lower than those of the schwertmannite samples. Only Al, Si and As were bound to precipitates in substantial amounts, up to several wt.%. In schwertmannites and goethites, Al, Cu, Co, Mn and Zn were mostly structural, substituting for Fe in an Fe oxyhydroxide structure or bound to surface adsorption sites in pores limited by diffusion. In ferrihydrites, heavy metals were also partly bound in adsorbed form dissolving in

  13. Preparation of iron oxide-impregnated spherical granular activated carbon-carbon composite and its photocatalytic removal of methylene blue in the presence of oxalic acid.

    Science.gov (United States)

    Kadirova, Zukhra C; Hojamberdiev, Mirabbos; Katsumata, Ken-Ichi; Isobe, Toshihiro; Matsushita, Nobuhiro; Nakajima, Akira; Sharipov, Khasan; Okada, Kiyoshi

    2014-01-01

    The spherical granular activated carbon-carbon composites (GAC-Fe) with different iron oxide contents (Fe mass% = 0.6-10) were prepared by a pore volume impregnation method. The X-ray diffraction (XRD), scanning electron microscopy (SEM), and N2-adsorption results confirm the presence of amorphous iron oxide, pyrolytic carbon, and graphitized globular carbon nanoparticles covered with amorphous carbon in the CAG-Fe. The rate of photodegradation of methylene blue (MB) in aqueous solution under UV light in the presence of oxalic acid correlates with porosity of the prepared materials. The total MB removal includes the combination of adsorption and photodegradation without the addition of H2O2. The results of total organic carbon (TOC) analysis reveal that the decolorization of MB in aqueous solution containing oxalic acid corresponds to the decomposition of organic compounds to CO2 and H2O.

  14. Preparation and characterization of a carbon-based magnetic nanostructure via co-precipitation method: Peroxidase-like activity assay with 3,3ʹ,5,5ʹ-tetramethylbenzidine

    Directory of Open Access Journals (Sweden)

    Navvabeh Salarizadeh

    2017-09-01

    Full Text Available Objective(S: Natural and artificial enzymes have shown important roles in biotechnological processes. Recently, design and synthesis of artificial enzymes especially peroxidase mimics has been interested by many researchers. Due to disadvantages of natural peroxidases, there is a desirable reason of current research interest in artificial peroxidase mimics. Methods: In this study, magnetic multiwall carbon nanotubes with a structure of Fe3O4/MWCNTs as enzyme mimetic were fabricated using in situ co-precipitation method. The structure, composition, and morphology of Fe3O4/MWCNTs nanocomposite were characterized using X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FTIR, and transmission electron microscopy (TEM. The magnetic properties were investigated by the vibrating sample magnetometer (VSM. Peroxidase-like catalytic activity of nanocomposite was investigated using colorimetric and electrochemical tests with 3,3ʹ,5,5ʹ-tetramethylbenzidine (TMB substrate. Results: The obtained data proved the synthesis of Fe3O4/MWCNTs nanocomposite. The average crystallite size of nanostructures was estimated about 12 nm by Debye–Scherer equation. It was found that Fe3O4/MWCNTs nanocomposite exhibit peroxidase-like activity. Colorimetric and electrochemical data demonstrated that prepared nanocomplex has higher catalytic activity toward H2O2 than pure MWCNT nanocatalyst. From electrochemical tests concluded that the Fe3O4/MWCNTs electrode exhibited the better redox response to H2O2, which is ~ 2 times larger than that of the MWCNTs. Conclusions: The synthesis of Fe3O4nanoparticles on MWCNTs was successfully performed by in situ co-precipitation process. Fe3O4/MWCNTs nanocatalyst exhibited a good peroxidase-like activity. These biomimetic catalysts have some advantages such as simplicity, stability and cost effectiveness that can be used in the design of enzyme-based devices for various applied fields.

  15. Diminution of oxalate induced renal tubular epithelial cell injury and inhibition of calcium oxalate crystallization in vitro by aqueous extract of Tribulus terrestris

    Directory of Open Access Journals (Sweden)

    A. Aggarwal

    2010-08-01

    Full Text Available PURPOSE: Recurrence and persistent side effects of present day treatment for urolithiasis restrict their use, so an alternate solution, using phytotherapy is being sought. The present study attempted to evaluate the antilithiatic properties of Tribulus terrestris commonly called as “gokhru” which is often used in ayurveda to treat various urinary diseases including urolithiasis. MATERIALS AND METHODS: The activity of Tribulus terrestris was investigated on nucleation and the growth of the calcium oxalate (CaOx crystals as well as on oxalate induced cell injury of NRK 52E renal epithelial cells. RESULTS: Tribulus terrestris extract exhibited a concentration dependent inhibition of nucleation and the growth of CaOx crystals. When NRK-52E cells were injured by exposure to oxalate for 72 h, Tribulus terrestris extract prevented the injury in a dose-dependent manner. On treatment with the different concentrations of the plant, the cell viability increased and lactate dehydrogenase release decreased in a concentration dependent manner. CONCLUSION: The current data suggests that Tribulus terrestris extract not only has a potential to inhibit nucleation and the growth of the CaOx crystals but also has a cytoprotective role. Our results indicate that it could be a potential candidate for phytotherapy against urolithiasis.

