Sample records for solution preparation method

  1. CTEPP STANDARD OPERATING PROCEDURE FOR PREPARATION OF SURROGATE RECOVERY STANDARD AND INTERNAL STANDARD SOLUTIONS FOR POLAR TARGET ANALYTES (SOP-5.26)

    EPA Science Inventory

    This SOP describes the method used for preparing surrogate recovery standard and internal standard solutions for the analysis of polar target analytes. It also describes the method for preparing calibration standard solutions for polar analytes used for gas chromatography/mass sp...

  2. Method and apparatus for the production of metal oxide powder

    DOEpatents

    Harris, Michael T.; Scott, Timothy C.; Byers, Charles H.

    1993-01-01

    The present invention provides a method for preparing metal oxide powder. A first solution, which is substantially organic, is prepared. A second solution, which is an aqueous solution substantially immiscible in the first solution, is prepared and delivered as drops to the first solution. The drops of the second solution are atomized by a pulsed electric field forming micro-drops of the second solution. Reagents in the first solution diffuse into and react with reactants in the micro-drops of the second solution forming metal hydroxide or oxalate particles. The metal hydroxide or metal oxalate particles are then recovered and dried to produce the metal oxide powder. An apparatus for preparing a metal oxide powder is also disclosed.

  3. Method and apparatus for the production of metal oxide powder

    DOEpatents

    Harris, Michael T.; Scott, Timothy C.; Byers, Charles H.

    1992-01-01

    The present invention provides a method for preparing metal oxide powder. A first solution, which is substantially organic, is prepared. A second solution, which is an aqueous solution substantially immiscible in the first solution, is prepared and delivered as drops to the first solution. The drops of the second solution are atomized by a pulsed electric field forming micro-drops of the second solution. Reagents in the first solution diffuse into and react with reactants in the micro-drops of the second solution forming metal hydroxide or oxalate particles. The metal hydroxide or metal oxalate particles are then recovered and dried to produce the metal oxide powder. An apparatus for preparing a metal oxide powder is also disclosed.

  4. Method and apparatus for the production of metal oxide powder

    DOEpatents

    Harris, M.T.; Scott, T.C.; Byers, C.H.

    1992-06-16

    The present invention provides a method for preparing metal oxide powder. A first solution, which is substantially organic, is prepared. A second solution, which is an aqueous solution substantially immiscible in the first solution, is prepared and delivered as drops to the first solution. The drops of the second solution are atomized by a pulsed electric field forming micro-drops of the second solution. Reagents in the first solution diffuse into and react with reactants in the micro-drops of the second solution forming metal hydroxide or oxalate particles. The metal hydroxide or metal oxalate particles are then recovered and dried to produce the metal oxide powder. An apparatus for preparing a metal oxide powder is also disclosed. 2 figs.

  5. Synthesis and Microstructure of Highly Oriented PbTiO3 Thin Films Prepared by a Sol-Gel Method

    DTIC Science & Technology

    1989-06-01

    lead acetate with titanium isopropoxide * in 2-methoxyethanol,* in a method similar to that reported by Gurkovitch and Blum." The resulting yellow-gold...orientation by a sol-gel processing method. EXPERIMENTAL Precursor Solution Preparation Stock solutions of complex Pb-Ti alkoxide were prepared by reacting... solution had an equivalent PbTiO 3 concentration of approximately 66 wt%. The alkoxide solutions were handled as moisture-sensitive reagents and, as

  6. Optical limiting device and method of preparation thereof

    DOEpatents

    Wang, Hsing-Lin; Xu, Su; McBranch, Duncan W.

    2003-01-01

    Optical limiting device and method of preparation thereof. The optical limiting device includes a transparent substrate and at least one homogeneous layer of an RSA material in polyvinylbutyral attached to the substrate. The device may be produced by preparing a solution of an RSA material, preferably a metallophthalocyanine complex, and a solution of polyvinylbutyral, and then mixing the two solutions together to remove air bubbles. The resulting solution is layered onto the substrate and the solvent is evaporated. The method can be used to produce a dual tandem optical limiting device.

  7. Method for preparing salt solutions having desired properties

    DOEpatents

    Ally, Moonis R.; Braunstein, Jerry

    1994-01-01

    The specification discloses a method for preparing salt solutions which exhibit desired thermodynamic properties. The method enables prediction of the value of the thermodynamic properties for single and multiple salt solutions over a wide range of conditions from activity data and constants which are independent of concentration and temperature. A particular application of the invention is in the control of salt solutions in a process to provide a salt solution which exhibits the desired properties.

  8. Lack of latex allergen contamination of solutions withdrawn from vials with natural rubber stoppers.

    PubMed

    Thomsen, D J; Burke, T G

    2000-01-01

    The effect on latex allergen contamination and microbial growth of a latex-allergy precaution technique for preparing injectable products was studied. The study consisted of three parts: (1) preparation of 20 samples from vials with latex-containing stoppers in accordance with conventional guidelines, (2) preparation of 20 samples in accordance with latex-allergy precaution guidelines, and (3) preparation of 5 latex-free samples and 1 latex-contaminated sample as negative and positive controls, respectively. The conventional method involved swabbing a vial top with an alcohol prep pad, puncturing the dry natural rubber stopper with an 18-gauge needle attached to a latex-free syringe, and withdrawing the contents of the vial into the syringe. The latex-allergy precaution preparation technique was similar, except that the stopper was removed before the vial contents were withdrawn. There was essentially no difference in latex allergen concentrations between the two drug preparation methods. None of the samples prepared with the standard method supported any microbial growth. One sample prepared with the latex-allergy precaution method grew bacteria. Removal of the dry rubber stopper from vials did not yield solutions with less latex allergen than solutions prepared according to conventional guidelines.

  9. [Nasal submicron emulsion of Scutellariae Radix extract preparation technology research based on phase transfer of solute technology].

    PubMed

    Shi, Ya-jun; Shi, Jun-hui; Chen, Shi-bin; Yang, Ming

    2015-07-01

    Based on the demand of nasal drug delivery high drug loadings, using the unique phase transfer of solute, integrating the phospholipid complex preparation and submicron emulsion molding process of Scutellariae Radix extract, the study obtained the preparation of the high drug loadings submicron emulsion of Scutellariae Radix extract. In the study of drug solution dispersion method, the uniformity of drug dispersed as the evaluation index, the traditional mixing method, grinding, homogenate and solute phase transfer technology were investigated, and the solute phase transfer technology was adopted in the last. With the adoption of new technology, the drug loading capacity reached 1.33% (phospholipid complex was 4%). The drug loading capacity was improved significantly. The transfer of solute method and timing were studied as follows,join the oil phase when the volume of phospholipid complex anhydrous ethanol solution remaining 30%, the solute phase transfer was completed with the continued recycling of anhydrous ethanol. After drug dissolved away to oil phase, the preparation technology of colostrum was determined with the evaluation index of emulsion droplet form. The particle size of submicron emulsion, PDI and stability parameters were used as evaluation index, orthogonal methodology were adopted to optimize the submicron emulsion ingredient and main influential factors of high pressure homogenization technology. The optimized preparation technology of Scutellariae Radix extract nasal submicron emulsion is practical and stable.

  10. Effects of preparation methods on the structure and mechanical properties of wet conditioned starch/montmorillonite nanocomposite films.

    PubMed

    Müller, Péter; Kapin, Éva; Fekete, Erika

    2014-11-26

    TPS/Na-montmorillonite nanocomposite films were prepared by solution and melt blending. Clay content changed between 0 and 25 wt% based on the amount of dry starch. Structure, tensile properties, and water content of wet conditioned films were determined as a function of clay content. Intercalated structure and VH-type crystallinity of starch were found for all the nanocomposites independently of clay and plasticizer content or preparation method, but at larger than 10 wt% clay content nanocomposites prepared by melt intercalation contained aggregated particles as well. In spite of the incomplete exfoliation clay reinforces TPS considerably. Preparation method has a strong influence on mechanical properties of wet conditioned films. Mechanical properties of the conditioned samples prepared by solution homogenization are much better than those of nanocomposites prepared by melt blending. Water, which was either adsorbed or bonded in the composites in conditioning or solution mixing process, respectively, has different effect on mechanical properties. Copyright © 2014 Elsevier Ltd. All rights reserved.

  11. Do centrally pre-prepared solutions achieve more reliable drug concentrations than solutions prepared on the ward?

    PubMed

    Dehmel, Carola; Braune, Stephan A; Kreymann, Georg; Baehr, Michael; Langebrake, Claudia; Hilgarth, Heike; Nierhaus, Axel; Dartsch, Dorothee C; Kluge, Stefan

    2011-08-01

    To compare the concentration conformity of infusion solutions manually prepared on intensive care units (ICU) with solutions from pharmacy-based, automated production. A prospective observational study conducted in a university hospital in Germany. Drug concentrations of 100 standardised infusion solutions manually prepared in the ICU and 100 matching solutions from automated production containing amiodarone, noradrenaline or hydrocortisone were measured by high-performance liquid chromatography analysis. Deviations from stated concentrations were calculated, and the quality of achieved concentration conformity of the two production methods was compared. Actual concentrations of 53% of the manually prepared and 16% of the machine-made solutions deviated by >5% above or below the stated concentration. A deviation of >10% was measured in 22% of the manually prepared samples and in 5% of samples from automated production. Of the manually prepared solutions, 15% deviated by >15% above or below the intended concentration. The mean concentration of the manually prepared solutions was 97.2% (SD 12.7%, range 45-129%) and of the machine-made solutions was 101.1% (SD 4.3%, range 90-114%) of the target concentration (p < 0.01). In this preliminary study, ward-based, manually prepared infusion solutions showed clinically relevant deviations in concentration conformity significantly more often than pharmacy-prepared, machine-made solutions. Centralised, automated preparation of standardised infusion solutions may be an effective means to reduce this type of medication error. Further confirmatory studies in larger settings and under conditions of routine automated production are required.

  12. Sol-gel preparation of lead magnesium niobate (PMN) powders and thin films

    DOEpatents

    Boyle, T.J.

    1999-01-12

    A method of preparing a lead magnesium niobium oxide (PMN), Pb(Mg{sub 1/3}Nb{sub 2/3})O{sub 3}, precursor solution by a solvent method wherein a liquid solution of a lead-complex PMN precursor is combined with a liquid solution of a niobium-complex PMN precursor, the combined lead- and niobium-complex liquid solutions are reacted with a magnesium-alkyl solution, forming a PMN precursor solution and a lead-based precipitate, and the precipitate is separated from the reacted liquid PMN precursor solution to form a precipitate-free PMN precursor solution. This precursor solution can be processed to form both ferroelectric powders and thin films. 3 figs.

  13. Sol-Gel Preparation Of Lead Magnesium Ni Obate (Pmn) Powdersand Thin Films

    DOEpatents

    Boyle, Timothy J.

    1999-01-12

    A method of preparing a lead magnesium niobium oxide (PMN), Pb(Mg.sub.1/3 Nb.sub.2/3)O.sub.3, precursor solution by a solvent method wherein a liquid solution of a lead-complex PMN precursor is combined with a liquid solution of a niobium-complex PMN precursor, the combined lead- and niobium-complex liquid solutions are reacted with a magnesium-alkyl solution, forming a PMN precursor solution and a lead-based precipitate, and the precipitate is separated from the reacted liquid PMN precursor solution to form a precipitate-free PMN precursor solution. This precursor solution can be processed to form both ferroelectric powders and thin films.

  14. Method of quantitating dsDNA

    DOEpatents

    Stark, Peter C.; Kuske, Cheryl R.; Mullen, Kenneth I.

    2002-01-01

    A method for quantitating dsDNA in an aqueous sample solution containing an unknown amount of dsDNA. A first aqueous test solution containing a known amount of a fluorescent dye-dsDNA complex and at least one fluorescence-attenutating contaminant is prepared. The fluorescence intensity of the test solution is measured. The first test solution is diluted by a known amount to provide a second test solution having a known concentration of dsDNA. The fluorescence intensity of the second test solution is measured. Additional diluted test solutions are similarly prepared until a sufficiently dilute test solution having a known amount of dsDNA is prepared that has a fluorescence intensity that is not attenuated upon further dilution. The value of the maximum absorbance of this solution between 200-900 nanometers (nm), referred to herein as the threshold absorbance, is measured. A sample solution having an unknown amount of dsDNA and an absorbance identical to that of the sufficiently dilute test solution at the same chosen wavelength is prepared. Dye is then added to the sample solution to form the fluorescent dye-dsDNA-complex, after which the fluorescence intensity of the sample solution is measured and the quantity of dsDNA in the sample solution is determined. Once the threshold absorbance of a sample solution obtained from a particular environment has been determined, any similarly prepared sample solution taken from a similar environment and having the same value for the threshold absorbance can be quantified for dsDNA by adding a large excess of dye to the sample solution and measuring its fluorescence intensity.

  15. Particle characterization of poorly water-soluble drugs using a spray freeze drying technique.

    PubMed

    Kondo, Masahiro; Niwa, Toshiyuki; Okamoto, Hirokazu; Danjo, Kazumi

    2009-07-01

    A spray freeze drying (SFD) method was developed to prepare the composite particles of poorly water-soluble drug. The aqueous solution dissolved drug and the functional polymer was sprayed directly into liquid nitrogen. Then, the iced droplets were lyophilized with freeze-dryer to prepare solid particles. Tolbutamide (TBM) and hydroxypropylmethylcellulose (HPMC) were used as a model drug and water-soluble polymeric carrier in this study, respectively. The morphological observation of particles revealed that the spherical particles having porous structure could be obtained by optimizing the loading amount of drug and polymer in the spray solution. Especially, SFD method was characterized that the prepared particles had significantly larger specific surface area comparing with those prepared by the standard spray drying technique. The physicochemical properties of the resultant particles were found to be dependent on the concentration of spray solution. When the solution with high content of drug and polymer was used, the particle size of the resulting composite particles increased and they became spherical. The specific surface area of the particles also increased as a result of higher concentration of solution. The evaluation of spray solution indicated that these results were dependent on the viscosity of spray solution. In addition, when composite particles of TBM were prepared using the SFD method with HPMC as a carrier, the crystallinity of TBM decreased as the proportion of HPMC increased. When the TBM : HPMC ratio reached 1 : 5, the crystallinity of the particles completely disappeared. The dissolution tests showed that the release profiles of poorly water-soluble TBM from SFD composite particles were drastically improved compared to bulk TBM. The 70% release time T(70) of composite particles prepared by the SFD method in a solution of pH 1.2 was quite smaller than that of bulk TBM, while in a solution of pH 6.8, it was slightly lower. In addition, the release rates were faster than those of standard spray dried (SD) composite particles for solutions of pH 1.2 and 6.8, respectively. When composite particles were prepared from mixtures with various composition ratios, T(70) was found to decrease as the proportion of HPMC increased; the release rate was faster than that of bulk TBM in a solution of pH 6.8, as well as solution of pH 1.2.

  16. [Study on two preparation methods for beta-CD inclusion compound of four traditional Chinese medicine volatile oils].

    PubMed

    Li, Hailiang; Cui, Xiaoli; Tong, Yan; Gong, Muxin

    2012-04-01

    To compare inclusion effects and process conditions of two preparation methods-colloid mill and saturated solution-for beta-CD inclusion compound of four traditional Chinese medicine volatile oils and study the relationship between each process condition and volatile oil physical properties and the regularity of selective inclusion of volatile oil components. Volatile oils from Nardostachyos Radix et Rhizoma, Amomi Fructus, Zingiberis Rhizoma and Angelicaesinensis Radix were prepared using two methods in the orthogonal test. These inclusion compounds by optimized processes were assessed and compared by such methods as TLC, IR and scanning electron microscope. Inclusion oils were extracted by steam distillation, and the components found before and after inclusion were analyzed by GC-MS. Analysis showed that new inclusion compounds, but inclusion compounds prepared by the two processes had differences to some extent. The colloid mill method showed a better inclusion effect than the saturated solution method, indicating that their process conditions had relations with volatile oil physical properties. There were differences in the inclusion selectivity of components between each other. The colloid mill method for inclusion preparation is more suitable for industrial requirements. To prepare volatile oil inclusion compounds with heavy gravity and high refractive index, the colloid mill method needs longer time and more water, while the saturated solution method requires higher temperature and more beta-cyclodextrin. The inclusion complex prepared with the colloid mill method contains extended molecular weight chemical composition, but the kinds of components are reduced.

  17. Solubilization and Stability of Mitomycin C Solutions Prepared for Intravesical Administration.

    PubMed

    Myers, Alan L; Zhang, Yan-Ping; Kawedia, Jitesh D; Zhou, Ximin; Sobocinski, Stacey M; Metcalfe, Michael J; Kramer, Mark A; Dinney, Colin P N; Kamat, Ashish M

    2017-06-01

    Mitomycin C (MMC) is an antitumor agent that is often administered intravesically to treat bladder cancer. Pharmacologically optimized studies have suggested varying methods to optimize delivery, with drug concentration and solution volume being the main drivers. However, these MMC concentrations (e.g. 2.0 mg/mL) supersede its solubility threshold, raising major concerns of inferior drug delivery. In this study, we seek to confirm that the pharmacologically optimized MMC concentrations are achievable in clinical practice through careful modifications of the solution preparation methods. MMC admixtures (1.0 and 2.0 mg/mL) were prepared in normal saline using conventional and alternative compounding methods. Conventional methodology resulted in poorly soluble solutions, with many visible particulates and crystallates. However, special compounding methods, which included incubation of solutions at 50 °C for 50 min followed by storage at 37 °C, were sufficient to solubilize drug. Chemical degradation of MMC solutions was determined over 6 h using high-performance liquid chromatography (HPLC) analytics, while physical stability was tested in parallel. Immediately following the 50 min incubation, both MMC solutions exhibited approximately 5-7% drug degradation. Based on the measured concentrations and linear regression of degradation plots, additional storage of these solutions at 37 °C for 5 h retained chemical stability criterion (< 10% overall drug loss). No physical changes were observed in any solutions at any test time points. We recommend that the described alternative preparation methods may improve intravesicular delivery of MMC in this urological setting, and advise that clinicians employing these changes should closely monitor patients for MMC toxicities and pharmacodynamics (change in clinical outcomes) that result from the potential enhancement of MMC exposure in the bladder.

  18. Method of forming catalyst layer by single step infiltration

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

    Gerdes, Kirk; Lee, Shiwoo; Dowd, Regis

    Provided herein is a method for electrocatalyst infiltration of a porous substrate, of particular use for preparation of a cathode for a solid oxide fuel cell. The method generally comprises preparing an electrocatalyst infiltrate solution comprising an electrocatalyst, surfactant, chelating agent, and a solvent; pretreating a porous mixed ionic-electric conductive substrate; and applying the electrocatalyst infiltration solution to the porous mixed ionic-electric conductive substrate.

  19. Process for fabricating PBI hollow fiber asymmetric membranes for gas separation and liquid separation

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

    Jayaweera, Indira; Krishnan, Gopala N.; Sanjurjo, Angel

    2016-04-26

    The invention provides methods for preparing an asymmetric hollow fiber, the asymmetric hollow fibers prepared by such methods, and uses of the asymmetric hollow fibers. One method involves passing a polymeric solution through an outer annular orifice of a tube-in-orifice spinneret, passing a bore fluid though an inner tube of the spinneret, dropping the polymeric solution and bore fluid through an atmosphere over a dropping distance, and quenching the polymeric solution and bore fluid in a bath to form an asymmetric hollow fiber.

  20. Superconductor precursor mixtures made by precipitation method

    DOEpatents

    Bunker, Bruce C.; Lamppa, Diana L.; Voigt, James A.

    1989-01-01

    Method and apparatus for preparing highly pure homogeneous precursor powder mixtures for metal oxide superconductive ceramics. The mixes are prepared by instantaneous precipitation from stoichiometric solutions of metal salts such as nitrates at controlled pH's within the 9 to 12 range, by addition of solutions of non-complexing pyrolyzable cations, such as alkyammonium and carbonate ions.

  1. 7 CFR 201.58d - Fungal endophyte test.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ...) Method of preparation of aniline blue stain for use in testing grass seed and plant material for the presence of fungal endophyte: (1) Prepare a 1 percent aqueous aniline blue solution by dissolving 1 gram aniline blue in 100 ml distilled water. (2) Prepare the endophyte staining solution of one part of 1...

  2. 7 CFR 201.58d - Fungal endophyte test.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ...) Method of preparation of aniline blue stain for use in testing grass seed and plant material for the presence of fungal endophyte: (1) Prepare a 1 percent aqueous aniline blue solution by dissolving 1 gram aniline blue in 100 ml distilled water. (2) Prepare the endophyte staining solution of one part of 1...

  3. 7 CFR 201.58d - Fungal endophyte test.

    Code of Federal Regulations, 2014 CFR

    2014-01-01

    ...) Method of preparation of aniline blue stain for use in testing grass seed and plant material for the presence of fungal endophyte: (1) Prepare a 1 percent aqueous aniline blue solution by dissolving 1 gram aniline blue in 100 ml distilled water. (2) Prepare the endophyte staining solution of one part of 1...

  4. Method for preparing actinide nitrides

    DOEpatents

    Bryan, G.H.; Cleveland, J.M.; Heiple, C.R.

    1975-12-01

    Actinide nitrides, and particularly plutonium and uranium nitrides, are prepared by reacting an ammonia solution of an actinide compound with an ammonia solution of a reactant or reductant metal, to form finely divided actinide nitride precipitate which may then be appropriately separated from the solution. The actinide nitride precipitate is particularly suitable for forming nuclear fuels.

  5. Iodine addition using triiodide solutions

    NASA Technical Reports Server (NTRS)

    Rutz, Jeffrey A.; Muckle, Susan V.; Sauer, Richard L.

    1992-01-01

    The study develops: a triiodide solution for use in preparing ground service equipment (GSE) water for Shuttle support, an iodine dissolution method that is reliable and requires minimal time and effort to prepare, and an iodine dissolution agent with a minimal concentration of sodium salt. Sodium iodide and hydriodic acid were both found to dissolve iodine to attain the desired GSE iodine concentrations of 7.5 +/- 2.5 mg/L and 25 +/- 5 mg/L. The 1.75:1 and 2:1 sodium iodide solutions produced higher iodine recoveries than the 1.2:1 hydriodic acid solution. A two-hour preparation time is required for the three sodium iodide solutions. The 1.2:1 hydriodic acid solution can be prepared in less than 5 min. Two sodium iodide stock solutions (2.5:1 and 2:1) were found to dissolve iodine without undergoing precipitation.

  6. Method for the preparation of thallium-containing superconducting materials by precipitation

    DOEpatents

    Bunker, Bruce C.; Lamppa, Diana L.; Voigt, James A.

    1991-01-01

    This invention provides improved methods for the preparation of precursor powders that are used in the preparation of superconducting ceramic materials that contain thallium. A first solution that contains the hydrogen peroxide and metal cations, other than thallium, that will be part of the ceramic is quickly mixed with a second solution that contains precipitating anions and thallium (I) to form a precipitate which is dried to yield precursor powders. The precursor powders are calcined an sintered to produce superconducting materials that contain thallium.

  7. Method for low temperature preparation of a noble metal alloy

    DOEpatents

    Even, Jr., William R.

    2002-01-01

    A method for producing fine, essentially contamination free, noble metal alloys is disclosed. The alloys comprise particles in a size range of 5 to 500 nm. The method comprises 1. A method for preparing a noble metal alloy at low temperature, the method comprising the steps of forming solution of organometallic compounds by dissolving the compounds into a quantity of a compatible solvent medium capable of solvating the organometallic, mixing a portion of each solution to provide a desired molarity ratio of ions in the mixed solution, adding a support material, rapidly quenching droplets of the mixed solution to initiate a solute-solvent phase separation as the solvent freezes, removing said liquid cryogen, collecting and freezing drying the frozen droplets to produce a dry powder, and finally reducing the powder to a metal by flowing dry hydrogen over the powder while warming the powder to a temperature of about 150.degree. C.

  8. CTEPP STANDARD OPERATING PROCEDURE FOR PREPARATION OF SURROGATE RECOVERY STANDARD AND INTERNAL STANDARD SOLUTIONS FOR NEUTRAL TARGET ANALYTES (SOP-5.25)

    EPA Science Inventory

    This standard operating procedure describes the method used for preparing internal standard, surrogate recovery standard and calibration standard solutions for neutral analytes used for gas chromatography/mass spectrometry analysis.

  9. Preparation of highly conductive, transparent, and flexible graphene/silver nanowires substrates using non-thermal laser photoreduction

    NASA Astrophysics Data System (ADS)

    Anis, Badawi; Mostafa, A. M.; El Sayed, Z. A.; Khalil, A. S. G.; Abouelsayed, A.

    2018-07-01

    We present the preparation of highly conducting, transparent, and flexible reduced graphene oxide/silver nanowires (rGO/SNWs) substrates using non-thermal laser photoreduction method. High quality monolayers graphene oxide (GO) solution has been prepared by the chemical oxidation of thermally expanded large area natural graphite. Silver nanowires was prepared by using the typical polyol method. Uniform hybrid GO/silver nanowires (GO/SNWs) was prepared by growing the nanowires from silver nuclei in the presence of GO. Uniform and high-quality rGO/SNWs thin films were prepared using a dip-coating technique and were reduced to highly electrically conductive graphene and transparent conductive films using non-thermal laser scribe method. The laser scribed rGO/SNWs hybrid film exhibited 80% transparency with 70 Ω □-1 after 20 min of dipping in GO/SNWs solution.

  10. Enzyme stabilization by glass-derived silicates in glass-exposed aqueous solutions

    USGS Publications Warehouse

    Ives, J.A.; Moffett, J.R.; Arun, P.; Lam, D.; Todorov, T.I.; Brothers, A.B.; Anick, D.J.; Centeno, J.; Namboodiri, M.A.A.; Jonas, W.B.

    2010-01-01

    Objectives: To analyze the solutes leaching from glass containers into aqueous solutions, and to show that these solutes have enzyme activity stabilizing effects in very dilute solutions. Methods: Enzyme assays with acetylcholine esterase were used to analyze serially succussed and diluted (SSD) solutions prepared in glass and plastic containers. Aqueous SSD preparations starting with various solutes, or water alone, were prepared under several conditions, and tested for their solute content and their ability to affect enzyme stability in dilute solution. Results: We confirm that water acts to dissolve constituents from glass vials, and show that the solutes derived from the glass have effects on enzymes in the resultant solutions. Enzyme assays demonstrated that enzyme stability in purified and deionized water was enhanced in SSD solutions that were prepared in glass containers, but not those prepared in plastic. The increased enzyme stability could be mimicked in a dose-dependent manner by the addition of silicates to the purified, deionized water that enzymes were dissolved in. Elemental analyses of SSD water preparations made in glass vials showed that boron, silicon, and sodium were present at micromolar concentrations. Conclusions: These results show that silicates and other solutes are present at micromolar levels in all glass-exposed solutions, whether pharmaceutical or homeopathic in nature. Even though silicates are known to have biological activity at higher concentrations, the silicate concentrations we measured in homeopathic preparations were too low to account for any purported in vivo efficacy, but could potentially influence in vitro biological assays reporting homeopathic effects. ?? 2009 The Faculty of Homeopathy.

  11. Purification of proteins from solutions containing residual host cell proteins via preparative crystallization.

    PubMed

    Hekmat, Dariusch; Breitschwerdt, Peter; Weuster-Botz, Dirk

    2015-09-01

    To investigate quantitatively and reproducibly a scalable, preparative crystallization method in novel stirred tanks using three different protein solutions containing residual microbial host cell proteins (HCP). Lysozyme from solutions being spiked with up to 15% host cell proteins (HCP) (corresponding to 176,500 ppm) was crystallized within a 2.4-4.6 h at 93.7% yield using NaCl and glycerol. Lipase was crystallized under comparable conditions using NaCl and a mixture of two polyethylene glycols (PEG). Enhanced green fluorescent protein (eGFP) was overexpressed in E. coli yielding a solution containing 23% target protein. Residual HCP content after pre-treatment was 7-16%. eGFP was crystallized from these solutions within 1.75-4 h at 88.7% step yield using ethanol and the same mixture of two PEG as in the case of lipase. HCP contained in the solvent channels of the protein crystals could be removed by diffusive washing yielding final purities at or above 99%. Preparative crystallization can be carried out with fast kinetics and high yields from solutions containing residual impurities and may represent an attractive alternative purification method compared to preparative chromatography, especially at large production scales.

  12. Stability of levamisole oral solutions prepared from tablets and powder.

    PubMed

    Chiadmi, Fouad; Lyer, Abdel; Cisternino, Salvatore; Toledano, Audrey; Schlatter, Joël; Ratiney, Robert; Fontan, Jean-Eudes

    2005-08-12

    To study the stability of levamisole oral solutions (25 mg/mL) prepared from powder and tablets stored at 4 +/- 3 degrees C and 23 +/- 2 degrees C in amber glass prescription bottles. Levamisole 25 mg/mL solutions were prepared from commercially available 50-mg tablets or from pure powder in sterile water. Levamisole concentrations were determined in duplicate by a stability-indicating HPLC method at 0, 1, 2, 3, 4, 7, 14, 30, 60 and 90 days. The initial and final pHs of solutions were measured. The recovery of levamisole from tablets was 100 +/- 2.1%. No color or odour changes were observed during the study period. The oral solutions prepared from powder were stable at least 90 days stored at 4 and 23 degrees C. The oral solutions prepared from tablets were stable at least 90 days at 4 degrees C and 15 days when stored at 23 degrees C. The initial pH of solutions prepared from powder and tablets were 5.30 and 4.55, respectively. Initial and final pH values were significantly different (p<0.001) for the two solutions. Levamisole 25 mg/mL oral solutions can be prepared from tablets or powder with sterile water for irrigation and stored for 90 days under refrigeration, taking account of the lack of microbiological contamination.

  13. Chlorhexidine ototoxicity in ear surgery part II: survey of preparation solution used by otolaryngologists in Canada: is there a cause for concern?