  16. Features of atopic dermatitis in children with oxalic acid dysmetabolism

    Directory of Open Access Journals (Sweden)

    T.V. Stoieva

    2018-03-01

    Full Text Available The article presents the features of atopic dermatitis in children with concomitant metabolic disturbances of oxalic acid. The influence of metabolic shifts was evaluated by clinical presentation, morphofunctional parameters of the skin and the features of oxalic acid metabolites excretion. In this study, a high incidence of dysmetabolic changes was identified, their significance was determined by the involvement of different systems for oxalic acid products excretion. The increased concentration of oxalate in the urine and in the exhaled air condensate had irritant effect and is associated with the hereditary metabolic disorders, early manifestation of atopy symptoms and the intensity of skin itching, with moderate increase of immunoglobulin E level.

  17. Bulk tungsten with uniformly dispersed La2O3 nanoparticles sintered from co-precipitated La2O3/W nanoparticles

    International Nuclear Information System (INIS)

    Xia, Min; Yan, Qingzhi; Xu, Lei; Guo, Hongyan; Zhu, Lingxu; Ge, Changchun

    2013-01-01

    Graphical abstract: La 2 O 3 doped La 2 O 3 /W nanoparticles with high-purity and uniform diameters have been fabricated by a co-precipitation process. The as-prepared nanoparticles demonstrate the potential of this method for fabricating uniformly structured bulk tungsten materials. -- Abstract: We report the preparation of 1 wt% La 2 O 3 doped La 2 O 3 /W nanoparticles by a co-precipitation process, using ammonium metatungstate (AMT) and lanthanum nitrate as raw materials. The as-synthesized nanoparticles were characterized by X-ray diffraction, Filed-emission scanning electron microscopy, Transmission electron microscopy (TEM), energy dispersive spectroscopy. Our results reveal that the as-synthesized particles possess uniform diameters of about 70 nm, and are of high purity. The TEM and the corresponding fast Fourier transform images demonstrated that La 2 O 3 precipitates were homogeneously doped into the nano-sized tungsten particles. When the as-synthesized nanoparticles were sintered by spark plasma sintering, the electron backscatter diffraction images of the bulk material reveal that La 2 O 3 nanoparticles were homogenously distributed in both the tungsten grains and the grain boundaries, and the sample exhibit a narrow micro-hardness distribution

  18. Liberation of Adsorbed and Co-Precipitated Arsenic from Jarosite, Schwertmannite, Ferrihydrite, and Goethite in Seawater

    Directory of Open Access Journals (Sweden)

    Rodrigo Alarcón

    2014-07-01

    Full Text Available Sea level rise is able to change the geochemical conditions in coastal systems. In these environments, transport of contaminants can be controlled by the stability and adsorption capacity of iron oxides. The behavior of adsorbed and co-precipitated arsenic in jarosite, schwertmannite, ferrihydrite, and goethite in sea water (common secondary minerals in coastal tailings was investigated. The aim of the investigation was to establish As retention and transport under a marine flood scenario, which may occur due to climate change. Natural and synthetic minerals with co-precipitated and adsorbed As were contacted with seawater for 25 days. During this period As, Fe, Cl, SO4, and pH levels were constantly measured. The larger retention capability of samples with co-precipitated As, in relation with adsorbed As samples, reflects the different kinetics between diffusion, dissolution, and surface exchange processes. Ferrihydrite and schwertmannite showed good results in retaining arsenic, although schwertmannite holding capacity was enhanced due its buffering capacity, which prevented reductive dissolution throughout the experiment. Arsenic desorption from goethite could be understood in terms of ion exchange between oxides and electrolytes, due to the charge difference generated by a low point-of-zero-charge and the change in stability of surface complexes between synthesis conditions and natural media.

  19. Synthesis and characterization of polyethylene glycol (PEG) coated Fe3O4 nanoparticles by chemical co-precipitation method for biomedical applications.

    Science.gov (United States)

    Anbarasu, M; Anandan, M; Chinnasamy, E; Gopinath, V; Balamurugan, K

    2015-01-25

    Polyethylene glycol (PEG) coated Fe3O4 nanoparticles were synthesized by chemical co-precipitation method. With polyethylene glycol (PEG) as a stabilizer and dispersant. The X-ray diffraction and selected area electron diffraction (SAED) results show that the cubic inverse spinel structure of pure phase polycrystalline Fe3O4 was obtained. The scanning electron microscopy (SEM) and field emission transmission electron microscopy (FE-TEM) results exhibited that the resulted Fe3O4 nanoparticles were roughly spherical in shape with narrow size distribution and homogenous shape. Fourier transform infrared spectroscopy (FT-IR) results suggested that PEG indicated with Fe3O4 via its carbonyl groups. Results of vibrating sample magnetometer (VSM) indicated that the prepared Fe3O4 nanoparticles exhibit superparamagnetic behavior and high saturation magnetization at room temperature. Such Fe3O4 nanoparticles with favorable size and tunable magnetic properties are promising biomedical applications. Copyright © 2014. Published by Elsevier B.V.