    PubMed

    Lai, Philip; Coulson, Chris; Pothier, David; Rutka, John

    2011-12-01

    To conduct a survey of the antiseptic preparations used for ear surgeries among otolaryngologists in Canada. An electronic survey was sent to active members of the Canadian Society of Otolaryngology-Head and Neck Surgery via e-mail. Questions included the use of antiseptic, choice of preparation solution, duration of preparation, use of a barrier method, and compliance with hospital protocol changes. The e-mail was received by 253 otolaryngologists, and 85 completed the survey. Four of 85 respondents did not perform tympanoplasty surgery and were not included in the analysis. Of those who performed tympanoplasty (n  =  81), 78 of the 81 respondents (96%) used an antiseptic preparation solution at surgery, whereas 3 respondents (4%) did not. Sixty-six of the 77 respondents (86%) used aqueous povidone-iodine, 4 (5%) used a chlorhexidine-based preparation, 3 (4%) used an alcohol-based solution, 3 (4%) used others, and 1 answered "I don't know." Thirty-eight of 75 (29%) respondents used a barrier method, 23 (31%) answered "always," 18 (24%) answered "sometimes," and 5 (7%) answered "I don't know." When asked if they would comply with a hypothetical hospital policy to use chlorhexidine in ear surgery, 15 of 79 (19%) respondents agreed, whereas 64 (81%) disagreed. Among the aqueous povidone-iodine users (n  =  66), 7 (11%) agreed to change to chlorhexidine. There is a wide variation in practice in the use of surgical preparation solution among otolaryngologists performing ear surgery. Surgeons must be vigilant to avoid ototoxicity. A national society consensus on appropriate preparation solutions for ear surgery would minimize patients' risk and minimize future medicolegal actions.

  14. Influence of pH on optoelectronic properties of zinc sulphide thin films prepared using hydrothermal and spin coating method

    NASA Astrophysics Data System (ADS)

    Choudapur, V. H.; Bennal, A. S.; Raju, A. B.

    2018-04-01

    The ZnS nanomaterial is synthesized by hydrothermal method under optimized conditions using Zinc acetate and sodium sulphide as precursors. The Zinc Sulphide thin films are obtained by simple spin coating method with high optical transmittance. The prepared thin films are adhesive and uniform. The x-ray diffraction analysis showed that the films are polycrystalline in cubic phase with the preferred orientation along (111) direction. Current-voltage curves were recorded at room temperature using Keithley 617 programmable electrometer and conductivity is calculated for the film coated on ITO by two probe method. The pH of the solution is varied by using ammonia and hydrochloric acid. The comparative studies of effect of pH on the morphology, crystallanity and optoelectronic properties of the films are studied. It is observed that the pH of the solution has large influence on optoelectronic properties. The thin film prepared with neutral pH has higher crystallanity, bandgap and conductivity as compared to the samples prepared in acidic or basic solutions.

  15. Effects of Temperature and Method of Solution Preparation on the Performance of a Typical Red Mud Flocculent

    NASA Astrophysics Data System (ADS)

    Ferland, Pierre; Malito, John T.; Phillips, Everett C.

    Alcan International Ltd. in collaboration with Ondeo Nalco Company have carried out a fundamental study on the dissolution and performance of a 100% anionic polymer. The effects of method of preparation, solvent composition, temperature and exposure time on flocculent activity under conditions relevant to both atmospheric and pressure decantation were investigated. Flocculent activity was determined using static and dynamic settling tests, and the results were correlated with the reduced specific viscosity (RSV). For any given method of preparation of the flocculent solutions (makeup/dilution) the RSV tended to decrease with increasing solution ionic strength, independent of ionic speciation. While a significant loss in flocculent activity occurred with long exposure of the solution to high temperature, only a minor loss occurred in the short time required to flocculate and settle the mud in a decanter operating at 150 °C. Recent results in an actual plant pressure decanter appear to validate this conclusion.

  16. Kevlar reinforced neoprene composites

    NASA Technical Reports Server (NTRS)

    Penn, B. G.; Daniels, J. G.; White, W. T.; Thompson, L. M.; Clemons, L. M.

    1985-01-01

    Kevlar/neoprene composites were prepared by two techniques. One method involved the fabrication of a composite from a rubber prepreg prepared by coating Kevlar with viscous neoprene solution and then allowing the solvent to evaporate (solution impregnation technique). The second method involved heating a stack of Kevlar/neoprene sheets at a temperature sufficient to cause polymer flow (melt flow technique). There was no significant difference in the breaking strength and percent elongation for samples obtained by the two methods; however the shear strength obtained for samples fabricated by the solution impregnation technique (275 psi) was significantly higher than that found for the melt flow fabricated samples (110 psi).

  17. A Multipurpose Apparatus to Measure Viscosity and Surface Tension of Solutions: The Measurement of the Molecular Cross-Sectional Area of N-Proposal

    ERIC Educational Resources Information Center

    Xin Zhang; Shouxin Liu; Booxin Li; Na An; Fan Zhang

    2004-01-01

    A multipurpose apparatus that can be used to measure the viscosity of solution by the Ostwald method and the surface tension of solution by the drop-weight method or by the capillary-rise method is developed. The apparatus is convenient for in-situ preparation of solutions of different concentrations and avoids the error that frothing of the…

  18. Microreactor and method for preparing a radiolabeled complex or a biomolecule conjugate

    DOEpatents

    Reichert, David E; Kenis, Paul J. A.; Wheeler, Tobias D; Desai, Amit V; Zeng, Dexing; Onal, Birce C

    2015-03-17

    A microreactor for preparing a radiolabeled complex or a biomolecule conjugate comprises a microchannel for fluid flow, where the microchannel comprises a mixing portion comprising one or more passive mixing elements, and a reservoir for incubating a mixed fluid. The reservoir is in fluid communication with the microchannel and is disposed downstream of the mixing portion. A method of preparing a radiolabeled complex includes flowing a radiometal solution comprising a metallic radionuclide through a downstream mixing portion of a microchannel, where the downstream mixing portion includes one or more passive mixing elements, and flowing a ligand solution comprising a bifunctional chelator through the downstream mixing portion. The ligand solution and the radiometal solution are passively mixed while in the downstream mixing portion to initiate a chelation reaction between the metallic radionuclide and the bifunctional chelator. The chelation reaction is completed to form a radiolabeled complex.

  19. URANIUM PURIFICATION PROCESS

    DOEpatents

    Winters, C.E.

    1957-11-12

    A method for the preparation of a diethyl ether solution of uranyl nitrate is described. Previously the preparation of such ether solutions has been difficult and expensive, since crystalline uranyl nitrate hexahydrate dissolves very slowly in ether. An improved method for effecting such dissolution has been found, and it comprises adding molten uranyl nitrate hexahydrate at a temperature of 65 to 105 deg C to the ether while maintaining the temperature of the ether solvent below its boiling point.

  20. Preparation of fullerene/glass composites

    DOEpatents

    Mattes, Benjamin R.; McBranch, Duncan W.; Robinson, Jeanne M.; Koskelo, Aaron C.; Love, Steven P.

    1995-01-01

    Synthesis of fullerene/glass composites. A direct method for preparing solid solutions of C.sub.60 in silicon dioxide (SiO.sub.2) glass matrices by means of sol-gel chemistry is described. In order to produce highly concentrated fullerene-sol-gel-composites it is necessary to increase the solubility of these "guests" in a delivery solvent which is compatible with the starter sol (receiving solvent). Sonication results in aggregate disruption by treatment with high frequency sound waves, thereby accelerating the rate of hydrolysis of the alkoxide precursor, and the solution process for the C.sub.60. Depending upon the preparative procedure, C.sub.60 dispersed within the glass matrix as microcrystalline domains, or dispersed as true molecular solutions of C.sub.60 in a solid glass matrix, is generated by the present method.

  1. Preparation of fullerene/glass composites

    DOEpatents

    Mattes, B.R.; McBranch, D.W.; Robinson, J.M.; Koskelo, A.C.; Love, S.P.

    1995-05-30

    Synthesis of fullerene/glass composites is described. A direct method for preparing solid solutions of C{sub 60} in silicon dioxide (SiO{sub 2}) glass matrices by means of sol-gel chemistry is described. In order to produce highly concentrated fullerene-sol-gel-composites it is necessary to increase the solubility of these ``guests`` in a delivery solvent which is compatible with the starter sol (receiving solvent). Sonication results in aggregate disruption by treatment with high frequency sound waves, thereby accelerating the rate of hydrolysis of the alkoxide precursor, and the solution process for the C{sub 60}. Depending upon the preparative procedure, C{sub 60} dispersed within the glass matrix as microcrystalline domains, or dispersed as true molecular solutions of C{sub 60} in a solid glass matrix, is generated by the present method.

  2. Simplified Method for Preparing Methylene-Blue-Sensitized Dichromated Gelatin

    NASA Astrophysics Data System (ADS)

    Kurokawa, Kazumasa; Koike, Satoshi; Namba, Sinji; Mizuno, Toru; Kubota, Toshihiro

    1998-05-01

    Methylene-blue-sensitized dichromated gelatin (MBDCG) is a suitable material for recording full-color holograms in a single layer. However, a drying process in an ammonia atmosphere is necessary to prepare the MBDCG plate. This process is time-consuming and unstable. A simplified method for preparing the MBDCG plate is presented in which the MBDCG can be dried without ammonia. Elimination of the drying process is possible when the methylene blue in MBDCG does not separate. This is achieved by a decrease in the concentration of dichromate in the photosensitized solution and the addition of an ammonia solution to the photosensitized solution. Last, the gelatin is allowed to gel. A Lippmann color hologram grating with a diffraction efficiency of more than 80% is obtained by use of this MBDCG.

  3. Preparation and Analysis of Solid Solutions in the Potassium Perchlorate-Permanganate System.

    ERIC Educational Resources Information Center

    Johnson, Garrett K.

    1979-01-01

    Describes an experiment, designed for and tested in an advanced inorganic laboratory methods course for college seniors and graduate students, that prepares and analyzes several samples in the nearly ideal potassium perchlorate-permanganate solid solution series. The results are accounted for by a theoretical treatment based upon aqueous…

  4. METHOD FOR PREPARING URANIUM MONOCARBIDE-PLUTONIUM MONOCARBIDE SOLID SOLUTION

    DOEpatents

    Ogard, A.E.; Leary, J.A.; Maraman, W.J.

    1963-03-19

    A method is given for preparing solid solutions of uranium monocarbide- plutonium monocarbide. In this method, the powder form of uranium dioxide, plutonium dioxide, and graphite are mixed in a ratio determined by the equation: xUO/sub 2/ + yPuO/sub 2/ + (2+z)C yields UxPu/sub y/C/sub z/ +2CO, where x + y equ al 1.0 and z is greater than 0.9 but less than 1.0. The resulting mixture is compacted and heated in a vacuum at a temperature of 1850 deg C. (AEC)

  5. Construction of super - hydrophobic copper alloy surface by one - step mixed solution immersion method

    NASA Astrophysics Data System (ADS)

    Gu, Qiang; Chen, Ying; Chen, Dong; Zhang, Zeting

    2018-01-01

    This paper presents a method for preparing a super hydrophobic surface with a fast, simple, low-cost, one-step reaction by immersing copper alloy in an ethanol solution containing silver nitrate and myristic acid. The effects of reaction time, reaction temperature, reactant concentration and reaction time on the wettability of the material were studied. The surface wettability, appearance, chemical composition, durability and chemical stability of the prepared samples was measured by water contact angle (CA), scanning electron microscopy (SEM), energy dispersive spectrometer (EDS), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). The results show that when the reaction time is only 10min, the surface WCA of the prepared material can reach 154.9. This study provides an effective method for the rapid preparation of stable super hydrophobic surfaces.

  6. Properties of ZnO nanocrystals prepared by radiation method

    NASA Astrophysics Data System (ADS)

    Čuba, Václav; Gbur, Tomáš; Múčka, Viliam; Nikl, Martin; Kučerková, Romana; Pospíšil, Milan; Jakubec, Ivo

    2010-01-01

    Zinc oxide nanoparticles were prepared by irradiation of aqueous solutions containing zinc(II) ions, propan-2-ol, polyvinyl alcohol, and hydrogen peroxide. Zinc oxide was found in solid phase either directly after irradiation, or after additional heat treatment. Various physicochemical parameters, including scintillation properties of prepared materials, were studied. After decomposition of impurities and annealing of oxygen vacancies, the samples showed intensive emission in visible spectral range and well-shaped exciton luminescence at 390-400 nm. The best scintillating properties had zinc oxide prepared from aqueous solutions containing zinc formate as initial precursor and hydrogen peroxide. Size of the crystalline particles ranged from tens to hundreds nm, depending on type of irradiated solution and post-irradiation thermal treatment.

  7. Method for preparation of thermally and mechanically stable metal/porous substrate composite membranes

    DOEpatents

    Damle, Ashok S.

    2004-07-13

    A method is provided for the preparation of metal/porous substrate composite membranes by flowing a solution of metal to be plated over a first surface of a porous substrate and concurrently applying a pressure of gas on a second surface of the porous substrate, such that the porous substrate separates the solution of metal from the gas, and the use of the resulting membrane for the production of highly purified hydrogen gas.

  8. Preparation and Characterization of Cabamazepine Cocrystal in Polymer Solution.

    PubMed

    Zhang, Hao; Zhu, Ying; Qiao, Ning; Chen, Yang; Gao, Linghuan

    2017-12-01

    In this study, we attempted to prepare carbamazepine (CBZ) cocrystal through the solution method in ethanol-water solvent mixture (volume ratio 1:1) and polyvinyl pyrrolidone (PVP) solution. Nicotinamide (NIC) and saccharin (SAC) were selected as cocrystal coformers. Cocrystal screening products were characterized by Fourier Transform Infrared Spectroscopy (FTIR), Differential Scanning Calorimetry (DSC), and Powder X-ray Diffraction (PXRD) techniques. Characterization results show that in ethanol-water solvent mixture, pure CBZ-NIC cocrystal can be prepared, while CBZ-SAC cocrystal cannot be obtained. The addition of PVP can inhibit CBZ-NIC cocrystal formation and facilitate CBZ-SAC cocrystal formation.

  9. Preparation and Characterization of Carbamazepine Cocrystal in Polymer Solution

    PubMed Central

    Zhang, Hao; Zhu, Ying; Chen, Yang; Gao, Linghuan

    2017-01-01

    In this study, we attempted to prepare carbamazepine (CBZ) cocrystal through the solution method in ethanol-water solvent mixture (volume ratio 1:1) and polyvinyl pyrrolidone (PVP) solution. Nicotinamide (NIC) and saccharin (SAC) were selected as cocrystal coformers. Cocrystal screening products were characterized by Fourier Transform Infrared Spectroscopy (FTIR), Differential Scanning Calorimetry (DSC), and Powder X-ray Diffraction (PXRD) techniques. Characterization results show that in ethanol-water solvent mixture, pure CBZ-NIC cocrystal can be prepared, while CBZ-SAC cocrystal cannot be obtained. The addition of PVP can inhibit CBZ-NIC cocrystal formation and facilitate CBZ-SAC cocrystal formation. PMID:29194387

  10. Conducting Compositions of Matter

    NASA Technical Reports Server (NTRS)

    Viswanathan, Tito (Inventor)

    1999-01-01

    The invention provides conductive compositions of matter, as well as methods for the preparation of the conductive compositions of matter, solutions comprising the conductive compositions of matter, and methods of preparing fibers or fabrics having improved anti-static properties employing the conductive compositions of matter.

  11. Conducting Compositions of Matter

    NASA Technical Reports Server (NTRS)

    Viswanathan, Tito (Inventor)

    2001-01-01

    The invention provides conductive compositions of matter, as well as methods for the preparation of the conductive compositions of matter, solutions comprising the conductive compositions of matter, and methods of preparing fibers or fabrics having improved anti-static properties employing the conductive compositions of matter.

  12. Conducting compositions of matter

    NASA Technical Reports Server (NTRS)

    Viswanathan, Tito (Inventor)

    2000-01-01

    The invention provides conductive compositions of matter, as well as methods for the preparation of the conductive compositions of matter, solutions comprising the conductive compositions of matter, and methods of preparing fibers or fabrics having improved anti-static properties employing the conductive compositions of matter.

  13. Resistivity behavior of optimized PbTiO3 thin films prepared by spin coating method

    NASA Astrophysics Data System (ADS)

    Nurbaya, Z.; Wahid, M. H.; Rozana, M. D.; Alrokayan, S. A. H.; Khan, H. A.; Rusop, M.

    2018-05-01

    Th is study presents the resistivity behavior of PbTiO3 thin films which were prepared towards metal-insulator-metal capacitor device fabrication. The PbTiO3 thin films were prepared through sol-gel spin coating method that involved various deposition parameters that is (1) different molar concentration of PbTiO3 solutions, (2) various additional PbAc-content in PbTiO3 solutions, and (3) various annealing temperature on PbTiO3 thin films. Hence, an electrical measurement of current versus voltage was done to determine the resistivity behavior of PbTiO3 thin films.

  14. Epitaxial ternary nitride thin films prepared by a chemical solution method

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

    Luo, Hongmei; Feldmann, David M; Wang, Haiyan

    2008-01-01

    It is indispensable to use thin films for many technological applications. This is the first report of epitaxial growth of ternary nitride AMN2 films. Epitaxial tetragonal SrTiN2 films have been successfully prepared by a chemical solution approach, polymer-assisted deposition. The structural, electrical, and optical properties of the films are also investigated.

  15. Preparation and the influencing factors of timozolomide liposomes.

    PubMed

    Kong, Bin; Sun, Yong; Li, Yongjian; Hu, Dejian

    2009-01-01

    To prepare timozolomide liposomes for administration through nasal mucous membrane, we studied the factors of the preparation of the liposomes. The timozolomide liposomes were prepared by the ammonium sulphate gradient method; electroscopy and laser particle analyzer were utilized to determine the conformation, size and distribution of timozolomide liposomes; high performance liquid chromatography (HPLC) was applied to determine the entrapping efficiency of timozolomide liposomes; then we studied the influences of the concentration of ammonium sulphate solution, temperature, and the drug-to-lipid ratio on the entrapping efficiency. The average size of timozolomide liposomes was 185 nm; the entrapping efficiency was 90.3%. The entrapping efficiency was enhanced with the increasing of the concentration of ammonium sulphate solution and the rising of temperature, and decreased with the increasing of the drug-to-lipid ratio. The timozolomide liposomes with high entrapping efficiency, small and even particle sizes could be prepared by the simple and convenient ammonium sulphate gradient method. The primary influencing factors on the entrapping efficiency of timozolomide liposomes were the concentration of ammonium sulphate solution, the temperature, and the drug-to-lipid ratio.

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

    Ivanov, Ilia N.; Simpson, John T.

    A method of preparing a network comprises disposing a solution comprising particulate materials in a solvent onto a superhydrophobic surface comprising a plurality of superhydrophobic features and interfacial areas between the superhydrophobic features. The plurality of superhydrophobic features has a water contact angle of at least about 150.degree.. The method of preparing the network also comprises removing the solvent from the solution of the particulate materials, and forming a network of the particulate materials in the interfacial areas, the particulate materials receding to the interfacial areas as the solvent is removed.

  17. Lithium-Air Battery: Study of Rechargeability and Scalability

    DTIC Science & Technology

    2012-07-01

    nanowires: MnO2 nanowires were prepared by hydrothermal method. In a typical procedure, an aqueous solution of KMnO4 (0.5 g KMnO4 in 60 ml DD water) was...reduction and oxygen evolution in Li-O2 cell. It was prepared by precipitation method, in which cerium source precipitated as cerium oxalate and...subsequent calcinations yield CeO2 nanoparticles. In a typical procedure, 0.15 M cerous nitrate solution was added drop wise to 1.5 M ammonium oxalate

  18. Effect of Preparation Methods on Crystallization Behavior and Tensile Strength of Poly(vinylidene fluoride) Membranes

    PubMed Central

    Liu, Jie; Lu, Xiaolong; Wu, Chunrui

    2013-01-01

    Poly(vinylidene fluoride) (PVDF) membranes were prepared by non solvent induced phase separation (NIPS), melt spinning and the solution-cast method. The effect of preparation methods with different membrane formation mechanisms on crystallization behavior and tensile strength of PVDF membranes was investigated. Fourier transform infrared spectroscopy-attenuated total reflectance (FTIR-ATR) and X-ray diffraction (XRD) were employed to examine the crystal form of the surface layers and the overall membranes, respectively. Spherulite morphologies and thermal behavior of the membranes were studied by polarized light optical microscopy (PLO) and differential scanning calorimetry (DSC) separately. It was found that the crystallization behavior of PVDF membranes was closely related to the preparation methods. For membranes prepared by the NIPS method, the skin layers had a mixture of α and β phases, the overall membranes were predominantly α phase, and the total crystallinity was 60.0% with no spherulite. For melt spinning membranes, the surface layers also showed a mixture of α and β phases, the overall membranes were predominantly α phase. The total crystallinity was 48.7% with perfect spherulites. Whereas the crystallization behavior of solution-cast membranes was related to the evaporation temperature and the additive, when the evaporation temperature was 140 °C with a soluble additive in the dope solution, obvious spherulites appeared. The crystalline morphology of PVDF exerted a great influence on the tensile strength of the membranes, which was much higher with perfect spherulites. PMID:24957064

  19. A new method for the radiochemical purity measurement of ¹¹¹In-pentetreotide.

    PubMed

    Salgado-Garcia, Carlos; Montoza-Aguado, Manuel; Luna-Alcaide, Ana B; Segovia-Gonzalez, Maria M; de Mora, Elena Sanchez; Lopez-Martin, Juana; Ramos-Font, Carlos; Jimenez-Heffernan, Amelia

    2011-12-01

    The recommended method for the measurement of radiochemical purity (RCP) of ¹¹¹In-labelled pentetreotide is thin-layer chromatography with a silica gel as the stationary phase and a 0.1 N sodium citrate solution (pH 5) as the mobile phase. According to the supplier's instructions, the mobile phase must be prepared before the test is carried out, and the recommended stationary phase is off-market. We propose a new method for RCP measurement in which the mobile phase is acid citrate dextrose, solution A, which does not need to be prepared beforehand, and thin-layer chromatography is performed with a silica gel-impregnated glass fibre sheet as the stationary phase. We used both methods to measure the percentages of radiopharmaceutical and impurities. The range of RCP values obtained was 98.0-99.9% (mean=99.3%) by the standard method and 98.1-99.9% (mean=99.2%) by the new method. We observed no differences between the RCP values of both methods (P=0.070). The proposed method is suitable for RCP testing because it yields results that are in good agreement with those of the standard method and because it is easier to perform as the mobile-phase solution need not be prepared in advance.

  20. Novel silk fibroin films prepared by formic acid/hydroxyapatite dissolution method.

    PubMed

    Ming, Jinfa; Liu, Zhi; Bie, Shiyu; Zhang, Feng; Zuo, Baoqi

    2014-04-01

    Bombyx mori silk fibroin from the silkworm was firstly found to be soluble in formic acid/hydroxyapatite system. The rheological behavior of silk fibroin solution was significantly influenced by HAp contents in dissolved solution. At the same time, silk fibroin nanofibers were observed in dissolved solution with 103.6±20.4nm in diameter. Moreover, the structure behavior of SF films prepared by formic acid/hydroxyapatite dissolution method was examined. The secondary structure of silk fibroin films was attributed to silk II structure (β-sheet), indicating that the hydroxyapatite contents in dissolved solution were not significantly affected by the structure of silk fibroin. The X-ray diffraction results exhibited obviously hydroxyapatite crystalline nature existing in silk fibroin films; however, when the hydroxyapatite content was 5.0wt.% in dissolved solution, some hydroxyapatite crystals were converted to calcium hydrogen phosphate dehydrate in silk fibroin dissolution process. This result was also confirmed by Fourier transform infrared analysis and DSC measurement. In addition, silk fibroin films prepared by this dissolution method had higher breaking strength and extension at break. Based on these analyses, an understanding of novel SF dissolution method may provide an additional tool for designing and synthesizing advanced materials with more complex structures, which should be helpful in different fields, including biomaterial applications. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Method for liquid chromatographic extraction of strontium from acid solutions

    DOEpatents

    Horwitz, E. Philip; Dietz, Mark L.

    1992-01-01

    A method and apparatus for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column is described. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water.

  2. Solution-mediated cladding doping of commercial polymer optical fibers

    NASA Astrophysics Data System (ADS)

    Stajanca, Pavol; Topolniak, Ievgeniia; Pötschke, Samuel; Krebber, Katerina

    2018-03-01

    Solution doping of commercial polymethyl methacrylate (PMMA) polymer optical fibers (POFs) is presented as a novel approach for preparation of custom cladding-doped POFs (CD-POFs). The presented method is based on a solution-mediated diffusion of dopant molecules into the fiber cladding upon soaking of POFs in a methanol-dopant solution. The method was tested on three different commercial POFs using Rhodamine B as a fluorescent dopant. The dynamics of the diffusion process was studied in order to optimize the doping procedure in terms of selection of the most suitable POF, doping time and conditions. Using the optimized procedure, longer segment of fluorescent CD-POF was prepared and its performance was characterized. Fiber's potential for sensing and illumination applications was demonstrated and discussed. The proposed method represents a simple and cheap way for fabrication of custom, short to medium length CD-POFs with various dopants.

  3. Intranasal scopolamine preparation and method

    NASA Technical Reports Server (NTRS)

    Putcha, Lakshmi (Inventor); Cintron, Nitza M. (Inventor)

    1991-01-01

    A new method and preparation for intranasal delivery of scopolamine provides a safe and effective treatment for motion sickness and other conditions requiring anticholinergic therapy. The preparation can be in the form of aqueous nasal drops, mist spray, gel or oinment. Intranasal delivery of scopolamine has similar bioavailability and effect of intravenous delivery and is far superior to oral dosage. Scopolamine is prepared in a buffered saline solution at the desired dosage rate for effective anticholinergic response.

  4. Fabrications of Polyaniline Films by Pulse Electrodeposition in Acidic Solutions with Different Anions and Their Thermoelectric Performances

    NASA Astrophysics Data System (ADS)

    Yang, Weifang; Xu, Han; Li, Yuanyuan; Wang, Wei

    2017-08-01

    Polymerization of aniline was prepared by the pulse potentiostatic method in H3PO4, HClO4 and H2SO4 acidic solutions. The morphologies and thermoelectric performances were analyzed by scanning electron microscopy, Seebeck coefficient ( S) and resistivity ( R) measurements. The results show that flake polyaniline (PANI) films can be obtained in H3PO4 and HClO4 acidic solutions, and porous PANI films with nanofiber-overlapped structures can be prepared in H2SO4 solution under the same pulse parameters. PANI films prepared in the three solutions are all p-type thermoelectric materials. PANI films polymerized in H2SO4 solution possess the highest S (30.2 μV K-1) and lowest R (1.6 × 10-3 Ω m) compared with those prepared in H3PO4 and HClO4 solutions, indicating that nanofiber-overlapped structures formed in H2SO4 solution contribute better thermoelectric performance. In addition, the effects of pulse parameters (anodic potential φ a, anodic pulse duration t a and cathodic pulse duration t c) on the surface morphologies and thermoelectric performances of PANI films were systematically investigated.

  5. Method for producing microcomposite powders using a soap solution

    DOEpatents

    Maginnis, Michael A.; Robinson, David A.

    1996-01-01

    A method for producing microcomposite powders for use in superconducting and non-superconducting applications. A particular method to produce microcomposite powders for use in superconducting applications includes the steps of: (a) preparing a solution including ammonium soap; (b) dissolving a preselected amount of a soluble metallic such as silver nitrate in the solution including ammonium soap to form a first solution; (c) adding a primary phase material such as a single phase YBC superconducting material in particle form to the first solution; (d) preparing a second solution formed from a mixture of a weak acid and an alkyl-mono-ether; (e) adding the second solution to the first solution to form a resultant mixture; (f) allowing the resultant mixture to set until the resultant mixture begins to cloud and thicken into a gel precipitating around individual particles of the primary phase material; (g) thereafter drying the resultant mixture to form a YBC superconducting material/silver nitrate precursor powder; and (h) calcining the YBC superconducting material/silver nitrate precursor powder to convert the silver nitrate to silver and thereby form a YBC/silver microcomposite powder wherein the silver is substantially uniformly dispersed in the matrix of the YBC material.

  6. Preparation of ethylenediamine dinitrate

    DOEpatents

    Lee, Kien-yin

    1985-01-01

    Method for the preparation of ethylenediamine dinitrate. Ethylenediamine dinitrate, a useful explosive, may readily be prepared by solvent extraction of nitrate ion from an acidic aqueous solution thereof using a high-molecular-weight, water-insoluble amine dissolved in an organic solvent, and reacting the resulting organic solution with ethylenediamine. The process of the instant invention avoids the use of concentrated nitric acid, as is currently practiced, resulting in a synthesis which is far less hazardous especially for large quantities of the explosive, and more efficient.

  7. Preparation of ethylenediamine dinitrate

    DOEpatents

    Lee, K.

    1984-05-17

    Method for the preparation of ethylenediamine dinitrate. Ethylenediamine dinitrate, a useful explosive, may readily be prepared by solvent extraction of nitrate ion from an acidic aqueous solution thereof using a high-molecular-weight, water-insoluble amine dissolved in an organic solvent, and reacting the resulting oraganic solution with ethylenediamine. The process of the instant invention avoids the use of concentrated nitric acid, as is currently practiced, resulting in a synthesis which is far less hazardous, especially for large quantities of the explosive, and more efficient.

  8. 75 FR 1650 - Notice of Intent To Prepare an Environmental Impact Statement for the Proposed HB Potash, LLC-“In...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-01-12

    ...] Notice of Intent To Prepare an Environmental Impact Statement for the Proposed HB Potash, LLC--``In-Situ... HB Potash, LLC--``In- Situ'' Solution Mine Project by any of the following methods: E-mail: Rebecca..., (Intrepid) is proposing to construct and operate an ``in-situ'' solution mining project that would involve...

  9. FC and ZFC magnetic properties of ferro-spinels (MFe2O4) prepared by solution-combustion method

    NASA Astrophysics Data System (ADS)

    Aravind, G.; Kumar, R. Vijaya; Nathaniyal, V.; Rambabu, T.; Ravinder, D.

    2017-07-01

    Magnetic ferro-spinels MFe2O4 (M= Co and Ni) prepared by citrate-gel solution combustion method using metal nitrates with low sintering temperature (500°C). From the XRD and TEM studies confirm that a nano crystalline nature of the prepared samples. Field Cooled (FC) and Zero Field Cooled (ZFC) magnetic studies of the prepared ferro-spinels are measured by using vibrating sample magnetometer (VSM). The resultant magnetization of the prepared samples as a function of an applied magnetic field 10 T was measured at two different temperatures 5 K and 310 K. Field Cooled (FC) and Zero Field Cooled (ZFC) magnetization measurements under an applied field of 100 Oe and 1000 Oe in the temperature range of 5-375 K were carried out, which shows the blocking temperature of these two samples at around 350 K.

  10. PREPARATION OF URANIUM TRIOXIDE

    DOEpatents

    Buckingham, J.S.

    1959-09-01

    The production of uranium trioxide from aqueous solutions of uranyl nitrate is discussed. The uranium trioxide is produced by adding sulfur or a sulfur-containing compound, such as thiourea, sulfamic acid, sulfuric acid, and ammonium sulfate, to the uranyl solution in an amount of about 0.5% by weight of the uranyl nitrate hexahydrate, evaporating the solution to dryness, and calcining the dry residue. The trioxide obtained by this method furnished a dioxide with a considerably higher reactivity with hydrogen fluoride than a trioxide prepared without the sulfur additive.

  11. Method of solution preparation of polyolefin class polymers for electrospinning processing included

    NASA Technical Reports Server (NTRS)

    Rabolt, John F. (Inventor); Givens, Steven R. (Inventor); Lee, Keun-Hyung (Inventor)

    2011-01-01

    A process to make a polyolefin fiber which has the following steps: mixing at least one polyolefin into a solution at room temperature or a slightly elevated temperature to form a polymer solution and electrospinning at room temperature said polymer solution to form a fiber.

  12. Method for forming energetic nanopowders

    DOEpatents

    Lee, Kien-Yin; Asay, Blaine W.; Kennedy, James E.

    2013-10-15

    A method for the preparation of neat energetic powders, having nanometer dimensions, is described herein. For these neat powder, a solution of a chosen energetic material is prepared in an aprotic solvent and later combined with liquid hexane that is miscible with such solvent. The energetic material chosen is less soluble in the liquid hexane than in the aprotic solvent and the liquid hexane is cooled to a temperature that is below that of the solvent solution. In order to form a precipitate of said neat powders, the solvent solution is rapidly combined with the liquid hexane. When the resulting precipitate is collected, it may be dried and filtered to yield an energetic nanopowder material.

  13. Preparation of zein fibers using solution blow spinning method

    USDA-ARS?s Scientific Manuscript database

    Zein fibers were successfully fabricated via solution blow spinning (SBS) using acetic acid as solvent. Surface tension, viscosity and modulus of zein solutions were respectively determined by force tensiometer and rheometer. Increases of these properties were observed with an increase of concentrat...

  14. Ocular Dorzolamide Nanoliposomes for Prolonged IOP Reduction: in-vitroand in-vivo Evaluation in Rabbits

    PubMed Central

    Kouchak, Maryam; Bahmandar, Reza; Bavarsad, Neda; Farrahi, Fereydoun

    2016-01-01

    Dorzolamide ophthalmic drop is one of the most common glaucoma medications but it has a short residence time in the eye. The aim of this study is to develop ocular dorzolamide HCl nanoliposomes (DRZ – nanoliposomes) and to evaluate their potential use for the treatment of ocular hypertension. Nanoliposomes were prepared using Reverse-phase evaporation vesicle (REV) and thin layer hydration (TLH) method with 7:3 and 7:4 molar ratios of phosphatidylcholine:cholesterol. The physicochemical properties of the formulations were investigated. Formulations with 7:4 lipid ratios were evaluated in terms of drug release, physical stability and ex-vivo permeation through the excised albino rabbit cornea. The rabbits in groups of 6 were treated with selected DRZ – nanoliposomes or dorzolamide solution or marketed dorzolamid preparation (Biosopt®) and intraocular pressure (IOP) was monitored. Formulations with 7:4 molar ratio entrapped greater amount of drug compared to those with 7:3 lipid components ratio. DRZ – nanoliposomes with 7:4 lipid ratio showed more transcorneal permeation than Dorzolamide solution (p<0.05); and the formulation prepared by TLH method exhibited higher permeability than that prepared by REV method (p<0.05). The selected DRZ – nanoliposomes showed greater IOP lowering activity and a more prolonged effect compared to dorzolamide solution and Biosopt®. DRZ – nanoliposomes prepared by TLH method with 7:4 ratios showed promising results as a candidate for the treatment of ocular hypertension. PMID:27610160

  15. Method for preparing membranes with adjustable separation performance

    DOEpatents

    Peterson, E.S.; Orme, C.J.; Stone, M.L.

    1995-01-31

    Methods for adjustable separation of solutes and solvents involve the combination of the use of a maximally swollen membrane and subsequent vacuum depressurization exerted on the permeate side of that membrane. By adjusting the extent of depressurization it is possible to separate solvent from solutes and solutes from each other. Improved control of separation parameters as well as improved flux rates characterize the present invention. 2 figs.

  16. Method for preparing membranes with adjustable separation performance

    DOEpatents

    Peterson, Eric S.; Orme, Christopher J.; Stone, Mark L.

    1995-01-01

    Methods for adjustable separation of solutes and solvents involve the combination of the use of a maximally swollen membrane and subsequent vacuum depressurization exerted on the permeate side of that membrane. By adjusting the extent of depressurization it is possible to separate solvent from solutes and solutes from each other. Improved control of separation parameters as well as improved flux rates characterize the present invention.

  17. Arsenic sulfide layers for dielectric reflection mirrors prepared from solution

    NASA Astrophysics Data System (ADS)

    Matějec, Vlastimil; Pedlikova, Jitka; BartoÅ, Ivo; Podrazký, Ondřej

    2017-12-01

    Chalcogenide materials due to high refractive indices, transparency in the mid-IR spectral region, nonlinear refractive indices, etc, have been employed as fibers and films in different photonic devices such as light amplifiers, optical regenerators, broadband radiation sources. Chalcogenide films can be prepared by physical methods as well as by solution-based techniques in which solutions of chalcogenides in amines are used. This paper presents results on the solution-based fabrication and optical characterization of single arsenic sulfide layers and multilayer stacks containing As2S3 layers together with porous silica layers coated on planar and fiber-optic substrates. Input As2S3 solutions for the layer fabrications were prepared by dissolving As2S3 powder in n-propylamine in a concentration of 0.50 mol/l. These solutions were applied on glass slides by dip-coating method and obtained layers were thermally treated in vacuum at temperatures up to 180 °C. Similar procedure was used for As2S3 layers in multilayer stacks. Such stacks were fabricated by repeating the application of one porous silica layer prepared by the sol-gel method and one As2S3 layer onto glass slides or silica fibers (a diameter of 0.3 mm) by using the dip-coating method. It has been found that the curing process of the applied layers has to be carefully controlled in order to obtain stacks with three pairs of such layers. Single arsenic and porous silica layers were characterized by optical microscopy, and by measuring their transmission spectra in a range of 200-2500 nm. Thicknesses and refractive indices were estimated from the spectra. Transmission spectra of planar multilayer stacks were measured, too. Interference bands have been determined from optical measurements on the multilayer stacks with a minimum transmittance of about 50% which indicates the possibility of using such stacks as reflecting mirrors.

  18. Preparation and characterisation of hydrocortisone particles using a supercritical fluids extraction process.

    PubMed

    Velaga, Sitaram P; Ghaderi, Raouf; Carlfors, Johan

    2002-01-14

    Crystallisation and subsequent milling of pharmaceutical powders by traditional methods often cause variations in physicochemical properties thereby influencing bioavailability of the formulation. Crystallisation of drug substances using supercritical fluids (SFs) offers some advantages over existing traditional methods in controlling particle characteristics. The novel particle formation method, solution enhanced dispersion by supercritical (SEDS) fluids was used for the preparation of hydrocortisone (HC) particles. The influence of processing conditions on the solid-state properties of the particles was studied. HC, an anti-inflammatory corticosteroid, particles were prepared from acetone and methanol solutions using the SEDS process. The solutions were dispersed with supercritical CO(2), acting as an anti-solvent, through a specially designed co-axial nozzle into a pressured vessel maintained at a specific constant temperature and pressure. The temperatures and pressures studied were 40-90 degrees C and 90-180 bar, respectively. The relative flow rates of drug solution to CO(2) were varied between 0.002 and 0.03. Solid-state characterisation of particles included differential scanning calorimetry (DSC), X-ray powder diffraction (XRPD), solubility studies and scanning electron microscopy (SEM) examination. The aerodynamic properties of SEDS prepared particles were determined by a multistage liquid impinger (MLI). Particles produced from acetone solutions were crystalline needles, melting at 221+/-2 degrees C. Their morphology was independent of processing conditions. With methanol solutions, particles were flakes or needles depending on the processing temperature and pressure. This material melted at 216+/-1 degrees C, indicating a different crystal structure from the original material, in agreement with observed differences in the position and intensity of the XRPD peaks. The simulated lung deposition, using the MLI, for HC powder was improved after SEDS processing. It was possible to produce and control the crystallinity, morphology, and aerodynamic properties of HC particles with the SEDS technique. This method may be useful for the processing of inhalation powders.

  19. CuIn(S,Se)(2) thin films prepared from a novel thioacetic acid-based solution and their photovoltaic application.

    PubMed

    Xie, Yian; Liu, Yufeng; Wang, Yaoming; Zhu, Xiaolong; Li, Aimin; Zhang, Lei; Qin, Mingsheng; Lü, Xujie; Huang, Fuqiang

    2014-04-28

    Low-cost and high-yield preparation of CuInSe2 films is the bottleneck for promising CuInSe2-based thin film solar cells. Here, we developed a simple, safe and cost-effective method using thioacetic acid to fabricate the absorber films of CuIn(S,Se)2 (CISSe). Dissolution of Cu2O and In(OH)3 in thioacetic acid was attributed to the strong coordination ability of S. The adhesive precursor solution can be prepared without any heating, centrifugation and inert gas protection, superior to the previously reported methods. The precursor CISSe layer was easily deposited in air by spin coating to ensure low cost. Uniform and compact CISSe thin films with well-crystallized and pure-phased CISSe grains were obtained after one step annealing. The as-prepared CISSe thin films were successfully applied to solar cells and a energy conversion efficiency of 6.75% was achieved. This facile preparation provides a low-cost and easy method to fabricate Cu-based thin film solar cells.

  20. Effect of gamma radiation on the physico-chemical properties of alginate-based films and beads

    NASA Astrophysics Data System (ADS)

    Huq, Tanzina; Khan, Avik; Dussault, Dominic; Salmieri, Stephane; Khan, Ruhul A.; Lacroix, Monique

    2012-08-01

    Alginate solution (3%, w/v) was prepared using deionized water from its powder. Then the solution was exposed to gamma radiation (0.1-25 kGy). The alginate films were prepared by solution casting. It was found that gamma radiation has strong effect on alginate solution. At low doses, mechanical strength of the alginate films improved but after 5 kGy dose, the strength started to decrease. The mechanism of alginate radiolysis in aqueous solution is discussed. Film formation was not possible from alginate solution at doses >5 kGy. The mechanical properties such as puncture strength (PS), puncture deformation (PD), viscoelasticity (Y) coefficient of the un-irradiated films were investigated. The values of PS, PD and Y coefficient of the films were 333 N/mm, 3.20 mm and 27%, respectively. Alginate beads were prepared from 3% alginate solution (w/v) by ionotropic gelation method in 5% CaCl2 solution. The rate of gel swelling improved in irradiated alginate-based beads at low doses (up to 0.5 kGy).

  1. Preparation and storage of isotopically labeled reduced nicotinamide adenine dinucleotide

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

    Northrop, D.B.; Duggleby, R.G.

    1987-09-01

    A method for obtaining highly purified NADH in a dry, solid, and stable form is described. The method involves improvements of the ion-exchange and reversed-phase chromatographic procedures of C. J. Newton and S. M. Faynor, and D. B. Northrop. The necessary time to prepare pure NADH has been reduced to a few hours. The final product, obtained by drying the nucleotide from absolute ethanol, shows no detectable decomposition either during the drying procedure or during storage under nitrogen gas at -20 degrees C for several months. Using dry product prepared from fixed volumes of ethanolic solution, standardized solutions of knownmore » amounts of the highly purified and stored NADH can be obtained in a few seconds.« less

  2. How-To-Do-It: Using Cauliflower to Demonstrate Plant Tissue Culture.

    ERIC Educational Resources Information Center

    Haldeman, Janice H.; Ellis, Jane P.

    1988-01-01

    Presents techniques used for disinfestation of plant material, preparation of equipment and media, and laboratory procedures for tissue culture using cauliflower. Details methods for preparing solutions and plant propagation by cloning. (CW)

  3. Synthesis and Reactivity of a New (Methylene)Phosphine.

    DTIC Science & Technology

    1981-01-27

    the synthesis of a variety of alkyl(silylamino)- 8phosphines Similarly, if two equivalents of the silylmethyl Grignard reagent were used (eq 3), the...n-BuLi (hexane solution), and t-BuLi (pentane solution). The Grignard reagent Me 3SiCH2 MgCl was prepared in Et 0 2 2 solution from Me3SiCH 2C and Mg...trimethylsilyl)amino] (chloro)- (trimethylsilylmethyl)phosphine (1) was prepared by the "one-pot" Grignard method (eqs 1 and 2) which we have used previously for

  4. Method for the preparation of inorganic single crystal and polycrystalline electronic materials

    NASA Technical Reports Server (NTRS)

    Groves, W. O. (Inventor)

    1969-01-01

    Large area, semiconductor crystals selected from group 3-5 compounds and alloys are provided for semiconductor device fabrication by the use of a selective etching operation which completely removes the substrate on which the desired crystal was deposited. The substrate, selected from the same group as the single crystal, has a higher solution rate than the epitaxial single crystal which is essentially unaffected by the etching solution. The preparation of gallium phosphide single crystals using a gallium arsenide substrate and a concentrated nitric acid etching solution is described.

  5. Assessment of glutathione levels in model solution and grape ferments supplemented with glutathione-enriched inactive dry yeast preparations using a novel UPLC-MS/MS method.

    PubMed

    Kritzinger, E C; Stander, M A; Du Toit, W J

    2013-01-01

    A novel, robust and fast ultra-high performance liquid chromatography-MS method has been developed for the simultaneous quantification of reduced glutathione (GSH) and oxidised glutathione (GSSG) in grape juice, wine and model wine solution. Sample preparation is minimal and does not require derivatisation. The method has very good performance in terms of sensitivity and selectivity. The limit of detection was 0.002 and 0.001 mg L(-1) for GSH and GSSG, respectively. The amount of GSH and GSSG released by commercial glutathione-enriched inactivated dry yeast preparations (GSH-IDYs) into a model solution was assessed. Significant differences in the amount of GSH and/or GSSG released into a model wine by different GSH-IDYs were observed, with ethanol influencing this release under certain conditions. The GSH and GSSG levels in grape juice fermentations supplemented with GSH-IDY were also assessed in relation to different addition times during fermentation. GSH-IDY addition can lead to elevated wine GSH levels, provided the supplementation is done early during alcoholic fermentation.

  6. Preparation of metallic nanoparticles by irradiation in starch aqueous solution

    NASA Astrophysics Data System (ADS)

    NemÅ£anu, Monica R.; Braşoveanu, Mirela; Iacob, Nicuşor

    2014-11-01

    Colloidal silver nanoparticles (AgNPs) were synthesized in a single step by electron beam irradiation reduction of silver ions in aqueous solution containing starch. The nanoparticles were characterized by spectrophotocolorimetry and compared with those obtained by chemical (thermal) reduction method. The results showed that the smaller sizes of AgNPs were prepared with higher yields as the irradiation dose increased. The broadening of particle size distribution occurred by increasing of irradiation dose and dose rate. Chromatic parameters such as b* (yellow-blue coordinate), C* (chroma) and ΔEab (total color difference) could characterize the nanoparticles with respect of their concentration. Hue angle ho was correlated to the particle size distribution. Experimental data of the irradiated samples were also subjected to factor analysis using principal component extraction and varimax rotation in order to reveal the relation between dependent variables and independent variables and to reduce their number. The radiation-based method provided silver nanoparticles with higher concentration and narrower size distribution than those produced by chemical reduction method. Therefore, the electron beam irradiation is effective for preparation of silver nanoparticles using starch aqueous solution as dispersion medium.

  7. Preparation, structure and magnetic properties of synthetic ferrihydrite nanoparticles

    NASA Astrophysics Data System (ADS)

    Stolyar, S. V.; Yaroslavtsev, R. N.; Bayukov, O. A.; Balaev, D. A.; Krasikov, A. A.; Iskhakov, R. S.; Vorotynov, A. M.; Ladygina, V. P.; Purtov, K. V.; Volochaev, M. N.

    2018-03-01

    Superparamagnetic ferrihydrite powders with average nanoparticle sizes of 2.5 nm produced by the chemical deposition method. Static and dynamic magnetic properties are measured. As a result of ultrasonic treatment in the cavitation regime of suspensions of ferrihydrite powders in a solution of the albumin protein, the Fe ions are reduced to the metallic state. A sol of ferrihydrite nanoparticles is prepared in an aqueous solution of arabinogalactan polysaccharide.

  8. Micro-structural characterization of precipitation-synthesized fluorapatite nano-material by transmission electron microscopy using different sample preparation techniques.

    PubMed

    Chinthaka Silva, G W; Ma, Longzhou; Hemmers, Oliver; Lindle, Dennis

    2008-01-01

    Fluorapatite is a naturally occurring mineral of the apatite group and it is well known for its high physical and chemical stability. There is a recent interest in this ceramic to be used as a radioactive waste form material due to its intriguing chemical and physical properties. In this study, the nano-sized fluorapatite particles were synthesized using a precipitation method and the material was characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM). Two well-known methods, called solution-drop and the microtome cutting, were used to prepare the sample for TEM analysis. It was found that the microtome cutting technique is advantageous for examining the particle shape and cross-sectional morphology as well as for obtaining ultra-thin samples. However, this method introduces artifacts and strong background contrast for high-resolution transmission electron microscopy (HRTEM) observation. On the other hand, phase image simulations showed that the solution-drop method is reliable and stable for HRTEM analysis. Therefore, in order to comprehensively analyze the microstructure and morphology of the nano-material, it is necessary to combine both solution-drop and microtome cutting techniques for TEM sample preparation.

  9. A randomized, controlled, double-blind trial of the adjunct use of Clebopride in polyethylene glycol electrolyte (PEG) solution for colonoscopy preparation.

    PubMed

    Abdullah, Murdani; Rani, A Aziz; Fauzi, Achmad; Syam, Ari Fahrial; Makmun, Dadang; Simadibrata, Marcellus; Manan, Chudahman; Harjodisastro, Daldiyono

    2010-01-01

    To study the benefit of Clebopride as an adjuvant in polyethylene glycol electrolyte (PEG) solution for colonoscopy preparation. Eighty one adult patients who underwent colonoscopy examination were recruited in this randomized double blind controlled study. First group received PEG and placebo, whereas second group received PEG and Clebopride. Two litres of PEG was taken at night before colonoscopy. The acceptability and tolerability of bowel preparation were assessed through interview method. The efficacy of bowel preparation was assessed using Aronchick's Criteria. In terms of acceptability, 64 patients (31 patients from placebo group vs 33 patients from Clebopride group) were able to drink two litres of PEG solution. Sixty patients (29 patients from placebo group and 31 patients from Clebopride group) were willing to accept PEG solution for their next bowel preparation. On the term of tolerability, nausea, abdominal distension, and borborygmus were more frequent in the placebo group (34.2% vs 27.9%; 44.7% vs 32.6%; 26.3% vs 4.6% respectively). However, only the difference at the incidence of borborygmus that was statistically significant (p<0.05). On the terms of efficacy, both groups showed a comparable bowel preparation quality with 88.4% of bowel preparation in Clebopride group and 81.6% of bowel preparation in placebo group were optimal (p = 0.585). The adjunct use of Clebopride in PEG solution for colonoscopy preparations tends to increase the acceptability, tolerability, and efficacy. The presence of borborygmus was significantly lower in the Clebopride group.

  10. Non-aqueous solution preparation of doped and undoped lixmnyoz

    DOEpatents

    Boyle, Timothy J.; Voigt, James A.

    1997-01-01

    A method for generation of phase-pure doped and undoped Li.sub.x Mn.sub.y O.sub.z precursors. The method of this invention uses organic solutions instead of aqueous solutions or nonsolution ball milling of dry powders to produce phase-pure precursors. These precursors can be used as cathodes for lithium-polymer electrolyte batteries. Dopants may be homogeneously incorporated to alter the characteristics of the powder.

  11. Efficient sample preparation method based on solvent-assisted dispersive solid-phase extraction for the trace detection of butachlor in urine and waste water samples.

    PubMed

    Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

    2016-10-01

    In this work, an efficient sample preparation method termed solvent-assisted dispersive solid-phase extraction was applied. The used sample preparation method was based on the dispersion of the sorbent (benzophenone) into the aqueous sample to maximize the interaction surface. In this approach, the dispersion of the sorbent at a very low milligram level was achieved by inserting a solution of the sorbent and disperser solvent into the aqueous sample. The cloudy solution created from the dispersion of the sorbent in the bulk aqueous sample. After pre-concentration of the butachlor, the cloudy solution was centrifuged and butachlor in the sediment phase dissolved in ethanol and determined by gas chromatography with flame ionization detection. Under the optimized conditions (solution pH = 7.0, sorbent: benzophenone, 2%, disperser solvent: ethanol, 500 μL, centrifuged at 4000 rpm for 3 min), the method detection limit for butachlor was 2, 3 and 3 μg/L for distilled water, waste water, and urine sample, respectively. Furthermore, the preconcentration factor was 198.8, 175.0, and 174.2 in distilled water, waste water, and urine sample, respectively. Solvent-assisted dispersive solid-phase extraction was successfully used for the trace monitoring of butachlor in urine and waste water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Method for making monolithic metal oxide aerogels

    DOEpatents

    Coronado, Paul R.

    1999-01-01

    Transparent, monolithic metal oxide aerogels of varying densities are produced using a method in which a metal alkoxide solution and a catalyst solution are prepared separately and reacted. The resulting hydrolyzed-condensed colloidal solution is gelled, and the wet gel is contained within a sealed, but gas permeable, containment vessel during supercritical extraction of the solvent. The containment vessel is enclosed within an aqueous atmosphere that is above the supercritical temperature and pressure of the solvent of the metal alkoxide solution.

  13. Electrochemical Preparation of Polyaniline Nanowires with the Used Electrolyte Solution Treated with the Extraction Process and Their Electrochemical Performance.

    PubMed

    Wu, Ying; Wang, Jixiao; Ou, Bin; Zhao, Song; Wang, Zhi; Wang, Shichang

    2018-02-12

    Electrochemical polymerization of aniline is one of the most promising methods to prepare polyaniline (PANI) materials. However, during this process, the electrolyte solution must be replaced after electropolymerization of a certain time because of the generation and the accumulation of the by-products, which have significant effects on the morphology, purity and properties of PANI products. Treatment and recycling of the used electrolyte solution are worthwhile to study to reduce the high treatment cost of the used electrolyte solution containing aniline and its polymerization by-products. Here, the composition of the used electrolyte solution was separated and determined by high performance liquid chromatography coupled with diode array detection (HPLC-DAD) in the range of ultraviolet and visible (UV-Vis) light. The analysis results revealed that the used electrolyte solution consisted of aniline, p-hydroquinone (HQ), p-benzoquinone (BQ), co-oligomers of aniline and p-benzoquinone (CAB) and acid. Then, n-octanol and 2-octanone were selected as extracts to remove HQ, BQ and CAB from the used electrolyte solution. Following that, the recycled electrolyte solution was prepared by adjusting the concentration of aniline and acid of the aqueous phase, and the electrochemical polymerization process was conducted. Finally, the obtained PANI was characterized by scanning electron microscope (SEM) and electrochemical methods. The experimental results clearly demonstrate that the morphology and specific capacitance of PANI produced from the recycled electrolyte solution can be recovered completely. This research paves the way for reusing the used electrolyte solution for aniline electrochemical polymerization.

  14. Electrochemical Preparation of Polyaniline Nanowires with the Used Electrolyte Solution Treated with the Extraction Process and Their Electrochemical Performance

    PubMed Central

    Wu, Ying; Wang, Jixiao; Ou, Bin; Zhao, Song; Wang, Zhi; Wang, Shichang

    2018-01-01

    Electrochemical polymerization of aniline is one of the most promising methods to prepare polyaniline (PANI) materials. However, during this process, the electrolyte solution must be replaced after electropolymerization of a certain time because of the generation and the accumulation of the by-products, which have significant effects on the morphology, purity and properties of PANI products. Treatment and recycling of the used electrolyte solution are worthwhile to study to reduce the high treatment cost of the used electrolyte solution containing aniline and its polymerization by-products. Here, the composition of the used electrolyte solution was separated and determined by high performance liquid chromatography coupled with diode array detection (HPLC-DAD) in the range of ultraviolet and visible (UV-Vis) light. The analysis results revealed that the used electrolyte solution consisted of aniline, p-hydroquinone (HQ), p-benzoquinone (BQ), co-oligomers of aniline and p-benzoquinone (CAB) and acid. Then, n-octanol and 2-octanone were selected as extracts to remove HQ, BQ and CAB from the used electrolyte solution. Following that, the recycled electrolyte solution was prepared by adjusting the concentration of aniline and acid of the aqueous phase, and the electrochemical polymerization process was conducted. Finally, the obtained PANI was characterized by scanning electron microscope (SEM) and electrochemical methods. The experimental results clearly demonstrate that the morphology and specific capacitance of PANI produced from the recycled electrolyte solution can be recovered completely. This research paves the way for reusing the used electrolyte solution for aniline electrochemical polymerization. PMID:29439514

  15. Method for synthesizing carbon nanotubes

    DOEpatents

    Fan, Hongyou

    2012-09-04

    A method for preparing a precursor solution for synthesis of carbon nanomaterials, where a polar solvent is added to at least one block copolymer and at least one carbohydrate compound, and the precursor solution is processed using a self-assembly process and subsequent heating to form nanoporous carbon films, porous carbon nanotubes, and porous carbon nanoparticles.

  16. Doped-carbon composites, synthesizing methods and applications of the same

    DOEpatents

    Viswanathan, Tito

    2017-05-09

    A method of synthesizing a doped carbon composite includes preparing a solution having a carbon source material and a heteroatom containing additive, evaporating the solution to yield a plurality of powders, and subjecting the plurality of powders to a heat treatment for a duration of time effective to produce the doped carbon composite.

  17. Reliability of chemotherapy preparation processes: Evaluating independent double-checking and computer-assisted gravimetric control.

    PubMed

    Carrez, Laurent; Bouchoud, Lucie; Fleury-Souverain, Sandrine; Combescure, Christophe; Falaschi, Ludivine; Sadeghipour, Farshid; Bonnabry, Pascal

    2017-03-01

    Background and objectives Centralized chemotherapy preparation units have established systematic strategies to avoid errors. Our work aimed to evaluate the accuracy of manual preparations associated with different control methods. Method A simulation study in an operational setting used phenylephrine and lidocaine as markers. Each operator prepared syringes that were controlled using a different method during each of three sessions (no control, visual double-checking, and gravimetric control). Eight reconstitutions and dilutions were prepared in each session, with variable doses and volumes, using different concentrations of stock solutions. Results were analyzed according to qualitative (choice of stock solution) and quantitative criteria (accurate, <5% deviation from the target concentration; weakly accurate, 5%-10%; inaccurate, 10%-30%; wrong, >30% deviation). Results Eleven operators carried out 19 sessions. No final preparation (n = 438) contained a wrong drug. The protocol involving no control failed to detect 1 of 3 dose errors made and double-checking failed to detect 3 of 7 dose errors. The gravimetric control method detected all 5 out of 5 dose errors. The accuracy of the doses measured was equivalent across the control methods ( p = 0.63 Kruskal-Wallis). The final preparations ranged from 58% to 60% accurate, 25% to 27% weakly accurate, 14% to 17% inaccurate and 0.9% wrong. A high variability was observed between operators. Discussion Gravimetric control was the only method able to detect all dose errors, but it did not improve dose accuracy. A dose accuracy with <5% deviation cannot always be guaranteed using manual production. Automation should be considered in the future.

  18. Corrosion resistant properties of polyaniline acrylic coating on magnesium alloy

    NASA Astrophysics Data System (ADS)

    Sathiyanarayanan, S.; Azim, S. Syed; Venkatachari, G.

    2006-12-01

    The performance of the paint coating based on acrylic-polyaniline on magnesium alloy ZM 21 has been studied by electrochemical impedance spectroscopy in 0.5% NaCl solution. The polyaniline was prepared by chemical oxidative method of aniline with ammonium persulphate in phosphoric acid medium. The phosphate-doped polyaniline was characterized by FTIR and XRD methods. Acrylic paint containing the phosphate-doped polyaniline was prepared and coated on magnesium ZM 21 alloy. The coating was able to protect the magnesium alloy and no base metal dissolution was noted even after 75 days exposure to sodium chloride solution.

  19. On the Preparation of Buffer Solutions.

    ERIC Educational Resources Information Center

    Thomson, Bruce M.; Kessick, Michael A.