  20. Total, Soluble and Insoluble Oxalate Contents of Ripe Green and Golden Kiwifruit.

    Science.gov (United States)

    Nguyễn, Hà Vũ Hồng; Savage, Geoffrey P

    2013-03-05

    Three bulk samples of two different cultivars of kiwifruit, green ( Actinidia deliciosa L . ) and golden ( Actinidia chinensis L . ) were bought ripe, ready to eat from a local market. The aim of the study was to determine the oxalate composition of each of the three fractions of kiwifruit, namely skin, pulp and seeds. The pulp consisted of 90.4% of the edible portion of the two cultivars while the skin and seeds made up a mean of 8.0% and 1.6% respectively. Total oxalate was extracted with 2.0 M HCL at 21 °C for 15 min and soluble oxalates extracted at 21 °C in water for 15 min from each fraction. The total and soluble oxalate compositions of each fraction were determined using ion exchange HPLC chromatography. The pulp of golden kiwifruit contained lower amounts of total oxalates (15.7 vs. 19.3 mg/100 g FW) and higher amounts of soluble oxalates (8.5 vs. 7.6 mg/100 g FW) when compared to the green cultivar. The skin of the green cultivar contained lower levels of insoluble oxalates (36.9 vs. 43.6 mg/100 g FW), while the seeds of the green cultivar contained higher levels of insoluble oxalates 106.7 vs. 84.7 mg/100 g FW.

  1. Mechanisms of Se(IV) Co-precipitation with Ferrihydrite at Acidic and Alkaline Conditions and Its Behavior during Aging

    DEFF Research Database (Denmark)

    Francisco, Paul Clarence M.; Sato, Tsutomu; Otake, Tsubasa

    2018-01-01

    in nanopore and defect structures. These results demonstrate a potential long-term immobilization pathway for Se(IV) even after phase transformation. This work presents one of the first direct insights on Se(IV) co-precipitation and its behavior in response to iron phase transformations.......Understanding the form of Se(IV) co-precipitated with ferrihydrite and its subsequent behavior during phase transformation is critical to predicting its long-term fate in a range of natural and engineered settings. In this work, Se(IV)-ferrihydrite co-precipitates formed at different pH were......, Se(IV) was removed dominantly as a ferric selenite-like phase intimately associated with ferrihydrite, while at pH 10, it was mostly present as a surface species on ferrihydrite. Similarly, the behavior of Se(IV) and the extent of its retention during phase transformation varied with pH. At pH 5, Se...

  2. Availability of calcium from chemically pure potassium oxalate to the buffalo (Bubalus bubalis)

    International Nuclear Information System (INIS)

    Singh, Sudarshan; Sareen, V.K.; Marwah, S.R.; Sharma, K.C.; Bhatia, I.S.

    1978-01-01

    Three experiments were conducted to determine the true dige'stibility of calcium in the buffalo calves fed chemically pure potassium oxalate. In each experiments 6 calves were divided into two groups, viz. control and oxalate-fed. The control group was given basal ration consisting of wheat straw, mustard-cake and maize grains. The oxalate-fed group was fed the basal ration supplemented with 60, 100 and 140 g potassium oxalate per day in experiments 1,2, and 3 respectively. The percent true digestibility of calcium was 51.7 and 52.5 in experiment 1, 60.5 and 44.1 in experiment 2, and 59.3 and 44.1 in experiment 3 in the control and oxalate-fed groups respectively. In all the experiments the oxalate was completely broken down in the rumen. The volume of water intake and urine excretion was more in the oxalate-fed groups. The daily alkali output in the urine in terms of N-acid was 0.7 and 1.3 in experiment 1, 1.5 and 2.5 in experiment 2, and 2.1 and 3.8 in experiment 3 in control and oxalate-fed groups respectively. The daily bicarbonate concentration in the urine (in g) was 26.5 and 53.4 in experiment 1, 83.2 and 146.2 in experiment 2, and 132.6 and 222.8 in experiment 3 in control and oxalate-fed groups respectively. Likewise the excretion of oxalate in the urine was more in oxalate-fed groups. On the basis of the results obtained, the reason for the somewhat low true digestibility of calcium in the calves consuming more than 60 g of potassium oxalate/day are discussed. Isotope-dilution technique using 45 CaCl 2 was employed in the study. (auth.)