    1981-01-01

    Presents a method, suitable for use on programmable calculators, which allows calculation of the pH and ionic strength (I) of a mixed solution of salts of an acid or amounts necessary to produce a solution of a particular pH and I. Includes limitations when using the calculations described. (SK)

  20. Process parameters and morphology in puerarin, phospholipids and their complex microparticles generation by supercritical antisolvent precipitation.

    PubMed

    Li, Ying; Yang, Da-Jian; Chen, Shi-Lin; Chen, Si-Bao; Chan, Albert Sun-Chi

    2008-07-09

    The aim of the study was to develop and evaluate a new method for the production of puerarin phospholipids complex (PPC) microparticles. The advanced particle formation method, solution enhanced dispersion by supercritical fluids (SEDS), was used for the preparation of puerarin (Pur), phospholipids (PC) and their complex particles for the first time. Evaluation of the processing variables on PPC particle characteristics was also conducted. The processing variables included temperature, pressure, solution concentration, the flow rate of supercritical carbon dioxide (SC-CO2) and the relative flow rate of drug solution to CO2. The morphology, particle size and size distribution of the particles were determined. Meanwhile Pur and phospholipids were separately prepared by gas antisolvent precipitation (GAS) method and solid characterization of particles by the two supercritical methods was also compared. Pur formed by GAS was more orderly, purer crystal, whereas amorphous Pur particles between 0.5 and 1microm were formed by SEDS. The complex was successfully obtained by SEDS exhibiting amorphous, partially agglomerated spheres comprised of particles sized only about 1microm. SEDS method may be useful for the processing of other pharmaceutical preparations besides phospholipids complex particles. Furthermore adopting a GAS process to recrystallize pharmaceuticals will provide a highly versatile methodology to generate new polymorphs of drugs in addition to conventional techniques.

  1. Pediatric oral solutions with propranolol hydrochloride for extemporaneous compounding: the formulation and stability study.

    PubMed

    Klovrzová, Sylva; Zahálka, Lukáš; Matysová, Ludmila; Horák, Petr; Sklubalová, Zdenka

    2013-02-01

    The aim of this study is to formulate an extemporaneous pediatric oral solution of propranolol hydrochloride (PRO) 2 mg/ml for the therapy of infantile haemangioma or hypertension in a target age group of 1 month to school children and to evaluate its stability. A citric acid solution and/or a citrate-phosphate buffer solution, respectively, were used as the vehicles to achieve pH value of about 3, optimal for the stability of PRO. In order to mask the bitter taste of PRO, simple syrup was used as the sweetener. All solutions were stored in tightly closed brown glass bottles at 5 ± 3 °C and/or 25 ± 3 °C, respectively. The validated HPLC method was used to evaluate the concentration of PRO and a preservative, sodium benzoate, at time intervals of 0-180 days. All preparations were stable at both storage temperatures with pH values in the range of 2.8-3.2. According to pharmacopoeial requirements, the efficacy of sodium benzoate 0.05 % w/v was proved (Ph.Eur., 5.1.3). The preparation formulated with the citrate-phosphate buffer, in our experience, had better palatability than that formulated with the citric acid solution. propranolol hydrochloride pediatric preparation extemporaneous preparation solution stability testing HPLC.

  2. Preparation of bone samples in the Gliwice Radiocarbon Laboratory for AMS radiocarbon dating.

    PubMed

    Piotrowska, N; Goslar, T

    2002-12-01

    In the Gliwice Radiocarbon Laboratory, a system for preparation of samples for AMS dating has been built. At first it was used to produce graphite targets from plant macrofossils and sediments. In this study we extended its capabilities with the preparation of bones. We dealt with 3 methods; the first was the classical Longin method of collagen extraction, the second one included additional treatment of powdered bone in alkali solution, while in the third one carboxyl carbon was separated from amino acids obtained after hydrolysis of protein. The suitability of the methods was tested on 2 bone samples. Most of our samples gave ages > 40 kyr BP, suggesting good performance of the adapted methods, except for one sample prepared with simple Longin method. For routine preparation of bones we chose the Longin method with additional alkali treatment.

  3. RAPID COMMUNICATION: Large-area uniform ultrahigh-Jc YBa2Cu3O7-x film fabricated by the metalorganic deposition method using trifluoroacetates

    NASA Astrophysics Data System (ADS)

    Araki, Takeshi; Yamagiwa, Katsuya; Hirabayashi, Izumi; Suzuki, Katsumi; Tanaka, Shoji

    2001-07-01

    Ultrahigh-Jc YBa2Cu3O7-x (YBCO) films have been successfully fabricated by the metalorganic deposition method using a trifluoroacetate coating solution which is prepared by a newly developed purification technique, the solvent-into-gel (SIG) method. The prepared pure coating solution has less than 0.25% impurities and has a wide flexibility in process conditions to obtain high-Jc YBCO film. Using this feature, we have successfully formed 50 mm diameter YBCO films, which have a critical current density over 10 MA cm-2 (77 K, 0 T) on LaAlO3 single crystalline substrates.

  4. Method of producing solution-derived metal oxide thin films

    DOEpatents

    Boyle, Timothy J.; Ingersoll, David

    2000-01-01

    A method of preparing metal oxide thin films by a solution method. A .beta.-metal .beta.-diketonate or carboxylate compound, where the metal is selected from groups 8, 9, 10, 11, and 12 of the Periodic Table, is solubilized in a strong Lewis base to form a homogeneous solution. This precursor solution forms within minutes and can be deposited on a substrate in a single layer or a multiple layers to form a metal oxide thin film. The substrate with the deposited thin film is heated to change the film from an amorphous phase to a ceramic metal oxide and cooled.

  5. Method for loading resin beds

    DOEpatents

    Notz, Karl J.; Rainey, Robert H.; Greene, Charles W.; Shockley, William E.

    1978-01-01

    An improved method of preparing nuclear reactor fuel by carbonizing a uranium loaded cation exchange resin provided by contacting a H.sup.+ loaded resin with a uranyl nitrate solution deficient in nitrate, comprises providing the nitrate deficient solution by a method comprising the steps of reacting in a reaction zone maintained between about 145.degree.-200.degree. C, a first aqueous component comprising a uranyl nitrate solution having a boiling point of at least 145.degree. C with a second aqueous component to provide a gaseous phase containing HNO.sub.3 and a reaction product comprising an aqueous uranyl nitrate solution deficient in nitrate.

  6. Size exclusion chromatography for analyses of fibroin in silk: optimization of sampling and separation conditions

    NASA Astrophysics Data System (ADS)

    Pawcenis, Dominika; Koperska, Monika A.; Milczarek, Jakub M.; Łojewski, Tomasz; Łojewska, Joanna

    2014-02-01

    A direct goal of this paper was to improve the methods of sample preparation and separation for analyses of fibroin polypeptide with the use of size exclusion chromatography (SEC). The motivation for the study arises from our interest in natural polymers included in historic textile and paper artifacts, and is a logical response to the urgent need for developing rationale-based methods for materials conservation. The first step is to develop a reliable analytical tool which would give insight into fibroin structure and its changes caused by both natural and artificial ageing. To investigate the influence of preparation conditions, two sets of artificially aged samples were prepared (with and without NaCl in sample solution) and measured by the means of SEC with multi angle laser light scattering detector. It was shown that dialysis of fibroin dissolved in LiBr solution allows removal of the salt which destroys stacks chromatographic columns and prevents reproducible analyses. Salt rich (NaCl) water solutions of fibroin improved the quality of chromatograms.

  7. Preparation and characterization of poly(acrylic acid)—corn starch blend for use as chemical sand-fixing materials

    NASA Astrophysics Data System (ADS)

    Dang, Xugang; Chen, Hui; Shan, Zhihua

    2017-07-01

    One chemical sand-fixing materials based on poly(acrylic acid)-corn starch (PACS) blend was studied in this work. The PACS blend was prepared by solution mixing method between PA and CS. In order to prepare sand-fixing materials for environmental applications using the well-established method of spraying evenly PACS blend solution on the surfaces of fine sand. Fourier transform infrared spectroscopy (FT-IR) revealed the existence of the intermolecular interactions between the blend components. Scanning electron microscope (SEM) analysis showed a continuous phase of blend, and it also showed the good sand-fixing capacity. The test results of hygroscopicity and water retention experiments indicated that the blends had excellent water-absorbing and water-retention capacity. The results of contact angle measurements between the PACS solutions and fine sand showed that the PACS blend has a satisfactory effect on fine sand wetting. And the PACS, as a sand-fixation material, has excellent sand-fixation rate up to 99.5%.

  8. Standard Reference Materials (SRMs) for the Calibration and Validation of Analytical Methods for PCBs (as Aroclor Mixtures)

    PubMed Central

    Poster, Dianne L.; Schantz, Michele M.; Leigh, Stefan D.; Wise, Stephen A.

    2004-01-01

    Six Standard Reference Materials (SRMs®) have been prepared by the National Institute of Standards and Technology (NIST) for the determination of PCBs as different Aroclor mixtures in methanol. Six additional SRMs of the same Aroclors in transformer oil have also been prepared. Specifically, solutions of Aroclors 1016, 1232, 1242, 1254, and 1260 have been gravimetrically prepared (individually) in methanol and transformer oil, mixed, and transferred to amber glass ampoules in approximately 1.2 mL aliquots. Gas chromatography with electron capture detection (GC-ECD) has been used to verify the gravimetric data for each solution and transformer oil SRM. Liquid chromatography was used for the isolation of the Aroclors from the transformer oil SRMs prior to GC-ECD analysis. Separate calibration solutions and oils were prepared with Aroclor levels similar to those in each methanol solution and transformer oil SRM and were processed alongside the samples. The GC-ECD response of each Aroclor was monitored relative to internal standards that were added to the complex mixtures for quantification. The gravimetric concentrations of Aroclors 1242 and 1254 in methanol were also examined by the same method of analysis (GC-ECD) using several different sources of Aroclors and two different capillary GC columns: a 5 % phenyl methylpolysiloxane phase and a relatively non-polar phase. The preparation of the materials, the gas chromatographic results, and the certified concentration values for each Aroclor SRM are described in this paper. PMID:27366608

  9. Study of Colloidal Gold Synthesis Using Turkevich Method

    NASA Astrophysics Data System (ADS)

    Rohiman, Asep; Anshori, Isa; Surawijaya, Akhmadi; Idris, Irman

    2011-12-01

    The synthesis of colloidal gold or Au-nanoparticles (Au-NPs) by reduction of chloroauric acid (HAuCl4) with sodium citrate was done using Turkevich method. We prepare HAuCl4 solution by dissolving gold wires (99.99%) into aqua regia solution. To initiate the Au-NPs synthesis 0.17 ml of 1 % chloroauric acid solution was heated to the boiling point and then 10 ml of 1 % sodium citrate was added to the boiling solution with a constant stirring in order to maintain a homogenous solution. A color of faint gray was observed in the solution approximately one minute and in a period of 2-3 minutes later, it further darkened to deep wine and red color. It showed that the gold solution has reduced to Au-NPs. The effect of process temperature on the size of Au-NPs prepared by sodium citrate reduction has also been investigated. With increasing temperature of Au-NPs synthesis, smaller-size Au-NPs were obtained. The higher temperatures shorten the time needed to achieve activation energy for reduction process. The resulting Au-NPs has been characterized by scanning Electron Microscope (SEM), showing the size of Au-NPs average diameter is ˜20-27 nm. The resulting colloidal gold will be used as catalyst for Si nanowires growth using VLS method.

  10. Simple synthesis of graphene nanocomposites MgO-rGO and Fe2O3-rGO for multifunctional applications

    NASA Astrophysics Data System (ADS)

    Abdel-Aal, Seham K.; Ionov, Andrey; Mozhchil, R. N.; Naqvi, Alim H.

    2018-05-01

    Hummer's method was used to prepare graphene oxide (GO) by chemical exfoliation of graphite. Simple precipitation method was used for the preparation of hybrid nanocomposites MgO-rGO and Fe2O3-rGO. A 0.3 Molar of corresponding metal nitrate solution and GO solution are used for the preparation process. XRD, FT-IR, and XPS were used to characterize the prepared nanocomposites. The reduction of GO into reduced rGO in the formed nanocomposites was confirmed. Morphological characterization showed the formation of needle-shaped nanocrystals of MgO successfully grown on graphene nanosheet with average crystallite size 8.4 nm. Hematite nanocomposite Fe2O3-rGO forms rod-shaped crystals with average crystallite size 27.5 nm. The saturation magnetization observed for Fe2O3-rGO is less than reported value for the pure Fe2O3 nanoparticles. Thermal properties of as-prepared hybrid nanocomposites MgO-rGO and Fe2O3-rGO showed thermal stability of the prepared nanocomposite over long range of temperature.

  11. Cellulose acetate fibers prepared from different raw materials with rapid synthesis method.

    PubMed

    Chen, Jinghuan; Xu, Jikun; Wang, Kun; Cao, Xuefei; Sun, Runcang

    2016-02-10

    Transesterification is a mild process to prepare cellulose acetate (CA) as compared with the traditional method. In this study, CA fibers were produced from six cellulose raw materials based on a simple and rapid transesterification method. The properties of the CA solutions and the obtained CA fibers were investigated in detail. Results showed that all of the cellulose raw materials were esterified within 15 min, and spinning dopes could be obtained by concentrating the CA solutions via vacuum distillation. The XRD, FT-IR, (1)H, (13)C and HSQC NMR analysis confirmed the successful synthesis of CA. The degree of substitution (DS) of the obtained CA was significantly affected by the degree of polymerization (DP) of cellulose raw materials, which further influenced the viscosity of CA solutions as well as the structural, thermal and mechanical properties of the CA fibers. Copyright © 2015 Elsevier Ltd. All rights reserved.

  12. Sillica Gel-Amine from Geothermal Sludge

    NASA Astrophysics Data System (ADS)

    Muljani, S.; Pujiastuti, C.; Wicaksono, P.; Lutfianingrum, R.

    2018-01-01

    Silica Gel-Amine (SGA) has been made from geothermal sludge by grafting amine method. Sodium silicate solution is prepared by extracted geothermal sludge powder using sodium hidroxide solution then acidification in the range of pH 5 - 9 by using tartaric acid 1N. The grafting process uses 1 ml of ammonia solution and 10 ml of toluene at a rate of 0.1 ml min-1 accompanied by a reflux process. The amine grafting is done in two methods. The first method is grafting amine in silicate solution and the second method is grafting amine in washed gel. Product SGA was confirmed by FTIR, TGA-DTG and BET characterization. The results show that the pH affects the amount of amine that is grafted onto silica gel. Differences in grafting method affect the size of the pore and surface area. SGA product prepared by grafting washed gel at pH 8 have pore diameter of 12.06 nm, surface area of 173.44 m2g-1, and mass of decomposed amine compound 0.4 mg. In the presence of amine groups on the silica gel surface, these adsorbents may be able to selectively adsorb CO2 gas from natural gas.

  13. Automated structure determination of proteins with the SAIL-FLYA NMR method.

    PubMed

    Takeda, Mitsuhiro; Ikeya, Teppei; Güntert, Peter; Kainosho, Masatsune

    2007-01-01

    The labeling of proteins with stable isotopes enhances the NMR method for the determination of 3D protein structures in solution. Stereo-array isotope labeling (SAIL) provides an optimal stereospecific and regiospecific pattern of stable isotopes that yields sharpened lines, spectral simplification without loss of information, and the ability to collect rapidly and evaluate fully automatically the structural restraints required to solve a high-quality solution structure for proteins up to twice as large as those that can be analyzed using conventional methods. Here, we describe a protocol for the preparation of SAIL proteins by cell-free methods, including the preparation of S30 extract and their automated structure analysis using the FLYA algorithm and the program CYANA. Once efficient cell-free expression of the unlabeled or uniformly labeled target protein has been achieved, the NMR sample preparation of a SAIL protein can be accomplished in 3 d. A fully automated FLYA structure calculation can be completed in 1 d on a powerful computer system.

  14. Method for synthesizing thin film electrodes

    DOEpatents

    Boyle, Timothy J [Albuquerque, NM

    2007-03-13

    A method for making a thin-film electrode, either an anode or a cathode, by preparing a precursor solution using an alkoxide reactant, depositing multiple thin film layers with each layer approximately 500 1000 .ANG. in thickness, and heating the layers to above 600.degree. C. to achieve a material with electrochemical properties suitable for use in a thin film battery. The preparation of the anode precursor solution uses Sn(OCH.sub.2C(CH.sub.3).sub.3).sub.2 dissolved in a solvent in the presence of HO.sub.2CCH.sub.3 and the cathode precursor solution is formed by dissolving a mixture of (Li(OCH.sub.2C(CH.sub.3).sub.3)).sub.8 and Co(O.sub.2CCH.sub.3).H.sub.2O in at least one polar solvent.

  15. Gravimetric preparation and characterization of primary reference solutions of molybdenum and rhodium.

    PubMed

    Kaltenbach, Angela; Noordmann, Janine; Görlitz, Volker; Pape, Carola; Richter, Silke; Kipphardt, Heinrich; Kopp, Gernot; Jährling, Reinhard; Rienitz, Olaf; Güttler, Bernd

    2015-04-01

    Gravimetrically prepared mono-elemental reference solutions having a well-known mass fraction of approximately 1 g/kg (or a mass concentration of 1 g/L) define the very basis of virtually all measurements in inorganic analysis. Serving as the starting materials of all standard/calibration solutions, they link virtually all measurements of inorganic analytes (regardless of the method applied) to the purity of the solid materials (high-purity metals or salts) they were prepared from. In case these solid materials are characterized comprehensively with respect to their purity, this link also establishes direct metrological traceability to The International System of Units (SI). This, in turn, ensures the comparability of all results on the highest level achievable. Several national metrology institutes (NMIs) and designated institutes (DIs) have been working for nearly two decades in close cooperation with commercial producers on making an increasing number of traceable reference solutions available. Besides the comprehensive characterization of the solid starting materials, dissolving them both loss-free and completely under strict gravimetric control is a challenging problem in the case of several elements like molybdenum and rhodium. Within the framework of the European Metrology Research Programme (EMRP), in the Joint Research Project (JRP) called SIB09 Primary standards for challenging elements, reference solutions of molybdenum and rhodium were prepared directly from the respective metals with a relative expanded uncertainty associated with the mass fraction of U rel(w) < 0.05 %. To achieve this, a microwave-assisted digestion procedure for Rh and a hotplate digestion procedure for Mo were developed along with highly accurate and precise inductively coupled plasma optical emission spectrometry (ICP OES) and multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) methods required to assist with the preparation and as dissemination tools.

  16. [Physical and chemical stability of fortified ophtalmic ready-to-use solutions: review of literature].

    PubMed

    Sourdeau, P; Evrard, J-M; Remy, G; Hecq, J-D

    2012-03-01

    Ophtalmic infections and inflammations are often encountered during hospitalization. They require the preparation of "fortified" ophtalmic solutions, i.e. pharmaceutical ophtalmic solutions which are hyperconcentrated in active substance. The data of physicochemical stabilities are modified and it is therefore essential to gather the results of the various publications devoted to this subject. In 2006, an initial literature review was undertaken to identify the molecules mostly used in the preparation of fortified ophtalmic solutions in hospital. A second review of the literature in 2010 has enriched the knowledge about it. Two new drugs have entered the summary table: amikacin and ticarcillin disodium. Date on 12 molecules already known in 2006 were updated to improve clinical practices. A review of the literature was undertaken in order to collect the results of the molecules mostly used for the preparation of the fortified ophtalmic solutions in hospitals. A summary table, indicating the active substance, its concentration, the assay method, the storage temperature and physicochemical modifications, presents all the results. This review of literature makes it possible to match stability and validity period to these preparations. Copyright © 2011 Elsevier Masson SAS. All rights reserved.

  17. Method for making monolithic metal oxide aerogels

    DOEpatents

    Droege, M.W.; Coronado, P.R.; Hair, L.M.

    1995-03-07

    Transparent, monolithic metal oxide aerogels of varying densities are produced using a method in which a metal alkoxide solution and a catalyst solution are prepared separately and reacted. The resulting hydrolyzed-condensed colloidal solution is gelled, and the wet gel is contained within a sealed, but gas permeable, containment vessel during supercritical extraction of the solvent. The present invention is especially advantageous for making metal oxides other than silica that are prone to forming opaque, cracked aerogels. 6 figs.

  18. Method for making monolithic metal oxide aerogels

    DOEpatents

    Droege, Michael W.; Coronado, Paul R.; Hair, Lucy M.

    1995-01-01

    Transparent, monolithic metal oxide aerogels of varying densities are produced using a method in which a metal alkoxide solution and a catalyst solution are prepared separately and reacted. The resulting hydrolyzed-condensed colloidal solution is gelled, and the wet gel is contained within a sealed, but gas permeable, containment vessel during supercritical extraction of the solvent. The present invention is especially advantageous for making metal oxides other than silica that are prone to forming opaque, cracked aerogels.

  19. Preparation of metallic nanoparticles by irradiation in starch aqueous solution

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

    Nemţanu, Monica R., E-mail: monica.nemtanu@inflpr.ro; Braşoveanu, Mirela, E-mail: monica.nemtanu@inflpr.ro; Iacob, Nicuşor, E-mail: monica.nemtanu@inflpr.ro

    Colloidal silver nanoparticles (AgNPs) were synthesized in a single step by electron beam irradiation reduction of silver ions in aqueous solution containing starch. The nanoparticles were characterized by spectrophotocolorimetry and compared with those obtained by chemical (thermal) reduction method. The results showed that the smaller sizes of AgNPs were prepared with higher yields as the irradiation dose increased. The broadening of particle size distribution occurred by increasing of irradiation dose and dose rate. Chromatic parameters such as b* (yellow-blue coordinate), C* (chroma) and ΔE{sub ab} (total color difference) could characterize the nanoparticles with respect of their concentration. Hue angle h{supmore » o} was correlated to the particle size distribution. Experimental data of the irradiated samples were also subjected to factor analysis using principal component extraction and varimax rotation in order to reveal the relation between dependent variables and independent variables and to reduce their number. The radiation-based method provided silver nanoparticles with higher concentration and narrower size distribution than those produced by chemical reduction method. Therefore, the electron beam irradiation is effective for preparation of silver nanoparticles using starch aqueous solution as dispersion medium.« less

  20. Thin films and uses

    DOEpatents

    Baskaran, Suresh; Graff, Gordon L.; Song, Lin

    1998-01-01

    The invention provides a method for synthesizing a titanium oxide-containing film comprising the following steps: (a) preparing an aqueous solution of a titanium chelate with a titanium molarity in the range of 0.01M to 0.6M. (b) immersing a substrate in the prepared solution, (c) decomposing the titanium chelate to deposit a film on the substrate. The titanium chelate maybe decomposed acid, base, temperature or other means. A preferred method provides for the deposit of adherent titanium oxide films from C2 to C5 hydroxy carboxylic acids. In another aspect the invention is a novel article of manufacture having a titanium coating which protects the substrate against ultraviolet damage. In another aspect the invention provides novel semipermeable gas separation membranes, and a method for producing them.

  1. Production of metals and compounds by radiation chemistry

    NASA Technical Reports Server (NTRS)

    Marsik, S. J.; Philipp, W. H.

    1969-01-01

    Preparation of metals and compounds by radiation induced chemical reactions involves irradiation of metal salt solutions with high energy electrons. This technique offers a method for the preparation of high purity metals with minimum contamination from the container material or the cover gas.

  2. Combination could be another tool for bowel preparation?

    PubMed Central

    Soh, Jae Seung; Kim, Kyung-Jo

    2016-01-01

    Optimal bowel preparation increases the cecal intubation rate and detection of neoplastic lesions while decreasing the procedural time and procedural-related complications. Although high-volume polyethylene glycol (PEG) solution is the most frequently used preparation for bowel cleansing, patients are often unwilling to take PEG solution due to its large volume, poor palatability, and high incidence of adverse events, such as abdominal bloating and nausea. Other purgatives include osmotic agents (e.g., sodium phosphate, magnesium citrate, and sodium sulfate), stimulant agents (e.g., senna, bisacodyl, and sodium picosulfate), and prokinetic agents (e.g., cisapride, mosapride, and itopride). A combination of PEG with an osmotic, stimulant, or prokinetic agent could effectively reduce the PEG solution volume and increase patients’ adherence. Some such solutions have been found in several published studies to not be inferior to PEG alone in terms of bowel cleansing quality. Although combination methods showed similar efficacy and safety, the value of these studies is limited by shortcomings in study design. New effective and well-tolerated combination preparations are required, in addition to rigorous new validated studies. PMID:26973388

  3. Templated Native Silk Smectic Gels

    NASA Technical Reports Server (NTRS)

    Park, Jae-Hyung (Inventor); Valluzzi, Regina (Inventor); Jin, Hyoung-Joon (Inventor)

    2013-01-01

    One aspect of the present invention relates to a method of preparing a fibrous protein smectic hydrogel by way of a solvent templating process, comprising the steps of pouring an aqueous fibrous protein solution into a container comprising a solvent that is not miscible with water; sealing the container and allowing it to age at about room temperature; and collecting the resulting fibrous protein smectic hydrogel and allowing it to dry. Another aspect of the present invention relates to a method of obtaining predominantly one enantiomer from a racemic mixture, comprising the steps of pouring an aqueous fibrous protein solution into a container comprising a solvent that is not miscible with water; sealing the container and allowing it to age at about room temperature; allowing the enantiomers of racemic mixture to diffuse selectively into the smectic hydrogel in solution; removing the smectic hydrogel from the solution; rinsing predominantly one enantiomer from the surface of the smectic hydrogel; and extracting predominantly one enantiomer from the interior of the smectic hydrogel. The present invention also relates to a smectic hydrogel prepared according to an aforementioned method.

  4. Templated Native Silk Smectic Gels

    NASA Technical Reports Server (NTRS)

    Park, Jae-Hyung (Inventor); Valluzzi, Regina (Inventor); Jin, Hyoung-Joon (Inventor)

    2016-01-01

    One aspect of the present invention relates to a method of preparing a fibrous protein smectic hydrogel by way of a solvent templating process, comprising the steps of pouring an aqueous fibrous protein solution into a container comprising a solvent that is not miscible with water; sealing the container and allowing it to age at about room temperature; and collecting the resulting fibrous protein smectic hydrogel and allowing it to dry. Another aspect of the present invention relates to a method of obtaining predominantly one enantiomer from a racemic mixture, comprising the steps of pouring an aqueous fibrous protein solution into a container comprising a solvent that is not miscible with water; sealing the container and allowing it to age at about room temperature; allowing the enantiomers of racemic mixture to diffuse selectively into the smectic hydrogel in solution; removing the smectic hydrogel from the solution; rinsing predominantly one enantiomer from the surface of the smectic hydrogel; and extracting predominantly one enantiomer from the interior of the smectic hydrogel. The present invention also relates to a smectic hydrogel prepared according to an aforementioned method.

  5. Water-assisted growth of graphene on carbon nanotubes by the chemical vapor deposition method.

    PubMed

    Feng, Jian-Min; Dai, Ye-Jing

    2013-05-21

    Combining carbon nanotubes (CNTs) with graphene has been proved to be a feasible method for improving the performance of graphene for some practical applications. This paper reports a water-assisted route to grow graphene on CNTs from ferrocene and thiophene dissolved in ethanol by the chemical vapor deposition method in an argon flow. A double injection technique was used to separately inject ethanol solution and water for the preparation of graphene/CNTs. First, CNTs were prepared from ethanol solution and water. The injection of ethanol solution was suspended and water alone was injected into the reactor to etch the CNTs. Thereafter, ethanol solution was injected along with water, which is the key factor in obtaining graphene/CNTs. Transmission electron microscopy, scanning electron microscopy, X-ray diffraction, and Raman scattering analyses confirmed that the products were the hybrid materials of graphene/CNTs. X-ray photo-electron spectroscopy analysis showed the presence of oxygen rich functional groups on the surface of the graphene/CNTs. Given the activity of the graphene/CNT surface, CdS quantum dots adhered onto it uniformly through simple mechanical mixing.

  6. Templated native silk smectic gels

    NASA Technical Reports Server (NTRS)

    Park, Jae-Hyung (Inventor); Valluzzi, Regina (Inventor); Jin, Hyoung-Joon (Inventor)

    2009-01-01

    One aspect of the present invention relates to a method of preparing a fibrous protein smectic hydrogel by way of a solvent templating process, comprising the steps of pouring an aqueous fibrous protein solution into a container comprising a solvent that is not miscible with water; sealing the container and allowing it to age at about room temperature; and collecting the resulting fibrous protein smectic hydrogel and allowing it to dry. Another aspect of the present invention relates to a method of obtaining predominantly one enantiomer from a racemic mixture, comprising the steps of pouring an aqueous fibrous protein solution into a container comprising a solvent that is not miscible with water; sealing the container and allowing it to age at about room temperature; allowing the enantiomers of racemic mixture to diffuse selectively into the smectic hydrogel in solution; removing the smectic hydrogel from the solution; rinsing predominantly one enantiomer from the surface of the smectic hydrogel; and extracting predominantly one enantiomer from the interior of the smectic hydrogel. The present invention also relates to a smectic hydrogel prepared according to an aforementioned method.

  7. Chemical stability of oseltamivir in oral solutions.

    PubMed

    Albert, K; Bockshorn, J

    2007-09-01

    The stability of oseltamivir in oral aqueous solutions containing the preservative sodium benzoate was studied by a stability indicating HPLC-method. The separation was achieved on a RP-18 ec column using a gradient of mobile phase A (aqueous solution of 50 mM ammonium acetate) and mobile phase B (60% (v/v) acetonitrile/40% (v/v) mobile phase A). The assay was subsequently validated according to the ICH guideline Q2(R1). The extemporaneously prepared "Oseltamivir Oral Solution 15 mg/ml for Adults or for Children" (NRF 31.2.) according to the German National Formulary ("Neues Rezeptur-Formularium") was stable for 84 days if stored under refrigeration. After storage at 25 degrees C the content of oseltamivir decreased to 98.4%. Considering the toxicological limit of 0.5% of the 5-acetylamino derivative (the so-called isomer I) the solution is stable for 46 days. Oseltamivir was less stable in a solution prepared with potable water instead of purified water. Due to an increasing pH the stability of this solution decreased to 14 days. Furthermore a white precipitate of mainly calcium phosphate was observed. The addition of 0.1% anhydrous citric acid avoided these problems and improved the stability of the solution prepared with potable water to 63 days. Sodium benzoate was stable in all oral solutions tested.

  8. A review of photocatalysts prepared by sol-gel method for VOCs removal.

    PubMed

    Tseng, Ting Ke; Lin, Yi Shing; Chen, Yi Ju; Chu, Hsin

    2010-05-28

    The sol-gel process is a wet-chemical technique (chemical solution deposition), which has been widely used in the fields of materials science, ceramic engineering, and especially in the preparation of photocatalysts. Volatile organic compounds (VOCs) are prevalent components of indoor air pollution. Among the approaches to remove VOCs from indoor air, photocatalytic oxidation (PCO) is regarded as a promising method. This paper is a review of the status of research on the sol-gel method for photocatalyst preparation and for the PCO purification of VOCs. The review and discussion will focus on the preparation and coating of various photocatalysts, operational parameters, and will provide an overview of general PCO models described in the literature.

  9. Non-aqueous solution preparation of doped and undoped Li{sub x}Mn{sub y}O{sub z}

    DOEpatents

    Boyle, T.J.; Voigt, J.A.

    1997-05-20

    A method is described for generation of phase-pure doped and undoped Li{sub x}Mn{sub y}O{sub z} precursors. The method of this invention uses organic solutions instead of aqueous solutions or nonsolution ball milling of dry powders to produce phase-pure precursors. These precursors can be used as cathodes for lithium-polymer electrolyte batteries. Dopants may be homogeneously incorporated to alter the characteristics of the powder. 1 fig.

  10. Consideration of Preventing Local Venous Pain by Dacarbazine.

    PubMed

    Ohtsubo, Tatsuya; Tsuji, Takumi; Umeyama, Takayo; Sudou, Miho; Komesu, Kana; Matsumoto, Minako; Yoshida, Yuya; Banno, Rie; Tomogane, Kanji; Fujita, Atsuo; Kohno, Takeyuki; Mikami, Tadashi

    2017-01-01

    Local venous pain caused by dacarbazine (DTIC) injection is due to its photodegradation product 5-diazoimidazole-4-carboxamide (Diazo-IC). The production of Diazo-IC can be decreased by protecting the drug from light. Furthermore, the production of Diazo-IC reportedly increases with time; however, there are no studies reporting the association between the injection preparation time and local venous pain caused by the DTIC injection. We evaluated the efficacy of the following: (1) method used to shorten the injection preparation time and (2) method used to change the diluting solution for DTIC. We found that shortening the injection preparation time tended to decrease the local venous pain expression due to DTIC, and Veen F decreased the production of Diazo-IC compared with the normal saline and 5% glucose solution. These results indicate that shortening the injection preparation time may be effective in preventing the local venous pain caused by the DTIC injection; moreover, using Veen F for DTIC may also reduce the pain.

  11. Extending the solvent-free MALDI sample preparation method.

    PubMed

    Hanton, Scott D; Parees, David M

    2005-01-01

    Matrix-assisted laser desorption/ionization (MALDI) mass spectrometry is an important technique to characterize many different materials, including synthetic polymers. MALDI mass spectral data can be used to determine the polymer average molecular weights, repeat units, and end groups. One of the key issues in traditional MALDI sample preparation is making good solutions of the analyte and the matrix. Solvent-free sample preparation methods have been developed to address these issues. Previous results of solvent-free or dry prepared samples show some advantages over traditional wet sample preparation methods. Although the results of the published solvent-free sample preparation methods produced excellent mass spectra, we found the method to be very time-consuming, with significant tool cleaning, which presents a significant possibility of cross contamination. To address these issues, we developed an extension of the solvent-free method that replaces the mortar and pestle grinding with ball milling the sample in a glass vial with two small steel balls. This new method generates mass spectra with equal quality of the previous methods, but has significant advantages in productivity, eliminates cross contamination, and is applicable to liquid and soft or waxy analytes.

  12. Liquid chromatographic extraction medium

    DOEpatents

    Horwitz, E. Philip; Dietz, Mark L.

    1994-01-01

    A method and apparatus for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column is described. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water.

  13. Polybenzoxazole via aromatic nucleophilic displacement

    NASA Technical Reports Server (NTRS)

    Hergenrother, Paul M. (Inventor); Connell, John W. (Inventor); Smith, Joseph G., Jr. (Inventor)

    1993-01-01

    Polybenzoxazoles (PBO) are heterocyclic macromolecules which were first synthesized in a two-step process by the initial formation of aromatic diacid chlorides with bis(o-aminophenol)s through solution condensation of aromatic diacid chlorides with bis(o-aminophenol)s followed by thermal cyclodehydration. Since then several methods were utilized in their synthesis. The most common synthetic method for PBO involves a polycondensation of bis(o-aminophenol)s with aromatic diacid diphenyl esters. Another preparative route involves the solution polycondensation of the hydrochloride salts of bis(o-amino phenol)s with aromatic diacids in polyphosphoric acid. Another synthetic method involves the initial formation of poly(o-hydroxy amide)s from silylated bis(o-aminophenol)s with aromatic diacid chlorides followed by thermal cyclodehydration to PBO. A recent preparative route involves the reaction of aromatic bisphenols with bis(fluorophenyl) benzoxazoles by the displacement reaction to form PBO. The novelty of the present invention is that high molecular weight PBO of new chemical structures are prepared that exhibit a favorable combination of physical and mechanical properties.

  14. METHOD OF PREPARING COMPLEXES OF PLUTONIUM WITH DIKETONES

    DOEpatents

    Dixon, J.S.; Katz, J.J.; Orlemann, E.F.

    1961-06-20

    A process is described for sepsrating Pu from an aqueous alkaline solution by either precipitating with a beta -diketone or extracting into a solution of the beta -dixetone in an organic water-immiscible solvent. Acetyl acetone and benzoyl acetone are the beta -diketones used.

  15. Fabrication of Semiconducting Methylammonium Lead Halide Perovskite Particles by Spray Technology

    NASA Astrophysics Data System (ADS)

    Ahmadian-Yazdi, Mohammad-Reza; Eslamian, Morteza

    2018-01-01

    In this "nano idea" paper, three concepts for the preparation of methylammonium lead halide perovskite particles are proposed, discussed, and tested. The first idea is based on the wet chemistry preparation of the perovskite particles, through the addition of the perovskite precursor solution to an anti-solvent to facilitate the precipitation of the perovskite particles in the solution. The second idea is based on the milling of a blend of the perovskite precursors in the dry form, in order to allow for the conversion of the precursors to the perovskite particles. The third idea is based on the atomization of the perovskite solution by a spray nozzle, introducing the spray droplets into a hot wall reactor, so as to prepare perovskite particles, using the droplet-to-particle spray approach (spray pyrolysis). Preliminary results show that the spray technology is the most successful method for the preparation of impurity-free perovskite particles and perovskite paste to deposit perovskite thin films. As a proof of concept, a perovskite solar cell with the paste prepared by the sprayed perovskite powder was successfully fabricated.

  16. Fabrication of Semiconducting Methylammonium Lead Halide Perovskite Particles by Spray Technology.

    PubMed

    Ahmadian-Yazdi, Mohammad-Reza; Eslamian, Morteza

    2018-01-10

    In this "nano idea" paper, three concepts for the preparation of methylammonium lead halide perovskite particles are proposed, discussed, and tested. The first idea is based on the wet chemistry preparation of the perovskite particles, through the addition of the perovskite precursor solution to an anti-solvent to facilitate the precipitation of the perovskite particles in the solution. The second idea is based on the milling of a blend of the perovskite precursors in the dry form, in order to allow for the conversion of the precursors to the perovskite particles. The third idea is based on the atomization of the perovskite solution by a spray nozzle, introducing the spray droplets into a hot wall reactor, so as to prepare perovskite particles, using the droplet-to-particle spray approach (spray pyrolysis). Preliminary results show that the spray technology is the most successful method for the preparation of impurity-free perovskite particles and perovskite paste to deposit perovskite thin films. As a proof of concept, a perovskite solar cell with the paste prepared by the sprayed perovskite powder was successfully fabricated.

  17. Method for preparing high specific activity 177Lu

    DOEpatents

    Mirzadeh, Saed; Du, Miting; Beets, Arnold L.; Knapp, Jr., Furn F.

    2004-04-06

    A method of separating lutetium from a solution containing Lu and Yb, particularly reactor-produced .sup.177 Lu and .sup.177 Yb, includes the steps of: providing a chromatographic separation apparatus containing LN resin; loading the apparatus with a solution containing Lu and Yb; and eluting the apparatus to chromatographically separate the Lu and the Yb in order to produce high-specific-activity .sup.177 Yb.

  18. Growth of antimony doped P-type zinc oxide nanowires for optoelectronics

    DOEpatents

    Wang, Zhong Lin; Pradel, Ken

    2016-09-27

    In a method of growing p-type nanowires, a nanowire growth solution of zinc nitrate (Zn(NO.sub.3).sub.2), hexamethylenetetramine (HMTA) and polyethylenemine (800 M.sub.w PEI) is prepared. A dopant solution to the growth solution, the dopant solution including an equal molar ration of sodium hydroxide (NaOH), glycolic acid (C.sub.2H.sub.4O.sub.3) and antimony acetate (Sb(CH.sub.3COO).sub.3) in water is prepared. The dopant solution and the growth solution combine to generate a resulting solution that includes antimony to zinc in a ratio of between 0.2% molar to 2.0% molar, the resulting solution having a top surface. An ammonia solution is added to the resulting solution. A ZnO seed layer is applied to a substrate and the substrate is placed into the top surface of the resulting solution with the ZnO seed layer facing downwardly for a predetermined time until Sb-doped ZnO nanowires having a length of at least 5 .mu.m have grown from the ZnO seed layer.

  19. Structure and magnetic/electrochemical properties of Cu-doped BiFeO3 nanoparticles prepared by a simple solution method

    NASA Astrophysics Data System (ADS)

    Khajonrit, Jessada; Phumying, Santi; Maensiri, Santi

    2016-06-01

    BiFe1- x Cu x O3 (x = 0, 0.05, 0.1, 0.2, and 0.3) nanoparticles were prepared by a simple solution method. The prepared nanoparticles were characterized by X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM), Brunauer-Emmett-Teller (BET) method analysis using the Barret-Joyner-Halenda (BJH) model, and X-ray absorption spectroscopy (XAS). Magnetization properties were obtained using a vibrating sample magnetometer (VSM) at room temperature. Magnetization was clearly enhanced by increasing Cu content and decreasing particle size. Zero-field-cooled (ZFC) and field-cooled (FC) temperature-dependent magnetization measurements showed that blocking temperature increased with increasing Cu content. Electrochemical properties were investigated by cyclic voltammetry (CV) and the galvanostatic charge-discharge (GCD) method. The performance of the fabricated supercapacitor was improved for the BiFe0.95Cu0.05O3 electrode. The highest specific capacitance was 568.13 F g-1 at 1 A g-1 and the capacity retention was 77.13% after 500 cycles.

  20. [Islet isolation outcome is influenced by pancreas preparation method].

    PubMed

    Pokrywczyńska, Marta; Drewa, Tomasz; Cieślak, Zaneta

    2008-09-01

    Pancreatic islet transplantation is a treatment method for type I diabetes. Its outcome is influenced by numerous factors, islet quantity and function being important ones of them. was to estimate the influence of pancreas preparation method on the outcome of islet isolation in rat. 6 pancreata harvested from Lewis rats were used in this research. Pancreatic duct was cannulated and pancreas was injected with 1 mg/ml collagenase P solution (Sigma) and then excised. After cutting into smaller fragments, it was digested in collagenase P solution for 15-20 min. Enzyme activity was then stopped by adding dilution medium. Heterogenous cell suspension was centrifuged in density gradient (Gradisol) to isolate islets. Pancreatic islets were collected and islet equivalent was calculated. Islet purity degree was estimated as islet cells to all cells, including exocrine, ratio. Islet viability was estimated using propidium iodide and fluorescein diacetate staining. Photographic documentation was made. Proper islet morphology, highest number and viability was obtained when pancreas was excised properly (isolation 3 and 4). Pancreas preparation method is one of which influences on islet isolation outcome.

  1. Development and validation of a single robust HPLC method for the characterization of a pharmaceutical starting material and impurities from three suppliers using three separate synthetic routes.

    PubMed

    Sheldon, E M; Downar, J B

    2000-08-15

    Novel approaches to the development of analytical procedures for monitoring incoming starting material in support of chemical/pharmaceutical processes are described. High technology solutions were utilized for timely process development and preparation of high quality clinical supplies. A single robust HPLC method was developed and characterized for the analysis of the key starting material from three suppliers. Each supplier used a different process for the preparation of this material and, therefore, each suppliers' material exhibited a unique impurity profile. The HPLC method utilized standard techniques acceptable for release testing in a QC/manufacturing environment. An automated experimental design protocol was used to characterize the robustness of the HPLC method. The method was evaluated for linearity, limit of quantitation, solution stability, and precision of replicate injections. An LC-MS method that emulated the release HPLC method was developed and the identities of impurities were mapped between the two methods.

  2. Color-tunable up-conversion emission in Y2O3:Yb3+, Er3+ nanoparticles prepared by polymer complex solution method

    PubMed Central

    2013-01-01

    Abstract Powders of Y2O3 co-doped with Yb3+ and Er3+ composed of well-crystallized nanoparticles (30 to 50 nm in diameter) with no adsorbed ligand species on their surface are prepared by polymer complex solution method. These powders exhibit up-conversion emission upon 978-nm excitation with a color that can be tuned from green to red by changing the Yb3+/Er3+ concentration ratio. The mechanism underlying up-conversion color changes is presented along with material structural and optical properties. PACS 42.70.-a, 78.55.Hx, 78.60.-b PMID:23522083

  3. Efficient solar-assisted O2 reduction by a cofacial iron porphyrin dimer integrated to a p-CuBi2O4 photocathode prepared by a simple novel method.

    PubMed

    Zahran, Zaki N; Mohamed, Eman A; Naruta, Yoshinori; Haleem, Ashraf

    2017-10-04

    A cofacial iron porphyrin hetero-dimer, Fe2TPFPP-TMP showed high electro-catalytic activity, selectivity, and stability for the O2 reduction to H2O both in homogeneous non-aqueous and heterogeneous neutral aqueous solutions. Moreover, when it is integrated to FTO/p-CuBi2O4 (FTO = fluorine doped tin oxide) photocathode prepared by a simple novel method, a remarkable efficient solar-assisted O2 reduction is achieved in neutral potassium phosphate (KPi) or basic NaOH solutions saturated with O2. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Facile and Rapid Growth of Nanostructured Ln-BTC Metal-Organic Framework Films by Electrophoretic Deposition for Explosives sensing in Gas and Cr 3+ Detection in Solution.

    PubMed

    Feng, Ji-Fei; Yang, Xue; Gao, Shui-Ying; Shi, Jianlin; Cao, Rong

    2017-12-19

    Until now, it has been a challenge to prepare lanthanide metal-organic framework films on traditional substrates, like zinc plate, indium oxide (ITO), and fluorine-doped tin oxide (FTO) glasses in a rapid and facile method. In this paper, continuous and dense Ln-BTC MOFs films on unmodified low-cost substrates have been rapidly and easily fabricated though the newly developed electrophoretic deposition (EPD) method in 5 min. Moreover, the as-prepared luminescent films were successfully used for the detection of nitrobenzene (NB), trinitrotoluene (TNT) in gas phases, as well as NB, Cr 3+ ions for detection in solution.

  5. Preparation of chitosan/tripolyphosphate nanoparticles with highly tunable size and low polydispersity.

    PubMed

    Sawtarie, Nader; Cai, Yuhang; Lapitsky, Yakov

    2017-09-01

    Nanoparticles prepared through the ionotropic gelation of chitosan with tripolyphosphate (TPP) have been extensively studied as vehicles for drug and gene delivery. Though a number of these works have focused on preparing particles with narrow size distributions, the monodisperse particles produced by these methods have been limited to narrow size ranges (where the average particle size was not varied by more than twofold). Here we show how, by tuning the NaCl concentration in the parent chitosan and TPP solutions, low-polydispersity particles with z-average diameters ranging between roughly 100 and 900nm can be prepared. Further, we explore how the size of these particles depends on the method by which the TPP is mixed into the chitosan solution, specifically comparing: (1) single-shot mixing; (2) dropwise addition; and (3) a dilution technique, where chitosan and TPP are codissolved at a high (gelation-inhibiting) ionic strength and then diluted to lower ionic strengths to trigger gelation. Though the particle size increases sigmoidally with the NaCl concentration for all three mixing methods, the dilution method delivers the most uniform/gradual size increase - i.e., it provides the most precise control. Also investigated are the effects of mixture composition and mixing procedure on the particle yield. These reveal the particle yield to increase with the chitosan/TPP concentration, decrease with the NaCl concentration, and vary only weakly with the mixing protocol; thus, at elevated NaCl concentrations, it may be beneficial to increase chitosan and TPP concentrations to ensure high particle yields. Finally, possible pitfalls of the salt-assisted size control strategy (and their solutions) are discussed. Taken together, these findings provide a simple and reliable method for extensively tuning chitosan/TPP particle size while maintaining narrow size distributions. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. A Novel Approach Toward Fabrication of High Performance Thin Film Composite Polyamide Membranes.

    PubMed

    Khorshidi, Behnam; Thundat, Thomas; Fleck, Brian A; Sadrzadeh, Mohtada

    2016-02-29

    A practical method is reported to enhance water permeability of thin film composite (TFC) polyamide (PA) membranes by decreasing the thickness of the selective PA layer. The composite membranes were prepared by interfacial polymerization (IP) reaction between meta-phenylene diamine (MPD)-aqueous and trimesoyl chloride (TMC)-organic solvents at the surface of polyethersulfone (PES) microporous support. Several PA TFC membranes were prepared at different temperatures of the organic solution ranging from -20 °C to 50 °C. The physico-chemical and morphological properties of the synthesized membranes were carefully characterized using serval analytical techniques. The results confirmed that the TFC membranes, synthesized at sub-zero temperatures of organic solution, had thinner and smoother PA layer with a greater degree of cross-linking and wettability compared to the PA films prepared at 50 °C. We demonstrated that reducing the temperature of organic solution effectively decreased the thickness of the PA active layer and thus enhanced water permeation through the membranes. The most water permeable membrane was prepared at -20 °C and exhibited nine times higher water flux compared to the membrane synthesized at room temperature. The method proposed in this report can be effectively applied for energy- and cost-efficient development of high performance nanofiltration and reverse osmosis membranes.

  7. Preparation of transition metal nanoparticles and surfaces modified with (CO)polymers synthesized by RAFT

    DOEpatents

    McCormick, III., Charles L.; Lowe, Andrew B.; Sumerlin, Brent S.

    2006-11-21

    A new, facile, general one-phase method of generating thio-functionalized transition metal nanoparticles and surfaces modified by (co)polymers synthesized by the RAFT method is described. The method includes the stops of forming a (co)polymer in aqueous solution using the RAFT methodology, forming a colloidal transition metal precursor solution from an appropriate transition metal; adding the metal precursor solution or surface to the (co)polymer solution, adding a reducing agent into the solution to reduce the metal colloid in situ to produce the stabilized nanoparticles or surface, and isolating the stabilized nanoparticles or surface in a manner such that aggregation is minimized. The functionalized surfaces generated using these methods can further undergo planar surface modifications, such as functionalization with a variety of different chemical groups, expanding their utility and application.

  8. Preparation of transition metal nanoparticles and surfaces modified with (co)polymers synthesized by RAFT

    DOEpatents

    McCormick, III, Charles L.; Lowe, Andrew B [Hattiesburg, MS; Sumerlin, Brent S [Pittsburgh, PA

    2011-12-27

    A new, facile, general one-phase method of generating thiol-functionalized transition metal nanoparticles and surfaces modified by (co)polymers synthesized by the RAFT method is described. The method includes the steps of forming a (co)polymer in aqueous solution using the RAFT methodology, forming a colloidal transition metal precursor solution from an appropriate transition metal; adding the metal precursor solution or surface to the (co)polymer solution, adding a reducing agent into the solution to reduce the metal colloid in situ to produce the stabilized nanoparticles or surface, and isolating the stabilized nanoparticles or surface in a manner such that aggregation is minimized. The functionalized surfaces generated using these methods can further undergo planar surface modifications, such as functionalization with a variety of different chemical groups, expanding their utility and application.

  9. Study of stability of methotrexate in acidic solution spectrofluorimetric determination of methotrexate in pharmaceutical preparations through acid-catalyzed degradation reaction.

    PubMed

    Sabry, Suzy M; Abdel-Hady, M; Elsayed, M; Fahmy, Osama T; Maher, Hadir M

    2003-07-14

    Study of the degradation reaction of methotrexate (MTX) in acidic solution was carried out. Optimization of the experimental parameters of MTX acid hydrolysis was investigated. Spectrofluorimetric method for determination of MTX through measurement of its acid-degradation product, 4-amino-4-deoxy-10-methylpteroic acid (AMP), was developed. Stability of the standard solution of MTX prepared in sulfuric acid was discussed in the view of accelerated stability analysis. Two other comparative spectroflourimetric methods based on measuring the fluorescence intensities from either a condensation reaction with acetylacetone-formaldehyde (Hantzsch reaction) or a reaction with fluorescamine were also described. Beer's law validation, accuracy, precision, limits of detection, limits of quantification, and other aspects of analytical merit are presented in the text. The proposed methods were successfully applied for the analysis of MTX in pure drug and tablets dosage form. The sensitivity of the developed methods was favorable, so it was possible to be adopted for determination of MTX in plasma samples for routine use in high-dose MTX therapy.

  10. Determination of berberine in pharmaceutical preparations using acidic hydrogen peroxide-nitrite chemiluminescence system.

    PubMed

    Liang, Yao-Dong; Yu, Chun-Xia

    2013-03-01

    A stronger chemiluminescence (CL) was observed when hydrogen peroxide was mixed with nitrite and berberine in sulfuric acid solution. The stronger CL originated from peroxidation of berberine by peroxynitrous acid that was synthesized online by the mixing of acidic hydrogen peroxide solution with nitrite solution in a flow system. The emitting species was excited state oxyberberine, a peroxidized product of berberine. Based on the stronger CL, a flow injection CL method for the determination of berberine was proposed. Under optimum experimental conditions, the stronger CL intensity was linearly related to the concentration of berberine over the range of 2.0 × 10(-7) -2.0 × 10(-5) mol L(-1) . The limit of detection (s/n = 3) was 6.2 × 10(-8) mol L(-1) . The proposed method has been evaluated by analyzing berberine in pharmaceutical preparations. Copyright © 2011 John Wiley & Sons, Ltd.

  11. Liquid chromatographic extraction medium

    DOEpatents

    Horwitz, E.P.; Dietz, M.L.

    1994-09-13

    A method and apparatus are disclosed for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water. 1 fig.

  12. Apparatus and method for preparing oxygen-15 labeled water H.sub.2 [.sup.15 O] in an injectable form for use in positron emission tomography

    DOEpatents

    Ferrieri, Richard A.; Schlyer, David J.; Alexoff, David

    1996-01-09

    A handling and processing apparatus for preparing Oxygen-15 labeled water (H.sub.2 [.sup.15 O]) in injectable form for use in Positron Emission Tomography from preferably H.sub.2 [.sup.15 O] produced by irradiating a flowing gas target of nitrogen and hydrogen. The apparatus includes a collector for receiving and directing a gas containing H.sub.2 [.sup.15 O] gas and impurities, mainly ammonia (NH.sub.3) gas into sterile water to trap the H.sub.2 [.sup.15 O] and form ammonium (NH.sub.4.sup.+) in the sterile water. A device for displacing the sterile water containing H.sub.2 [.sup.15 O] and NH.sub.4.sup.+ through a cation resin removes NH.sub.4.sup.+ from the sterile water. A device for combining the sterile water containing H.sub.2 [.sup.15 O] with a saline solution produces an injectable solution. Preferably, the apparatus includes a device for delivering the solution to a syringe for injection into a patient. Also, disclosed is a method for preparing H.sub.2 [.sup.15 O] in injectable form for use in Positron Emission Tomography in which the method neither requires isotopic exchange reaction nor application of high temperature.

  13. Can intra-radicular cleaning protocols increase the retention of fiberglass posts? A systematic review.

    PubMed

    Oliveira, Lilian Vieira; Maia, Thais Souza; Zancopé, Karla; Menezes, Murilo de Souza; Soares, Carlos José; Moura, Camilla Christian Gomes

    2018-03-15

    The presence of residues within the root canal after post-space preparation can influence the bond strength between resin cement and root dentin when using fiberglass posts (FGPs). Currently, there is no consensus in the literature regarding what is the best solution for the removal of debris after post-space preparation. This systematic review involved "in vitro" studies to investigate if cleaning methods of the root canal after post-space preparation can increase the retention of FGPs evaluated by the push-out test. Searches were carried out in PubMed (MEDLINE) and Scopus databases up to July2017. English language studies published from 2007 to July 2017 were selected. 475 studies were found, and 9 were included in this review. Information from the 9 studies were collected regarding the number of samples, storage method after extraction, root canal preparation, method of post-space preparation, endodontic sealer, resin cement, cleaning methods after post-space and presence of irrigant activation. Five studies presented the best results for the association of sodium hypochlorite (NaOCl) and ethylenediamine tetra-acetic acid (EDTA), while in the other 4 studies, the solutions that showed improved retention of FGPs were photon-induced photoacoustic streaming (PIPS), Qmix, Sikko and EDTA. The results showed heterogeneity in all comparisons due to a high variety of information about cleaning methods, different concentrations, application time, type of adhesive system and resin cements used. In conclusion, this review suggests that the use of NaOCl/EDTA results in the retention of FGPs and may thus be recommended as a post-space cleaning method influencing the luting procedure.

  14. Implementation Study of Patient-Ready Syringes Containing 25 mg/mL Methotrexate Solution for Use in Treating Ectopic Pregnancy

    PubMed Central

    Respaud, R.; Gaudy, A. S.; Arlicot, C.; Tournamille, J. F.; Viaud-Massuard, M. C.; Elfakir, C.; Antier, D.

    2014-01-01

    Background. Ectopic pregnancy (EP) is a significant cause of morbidity and mortality during the first trimester of pregnancy. Small unruptured tubal pregnancies can be treated medically with a single dose of methotrexate (MTX). Objective. The aim of this study was to evaluate the stability of a 25 mg/mL solution of MTX to devise a secure delivery circuit for the preparation and use of this medication in the management of EP. Method. MTX solutions were packaged in polypropylene syringes, stored over an 84-day period, and protected from light either at +2 to +8°C or at 23°C. We assessed the physical and chemical stability of the solutions at various time points over the storage period. A pharmaceutical delivery circuit was implemented that involved the batch preparation of MTX syringes. Results. We show that 25 mg/mL MTX solutions remain stable over an 84-day period under the storage conditions tested. Standard doses were prepared, ranging from 50 mg to 100 mg. The results of this study suggest that MTX syringes can be prepared in advance by the pharmacy, ready to be dispensed at any time that a diagnosis of EP is made. Conclusion. The high stability of a 25 mg/mL MTX solution in polypropylene syringes makes it possible to implement a flexible and cost-effective delivery circuit for ready-to-use preparations of this drug, providing 24-hour access and preventing treatment delays. PMID:24900977

  15. A Review of Photocatalysts Prepared by Sol-Gel Method for VOCs Removal

    PubMed Central

    Tseng, Ting Ke; Lin, Yi Shing; Chen, Yi Ju; Chu, Hsin

    2010-01-01

    The sol-gel process is a wet-chemical technique (chemical solution deposition), which has been widely used in the fields of materials science, ceramic engineering, and especially in the preparation of photocatalysts. Volatile organic compounds (VOCs) are prevalent components of indoor air pollution. Among the approaches to remove VOCs from indoor air, photocatalytic oxidation (PCO) is regarded as a promising method. This paper is a review of the status of research on the sol-gel method for photocatalyst preparation and for the PCO purification of VOCs. The review and discussion will focus on the preparation and coating of various photocatalysts, operational parameters, and will provide an overview of general PCO models described in the literature. PMID:20640156

  16. Preparation of colloidal gold for staining proteins electrotransferred onto nitrocellulose membranes.

    PubMed

    Yamaguchi, K; Asakawa, H

    1988-07-01

    This paper describes a simple method of preparing colloidal gold for staining protein blots. Colloidal gold was prepared from 0.005 or 0.01% HAuCl4 by the addition of formalin as a reductant and potassium hydroxide. Staining of small cell carcinoma tissue extract blotted onto nitrocellulose membranes with this colloidal gold solution resulted in the appearance of a large number of clear wine-red bands. The sensitivity of gold staining was 60 times higher than that of Coomassie brilliant blue staining and almost comparable to that of silver staining of proteins in polyacrylamide gel. The sensitivity of this method was also satisfactory in comparison with that of enzyme immunoblotting. The colloidal gold prepared by this method is usable for routine work.