  3. 1D and 2D Cobalt(II) Coordination Polymers, Co(ox)(en):Synthesis, Structures and Magnetic Properties

    International Nuclear Information System (INIS)

    Kang, Jae Un; Lee, Yu Mi; Kim, Seung Joo; Yun, Ho Seop; Do, Jung Hwan

    2014-01-01

    Two ethylenediamine cobalt(II) oxalate complexes Co(ox)(en), 1 and Co(ox)(en)·2H 2 O, 2 have been hydrothermally synthesized and characterized by single crystal X-ray diffraction, IR spectrum, TG analysis, and magnetic measurements. In 1, Co atoms are coordinated by two bis-bidentate oxalate ions in transconfiguration to form Co(ox) chains, which are further bridged by ethylenediamine molecules to produce 2D grid layers, Co(ox)(en). In 2, Co atoms are coordinated by bridging oxalate ions in cis - configuration to form Co(ox) chains, and the additional chelation of ethylenediamine to Co atoms completes 1D zigzag chain, Co(en)(ox). Two lattice water molecules stabilize the chains through hydrogen bonding. Magnetic susceptibility measurements indicate that both complexes exhibit weak antiferromagnetic coupling between cobalt(II) ions with the susceptibility maxima at 23 K for 1 and 20 K for 2, respectively. In 1 and 2, the oxalate ligands afford a much shorter and more effective pathway for the magnetic interaction between cobalt ions compared to the ethylenediamine ligands, so the magnetic behaviors of both complexes could be well described with 1D infinite magnetic chain model

  4. Hydrothermal synthesis of uranyl squarates and squarate-oxalates: hydrolysis trends and in situ oxalate formation.

    Science.gov (United States)

    Rowland, Clare E; Cahill, Christopher L

    2010-07-19

    We report the synthesis of two uranyl squarates and two mixed-ligand uranyl squarate-oxalates from aqueous solutions under hydrothermal conditions. These products exhibit a range of uranyl building units from squarates with monomers in (UO(2))(2)(C(4)O(4))(5).6NH(4).4H(2)O (1; a = 16.731(17) A, b = 7.280(8) A, c = 15.872(16) A, beta = 113.294(16) degrees , monoclinic, P2(1)/c) and chains in (UO(2))(2)(OH)(2)(H(2)O)(2)(C(4)O(4)) (2; a = 12.909(5) A, b = 8.400(3) A, c = 10.322(4) A, beta = 100.056(7) degrees , monoclinic, C2/c) to two squarate-oxalate polymorphs with dimers in (UO(2))(2)(OH)(C(4)O(4))(C(2)O(4)).NH(4).H(2)O (3; a = 9.0601(7) A, b = 15.7299(12) A, c = 10.5108(8) A, beta = 106.394(1) degrees , monoclinic, P2(1)/n; and 4; a = 8.4469(6) A, b = 7.7589(5) A, c = 10.5257(7) A, beta = 105.696(1) degrees , monoclinic, P2(1)/m). The dominance at low pH of monomeric species and the increasing occurrence of oligomeric species with increasing pH suggests that uranyl hydrolysis, mUO(2)(2+) + nH(2)O right harpoon over left harpoon [(UO(2))(m)(OH)(n)](2m-n) + nH(+), has a significant role in the identity of the inorganic building unit. Additional factors that influence product assembly include in situ hydrolysis of squaric acid to oxalic acid, dynamic metal to ligand concentration, and additional binding modes resulting from the introduction of oxalate anions. These points and the effects of uranyl hydrolysis with changing pH are discussed in the context of the compounds presented herein.

  5. Unusual calcium oxalate crystals in ethylene glycol poisoning.

    Science.gov (United States)

    Godolphin, W; Meagher, E P; Sanders, H D; Frohlich, J

    1980-06-01

    A patient poisoned with ethylene glycol exhibited the symptoms of (1) hysteria, (2) metabolic acidosis with both a large anion gap and osmolal gap, and (3) crystalluria. However, the shape of the urinary crystals was prismatic and resembled hippurate rather than the expected dipyramidal calcium oxalate dihydrate. X-ray crystallography positively identified them as calcium oxalate monohydrate.

  6. [Clinical, laboratory, and functional characteristic of patients with bronchial asthma and chronic obstructive pulmonary disease with disturbances of oxalic acid metabolism].

    Science.gov (United States)

    Shaĭlieva, L O; Fedoseev, G B; Zorina, M L; Petrova, M A; Trofimov, V I; Kakliugin, A P

    2013-01-01

    We studied the role of oxalate release through the airways as a potential injurious factor in the development of inflammation, bronchial obstruction and cough syndrome (respiratory oxalosis). Detection of oxalates in bronhcoalveolar lavage fluid and daily urine is the most valuable method for diagnostics of oxalates. Systemic effects, such as cholelithiasis, urolithiasis, and spinal osteochondrosis are characteristic clinical signs of respiratory oxalosis, besides purely respiratory symptoms.