  17. Quantitative Analysis of Heavy Metals in Water Based on LIBS with an Automatic Device for Sample Preparation

    NASA Astrophysics Data System (ADS)

    Hu, Li; Zhao, Nanjing; Liu, Wenqing; Meng, Deshuo; Fang, Li; Wang, Yin; Yu, Yang; Ma, Mingjun

    2015-08-01

    Heavy metals in water can be deposited on graphite flakes, which can be used as an enrichment method for laser-induced breakdown spectroscopy (LIBS) and is studied in this paper. The graphite samples were prepared with an automatic device, which was composed of a loading and unloading module, a quantitatively adding solution module, a rapid heating and drying module and a precise rotating module. The experimental results showed that the sample preparation methods had no significant effect on sample distribution and the LIBS signal accumulated in 20 pulses was stable and repeatable. With an increasing amount of the sample solution on the graphite flake, the peak intensity at Cu I 324.75 nm accorded with the exponential function with a correlation coefficient of 0.9963 and the background intensity remained unchanged. The limit of detection (LOD) was calculated through linear fitting of the peak intensity versus the concentration. The LOD decreased rapidly with an increasing amount of sample solution until the amount exceeded 20 mL and the correlation coefficient of exponential function fitting was 0.991. The LOD of Pb, Ni, Cd, Cr and Zn after evaporating different amounts of sample solution on the graphite flakes was measured and the variation tendency of their LOD with sample solution amounts was similar to the tendency for Cu. The experimental data and conclusions could provide a reference for automatic sample preparation and heavy metal in situ detection. supported by National Natural Science Foundation of China (No. 60908018), National High Technology Research and Development Program of China (No. 2013AA065502) and Anhui Province Outstanding Youth Science Fund of China (No. 1108085J19)

  18. Antireflective graded index silica coating, method for making

    DOEpatents

    Yoldas, Bulent E.; Partlow, Deborah P.

    1985-01-01

    Antireflective silica coating for vitreous material is substantially non-reflecting over a wide band of radiations. This is achieved by providing the coating with a graded degree of porosity which grades the index of refraction between that of air and the vitreous material of the substrate. To prepare the coating, there is first prepared a silicon-alkoxide-based coating solution of particular polymer structure produced by a controlled proportion of water to alkoxide and a controlled concentration of alkoxide to solution, along with a small amount of catalyst. The primary solvent is alcohol and the solution is polymerized and hydrolized under controlled conditions prior to use. The prepared solution is applied as a film to the vitreous substrate and rapidly dried. It is thereafter heated under controlled conditions to volatilize the hydroxyl radicals and organics therefrom and then to produce a suitable pore morphology in the residual porous silica layer. The silica layer is then etched in order to enlarge the pores in a graded fashion, with the largest of the pores remaining being sufficiently small that radiations to be passed through the substrate are not significantly scattered. For use with quartz substrates, extremely durable coatings which display only 0.1% reflectivity have been prepared.

  19. Effect of heterocyclic based organoclays on the properties of polyimide-clay nanocomposites.

    PubMed

    Krishnan, P Santhana Gopala; Joshi, Mangala; Bhargava, Prachur; Valiyaveettil, Suresh; He, Chaobin

    2005-07-01

    Polyimide-clay nanocomposites were prepared from their precursor, namely, polyamic acid, by the solution-casting method. Organomodified montmorillonite (MMT) clay was prepared by treating Na+MMT (Kunipia F) with three different intercalating agents, namely, piperazine dihydrochloride, 1,3-bis(4-piperidinylpropane) dihydrochloride and 4,4'-bipiperidine dihydrochloride at 80 degrees C. Polyamic acid solutions containing various weight percentages of organomodified MMT were prepared by reacting 4,4'-(1,1'-biphenyl-4,4'-diyldioxy)dianiline with bicyclo[2.2.2]oct-7-ene-2,3,5,6-tetracarboxylic dianhydride in N-methyl-2-pyrrolidinone containing dispersed particles of organomodified MMT at 20 degrees C. Nanocomposite films were prepared from these solutions by solution casting and heated subsequently at a programmed heating rate. These films were transparent and brown in color. The extent of layer separation in nanocomposite films depends upon the chemical structure of the organoclay. These films were characterized by inherent viscosity, FT-IR, DSC, TMA, WAXD, TEM, UV, and TGA. The tensile behavior and surface energy studies were also investigated. The nanocomposite films had superior tensile properties, thermal behavior, and solvent resistance. Among the three organoclays, piperazine dihydrochloride was the best modifier.

  20. Binary ferrihydrite catalysts

    DOEpatents

    Huffman, Gerald P.; Zhao, Jianmin; Feng, Zhen

    1996-01-01

    A method of preparing a catalyst precursor comprises dissolving an iron salt and a salt of an oxoanion forming agent, in water so that a solution of the iron salt and oxoanion forming agent salt has a ratio of oxoanion/Fe of between 0.0001:1 to 0.5:1. Next is increasing the pH of the solution to 10 by adding a strong base followed by collecting of precipitate having a binary ferrihydrite structure. A binary ferrihydrite catalyst precursor is also prepared by dissolving an iron salt in water. The solution is brought to a pH of substantially 10 to obtain ferrihydrite precipitate. The precipitate is then filtered and washed with distilled water and subsequently admixed with a hydroxy carboxylic acid solution. The admixture is mixed/agitated and the binary ferrihydrite precipitate is then filtered and recovered.

  1. Method for producing UO$sub 2$ loaded refractory metals

    DOEpatents

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

    1973-12-11

    A finely divided dispersion of UO/sub 2/ in tungsten or molybdenum is prepared by co-precipitating the metals from mixed aqueous solution with oxine. The co-precipitate thus formed is separated from the solution, dried, calcined, and finally reduced to UO/sub 2/ and refractory metal. (Official Gazette)

  2. Specimen preparation for x-ray fluorescence analysis of solutions

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

    Eksperiandova, L.P.; Spolnik, Z.M.; Blank, A.B.

    1995-12-31

    Specimens for x-ray fluorescence analysis (XRFA) were prepared by adding dry gelatine (10%) to the analysis solution, homogenizing the mixture and cooling for 20 minutes. Thus, a compact resilient mass could be formed with the required shape and size; the roughness of the surface was determined by the roughness of the surface on which the specimen was formed, much the same as highly polished. Various calibration methods can be applied in the XRFA of a variety of materials if such specimens are used. 12 refs., 1 fig., 2 tabs.

  3. Preparation and use of crystalline bis-monoorganic phosphonate and phosphate salts of tetravalent metals

    DOEpatents

    Maya, L.

    1980-06-26

    A method of preparing and using the crystalline organic derivatives of the tetravalent metal phosphates and phosphonates provides for the contacting of an aqueous solution of a metal nitrate, with a solution of an organophosphorus acid for a period of time at room temperature that is sufficient for the formation of a metal phosphate product, and thereafter recovering said product. According to the invention, the product of the disclosed process is used in effecting analytical separations, such as ion exchange and chromatography.

  4. The Synthesis of 1,1’-Bicobaltocene Salts of Tetracyano-P-Quinodimethanide and the Sturcture of 1,1’-Bicobaltocene (Co (III) Co (III)) (TCNQ)3,

    DTIC Science & Technology

    1981-06-03

    Salts of Bicobaltocenet-The hexafluorophosphate salt of bicobaltocene(III,III) was prepared by the method of Davison and Smart 4 and the orange product...tetrahydrofuran. The lithium salt of TCNO was prepared by adding a boiling solution of lithium iodide in acetonitrile to a boiling solution of TCNQ in...compound 1,1’-bicobaltocene[Co(III)Co(III)[TCNQJ 3 resulted from the reaction of the mixed valence hexafluorophosphate salt with a mixture of [Et3NH

  5. Preparation of polymer-blended quinine nanocomposite particles by spray drying and assessment of their instrumental bitterness-masking effect using a taste sensor.

    PubMed

    Taki, Moeko; Tagami, Tatsuaki; Ozeki, Tetsuya

    2017-05-01

    The development of taste-masking technologies for foods and drugs is essential because it would enable people to consume and receive healthy and therapeutic effect without distress. In the current study, in order to develop a novel method to prepare nanocomposite particles (microparticles containing bitter nanoparticles) in only one step, by using spray drying, a two-solution mixing nozzle-equipped spray dryer that we previously reported was used. The nanocomposite particles with or without poorly water-soluble polymers prepared using our spray-drying technique were characterized. (1) The organic solution containing quinine, a model of bitter compound and poorly water-soluble polymers and (2) sugar alcohol (mannitol) aqueous solution were separately flown in tubes and two solutions were spray dried through two-solution type spray nozzle to prepare polymer-blended quinine nanocomposite particles. Mean diameters of nanoparticles, taste-masking effect and dissolution rate of quinine were evaluated. The results of taste masking by taste sensor suggested that the polymer (Eudragit EPO, Eudragit S100 or Ethyl cellulose)-blended quinine nanocomposite particles exhibited marked masking of instrumental quinine bitterness compared with the quinine nanocomposite particles alone. Quinine nanocomposite formulations altered the quinine dissolution rate, indicating that they can control intestinal absorption of quinine. These results suggest that polymer-blended quinine composite particles prepared using our spray-drying technique are useful for masking bitter tastes in the field of food and pharmaceutical industry.

  6. Preparation before colonoscopy: a randomized controlled trial comparing different regimes.

    PubMed

    Jansen, Sita V; Goedhard, Jelle G; Winkens, Bjorn; van Deursen, Cees Th B M

    2011-10-01

    A good bowel preparation is essential for optimal visualization of the large intestine. Several preparations with a difference in composition and volume are available. We compared five methods for bowel cleansing quality and patients' acceptability. Adult ambulatory outpatients scheduled for elective colonoscopy were randomized to receive 4-l polyethylene glycol (PEG) solution (Klean-prep), 2-l PEG solution+ascorbic acid (Moviprep), or a sodium phosphate (NaP) solution, Phosphoral. Patients with the PEG solutions were also randomized to receive simethicone (Aeropax), to investigate whether this improves the bowel cleansing efficacy. Before colonoscopy patients completed a questionnaire about the acceptability and tolerability of the preparation. Endoscopists blinded to the type of preparation gave a bowel cleansing score. Data were available for 461 patients. 2-l PEG+ascorbic acid was noninferior to 4-l PEG in bowel cleansing quality of rectosigmoid and colon. NaP was noninferior to 4-l PEG in bowel cleansing quality of rectosigmoid but inferior for the whole colon. Compliance was significantly less in the group with 4-l PEG compared with the 2-l PEG and NaP group. No difference was found for abdominal cramps. Taste was significantly better in the 2-l PEG group. Simethicone did not improve the bowel cleansing quality. 2-l PEG+ascorbic acid was noninferior to the 4-l PEG solution in bowel cleansing quality and was better in taste and compliance. NaP was inferior to 4-l PEG in bowel cleansing quality. Addition of simethicone gave no improvement.

  7. Synthesis and Photoluminescence Characteristics of Eu(3+)-Doped Molybdates Nanocrystals.

    PubMed

    Li, Fuhai; Yu, Lixin; Wei, Shuilin; Sun, Jiaju; Chen, Weiqing; Sun, Wei

    2015-12-01

    In this paper, the Eu(3+)-doped molybdate (CaMoO4, ZnMoO4 and BaMoO4) phosphors have been prepared by a hydrothermal method through modulating the pH value of the precursor solution (pH = 8, 10, and 12, respectively). The crystalline phase, morphology, photoluminescent properties of the prepared samples were systematically characterized by means of X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and photoluminescence (PL) spectra. The results indicate that the photoluminescence and morphology can be affected by the precursor solution. And the growth of the ZnMoO4 crystals also can be affected by the pH value of the precursor solution.

  8. Mechanism of Action and Toxicities of Purgatives Used for Colonoscopy Preparation

    PubMed Central

    Adamcewicz, Margaret; Bearelly, Dilip; Porat, Gail; Friedenberg, Frank K.

    2011-01-01

    Importance of the field In developed countries colonoscopy volume has increased dramatically over the past 15 years and is the principle method used to screen for colon cancer. Preparations used for colon cleaning have evolved over the past 30 years. Some preparations have been shown to be unsafe and are now used on a limited basis. There has been progress on limiting the volume required and on taste improvement. Areas covered in this review This review provides an account of preparations used from 1980 when polyethylene glycol-based preparations became widely available, until the present day. The review highlights their mechanism of action and principle toxicities. The handling of solutes and solute-free fluid by the colon is also reviewed. What the reader will gain The reader will gain a perspective on the factors considered in developing colonic purgatives and the rationale for choosing selected preparations based on patient factors such as age, co-morbidities, and concomitant medications. Take home message Although generally safe and effective, colonic purgatives have both acute and permanent toxicities. The safest preparations utilize polyethylene glycol combined with a balanced electrolyte solution. Limitations of this preparation center on the volume required and poor taste. Alternative formulations are now available; however those using sodium phosphate have fallen out of favor due to a risk of renal toxicity. PMID:21162694

  9. Temperature calibration of cryoscopic solutions used in the milk industry by adiabatic calorimetry

    NASA Astrophysics Data System (ADS)

    Méndez-Lango, E.; Lira-Cortes, L.; Quiñones-Ibarra, R.

    2013-09-01

    One method to detect extraneous water in milk is through cryoscopy. This method is used to measure the freezing point of milk. For calibration of a cryoscope there are is a set of standardized solution with known freezing points values. These values are related with the solute concentration, based in almost a century old data; it was no found recent results. It was found that reference solution are not certified in temperature: they do not have traceability to the temperature unit or standards. We prepared four solutions and measured them on a cryoscope and on an adiabatic calorimeter. It was found that results obtained with one technique dose not coincide with the other one.

  10. Preparation of thin ceramic films via an aqueous solution route

    DOEpatents

    Pederson, Larry R.; Chick, Lawrence A.; Exarhos, Gregory J.

    1989-01-01

    A new chemical method of forming thin ceramic films has been developed. An aqueous solution of metal nitrates or other soluble metal salts and a low molecular weight amino acid is coated onto a substrate and pyrolyzed. The amino acid serves to prevent precipitation of individual solution components, forming a very viscous, glass-like material as excess water is evaporated. Using metal nitrates and glycine, the method has been demonstrated for zirconia with various levels of yttria stabilization, for lanthanum-strontium chromites, and for yttrium-barium-copper oxide superconductors on various substrates.

  11. [Development of ICP-OES, ICP-MS and GF-AAS Methods for Simultaneous Quantification of Lead, Total Arsenic and Cadmium in Soft Drinks].

    PubMed

    Kataoka, Yohei; Watanabe, Takahiro; Hayashi, Tomoko; Teshima, Reiko; Matsuda, Rieko

    2015-01-01

    In this study, we developed methods to quantify lead, total arsenic and cadmium contained in various kinds of soft drinks, and we evaluated their performance. The samples were digested by common methods to prepare solutions for measurement by ICP-OES, ICP-MS and graphite furnace atomic absorption spectrometry (GF-AAS). After digestion, internal standard was added to the digestion solutions for measurements by ICP-OES and ICP-MS. For measurement by GF-AAS, additional purification of the digestion solution was conducted by back-extraction of the three metals into nitric acid solution after extraction into an organic solvent with ammonium pyrrolidine dithiocarbamate. Performance of the developed methods were evaluated for eight kinds of soft drinks.

  12. Administration of Substances to Laboratory Animals: Equipment Considerations, Vehicle Selection, and Solute Preparation

    PubMed Central

    Turner, Patricia V; Pekow, Cynthia; Vasbinder, Mary Ann; Brabb, Thea

    2011-01-01

    Administration of substances to laboratory animals requires careful consideration and planning to optimize delivery of the agent to the animal while minimizing potential adverse experiences from the procedure. The equipment selected to deliver substances to animals depends on the length of the study and the nature of the material being administered. This selection provides a significant opportunity for refining animal treatment. Similarly, when substances are administered as solutions or suspensions, attention should be given to selection of vehicles and methods used for preparing the solutions and suspensions. The research team, veterinarian, technical personnel, and IACUC members should be aware of reasons underlying selection of equipment for substance delivery and should consider carefully how substances will be prepared and stored prior to administration to animals. Failure to consider these factors during experimental planning may result in unintentional adverse effects on experimental animals and confounded results. PMID:22330706

  13. The preparation and degradation performance of CdS photocatalysts to methyl orange solution.

    PubMed

    Duan, Limei; Zhao, Weiqiang; Xu, Ling; Chen, Xiaohong; Lita, A; Liu, Zongrui

    2013-03-01

    In this paper, the CdS samples were prepared using thiourea or sodium sulfide as sulfur source by hydrothermal or solvothermal synthesis method, the results of XRD, TEM and SEM showed all the samples belong to hexagonal CdS nano-material with different morphologies. Using the degradation of methyl orange solution as a model reaction, the photocatalytic performance of different CdS samples was measured, and the samples prepared using thiourea as sulfur source exhibited better photocatalytic activity than those using sodium sulfide as sulfur source. The factors on degradation effect were discussed including the pH value of degradation system and the type of light source. The degradation effect of CdS samples increased with the pH value decreased, and the degradation effect was better when the methyl orange solution was irradiated under sunlight than under 250 W mercury lamp.

  14. Heterogeneity of activated carbons in adsorption of aniline from aqueous solutions

    NASA Astrophysics Data System (ADS)

    Podkościelny, P.; László, K.

    2007-08-01

    The heterogeneity of activated carbons (ACs) prepared from different precursors is investigated on the basis of adsorption isotherms of aniline from dilute aqueous solutions at various pH values. The APET carbon prepared from polyethyleneterephthalate (PET), as well as, commercial ACP carbon prepared from peat were used. Besides, to investigate the influence of carbon surface chemistry, the adsorption was studied on modified carbons based on ACP carbon. Its various oxygen surface groups were changed by both nitric acid and thermal treatments. The Dubinin-Astakhov (DA) equation and Langmuir-Freundlich (LF) one have been used to model the phenomenon of aniline adsorption from aqueous solutions on heterogeneous carbon surfaces. Adsorption-energy distribution (AED) functions have been calculated by using an algorithm based on a regularization method. Analysis of these functions for activated carbons studied provides important comparative information about their surface heterogeneity.

  15. Characterization of Polysulfone Membranes Prepared with Thermally Induced Phase Separation Technique

    NASA Astrophysics Data System (ADS)

    Tiron, L. G.; Pintilie, Ș C.; Vlad, M.; Birsan, I. G.; Baltă, Ș

    2017-06-01

    Abstract Membrane technology is one of the most used water treatment technology because of its high removal efficiency and cost effectiveness. Preparation techniques for polymer membranes show an important aspect of membrane properties. Generally, polysulfone (PSf) and polyethersulfone (PES) are used for the preparation of ultrafiltration (UF) membranes. Polysulfone (PSf) membranes have been widely used for separation and purification of different solutions because of their excellent chemical and thermal stability. Polymeric membranes were obtained by phase inversion method. The polymer solution introduced in the nonsolvent bath (distilled water) initiate the evaporation of the solvent from the solution, this phenomenon has a strong influence on the transport properties. The effect of the coagulation bath temperature on the membrane properties is of interest for this study. Membranes are characterized by pure water flux, permeability, porosity and retention of methylene blue. The low temperature of coagulation bath improve the membrane’s rejection and its influence was most notable.

  16. Preparation of Zeolite/Zinc Oxide Nanocomposites for toxic metals removal from water

    NASA Astrophysics Data System (ADS)

    Alswata, Abdullah A.; Ahmad, Mansor Bin; Al-Hada, Naif Mohammed; Kamari, Halimah Mohamed; Hussein, Mohd Zobir Bin; Ibrahim, Nor Azowa

    This research work has proposed preparation of Zeolite/Zinc Oxide Nanocomposite (Zeolite/ZnO NCs) by using a co-precipitation method. Then, the prepared Nanocomposite has been tested for adsorption of Lead Pb (II) and Arsenic As (V) from aqueous solution under the room pressure and temperature. After that, the prepared adsorbent has been studied by several techniques. For adsorption process; the effect of the adsorbent masses, contact time, PH and initial metals concentration as well as, the kinetics and isotherm for adsorption process have been investigated. The results revealed that; ZnO nanoparticles (NPs) with average diameter 4.5 nm have successfully been loaded into Zeolite. The optimum parameters for the removal of the toxic metals 93% and 89% of Pb (II) and As (V), respectively, in 100 mg/L aqua solutions were pH4, 0.15 g and 30 min. According to the obtained results; pseudo second-order kinetic and Langmuir isotherm model have higher correlation coefficients and provided a better agreement with the experimental data. The prepared sorbent showed an economical and effective way to remove the heavy toxic metals due to its ambient operation conditions, low- consumption energy and facile regeneration method.

  17. Using Silica Sol as a Nanoglue to Prepare Nanoscale Mesoporous Composite Gel and Aerogels

    DTIC Science & Technology

    2000-03-31

    solution-phase reactants remain unaltered. Furthermore, the composite constitutes a rigid solid architecture, such that the silica aerogel structure...nm) was immobilized in a silica aerogel structure according to the method of the present invention. The optical properties of 9 these materials...Aerogel Preparation. Acid- and base-catalyzed silica aerogels were prepared by procedures similarto those previously published in Russo et al.J.Non

  18. Surface engineered nanoparticles for improved surface enhanced Raman scattering applications and method for preparing same

    DOEpatents

    Simmons, Blake A [San Francisco, CA; Talin, Albert Alec [Livermore, CA

    2009-11-27

    A method for producing metal nanoparticles that when associated with an analyte material will generate an amplified SERS spectrum when the analyte material is illuminated by a light source and a spectrum is recorded. The method for preparing the metal nanoparticles comprises the steps of (i) forming a water-in-oil microemulsion comprising a bulk oil phase, a dilute water phase, and one or more surfactants, wherein the water phase comprises a transition metal ion; (ii) adding an aqueous solution comprising a mild reducing agent to the water-in-oil microemulsion; (iii) stirring the water-in-oil microemulsion and aqueous solution to initiate a reduction reaction resulting in the formation of a fine precipitate dispersed in the water-in-oil microemulsion; and (iv) separating the precipitate from the water-in-oil microemulsion.

  19. Voltammetric determination of copper in selected pharmaceutical preparations--validation of the method.

    PubMed

    Lutka, Anna; Maruszewska, Małgorzata

    2011-01-01

    It were established and validated the conditions of voltammetric determination of copper in pharmaceutical preparations. The three selected preparations: Zincuprim (A), Wapń, cynk, miedź z wit. C (B), Vigor complete (V) contained different salts and different quantity of copper (II) and increasing number of accompanied ingredients. For the purpose to transfer copper into solution, the samples of powdered tablets of the first and second preparation were undergone extraction and of the third the mineralization procedures. The concentration of copper in solution was determined by differential pulse voltammetry (DP) using comparison with standard technique. In the validation process, the selectivity, accuracy, precision and linearity of DP determination of copper in three preparations were estimated. Copper was determined within the concentration range of 1-9 ppm (1-9 microg/mL): the mean recoveries approached 102% (A), 100% (B), 102% (V); the relative standard deviations of determinations (RSD) were 0.79-1.59% (A), 0.62-0.85% (B) and 1.68-2.28% (V), respectively. The mean recoveries and the RSDs of determination satisfied the requirements for the analyte concentration at the level 1-10 ppm. The statistical verification confirmed that the tested voltammetric method is suitable for determination of copper in pharmaceutical preparation.

  20. Method of preparing silicon carbide particles dispersed in an electrolytic bath for composite electroplating of metals

    DOEpatents

    Peng, Yu-Min; Wang, Jih-Wen; Liue, Chun-Ying; Yeh, Shinn-Horng

    1994-01-01

    A method for preparing silicon carbide particles dispersed in an electrolytic bath for composite electroplating of metals includes the steps of washing the silicon carbide particles with an organic solvent; washing the silicon carbide particles with an inorganic acid; grinding the silicon carbide particles; and heating the silicon carbide particles in a nickel-containing solution at a boiling temperature for a predetermined period of time.

  1. Method of preparing high specific activity platinum-195m

    DOEpatents

    Mirzadeh, Saed; Du, Miting; Beets, Arnold L.; Knapp, Jr., Furn F.

    2004-06-15

    A method of preparing high-specific-activity .sup.195m Pt includes the steps of: exposing .sup.193 Ir to a flux of neutrons sufficient to convert a portion of the .sup.193 Ir to .sup.195m Pt to form an irradiated material; dissolving the irradiated material to form an intermediate solution comprising Ir and Pt; and separating the Pt from the Ir by cation exchange chromatography to produce .sup.195m Pt.

  2. Methods for dispersing hydrocarbons using autoclaved bacteria

    DOEpatents

    Tyndall, Richard L.

    1996-01-01

    A method of dispersing a hydrocarbon includes the steps: providing a bacterium selected from the following group: ATCC 85527, ATCC 75529, and ATCC 55638, a mutant of any one of these bacteria possessing all the identifying characteristics of any one of these bacteria, and mixtures thereof; autoclaving the bacterium to derive a dispersant solution therefrom; and contacting the dispersant solution with a hydrocarbon to disperse the hydrocarbon. Moreover, a method for preparing a dispersant solution includes the following steps: providing a bacterium selected from the following group: ATCC 75527, ATCC 75529, and ATCC 55638, a mutant of any one of these bacteria possessing all the identifying characteristics of any one of these bacteria, and mixtures thereof; and autoclaving the bacterium to derive a dispersant solution therefrom.

  3. Methods for dispersing hydrocarbons using autoclaved bacteria

    DOEpatents

    Tyndall, R.L.

    1996-11-26

    A method of dispersing a hydrocarbon includes the following steps: providing a bacterium selected from the following group: ATCC 85527, ATCC 75529, and ATCC 55638, a mutant of any one of these bacteria possessing all the identifying characteristics of any one of these bacteria, and mixtures; autoclaving the bacterium to derive a dispersant solution; and contacting the dispersant solution with a hydrocarbon to disperse the hydrocarbon. Moreover, a method for preparing a dispersant solution includes the following steps: providing a bacterium selected from the following group: ATCC 75527, ATCC 75529, and ATCC 55638, a mutant of any one of these bacteria possessing all the identifying characteristics of any one of these bacteria, and mixtures; and autoclaving the bacterium to derive a dispersant solution.

  4. Use of gamma radiation for preparation of nutrient culture media

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

    Speranskaya, I.D.; Tumanyan, M.A.; Mironova, L.L.

    1977-01-01

    A technique was developed for sterilization of nutrient culture media using ..gamma..-radiation. For this purpose, dry preparations were exposed to 3 to 6 Mrad radiation, then dissolved in sterile distilled water. The quality of media and solutions thus obtained is as good as that of preparations sterilized by filtration. The advantage of the proposed sterilization method is that liquid media can be rapidly prepared and dry sterile media can be stored at room temperature for long periods of time.

  5. Combined low-volume polyethylene glycol solution plus stimulant laxatives versus standard-volume polyethylene glycol solution: A prospective, randomized study of colon cleansing before colonoscopy

    PubMed Central

    Hookey, Lawrence C; Depew, William T; Vanner, Stephen J

    2006-01-01

    INTRODUCTION The effectiveness of polyethylene glycol solutions (PEG) for colon cleansing is often limited by the inability of patients to drink adequate portions of the 4 L solution. The aim of the present study was to determine whether a reduced volume of PEG combined with stimulant laxatives would be better tolerated and as or more effective than the standard dose. METHODS Patients undergoing outpatient colonoscopy were randomly assigned to receive either low-volume PEG plus sennosides (120 mg oral sennosides syrup followed by 2 L PEG) or the standard volume preparation (4 L PEG). The subjects rated the tolerability of the preparations and their symptoms. Colonoscopists were blind to the colonic cleansing preparation and graded the cleansing efficacy using a validated tool (the Ottawa scale). RESULTS The low-volume PEG plus sennosides preparation was significantly better tolerated than the standard large volume PEG (P<0.001) but was less efficacious (P=0.03). Thirty-eight per cent of patients in the large volume PEG group were unable to finish the preparation, compared with only 6% in the reduced volume group. There were no adverse events reported. CONCLUSIONS Although the low-volume PEG plus sennosides preparation was better tolerated, it was not as effective as standard large-volume PEG. However, in view of the significant difference in tolerance, further research investigating possible improvements in the reduced-volume regimen seems warranted. PMID:16482236

  6. [Adaptation of the (18)FDG module for the preparation of a sodium fluoride [(18)F] injection solution in agreement with the United States (USP 32) and European Pharmacopeia (PhEur 6)].

    PubMed

    Martínez, T; Cordero, B; Medín, S; Sánchez Salmón, A

    2011-01-01

    To establish an automated procedure for the preparation of sodium fluoride (18)F injection using the resources available in our laboratory for the preparation of (18)FDG and to analyze the repercussion of the conditioning column of the fluoride ion entrapment on the characteristics of the final product. The sequence of an (18)FDG synthesis module prepared so that it traps the fluoride ion from the cyclotron in ion-exchange resin diluted with 0.9% sodium chloride. The final solution was dosified and sterilized in a final vial in an automatized dispensing module. Three different column conditioning protocols within the process were tested. Quality controls were run according to USP 32 and EurPh 6, adding control of ethanol levels of residual solvent and quality controls of the solution at 8 h post-preparation. Activation of the resin cartridges with ethanol and water was the chosen procedure, with fluoride ion trapping > 95% and pH around 7. Ethanol levels were < 5.000 ppm. Quality controls at 8 h indicated that the solution was in compliance with the USP 32 and EurPh 6 specifications. This is an easy, low-cost, reliable automated method for sodium fluoride preparation in PET facilities with existing equipment for (18)FDG synthesis and quality control. Copyright © 2010 Elsevier España, S.L. y SEMNIM. All rights reserved.

  7. Preparation of Electrically Conductive Polystyrene/Carbon Nanofiber Nanocomposite Films

    ERIC Educational Resources Information Center

    Sun, Luyi; O'Reilly, Jonathan Y.; Tien, Chi-Wei; Sue, Hung-Jue

    2008-01-01

    A simple and effective approach to prepare conductive polystyrene/carbon nanofiber (PS/CNF) nanocomposite films via a solution dispersion method is presented. Inexpensive CNF, which has a structure similar to multi-walled carbon nanotubes, is chosen as a nanofiller in this experiment to achieve conductivity in PS films. A good dispersion is…

  8. METHOD FOR PREPARATION OF SINTERABLE BERYLLIUM OXIDE

    DOEpatents

    Sturm, B.J.

    1963-08-13

    High-purity beryllium oxide for nuclear reactor applications can be prepared by precipitation of beryllium oxalate monohydrate from aqueous solution at a temperature above 50 deg C and subsequent calcination of the precipitate. Improved purification with respect to metallic impurities is obtained, and the product beryllium oxide sinters reproducibly to a high density. (AEC)

  9. Preparation of U.sub.3 O.sub.8

    DOEpatents

    Johnson, David R.

    1980-01-01

    A method is described for the preparation of U.sub.3 O.sub.8 nuclear fuel material by direct precipitation of uranyl formate monohydrate from uranyl nitrate solution. The uranyl formate monohydrate precipitate is removed, dried and calcined to produce U.sub.3 O.sub.8 having a controlled particle size distribution.

  10. Beet juice utilization: Expeditious green synthesis of nobel metal nanoparticles (Ag, Au, Pt, and Pd) using microwaves

    EPA Science Inventory

    Metal nanoparticles of Ag, Au, Pt, and Pd were prepared in aqueous solutions via a rapid microwave-assisted green method using beet juice, an abundant sugar-rich agricultural produce, served as both a reducing and a capping reagent. The Ag nanoparticles with capping prepared by b...

  11. Noble metal superparticles and methods of preparation thereof

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

    Sun, Yugang; Hu, Yongxing

    A method comprises heating an aqueous solution of colloidal silver particles. A soluble noble metal halide salt is added to the aqueous solution which undergoes a redox reaction on a surface of the silver particles to form noble metal/silver halide SPs, noble metal halide/silver halide SPs or noble metal oxide/silver halide SPs on the surface of the silver particles. The heat is maintained for a predetermined time to consume the silver particles and release the noble metal/silver halide SPs, the noble metal halide/silver halide SPs or the noble metal oxide/silver halide SPs into the aqueous solution. The aqueous solution ismore » cooled. The noble metal/silver halide SPs, the noble metal halide/silver halide SPs or noble metal oxide/silver halide SPs are separated from the aqueous solution. The method optionally includes adding a soluble halide salt to the aqueous solution.« less

  12. A new sol-gel processing routine without chelating agents for preparing highly transparent solutions and nanothin films: engineering the role of chemistry to design the process

    NASA Astrophysics Data System (ADS)

    Ashiri, Rouholah

    2015-01-01

    The great sensitivity of titanium alkoxides to hydrolysis makes their sol-gel transformation very fast and thus difficult to control. A method was proposed to alleviate this drawback. Preparation of highly transparent solutions and nanothin films is another objective of the present research. Employing nanoemulsion method and optimizing the processing conditions, a clear solution of well-dispersed nanosized particles was obtained. With the proposed process BaTiO3 precursor sols and nanothin films with enhanced optical transparency towards the visible were prepared. The optimal formulation of the sol consists of acetic acid, barium acetate, 2-propanol, TTIP and deionized water with 6:1:1:1:150 M ratios, respectively. It was found that the reduction of the temperature in the initial stage of mixing of precursors controls the size of the forming species and accordingly improves the stability and transparency of the sol. The results also showed that the applied modifications and optimizations significantly downsize the particles within the sol to the nanometric scale and accordingly result in a significant improvement in the optical response of the products.

  13. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; preparation procedure for aquatic biological material determined for trace metals

    USGS Publications Warehouse

    Hoffman, Gerald L.

    1996-01-01

    A method for the chemical preparation of tissue samples that are subsequently analyzed for 22 trace metals is described. The tissue-preparation procedure was tested with three National Institute of Standards and Technology biological standard reference materials and two National Water Quality Laboratory homogenized biological materials. A low-temperature (85 degrees Celsius) nitric acid digestion followed by the careful addition of hydrogen peroxide (30-percent solution) is used to decompose the biological material. The solutions are evaporated to incipient dryness, reconstituted with 5 percent nitric acid, and filtered. After filtration the solutions were diluted to a known volume and analyzed by inductively coupled plasma-mass spectrometry (ICP-MS), inductively coupled plasma-atomic emission spectrometry (ICP-AES), and cold vapor-atomic absorption spectrophotometry (CV-AAS). Many of the metals were determined by both ICP-MS and ICP-AES. This report does not provide a detailed description of the instrumental procedures and conditions used with the three types of instrumentation for the quantitation of trace metals determined in this study. Statistical data regarding recovery, accuracy, and precision for individual trace metals determined in the biological material tested are summarized.

  14. Preparation of UO2, ThO2 and (Th,U)O2 pellets from photochemically-prepared nano-powders

    NASA Astrophysics Data System (ADS)

    Pavelková, Tereza; Čuba, Václav; de Visser-Týnová, Eva; Ekberg, Christian; Persson, Ingmar

    2016-02-01

    Photochemically-induced preparation of nano-powders of crystalline uranium and/or thorium oxides and their subsequent pelletizing has been investigated. The preparative method was based on the photochemically induced formation of amorphous solid precursors in aqueous solution containing uranyl and/or thorium nitrate and ammonium formate. The EXAFS analyses of the precursors shown that photon irradiation of thorium containing solutions yields a compound with little long-range order but likely "ThO2 like" and the irradiation of uranium containing solutions yields the mixture of U(IV) and U(VI) compounds. The U-containing precursors were carbon free, thus allowing direct heat treatment in reducing atmosphere without pre-treatment in the air. Subsequent heat treatment of amorphous solid precursors at 300-550 °C yielded nano-crystalline UO2, ThO2 or solid (Th,U)O2 solutions with high purity, well-developed crystals with linear crystallite size <15 nm. The prepared nano-powders of crystalline oxides were pelletized without any binder (pressure 500 MPa), the green pellets were subsequently sintered at 1300 °C under an Ar:H2 (20:1) mixture (UO2 and (Th,U)O2 pellets) or at 1600 °C in ambient air (ThO2 pellets). The theoretical density of the sintered pellets varied from 91 to 97%.

  15. Solid lithium ion conducting electrolytes and methods of preparation

    DOEpatents

    Narula, Chaitanya K; Daniel, Claus

    2013-05-28

    A composition comprised of nanoparticles of lithium ion conducting solid oxide material, wherein the solid oxide material is comprised of lithium ions, and at least one type of metal ion selected from pentavalent metal ions and trivalent lanthanide metal ions. Solution methods useful for synthesizing these solid oxide materials, as well as precursor solutions and components thereof, are also described. The solid oxide materials are incorporated as electrolytes into lithium ion batteries.

  16. Solid lithium ion conducting electrolytes and methods of preparation

    DOEpatents

    Narula, Chaitanya K.; Daniel, Claus

    2015-11-19

    A composition comprised of nanoparticles of lithium ion conducting solid oxide material, wherein the solid oxide material is comprised of lithium ions, and at least one type of metal ion selected from pentavalent metal ions and trivalent lanthanide metal ions. Solution methods useful for synthesizing these solid oxide materials, as well as precursor solutions and components thereof, are also described. The solid oxide materials are incorporated as electrolytes into lithium ion batteries.

  17. Matter in general relativity

    NASA Technical Reports Server (NTRS)

    Ray, J. R.

    1982-01-01

    Two theories of matter in general relativity, the fluid theory and the kinetic theory, were studied. Results include: (1) a discussion of various methods of completing the fluid equations; (2) a method of constructing charged general relativistic solutions in kinetic theory; and (3) a proof and discussion of the incompatibility of perfect fluid solutions in anisotropic cosmologies. Interpretations of NASA gravitational experiments using the above mentioned results were started. Two papers were prepared for publications based on this work.

  18. A novel preparation method for silicone oil nanoemulsions and its application for coating hair with silicone

    PubMed Central

    Hu, Zhenhua; Liao, Meiling; Chen, Yinghui; Cai, Yunpeng; Meng, Lele; Liu, Yajun; Lv, Nan; Liu, Zhenguo; Yuan, Weien

    2012-01-01

    Background Silicone oil, as a major component in conditioner, is beneficial in the moisture preservation and lubrication of hair. However, it is difficult for silicone oil to directly absorb on the hair surface because of its hydrophobicity. Stable nanoemulsions containing silicone oil may present as a potential solution to this problem. Methods Silicone oil nanoemulsions were prepared using the oil-in-water method with nonionic surfactants. Emulsion particle size and distribution were characterized by scanning electron microscopy. The kinetic stability of this nanoemulsion system was investigated under accelerated stability tests and long-term storage. The effect of silicone oil deposition on hair was examined by analyzing the element of hair after treatment of silicone oil nanoemulsions. Results Nonionic surfactants such as Span 80 and Tween 80 are suitable emulsifiers to prepare oil-in-water nanoemulsions that are both thermodynamically stable and can enhance the absorption of silicone oil on hair surface. Conclusion The silicone oil-in-water nanoemulsions containing nonionic surfactants present as a promising solution to improve the silicone oil deposition on the hair surface for hair care applications. PMID:23166436

  19. Performance of mesoporous organosilicates on the adsorption of heavy oil from produced water

    NASA Astrophysics Data System (ADS)

    Twaiq, Farouq A.; Nasser, Mustafa S.; Al-Ryiami, Samyia; Al-Ryiami, Hanan

    2012-09-01

    The performance of mesoporous organosilicate materials in removal of soluble oil from wastewater is investigated. The aim of the study is to evaluate the oil adsorption over organosilicate prepared using pre-synthesis methods and compare the results with adsorption over pure siliceous mesoporous material. The materials were prepared using sol-gel technique using Dodecylamine (D) and Cetyltrimethylammonium bromide (CTAB) as surfactant templates, and Tetraethylorthosilicate (TEOS) as silica precursor. The as-synthesized mesoporous materials were treated using three different methods to remove the surfactant from the mesoporous silica including calcinations method for total removal of the surfactant, the water vapor stripping and ethanol vapor stripping were used for partial removal of the surfactants. The synthesized materials were characterized using X-ray diffraction (XRD) and nitrogen adsorption. The materials were tested for heavy oils removal from oil-water solution. The results showed that neutral surfactant organosilicates have less adsorption compare to cationic surfactant organosilicates. The results also showed that among organosilicates prepared using neutral surfactant, treated organosilicate by ethanol vapor have the highest activity in removing the oil from the oil-water solution.

  20. Effective Design of Educational Virtual Reality Applications for Medicine Using Knowledge-Engineering Techniques

    ERIC Educational Resources Information Center

    Górski, Filip; Bun, Pawel; Wichniarek, Radoslaw; Zawadzki, Przemyslaw; Hamrol, Adam

    2017-01-01

    Effective medical and biomedical engineering education is an important problem. Traditional methods are difficult and costly. That is why Virtual Reality is often used for that purpose. Educational medical VR is a well-developed IT field, with many available hardware and software solutions. Current solutions are prepared without methodological…

  1. Clean thermal decomposition of tertiary-alkyl metal thiolates to metal sulfides: environmentally-benign, non-polar inks for solution-processed chalcopyrite solar cells.

    PubMed

    Heo, Jungwoo; Kim, Gi-Hwan; Jeong, Jaeki; Yoon, Yung Jin; Seo, Jung Hwa; Walker, Bright; Kim, Jin Young

    2016-11-09

    We report the preparation of Cu 2 S, In 2 S 3 , CuInS 2 and Cu(In,Ga)S 2 semiconducting films via the spin coating and annealing of soluble tertiary-alkyl thiolate complexes. The thiolate compounds are readily prepared via the reaction of metal bases and tertiary-alkyl thiols. The thiolate complexes are soluble in common organic solvents and can be solution processed by spin coating to yield thin films. Upon thermal annealing in the range of 200-400 °C, the tertiary-alkyl thiolates decompose cleanly to yield volatile dialkyl sulfides and metal sulfide films which are free of organic residue. Analysis of the reaction byproducts strongly suggests that the decomposition proceeds via an SN 1 mechanism. The composition of the films can be controlled by adjusting the amount of each metal thiolate used in the precursor solution yielding bandgaps in the range of 1.2 to 3.3 eV. The films form functioning p-n junctions when deposited in contact with CdS films prepared by the same method. Functioning solar cells are observed when such p-n junctions are prepared on transparent conducting substrates and finished by depositing electrodes with appropriate work functions. This method enables the fabrication of metal chalcogenide films on a large scale via a simple and chemically clear process.

  2. Clean thermal decomposition of tertiary-alkyl metal thiolates to metal sulfides: environmentally-benign, non-polar inks for solution-processed chalcopyrite solar cells

    NASA Astrophysics Data System (ADS)

    Heo, Jungwoo; Kim, Gi-Hwan; Jeong, Jaeki; Yoon, Yung Jin; Seo, Jung Hwa; Walker, Bright; Kim, Jin Young

    2016-11-01

    We report the preparation of Cu2S, In2S3, CuInS2 and Cu(In,Ga)S2 semiconducting films via the spin coating and annealing of soluble tertiary-alkyl thiolate complexes. The thiolate compounds are readily prepared via the reaction of metal bases and tertiary-alkyl thiols. The thiolate complexes are soluble in common organic solvents and can be solution processed by spin coating to yield thin films. Upon thermal annealing in the range of 200-400 °C, the tertiary-alkyl thiolates decompose cleanly to yield volatile dialkyl sulfides and metal sulfide films which are free of organic residue. Analysis of the reaction byproducts strongly suggests that the decomposition proceeds via an SN1 mechanism. The composition of the films can be controlled by adjusting the amount of each metal thiolate used in the precursor solution yielding bandgaps in the range of 1.2 to 3.3 eV. The films form functioning p-n junctions when deposited in contact with CdS films prepared by the same method. Functioning solar cells are observed when such p-n junctions are prepared on transparent conducting substrates and finished by depositing electrodes with appropriate work functions. This method enables the fabrication of metal chalcogenide films on a large scale via a simple and chemically clear process.

  3. Preparation of Sic/AIN Solid Solutions Using Organometallic Precursors

    DTIC Science & Technology

    1989-02-15

    pyrolysis of organoaluminum and organosilicon compounds was investigated as a potential source of SiC /AUI solid solutions. Using two different co... pyrolysis methods, homogeneous mixtures of organoaluminum amides and both a vinylic polysilane and a poly- carbosilane were convertec to a preceramic ...solid that transformed to crystalline SiC /AiN solid solutions at 򒸀 C. Moreover, the liquid, polymeric , form of these precursor mixtures provides a

  4. Establishing the traceability of a uranyl nitrate solution to a standard reference material

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

    Jackson, C.H.; Clark, J.P.

    1978-01-01

    A uranyl nitrate solution for use as a Working Calibration and Test Material (WCTM) was characterized, using a statistically designed procedure to document traceability to National Bureau of Standards Reference Material (SPM-960). A Reference Calibration and Test Material (PCTM) was prepared from SRM-960 uranium metal to approximate the acid and uranium concentration of the WCTM. This solution was used in the characterization procedure. Details of preparing, handling, and packaging these solutions are covered. Two outside laboratories, each having measurement expertise using a different analytical method, were selected to measure both solutions according to the procedure for characterizing the WCTM. Twomore » different methods were also used for the in-house characterization work. All analytical results were tested for statistical agreement before the WCTM concentration and limit of error values were calculated. A concentration value was determined with a relative limit of error (RLE) of approximately 0.03% which was better than the target RLE of 0.08%. The use of this working material eliminates the expense of using SRMs to fulfill traceability requirements for uranium measurements on this type material. Several years' supply of uranyl nitrate solution with NBS traceability was produced. The cost of this material was less than 10% of an equal quantity of SRM-960 uranium metal.« less

  5. Copper Oxide Nanomaterials Prepared by Solution Methods, Some Properties, and Potential Applications: A Brief Review

    PubMed Central

    Tran, Thi Ha; Nguyen, Viet Tuyen

    2014-01-01

    Cupric oxide (CuO), having a narrow bandgap of 1.2 eV and a variety of chemophysical properties, is recently attractive in many fields such as energy conversion, optoelectronic devices, and catalyst. Compared with bulk material, the advanced properties of CuO nanostructures have been demonstrated; however, the fact that these materials cannot yet be produced in large scale is an obstacle to realize the potential applications of this material. In this respect, chemical methods seem to be efficient synthesis processes which yield not only large quantities but also high quality and advanced material properties. In this paper, the effect of some general factors on the morphology and properties of CuO nanomaterials prepared by solution methods will be overviewed. In terms of advanced nanostructure synthesis, microwave method in which copper hydroxide nanostructures are produced in the precursor solution and sequentially transformed by microwave into CuO may be considered as a promising method to explore in the near future. This method produces not only large quantities of nanoproducts in a short reaction time of several minutes, but also high quality materials with advanced properties. A brief review on some unique properties and applications of CuO nanostructures will be also presented. PMID:27437488

  6. Binary ferrihydrite catalysts

    DOEpatents

    Huffman, G.P.; Zhao, J.; Feng, Z.

    1996-12-03

    A method of preparing a catalyst precursor comprises dissolving an iron salt and a salt of an oxoanion forming agent, in water so that a solution of the iron salt and oxoanion forming agent salt has a ratio of oxoanion/Fe of between 0.0001:1 to 0.5:1. Next is increasing the pH of the solution to 10 by adding a strong base followed by collecting of precipitate having a binary ferrihydrite structure. A binary ferrihydrite catalyst precursor is also prepared by dissolving an iron salt in water. The solution is brought to a pH of substantially 10 to obtain ferrihydrite precipitate. The precipitate is then filtered and washed with distilled water and subsequently admixed with a hydroxy carboxylic acid solution. The admixture is mixed/agitated and the binary ferrihydrite precipitate is then filtered and recovered. 3 figs.

  7. Alternatives to Sedation and General Anesthesia in Pediatric Magnetic Resonance Imaging: A Literature Review.

    PubMed

    McGuirt, Delaney

    2016-09-01

    To assess alternatives to sedation and general anesthesia to prepare children for magnetic resonance (MR) imaging examinations. Online databases were searched for articles discussing methods of preparing children for MR imaging procedures. Because of the large number of articles returned, criteria were limited to only studies that prepared patients without the use of sedation or general anesthesia. Twenty-four studies were deemed appropriate for inclusion in the review. The following methods emerged as alternatives to pediatric sedation: mock scanners, MR-compatible audiovisual systems, feed-sleep manipulation, play therapy, infant incubators/immobilizers, photo diaries, sucrose solutions, and guided imagery. The approaches with the most extensive research were mock MR scanners and feed-sleep manipulation. Evidence supports the use of these alternative techniques as valid substitutes for pediatric sedation and general anesthesia. To reduce the risks associated with sedation of pediatric patients, institutions could implement the alternatives discussed in this review. Cost analyses should be conducted first because some methods are more expensive than others. Finally, further research is needed to better assess the effectiveness of lesser-practiced methods, including photo diaries, sucrose solutions, and guided imagery. ©2016 American Society of Radiologic Technologists.

  8. Multi-instrumental characterization of carbon nanotubes dispersed in aqueous solutions

    EPA Science Inventory

    Previous studies showed that the dispersion extent and physicochemical properties of carbon nanotubes are highly dependent upon the preparation methods (e.g., dispersion methods and dispersants). In the present work, multiwalled carbon nanotubes (MWNTs) are dispersed in aqueous s...

  9. METHOD FOR PREPARATION OF SPHERICAL UO$sub 4$

    DOEpatents

    Gregory, J.F. Jr.; Levey, R.P. Jr.

    1962-06-01

    A method is given for continuously precipitating ura nium peroxide in the form of spherical particles. Seed crystals are formed in a first reaction zone by introducing an acidified aqueous uranyl nitrate solution and an aqueous hydrogen peroxide solution at a ratio of 5 to 20 per cent of the stoichiometric amount required for complete precipitation. After a mean residence time of 2 to 5 minutes in the first reaction zone, the resulting mixture is introduced into a second reaction zone, together with a large excess of hydrogen peroxide solution. The resulting UO4 is rapidly separated from the mother liquor after an over-all residence time of 5 to 11 minutes. The first reaction is maintained at a temperature of 85 to 90 deg C and the second zone above 50 deg C. Additional reaction zones may be employed for further crystal growth. The UO/sub 4/ is converted to U/sub 3/O/sub 8/ or UO/sub 2/ by heating in air or hydrogen atmosphere. This method is particularly useful for the preparation of spherical UO/sub 2/ particles 10 to 25 microns in diameter. (AEC)

  10. Improved performance of mesostructured perovskite solar cells via an anti-solvent method

    NASA Astrophysics Data System (ADS)

    Hao, Jiabin; Hao, Huiying; Cheng, Feiyu; Li, Jianfeng; Zhang, Haiyu; Dong, Jingjing; Xing, Jie; Liu, Hao; Wu, Jian

    2018-06-01

    One-step solution process is a facile and widely used procedure to prepare organic-inorganic perovskite materials. However, the poor surface morphology of the films attributed to the uncontrollable nucleation and crystal growth in the process is unfavorable to solar cells. In this study, an anti-solvent treatment during the one-step solution process, in which ethyl acetate (EA) was dropped on the sample during spinning the precursor solution containing CH3NH3Cl, was adopted to fabricate perovskite materials and solar cells. It was found that the morphology of the perovskite film was significantly improved due to the rapid nucleation and slow crystal growth process. The modified process enabled us to fabricate the mesoporous solar cell with power conversion efficiency of 14%, showing an improvement of 40% over the efficiency of 9.7% of the device prepared by conventional one-step method. The controlling effect of annealing time on the morphology, crystal structure and transport properties of perovskite layer as well as the performance of device fabricated by the anti-solvent method were investigated and the possible mechanism was discussed.

  11. Design and preparation of polymeric scaffolds for tissue engineering.

    PubMed

    Weigel, Thomas; Schinkel, Gregor; Lendlein, Andreas

    2006-11-01

    Polymeric scaffolds for tissue engineering can be prepared with a multitude of different techniques. Many diverse approaches have recently been under development. The adaptation of conventional preparation methods, such as electrospinning, induced phase separation of polymer solutions or porogen leaching, which were developed originally for other research areas, are described. In addition, the utilization of novel fabrication techniques, such as rapid prototyping or solid free-form procedures, with their many different methods to generate or to embody scaffold structures or the usage of self-assembly systems that mimic the properties of the extracellular matrix are also described. These methods are reviewed and evaluated with specific regard to their utility in the area of tissue engineering.

  12. Apparatus and method for preparing oxygen-15 labeled water H{sub 2}[{sup 15}O] in an injectable form for use in positron emission tomography

    DOEpatents

    Ferrieri, R.A.; Schlyer, D.J.; Alexoff, D.

    1996-01-09

    A handling and processing apparatus is revealed for preparing Oxygen-15 labeled water (H{sub 2}[{sup 15}O]) in injectable form for use in Positron Emission Tomography from preferably H{sub 2}[{sup 15}O] produced by irradiating a flowing gas target of nitrogen and hydrogen. The apparatus includes a collector for receiving and directing a gas containing H{sub 2}[{sup 15}O] gas and impurities, mainly ammonia (NH{sub 3}) gas into sterile water to trap the H{sub 2}[{sup 15}O] and form ammonium (NH{sub 4}{sup +}) in the sterile water. A device for displacing the sterile water containing H{sub 2}[{sup 15}O] and NH{sub 4}{sup +} through a cation resin removes NH{sub 4}{sup +} from the sterile water. A device for combining the sterile water containing H{sub 2}[{sup 15}O] with a saline solution produces an injectable solution. Preferably, the apparatus includes a device for delivering the solution to a syringe for injection into a patient. Also, disclosed is a method for preparing H{sub 2}[{sup 15}O] in injectable form for use in Positron Emission Tomography in which the method neither requires isotopic exchange reaction nor application of high temperature. 7 figs.

  13. Assessment of Sample Preparation Bias in Mass Spectrometry-Based Proteomics.

    PubMed

    Klont, Frank; Bras, Linda; Wolters, Justina C; Ongay, Sara; Bischoff, Rainer; Halmos, Gyorgy B; Horvatovich, Péter

    2018-04-17

    For mass spectrometry-based proteomics, the selected sample preparation strategy is a key determinant for information that will be obtained. However, the corresponding selection is often not based on a fit-for-purpose evaluation. Here we report a comparison of in-gel (IGD), in-solution (ISD), on-filter (OFD), and on-pellet digestion (OPD) workflows on the basis of targeted (QconCAT-multiple reaction monitoring (MRM) method for mitochondrial proteins) and discovery proteomics (data-dependent acquisition, DDA) analyses using three different human head and neck tissues (i.e., nasal polyps, parotid gland, and palatine tonsils). Our study reveals differences between the sample preparation methods, for example, with respect to protein and peptide losses, quantification variability, protocol-induced methionine oxidation, and asparagine/glutamine deamidation as well as identification of cysteine-containing peptides. However, none of the methods performed best for all types of tissues, which argues against the existence of a universal sample preparation method for proteome analysis.

  14. Development of second generation gold-supported palladium material with low-leaching and recyclable characteristics in aromatic amination.

    PubMed

    Al-Amin, Mohammad; Arai, Satoshi; Hoshiya, Naoyoki; Honma, Tetsuo; Tamenori, Yusuke; Sato, Takatoshi; Yokoyama, Mami; Ishii, Akira; Takeuchi, Masashi; Maruko, Tomohiro; Shuto, Satoshi; Arisawa, Mitsuhiro

    2013-08-02

    An improved process for the preparation of sulfur-modified gold-supported palladium material [SAPd, second generation] is presented. The developed preparation method is safer and generates less heat (aqueous Na2S2O8 and H2SO4) for sulfur fixation on a gold surface, and it is superior to the previous method of preparing SAPd (first generation), which requires the use of the more heat-generating and dangerous piranha solution (concentrated H2SO4 and 35% H2O2) in the sulfur fixation step. This safer and improved preparation method is particularly important for the mass production of SAPd (second generation) for which the catalytic activity was examined in ligand-free Buchwald-Hartwig cross-coupling reactions. The catalytic activities were the same between the first and second generation SAPds in aromatic aminations, but the lower palladium leaching properties and safer preparative method of second generation SAPd are a significant improvement over the first generation SAPd.

  15. Remediation using trace element humate surfactant

    DOEpatents

    Riddle, Catherine Lynn; Taylor, Steven Cheney; Bruhn, Debra Fox

    2016-08-30

    A method of remediation at a remediation site having one or more undesirable conditions in which one or more soil characteristics, preferably soil pH and/or elemental concentrations, are measured at a remediation site. A trace element humate surfactant composition is prepared comprising a humate solution, element solution and at least one surfactant. The prepared trace element humate surfactant composition is then dispensed onto the remediation site whereby the trace element humate surfactant composition will reduce the amount of undesirable compounds by promoting growth of native species activity. By promoting native species activity, remediation occurs quickly and environmental impact is minimal.

  16. A new ex vivo method for the study of nasal drops on ciliary function.

    PubMed

    Levrier, J; Molon-Noblot, S; Duval, D; Lloyd, K G

    1989-01-01

    Any pharmaceutical nasal preparation should respect the physiological function of the mucociliary transport system and should undergo testing to this effect. An experimental protocol has been developed using the guinea pig in order to assess the effects of commercial nasal drop preparations on mucociliary function. The method presented here consists of applying in vivo the test solution on the nasal respiratory epithelium. After a specified contact time and following rapid sacrifice of the animal, the mucosa is removed; the beating frequency of the cilia is then recorded ex vivo by micro-photo-oscillography. The method is sensitive to compounds known to diminish mucociliary function as sodium mercurothiolate inhibits ciliary movement of the nasal epithelium ex vivo. This inhibition of ciliary movement is long-lasting, although reversible. This method can be used to test the action of intranasally administered pharmaceutical preparations on mucociliary function. Commercially available solutions of the nasal vasoconstrictors tymazoline, fenoxazoline or oxymetazoline do not alter ciliary movement ex vivo at dose levels equal to or greater than those clinically utilized. ATP significantly enhances nasal ciliary frequency in instances where a low basal rate occurred. Thus, this method can be used for the testing of the maintenance of nasal ciliary function in the presence of compounds and preparations which will be applied into the nostrils. The advantages over previous techniques include a closer approach to the therapeutic utilization and the maintained physiological conditions of the mucosa during drug administration.

  17. Indoor Pedestrian Navigation Using Foot-Mounted IMU and Portable Ultrasound Range Sensors

    PubMed Central

    Girard, Gabriel; Côté, Stéphane; Zlatanova, Sisi; Barette, Yannick; St-Pierre, Johanne; van Oosterom, Peter

    2011-01-01

    Many solutions have been proposed for indoor pedestrian navigation. Some rely on pre-installed sensor networks, which offer good accuracy but are limited to areas that have been prepared for that purpose, thus requiring an expensive and possibly time-consuming process. Such methods are therefore inappropriate for navigation in emergency situations since the power supply may be disturbed. Other types of solutions track the user without requiring a prepared environment. However, they may have low accuracy. Offline tracking has been proposed to increase accuracy, however this prevents users from knowing their position in real time. This paper describes a real time indoor navigation system that does not require prepared building environments and provides tracking accuracy superior to previously described tracking methods. The system uses a combination of four techniques: foot-mounted IMU (Inertial Motion Unit), ultrasonic ranging, particle filtering and model-based navigation. The very purpose of the project is to combine these four well-known techniques in a novel way to provide better indoor tracking results for pedestrians. PMID:22164034

  18. Automated MALDI Matrix Coating System for Multiple Tissue Samples for Imaging Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Mounfield, William P.; Garrett, Timothy J.

    2012-03-01

    Uniform matrix deposition on tissue samples for matrix-assisted laser desorption/ionization (MALDI) is key for reproducible analyte ion signals. Current methods often result in nonhomogenous matrix deposition, and take time and effort to produce acceptable ion signals. Here we describe a fully-automated method for matrix deposition using an enclosed spray chamber and spray nozzle for matrix solution delivery. A commercial air-atomizing spray nozzle was modified and combined with solenoid controlled valves and a Programmable Logic Controller (PLC) to control and deliver the matrix solution. A spray chamber was employed to contain the nozzle, sample, and atomized matrix solution stream, and to prevent any interference from outside conditions as well as allow complete control of the sample environment. A gravity cup was filled with MALDI matrix solutions, including DHB in chloroform/methanol (50:50) at concentrations up to 60 mg/mL. Various samples (including rat brain tissue sections) were prepared using two deposition methods (spray chamber, inkjet). A linear ion trap equipped with an intermediate-pressure MALDI source was used for analyses. Optical microscopic examination showed a uniform coating of matrix crystals across the sample. Overall, the mass spectral images gathered from tissues coated using the spray chamber system were of better quality and more reproducible than from tissue specimens prepared by the inkjet deposition method.