  7. Sonocatalytic degradation of malachite green oxalate by a semiconductor metal oxide nanocatalyst.

    Science.gov (United States)

    Bhavani, R; Sivasamy, A

    2016-12-01

    Advanced Oxidation Process (AOP) technologies are considered to be better technique for the degradation or mineralization of many recalcitrant compounds and pollutants. In the present study heterogeneous sonocatalytic degradation of a model organic compound such as Malachite green oxalate (MGO) was carried out in the aqueous phase. Zinc oxide nanorods were prepared by precipitation method employing zinc acetates as precursors and were characterized by FT-IR, XRD, FE-SEM and EDAX analysis. Degradation of MGO in the aqueous phase was studied in detail under the sonocatalytic process. Effects of pH, dye concentration, oxidant concentration, kinetics and effect of electrolytes on dye degradation were carried out to check the efficiency of the sonocatalyst. Effect of energy input on the degradation processes was also investigated. The degradation of dye molecules were monitored by UV-visible spectrophotometer and Chemical Oxygen demand (COD). The dye molecules were readily degraded at above 90% in the pH range 5.0-7.0 under ultrasound with zinc oxide nanorods. The interference of electrolytes like NaCl, KCl, Na 2 CO 3 , NaHCO 3 and MgSO 4 on the degradation of dye molecules were also studied on the sonocatalytic degradation of MGO. From the kinetic studies it was observed that at lower initial concentration of dye molecules the degradation efficiency was above 90%. The rate of the reaction decreased on increasing the initial dye concentrations of the dye molecules. It was observed that the complete mineralization of dye molecules was achieved without the formation of toxic by-products. The reusability of the catalyst also showed the effective degradation of the dye molecules up to five cycles without loss of the catalytic activities. Copyright © 2015 Elsevier Inc. All rights reserved.

  8. Comparison of direct and precipitation methods for the estimation of ...

    African Journals Online (AJOL)

    Background: There is increase in use of direct assays for analysis of high and low density lipoprotein cholesterol by clinical laboratories despite differences in performance characteristics with conventional precipitation methods. Calculation of low density lipoprotein cholesterol in precipitation methods is based on total ...

  9. Crystallization of calcium oxalate in minimally diluted urine

    Science.gov (United States)

    Bretherton, T.; Rodgers, A.

    1998-09-01

    Crystallization of calcium oxalate was studied in minimally diluted (92%) urine using a mixed suspension mixed product crystallizer in series with a Malvern particle sizer. The crystallization was initiated by constant flow of aqueous sodium oxalate and urine into the reaction vessel via two independent feed lines. Because the Malvern cell was in series with the reaction vessel, noninvasive measurement of particle sizes could be effected. In addition, aliquots of the mixed suspension were withdrawn and transferred to a Coulter counter for crystal counting and sizing. Steady-state particle size distributions were used to determine nucleation and growth kinetics while scanning electron microscopy was used to examine deposited crystals. Two sets of experiments were performed. In the first, the effect of the concentration of the exogenous sodium oxalate was investigated while in the second, the effect of temperature was studied. Calcium oxalate nucleation and growth rates were found to be dependent on supersaturation levels inside the crystallizer. However, while growth rate increased with increasing temperature, nucleation rates decreased. The favored phases were the trihydrate at 18°C, the dihydrate at 38° and the monohydrate at 58°C. The results of both experiments are in agreement with those obtained in other studies that have been conducted in synthetic and in maximally diluted urine and which have employed invasive crystal counting and sizing techniques. As such, the present study lends confidence to the models of urinary calcium oxalate crystallization processes which currently prevail in the literature.

  10. Effect of synthesis methods on the Ca{sub 3}Co{sub 4}O{sub 9} thermoelectric ceramic performances

    Energy Technology Data Exchange (ETDEWEB)

    Sotelo, A.; Rasekh, Sh.; Torres, M.A. [Instituto de Ciencia de Materiales de Aragón, CSIC—Universidad de Zaragoza, M" a de Luna, 3, 50018-Zaragoza (Spain); Bosque, P. [Centro Universitario de la Defensa de Zaragoza. Academia General Militar. Ctra. de Huesca s/n. 50090, Zaragoza (Spain); Madre, M.A., E-mail: amadre@unizar.es [Instituto de Ciencia de Materiales de Aragón, CSIC—Universidad de Zaragoza, M" a de Luna, 3, 50018-Zaragoza (Spain); Diez, J.C. [Instituto de Ciencia de Materiales de Aragón, CSIC—Universidad de Zaragoza, M" a de Luna, 3, 50018-Zaragoza (Spain)

    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 ones 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.

  11. Effect of Co2+ and Y3+ ions insertion on the microstructure development and magnetic properties of Ni0.5Zn0.5Fe2O4 powders synthesized using Co-precipitation method

    Science.gov (United States)

    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.

  12. Heterogeneous nucleation of calcium oxalate on native oxide surfaces

    International Nuclear Information System (INIS)

    Song, L.; Pattillo, M.J.; Graff, G.L.; Campbell, A.A.; Bunker, B.C.

    1994-04-01

    The aqueous deposition of calcium oxalate onto colloidal oxides has been studied as a model system for understanding heterogeneous nucleation processes of importance in biomimetic synthesis of ceramic thin films. Calcium oxalate nucleation has been monitored by measuring induction times for nucleation using Constant Composition techniques and by measuring nucleation densities on extended oxide surfaces using an atomic force microscope. Results show that the dependence of calcium oxalate nucleation on solution supersaturation fits the functional form predicted by classical nucleation theories. Anionic surfaces appear to promote nucleation better than cationic surfaces, lowering the effective energy barrier to heterogeneous nucleation

  13. 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.

    Science.gov (United States)

    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.

  14. Total, Soluble and Insoluble Oxalate Contents of Ripe Green and Golden Kiwifruit

    Directory of Open Access Journals (Sweden)

    Hà Vũ Hồng Nguyễn

    2013-03-01

    Full Text Available Three bulk samples of two different cultivars of kiwifruit, green (Actinidia deliciosa L. and golden (Actinidia chinensis L. were bought ripe, ready to eat from a local market. The aim of the study was to determine the oxalate composition of each of the three fractions of kiwifruit, namely skin, pulp and seeds. The pulp consisted of 90.4% of the edible portion of the two cultivars while the skin and seeds made up a mean of 8.0% and 1.6% respectively. Total oxalate was extracted with 2.0 M HCL at 21 °C for 15 min and soluble oxalates extracted at 21 °C in water for 15 min from each fraction. The total and soluble oxalate compositions of each fraction were determined using ion exchange HPLC chromatography. The pulp of golden kiwifruit contained lower amounts of total oxalates (15.7 vs. 19.3 mg/100 g FW and higher amounts of soluble oxalates (8.5 vs. 7.6 mg/100 g FW when compared to the green cultivar. The skin of the green cultivar contained lower levels of insoluble oxalates (36.9 vs. 43.6 mg/100 g FW, while the seeds of the green cultivar contained higher levels of insoluble oxalates 106.7 vs. 84.7 mg/100 g FW.

  15. Mercury (II) reduction and co-precipitation of metallic mercury on hydrous ferric oxide in contaminated groundwater.

    Science.gov (United States)

    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.

  16. Correlation between oxalic acid production and copper tolerance in Wolfiporia cocos

    Science.gov (United States)

    C. A. Clausen; Frederick Green; B. M. Woodward; J. W. Evans; R. C. DeGroot

    2000-01-01

    The increased interest in copper-based wood preservatives has hastened the need for understanding why some fungi are able to attack copper-treated wood. Due in part to accumulation of oxalic acid by brown-rot fungi and visualization of copper oxalate crystals in wood decayed by known copper-tolerant decay fungi, oxalic acid has been implicated in copper tolerance by...

  17. Evaluation of soluble oxalates content in infusions of different kinds of tea and coffee available on the Polish market.

    Science.gov (United States)

    Rusinek, Elzbieta

    2012-01-01

    Tea and coffee are the potentially rich source of oxalic acid, which can act as a antinutrient. The aim of this study was to determine and evaluate the content of soluble oxalates in teas and coffees available on the Polish market. The green, red and black teas, and black natural ground and instant coffees were used for preparing the infusions. The manganometric method was used for the determination of the oxalates in the infusions. The mean oxalates content in the infusions from 3 g of black teas was 115.68 mg/100 cm3 and was higher as compared to red teas (101.91 mg/100 cm3) and green teas (87.64 mg/100 cm3). Disregarding the variety of analyzed teas, the largest oxalates content was in infusions of pure one-component tea--"Sir Roger" (164.82-174.22 mg/100 cm3), while the lowest oxalates content was noted in the tea containing the components from other plants ("Bio-Active" with grapefruit juice--reaching as low level as 39.00 mg/100 cm3). Instant coffees contained larger amount of oxalates than natural ground coffees. Irrespective of the kind of the tested coffees, the lowest oxalates content was found in the infusions from the following coffees: Tchibo Exclusive--19.62 mg/100 cm3, Gala ulubiona--37.32 mg/100 cm3, and Maxwell House--38.40 mg/100 cm3, while the highest oxalates content in instant coffee--Nescafe Espiro 51.80 mg/100 cm3. The results revealed a significant relation between phytochemical composition of analyzed teas and coffees and the level of soluble oxalates in infusions prepared from the tested products.

  18. Method of precipitating uranium from an aqueous solution and/or sediment

    Science.gov (United States)

    Tokunaga, Tetsu K; Kim, Yongman; Wan, Jiamin

    2013-08-20

    A method for precipitating uranium from an aqueous solution and/or sediment comprising uranium and/or vanadium is presented. The method includes precipitating uranium as a uranyl vanadate through mixing an aqueous solution and/or sediment comprising uranium and/or vanadium and a solution comprising a monovalent or divalent cation to form the corresponding cation uranyl vanadate precipitate. The method also provides a pathway for extraction of uranium and vanadium from an aqueous solution and/or sediment.

  19. Synthesis, Optical and Electrochemical Properties of Y2O3 Nanoparticles Prepared by Co-Precipitation Method.

    Science.gov (United States)

    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.

  20. Modified structural and magnetic properties of nanocrystalline MnFe{sub 2}O{sub 4} by pH in capping agent free co-precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Iranmanesh, P., E-mail: p.iranmanesh@vru.ac.ir [Department of Physics, Vali-e-Asr University of Rafsanjan, 77139-36417 Rafsanjan (Iran, Islamic Republic of); Saeednia, S. [Department of Chemistry, Vali-e-Asr University of Rafsanjan, 77139-36417 Rafsanjan (Iran, Islamic Republic of); Mehran, M.; Dafeh, S. Rashidi [Department of Physics, Vali-e-Asr University of Rafsanjan, 77139-36417 Rafsanjan (Iran, Islamic Republic of)

    2017-03-01

    Nano-sized manganese ferrite (MnFe{sub 2}O{sub 4}) particles were prepared using co-precipitation method in two different pH (9 and 11). The structural, morphological, optical and magnetic properties of as-synthesized nanoparticles were characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), transmission electron microscopy (TEM), UV–vis absorption and vibrating sample magnetometer (VSM). The FTIR spectra revealed two strong peaks at about 600 and 400 cm{sup −1} that can be attributed to the vibration mode of octahedral and tetrahedral sites of spinel structure of MnFe{sub 2}O{sub 4}, respectively. The XRD results showed that the nanocrystalline MnFe{sub 2}O{sub 4} has pure cubic spinel crystal structure with average crystallite size of 11 nm. The cation distribution of these nanoparticles was estimated by X-ray analysis data. The blue shift was observed in the band gap when compared with bulk sample which is due to the quantum size effect. The absence of hysteresis for MnFe{sub 2}O{sub 4} nanoparticles indicated the superparamagnetic behaviour, as expected for single domain nanoparticles. The obtained value for saturation magnetization being less than its value of bulk ones and larger pH is due to surface effects. The calculated magnetic particle size was smaller than crystallite size estimated from the XRD results; which indicate the presence of dead layer on particle surface. - Highlights: • We study effect of pH on the size and magnetic properties of MnFe{sub 2}O{sub 4} nanoparticles. • MnFe{sub 2}O{sub 4} were synthesized by co-precipitation method without any capping agent. • The physical properties are affected by cation contribution and surface effects. • The smaller nanoparticles with larger pH show a red shift in the band gap energy. • The M{sub s} is less than its value of bulk ones due to surface effects.

  1. A method for determination of 90Sr in vegetation

    International Nuclear Information System (INIS)

    Nygren, U.

    1998-12-01

    This report describes a method for determination of 90 Sr in vegetation. The method consists of wet-ashing the samples and separating Sr from the sample matrix by oxalate precipitation and extraction chromatography. 90 Y ingrowth is awaited after which Y is separated from Sr and 90 Y measured in a proportional counter. The method has been applied on two reference materials and the 90 Sr results agree well with the recommended values. The method has also been used on 20 samples of blueberry twigs and the mean recovery of Sr was 74%

  2. Preparation and Heat-Treatment of DWPF Simulants With and Without Co-Precipitated Noble Metals

    International Nuclear Information System (INIS)

    Koopman, David C.:Eibling, Russel E

    2005-01-01

    The Savannah River National Laboratory is in the process of investigating factors suspected of impacting catalytic hydrogen generation in the Chemical Process Cell of the Defense Waste Processing Facility, DWPF. Noble metal catalyzed hydrogen generation in simulation work constrains the allowable acid addition operating window in DWPF. This constraint potentially impacts washing strategies during sludge batch preparation. It can also influence decisions related to the addition of secondary waste streams to a sludge batch. Noble metals have historically been added as trim chemicals to process simulations. The present study investigated the potential conservatism that might be present from adding the catalytic species as trim chemicals to the final sludge simulant versus co-precipitating the noble metals into the insoluble sludge solids matrix. Parallel preparations of two sludge simulants targeting the composition of Sludge Batch 3 were performed in order to evaluate the impact of the form of noble metals. Identical steps were used except that one simulant had dissolved palladium, rhodium, and ruthenium present during the precipitation of the insoluble solids. Noble metals were trimmed into the other stimulant prior to process tests. Portions of both sludge simulants were held at 97 C for about eight hours to qualitatively simulate the effects of long term storage on particle morphology and speciation. The simulants were used as feeds for Sludge Receipt and Adjustment Tank, SRAT, process simulations. The following conclusions were drawn from the simulant preparation work: (1) The first preparation of a waste slurry simulant with co-precipitated noble metals was successful, based on the data obtained. It appears that 99+% of the noble metals were retained in the simulant. (2) Better control of carbonate, hydroxide, and post-wash trim chemical additions is needed before the new method of simulant preparation will be as reproducible as the old method. (3) The two new

  3. Investigating the effect of Mn-doped CeO2 nanoparticles by co-precipitation method

    International Nuclear Information System (INIS)

    Prabaharan, D.D.M.; Sadaiyandi, K.; Mahendran, M.; Sagadevan, Suresh

    2018-01-01

    The paper exhibits a detailed study about the synthesis and characterization in analysis of structural, morphological, optical and electrical investigations of pure and Mn-doped Cerium oxide (CeO 2 ) nanoparticles which were synthesized by co-precipitation technique. Phase formation of the prepared sample was analyzed with powder X-ray diffraction (PXRD) examines, scanning electron microscopy (SEM) examination. The PXRD comes about affirmed partial crystallinity having cubic phases and the crystallite sizes of the pure and Mn-doped Cerium oxide (CeO 2 ) were estimated by utilizing Debye-Scherrer's formula and they were calculated to be 12 and 14 nm individually. SEM pictures revealed that the particles were profoundly accumulated and were of permeable nature. The optical properties of pure and Mn-doped CeO 2 were ascertained by using UV-visible absorption spectrum. The estimated band gap values for the pure and the Mn-doped CeO 2 nanoparticles were observed to be 2.7 and 2.6 eV, respectively, utilizing UV-Vis spectroscopy. At different frequencies and temperatures the dielectric properties of the Mn-doped Cerium oxide (CeO 2 ) nanoparticles, for example, the dielectric consistent, the dielectric loss and the AC conductivity, were studied. (orig.)

  4. Thermoluminescent properties of CaSO4:Dy prepared by precipitation method

    International Nuclear Information System (INIS)

    Roman, J.; Rivera, T.; Azorin, J.

    2009-10-01

    This paper reports the synthesis and thermoluminescent (Tl) characterization of CaSO 4 :Dy obtained by the precipitation method. Thermoluminescent CaSO 4 :Dy powder and Teflon (PTFE) were mixed in order to obtain samples in pellets form. Samples of CaSO 4 :Dy were exposed to a radiation gamma source of 60 Co and 90 Sr beta particles. Tl response of CaSO 4 :Dy showed a glow curve with two peaks centered at around 164 and 302 C. Tl phosphor showed a good linearity in the range from 0.5 to 30 Gy. Fading of the Tl information was 5.19 % in 37 days and presented a standard deviation of 4% for reproducibility. (Author)

  5. Oxalic acid as an assisting agent for the electrodialytic remediation of chromated copper arsenate treated timber waste

    DEFF Research Database (Denmark)

    Ribeiro, Alexandra B.; Mateus, Eduardo P.; Ottosen, Lisbeth M.

    1999-01-01

    The electrodialytic process is proposed as a technique for the remediation of chromated copper arsenate treated timber waste, using oxalic acid as assisting agent. The method prowed succesfull 93% Cu, 95% Cr and 99% As was removed from the timber.......The electrodialytic process is proposed as a technique for the remediation of chromated copper arsenate treated timber waste, using oxalic acid as assisting agent. The method prowed succesfull 93% Cu, 95% Cr and 99% As was removed from the timber....

  6. Reaction of Hydrazine Hydrate with Oxalic Acid: Synthesis and ...

    African Journals Online (AJOL)

    NICO

    2013-11-28

    Nov 28, 2013 ... The title compound is a molecular salt containing two discrete hydrazinium cations and an oxalate anion. The oxalate ... RESEARCH ARTICLE ... Scheme and reaction showing the simple experimental procedure for the preparation of .... 7 A.I. Vogel, A Text Book of Quantitative Inorganic Analysis, 4th edn.,.

  7. Studies on the decomposition of oxalic acid by nitric acid in presence of catalysts

    International Nuclear Information System (INIS)

    Noronha, D.M.; Pius, I.C.; Chaudhury, S.

    2015-01-01

    Impure Plutonium oxalate generated from the recovery of plutonium from waste solutions may require further purification via anion exchange. Conventionally, plutonium oxalate is converted to oxide in a furnace and the oxide is dissolved in Conc. HNO 3 containing HF and purified by anion exchange route. Studies initiated on the decomposition of oxalic acid with Conc. HNO 3 to facilitate direct dissolution of plutonium oxalate and quantitative destruction of oxalate are discussed in this paper. (author)

  8. Preliminary assessment of a method utilizing carbon dioxide and steelmaking slags to produce precipitated calcium carbonate

    International Nuclear