  19. Automated MALDI matrix coating system for multiple tissue samples for imaging mass spectrometry.

    PubMed

    Mounfield, William P; Garrett, Timothy J

    2012-03-01

    Uniform matrix deposition on tissue samples for matrix-assisted laser desorption/ionization (MALDI) is key for reproducible analyte ion signals. Current methods often result in nonhomogenous matrix deposition, and take time and effort to produce acceptable ion signals. Here we describe a fully-automated method for matrix deposition using an enclosed spray chamber and spray nozzle for matrix solution delivery. A commercial air-atomizing spray nozzle was modified and combined with solenoid controlled valves and a Programmable Logic Controller (PLC) to control and deliver the matrix solution. A spray chamber was employed to contain the nozzle, sample, and atomized matrix solution stream, and to prevent any interference from outside conditions as well as allow complete control of the sample environment. A gravity cup was filled with MALDI matrix solutions, including DHB in chloroform/methanol (50:50) at concentrations up to 60 mg/mL. Various samples (including rat brain tissue sections) were prepared using two deposition methods (spray chamber, inkjet). A linear ion trap equipped with an intermediate-pressure MALDI source was used for analyses. Optical microscopic examination showed a uniform coating of matrix crystals across the sample. Overall, the mass spectral images gathered from tissues coated using the spray chamber system were of better quality and more reproducible than from tissue specimens prepared by the inkjet deposition method.

  20. Effect of cationic monomer content on polyacrylamide copolymers by frit-inlet asymmetrical flow field-flow fractionation/multi-angle light scattering.

    PubMed

    Lee, Hyejin; Kim, Jin Yong; Choi, Woonjin; Moon, Myeong Hee

    2017-06-23

    In this study, ultrahigh-molecular-weight (MW) (>10 7 Da) cationic polyacrylamides (C-PAMs), which are water-soluble polymers used in waste water treatment, were characterized using frit-inlet asymmetrical flow field-flow fractionation coupled with multi-angle light scattering and differential refractive detection. C-PAMs copolymerized with acryloxyethyltrimethyl ammonium chloride (DAC) were prepared by varying the feed amount of cationic monomer, polymerization method (solution vs. emulsion), and degree of branching. The MW of the copolymers prepared using emulsion polymerization (10 7 -10 9 Da) was generally larger than that of copolymers prepared using solution polymerization (4×10 7 -10 8 Da). When the amount of cationic monomer was increased from 10 to 55mol% in solution polymerization, hydrophobic contraction of the core induced formation of more compact C-PAMs. The copolymers prepared using emulsion polymerization formed highly aggregated or supercoil structures owing to increased intermolecular hydrophobic interaction when less cationic monomer was used. However, the MW decreased with increased cationic group content. In addition, C-PAMs larger than ∼10 8 Da prepared using the emulsion method were separated by steric/hyperlayer elution mode while those in the 10 7 -10 8 Da range were analyzed in either normal or steric/hyperlayer mode depending on the decay patterns of field programming. Moreover, branched copolymers were found to be resolved with different elution modes under the same field decay pattern depending on the degree of branching: steric/hyperlayer for low-branching and normal for high-branching C-PAMs. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. A moderate method for preparation DMSA coated Fe3O4 nanoparticles

    NASA Astrophysics Data System (ADS)

    Song, L. N.; Gu, N.; Zhang, Y.

    2017-01-01

    A moderate way to prepare water soluble magnetic Fe3O4 nanoparticles has been developed. Firstly, oleic acid coated Fe3O4 is prepared by coprecipitation. Second, oleic acid were replaced by 2,3-dimercaptosuccinnic acid (DMSA) to prepare DMSA/Fe3O4 in the mixed solution of n-hexane and acetone. After dialysis and filtration the DMSA/Fe3O4 can be transferred into distilled water to form stable Fe3O4 nanoparticle solutions. The TEM images indicated that the particles had spherical shape and the nanoparticles were found to be 12 nm with a relatively narrow size distribution with the hydrodynamic size of 30 nm. And the result of VSM shows that DMSA/Fe3O4 nanoparticles have a saturation magnetization of 31 emu/g. The IR spectra indicated that the iron oxide was located by carboxyl matrix.

  2. Adsorption of NO on alumina-supported oxides and oxide-hydroxides of manganese.

    PubMed

    Spasova, I; Nikolov, P; Mehandjiev, D

    2005-10-15

    The adsorption capacity for NO of alumina-supported oxides and oxide-hydroxides of manganese have been studied. Two series of samples have been prepared by precipitation on gamma-alumina and appropriate thermal treatment. The samples have been characterized by adsorption methods, magnetic methods, electronic paramagnetic resonance (EPR), transient response technique, and temperature-programmed desorption (TPD). The influence of the concentration of the initial manganese-containing solution has been investigated. The sample, prepared with a solution with Mn concentration of 4 g/100 ml, has been shown to be the best adsorbent for NO under the conditions of the experiment. It has been found that the presence mainly of Mn3+ ions on the surface of the support is probably responsible for the enhanced adsorption capacity.

  3. Method for etching thin films of niboium and niobium-containing compounds for preparing superconductive circuits

    DOEpatents

    Kampwirth, R.T.; Schuller, I.K.; Falco, C.M.

    1979-11-23

    An improved method of preparing thin film superconducting electrical circuits of niobium or niobium compounds is provided in which a thin film of the niobium or niobium compound is applied to a nonconductive substrate and covered with a layer of photosensitive material. The sensitive material is in turn covered with a circuit pattern exposed and developed to form a mask of the circuit in photoresistive material on the surface of the film. The unmasked excess niobium film is removed by contacting the substrate with an aqueous etching solution of nitric acid, sulfuric acid, and hydrogen fluoride, which will rapidly etch the niobium compound without undercutting the photoresist. A modification of the etching solution will permit thin films to be lifted from the substrate without further etching.

  4. Facile method for preparing organic/inorganic hybrid capsules using amino-functional silane coupling agent in aqueous media.

    PubMed

    Kurayama, Fumio; Suzuki, Satoru; Oyamada, Tetsuro; Furusawa, Takeshi; Sato, Masahide; Suzuki, Noboru

    2010-09-01

    A new and facile method for preparing microcapsules with 3-aminopropyltriethoxysilane (APTES)/alginate hybrid shell (AP-capsule) is proposed based on gelling and sol-gel processes. In this method, conventional capsules with alginate shells (Alg-capsule) are produced by dripping carboxymethyl cellulose solution containing calcium chloride into a sodium alginate solution. Subsequently, addition of the Alg-capsules to an aqueous APTES solution induces the formation of APTES/alginate hybrid shells. The optical observation shows that the texture of AP-capsules is more glossy and transparent than that of Alg-capsules. The surface morphology and elemental composition of microcapsules were characterized by Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FT-IR) and X-ray Photoelectron Spectroscopy (XPS). The results suggest that APTES molecules are incorporated to the framework of the alginate shells via electrostatic interaction between amino groups of APTES and carboxyl groups of alginate and the hybrid shells have a dense and homogeneous structure. In the formation reaction, the shrinking of the capsule shells occurs and the accumulation of APTES in the capsule shells proceeds with pseudo first-order kinetics. Moreover, these behaviors are greatly influenced by pH of the reaction solution, especially promoted under acidic and alkaline conditions. Copyright 2010 Elsevier Inc. All rights reserved.

  5. Band gap grading and photovoltaic performance of solution-processed Cu(In,Ga)S2 thin-film solar cells.

    PubMed

    Sohn, So Hyeong; Han, Noh Soo; Park, Yong Jin; Park, Seung Min; An, Hee Sang; Kim, Dong-Wook; Min, Byoung Koun; Song, Jae Kyu

    2014-12-28

    The photophysical properties of CuInxGa1-xS2 (CIGS) thin films, prepared by solution-based coating methods, are investigated to understand the correlation between the optical properties of these films and the electrical characteristics of solar cells fabricated using these films. Photophysical properties, such as the depth-dependent band gap and carrier lifetime, turn out to be at play in determining the energy conversion efficiency of solar cells. A double grading of the band gap in CIGS films enhances solar cell efficiency, even when defect states disturb carrier collection by non-radiative decay. The combinational stacking of different density films leads to improved solar cell performance as well as efficient fabrication because a graded band gap and reduced shunt current increase carrier collection efficiency. The photodynamics of minority-carriers suggests that the suppression of defect states is a primary area of improvement in CIGS thin films prepared by solution-based methods.

  6. Process for preparing energetic materials

    DOEpatents

    Simpson, Randall L [Livermore, CA; Lee, Ronald S [Livermore, CA; Tillotson, Thomas M [Tracy, CA; Hrubesh, Lawrence W [Pleasanton, CA; Swansiger, Rosalind W [Livermore, CA; Fox, Glenn A [Livermore, CA

    2011-12-13

    Sol-gel chemistry is used for the preparation of energetic materials (explosives, propellants and pyrotechnics) with improved homogeneity, and/or which can be cast to near-net shape, and/or made into precision molding powders. The sol-gel method is a synthetic chemical process where reactive monomers are mixed into a solution, polymerization occurs leading to a highly cross-linked three dimensional solid network resulting in a gel. The energetic materials can be incorporated during the formation of the solution or during the gel stage of the process. The composition, pore, and primary particle sizes, gel time, surface areas, and density may be tailored and controlled by the solution chemistry. The gel is then dried using supercritical extraction to produce a highly porous low density aerogel or by controlled slow evaporation to produce a xerogel. Applying stress during the extraction phase can result in high density materials. Thus, the sol-gel method can be used for precision detonator explosive manufacturing as well as producing precision explosives, propellants, and pyrotechnics, along with high power composite energetic materials.

  7. The Influence of Conditions on Synthesis Hydroxyapatite By Chemical Precipitation Method

    NASA Astrophysics Data System (ADS)

    Zhu, Jianping; Kong, Deshuang; Zhang, Yin; Yao, Nengjian; Tao, Yaqiu; Qiu, Tai

    2011-10-01

    Particles of Hydroxyapatite (HAp) were synthesized by means of chemical precipitation method, under atmosphere pressure. The starting solution with the Ca/P ratio of 1.67 was prepared by mixing 0.167 mol·dm-3 Ca(NO3)2·4H2O, 0.100 mol·dm-3 (NH4)2HPO4, 0.500 mol·dm-3 (NH2)2CO and 0.10 mol·dm-3 HNO3 aqueous solutions. The hydroxyapatite were prepared by heating the solution at 80 °C for 24 hour and then at 90°C for 72 hour. Then followed, the dry powers were heat treatment at 660°C temperatures for 8 hour. The obtained powder was analyzed using XRD, XRF, FT-IR, SEM, TG-DTA. The results showed that obtained HAp powers were greatly influenced by synthetic conditions. HAp powders with various morphologies, such as sphere, rod, layered, dumbbell, fibre, scaly, were obtained by controlling the synthetic conditions.

  8. Preparation and evaluation of a mixed-bed immunoaffinity column for selective purification of sixteen sulfonamides in pork muscle.

    PubMed

    Li, Yingguo; Chen, Yiqiang; Li, Zhengguo; Zhang, Lei; Li, Xianliang; Xi, Cunxian; Wang, Guomin; Wang, Xiong; Guo, Qi; Li, Na

    2012-03-01

    This paper describes the preparation of a novel mixed-bed immunoaffinity chromatography (IAC) column by coupling four monoclonal antibodies against different sulfonamides (SAs) to Sepharose 4B. The IAC column can be used to simultaneously extract and purify 16 SAs in pork muscle. The dynamic column capacities for all SAs in mixed standard solution were between 312 and 479 ng/mL gel. After simple extraction and IAC cleanup, the sample solution can be directly injected for liquid chromatography-ultraviolet analysis. The recoveries of SAs from spiked samples at levels of 25, 50 and 100 µg/kg ranged from 83.3 to 103.1% with variation coefficient less than 8.6%. The comparison of IAC with liquid-liquid extraction and solid phase extraction indicated that IAC has better purification effect and needs less organic solution than conventional methods, thus it would be an ideal method for selective purification of SAs in pork muscle.

  9. Continuous Preparation of 1:1 Haloperidol-Maleic Acid Salt by a Novel Solvent-Free Method Using a Twin Screw Melt Extruder.

    PubMed

    Lee, Hung Lin; Vasoya, Jaydip M; Cirqueira, Marilia de Lima; Yeh, Kuan Lin; Lee, Tu; Serajuddin, Abu T M

    2017-04-03

    Salts are generally prepared by acid-base reaction in relatively large volumes of organic solvents, followed by crystallization. In this study, the potential for preparing a pharmaceutical salt between haloperidol and maleic acid by a novel solvent-free method using a twin-screw melt extruder was investigated. The pH-solubility relationship between haloperidol and maleic acid in aqueous medium was first determined, which demonstrated that 1:1 salt formation between them was feasible (pH max 4.8; salt solubility 4.7 mg/mL). Extrusion of a 1:1 mixture of haloperidol and maleic acid at the extruder barrel temperature of 60 °C resulted in the formation of a highly crystalline salt. The effects of operating temperature and screw configuration on salt formation were also investigated, and those two were identified as key processing parameters. Salts were also prepared by solution crystallization from ethyl acetate, liquid-assisted grinding, and heat-assisted grinding and compared with those obtained by melt extrusion by using DSC, PXRD, TGA, and optical microscopy. While similar salts were obtained by all methods, both melt extrusion and solution crystallization yielded highly crystalline materials with identical enthalpies of melting. During the pH-solubility study, a salt hydrate form was also identified, which, upon heating, converted to anhydrate similar to that obtained by other methods. There were previous reports of the formation of cocrystals, but not salts, by melt extrusion. 1 H NMR and single-crystal X-ray diffraction confirmed that a salt was indeed formed in the present study. The haloperidol-maleic acid salt obtained was nonhygroscopic in the moisture sorption study and converted to the hydrate form only upon mixing with water. Thus, we are reporting for the first time a relatively simple and solvent-free twin-screw melt extrusion method for the preparation of a pharmaceutical salt that provides material comparable to that obtained by solution crystallization and is amenable to continuous manufacturing and easy scale up.

  10. An Analytical Chemistry Experiment in Simultaneous Spectrophotometric Determination of Fe(III) and Cu(II) with Hexacyanoruthenate(II) Reagent.

    ERIC Educational Resources Information Center

    Mehra, M. C.; Rioux, J.

    1982-01-01

    Experimental procedures, typical observations, and results for the simultaneous analysis of Fe(III) and Cu(II) in a solution are discussed. The method is based on selective interaction between the two ions and potassium hexacyanoruthenate(II) in acid solution involving no preliminary sample preparations. (Author/JN)

  11. Sol-gel method for encapsulating molecules

    DOEpatents

    Brinker, C. Jeffrey; Ashley, Carol S.; Bhatia, Rimple; Singh, Anup K.

    2002-01-01

    A method for encapsulating organic molecules, and in particular, biomolecules using sol-gel chemistry. A silica sol is prepared from an aqueous alkali metal silicate solution, such as a mixture of silicon dioxide and sodium or potassium oxide in water. The pH is adjusted to a suitably low value to stabilize the sol by minimizing the rate of siloxane condensation, thereby allowing storage stability of the sol prior to gelation. The organic molecules, generally in solution, is then added with the organic molecules being encapsulated in the sol matrix. After aging, either a thin film can be prepared or a gel can be formed with the encapsulated molecules. Depending upon the acid used, pH, and other processing conditions, the gelation time can be from one minute up to several days. In the method of the present invention, no alcohols are generated as by-products during the sol-gel and encapsulation steps. The organic molecules can be added at any desired pH value, where the pH value is generally chosen to achieve the desired reactivity of the organic molecules. The method of the present invention thereby presents a sufficiently mild encapsulation method to retain a significant portion of the activity of the biomolecules, compared with the activity of the biomolecules in free solution.

  12. Buffer-free therapeutic antibody preparations provide a viable alternative to conventionally buffered solutions: from protein buffer capacity prediction to bioprocess applications.

    PubMed

    Bahrenburg, Sven; Karow, Anne R; Garidel, Patrick

    2015-04-01

    Protein therapeutics, including monoclonal antibodies (mAbs), have significant buffering capacity, particularly at concentrations>50 mg/mL. This report addresses pH-related issues critical to adoption of self-buffered monoclonal antibody formulations. We evaluated solution conditions with protein concentrations ranging from 50 to 250 mg/mL. Samples were both buffer-free and conventionally buffered with citrate. Samples were non-isotonic or adjusted for isotonicity with NaCl or trehalose. Studies included accelerated temperature stability tests, shaking stability studies, and pH changes in infusion media as protein concentrate is added. We present averaged buffering slopes of capacity that can be applied to any mAb and present a general method for calculating buffering capacity of buffer-free, highly concentrated antibody liquid formulations. In temperature stability tests, neither buffer-free nor conventionally buffered solution conditions showed significant pH changes. Conventionally buffered solutions showed significantly higher opalescence than buffer-free ones. In general, buffer-free solution conditions showed less aggregation than conventionally buffered solutions. Shaking stability tests showed no differences between buffer-free and conventionally buffered solutions. "In-use" preparation experiments showed that pH in infusion bag medium can rapidly approximate that of self-buffered protein concentrate as concentrate is added. In summary, the buffer capacity of proteins can be predicted and buffer-free therapeutic antibody preparations provide a viable alternative to conventionally buffered solutions. Copyright © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Trace element analysis of extraterrestrial metal samples by inductively coupled plasma mass spectrometry: the standard solutions and digesting acids.

    PubMed

    Wang, Guiqin; Wu, Yangsiqian; Lin, Yangting

    2016-02-28

    Nearly 99% of the total content of extraterrestrial metals is composed of Fe and Ni, but with greatly variable trace element contents. The accuracy obtained in the inductively coupled plasma mass spectrometry (ICP-MS) analysis of solutions of these samples can be significantly influenced by matrix contents, polyatomic ion interference, and the concentrations of external standard solutions. An ICP-MS instrument (X Series 2) was used to determine 30 standard solutions with different concentrations of trace elements, and different matrix contents. Based on these measurements, the matrix effects were determined. Three iron meteorites were dissolved separately in aqua regia and HNO3. Deviations due to variation of matrix contents in the external standard solutions were evaluated and the analysis results of the two digestion methods for iron meteorites were assessed. Our results show obvious deviations due to unmatched matrix contents in the external standard solutions. Furthermore, discrepancy in the measurement of some elements was found between the sample solutions prepared with aqua regia and HNO3, due to loss of chloride during sample preparation and/or incomplete digestion of highly siderophile elements in iron meteorites. An accurate ICP-MS analysis method for extraterrestrial metal samples has been established using external standard solutions with matched matrix contents and digesting the samples with HNO3 and aqua regia. Using the data from this work, the Mundrabilla iron meteorite previously classified as IAB-ung is reclassified as IAB-MG. Copyright © 2016 John Wiley & Sons, Ltd.

  14. Enhanced Performance of Perovskite CH3NH3PbI3 Solar Cell by Using CH3NH3I as Additive in Sequential Deposition.

    PubMed

    Xie, Yian; Shao, Feng; Wang, Yaoming; Xu, Tao; Wang, Deliang; Huang, Fuqiang

    2015-06-17

    Sequential deposition is a widely adopted method to prepare CH3NH3PbI3 on mesostructured TiO2 electrode for organic lead halide perovskite solar cells. However, this method often suffers from the uncontrollable crystal size, surface morphology, and residual PbI2 in the resulting CH3NH3PbI3, which are all detrimental to the device performance. We herein present an optimized sequential solution deposition method by introducing different amount of CH3NH3I in PbI2 precursor solution in the first step to prepare CH3NH3PbI3 absorber on mesoporous TiO2 substrates. The addition of CH3NH3I in PbI2 precursor solution can affect the crystallization and composition of PbI2 raw films, resulting in the variation of UV-vis absorption and surface morphology. Proper addition of CH3NH3I not only enhances the absorption but also improves the efficiency of CH3NH3PbI3 solar cells from 11.13% to 13.37%. Photoluminescence spectra suggest that the improvement of device performance is attributed to the decrease of recombination rate of carriers in CH3NH3PbI3 absorber. This current method provides a highly repeatable route for enhancing the efficiency of CH3NH3PbI3 solar cell in the sequential solution deposition method.

  15. Preparation of silver-hydroyapatite/PVA nanocomposites: Giant dielectric material for industrial and clinical applications

    NASA Astrophysics Data System (ADS)

    Uddin, Md Jamal; Middya, T. R.; Chaudhuri, B. K.

    2015-02-01

    Pure hydroxyappatite Ca10(PO4)6(OH)2 (or HAP) was prepared from eggshell and potassium dihydrogen phosphate (KH2PO4) by a simple self-chemical reaction method. The clean eggshell was heated at 800 °C in air giving the source of CaO. Appropriate amount of CaO was dissolved in KH2PO4 solution at 37°C for few days. The PH value decreases with increasing the duration of preparation of HAP. Silver nanoparticles derived from silver nitrate solution using black tea leaf extract had been introduced to hydroxyapatite due to its biocompatibility. The unique size- dependent properties of nanomaterials make them superior and indispensable. In this work, hydroxyapatite-silver nanoparticles/polyvinyl alcohol (PVA) composites with 4 different concentrations of hydroxyapatite (1-4 wt %) were prepared by bio-reduction method. Several techniques like XRD and SEM were used to characterize the prepared samples. Frequency dependent capacitance and conductance of the samples were measured using an impedance analyzer. The results showed a remarkable increase in dielectric permittivity (~5117) with low loss (~0.23) at1000 HZ and room temperature (300K) for 4wt% Hydroxapatie-Silver/PVA nanocomposite. Such nanocomposite might be directly applied in manufacturing clinical devices and also for embedding capacitor applications.

  16. Carbon nanotube fiber spun from wetted ribbon

    DOEpatents

    Zhu, Yuntian T; Arendt, Paul; Zhang, Xiefei; Li, Qingwen; Fu, Lei; Zheng, Lianxi

    2014-04-29

    A fiber of carbon nanotubes was prepared by a wet-spinning method involving drawing carbon nanotubes away from a substantially aligned, supported array of carbon nanotubes to form a ribbon, wetting the ribbon with a liquid, and spinning a fiber from the wetted ribbon. The liquid can be a polymer solution and after forming the fiber, the polymer can be cured. The resulting fiber has a higher tensile strength and higher conductivity compared to dry-spun fibers and to wet-spun fibers prepared by other methods.

  17. 'It's Fast, It's Quick, It Stops Me Being Sick': How to influence preparation of opioid tablets for injection.

    PubMed

    Lafferty, Lise; Treloar, Carla; van Breda, Nick; Steele, Maureen; Hiley, Sarah; Flaherty, Ian; Salmon, Allison

    2017-09-01

    Injection of pharmaceutical opioids (PO) among people who inject drugs has increased in many countries. The common method for preparing PO tablets for injection uses heat, resulting in greater particulate matter and therefore increased risk of local infection risk and damage to veins and organs. A cold preparation process has fewer risks, but this preparation method is not commonly used. This study seeks to explore how people who inject PO learn to prepare injections and how health promotion efforts could influence practice. Between March and December 2013, qualitative interviews were undertaken with 33 clients of Sydney's Medically Supervised Injecting Centre who inject PO tablets regarding sources of knowledge and current preparation methods for injection of POs. Overwhelmingly, the most commonly reported source of knowledge around injection of tablets was others who inject. Most participants reported heating the solution as the quickest way to administer the drug. Attitudes to the use of wheel filters varied, with some participants reporting that they would use the filters if they were shown how, while others reported a number of barriers to using filters, including complexity of use. Harnessing the power of social connections may provide avenues for education about safer injecting of tablets, including the use of wheel filters. Further work is required to debunk myths about the relative potencies of cold versus hot drug solution. Collaborations between harm reduction workers and peer workers would assist in knowledge dissemination regarding safer injecting practices. © 2017 Australasian Professional Society on Alcohol and other Drugs.

  18. Different amorphous solid-state forms of roxithromycin: A thermodynamic and morphological study.

    PubMed

    Milne, Marnus; Liebenberg, Wilna; Aucamp, Marique Elizabeth

    2016-02-10

    The striking impact that different preparation methods have on the characteristics of amorphous solid-state forms has attracted considerable attention during the last two decades. The pursuit of more extensive knowledge regarding polyamorphism therefore continues. The aim of this study was firstly, to investigate the influence of different preparation techniques to obtain amorphous solid-state forms for the same active pharmaceutical ingredient, namely roxithromycin. The preparation techniques also report on a method utilizing hot air, which although it is based on a melt intermediary step, is considered a novel preparation method. Secondly, to conduct an in-depth investigation into any physico-chemical differences between the resulting amorphous forms and thirdly, to bring our findings into context with that of previous work done, whilst simultaneously discussing a well-defined interpretation for the term polyamorphism and propose a discernment between true polyamorphism and pseudo-polyamorphism/atypical-polyamorphism. The preparation techniques included melt, solution, and a combination of solution-mechanical disruption as intermediary steps. The resulting amorphous forms were investigated using differential scanning calorimetry, X-ray powder diffraction, hot-stage microscopy, scanning electron microscopy, and vapor sorption. Clear and significant thermodynamic differences were determined between the four amorphous forms. It was also deduced from this study that different preparation techniques have a mentionable impact on the morphological properties of the resulting amorphous roxithromycin powders. Thermodynamic properties as well as the physical characteristics of the amorphous forms greatly governed other physico-chemical properties i.e. solubility and dissolution. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Characterization of molecularly imprinted polymers using a new polar solvent titration method.

    PubMed

    Song, Di; Zhang, Yagang; Geer, Michael F; Shimizu, Ken D

    2014-07-01

    A new method of characterizing molecularly imprinted polymers (MIPs) was developed and tested, which provides a more accurate means of identifying and measuring the molecular imprinting effect. In the new polar solvent titration method, a series of imprinted and non-imprinted polymers were prepared in solutions containing increasing concentrations of a polar solvent. The polar solvent additives systematically disrupted the templation and monomer aggregation processes in the prepolymerization solutions, and the extent of disruption was captured by the polymerization process. The changes in binding capacity within each series of polymers were measured, providing a quantitative assessment of the templation and monomer aggregation processes in the imprinted and non-imprinted polymers. The new method was tested using three different diphenyl phosphate imprinted polymers made using three different urea functional monomers. Each monomer had varying efficiencies of templation and monomer aggregation. The new MIP characterization method was found to have several advantages. To independently verify the new characterization method, the MIPs were also characterized using traditional binding isotherm analyses. The two methods appeared to give consistent conclusions. First, the polar solvent titration method is less susceptible to false positives in identifying the imprinting effect. Second, the method is able to differentiate and quantify changes in binding capacity, as measured at a fixed guest and polymer concentration, arising from templation or monomer aggregation processes in the prepolymerization solution. Third, the method was also easy to carry out, taking advantage of the ease of preparing MIPs. Copyright © 2014 John Wiley & Sons, Ltd.

  20. A NOVEL SEPARATION TECHNOLOGY FOR REMOVAL RECOVERY OF METALS FROM AQUEOUS SOLUTIONS

    EPA Science Inventory

    Recovery/Recycling of metal ions from industrial process waste streams is a preferred alternative to disposal by conventional techniques. This paper presents methods for preparation of inorganic chemically active adsorbents to be used in fixed bed adsorbers. Methods for immobiliz...

  1. Method of preparing a high heating value fuel product

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

    Somerville, R.; Fan, L.T.

    1989-10-24

    This patent describes a method of preparing a high heating value fuel product. The method comprising the steps of: blending a high heating value waste material with a cellulosic material; mixing an organic reagent to the blended mixture of the waste material and the cellulosic material, the organic reagent being a mixture having a 4-15 weight percent of a chemical selected from the group consisting of: triethylene, glycol, diethylene glycol, and glycerin propylene glycol; introducing a pozzolanic agent to the blended mixture for controlling the rate of solidification; and forming the blended mixture into a form suitable for handling. Alsomore » described is the same method with the mixture of the organic reagent further comprising: a 20-32 weight percent calcium chloride solution. Another method of preparing a fuel product is also described.« less

  2. Electrochemical Polishing Applications and EIS of a Novel Choline Chloride-Based Ionic Liquid

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

    Wixtrom, Alex I.; Buhler, Jessica E.; Reece, Charles E.

    2013-06-01

    Minimal surface roughness is a critical feature for high-field superconducting radio frequency (SRF) cavities used to engineer particle accelerators. Current methods for polishing Niobium cavities typically utilize solutions containing a mixture of concentrated sulfuric and hydrofluoric acid. Polishing processes such as these are effective, yet there are many hazards and costs associated with the use (and safe disposal) of the concentrated acid solutions. An alternative method for electrochemical polishing of the cavities was explored using a novel ionic liquid solution containing choline chloride. Potentiostatic electrochemical impedance spectroscopy (EIS) was used to analyze the ionic polishing solution. Final surface roughness ofmore » the Nb was found to be comparable to that of the acid-polishing method, as assessed by atomic force microscopy (AFM). This indicates that ionic liquid-based electrochemical polishing of Nb is a viable replacement for acid-based methods for preparation of SRF cavities.« less

  3. [Application of polyguanidine solution for fixation of biological and anatomical specimens].

    PubMed

    Anichkov, N M; Danilova, I A; Riabinin, I A; Kipenko, A V

    2010-01-01

    A new method for fixation of biological material is described, and its effectiveness is compared to that one of formalin fixation. As an embalming agent, polyhexamethylenguanidine (PHMG) hydrochloride was used. Using the proposed method of fixation, the anatomical and histological preparations of human organs and of chick embryos at developmental 12 days, were produced. The anatomical preparations obtained show the appearance, similar to that of the recently removed organs. Histological preparations were free from significant distortions of the microscopic characteristics of the specimens, which are typical to the material fixed with formalin. The results of the study suggest the possibility of PHMG application in the morphological studies.

  4. Cellular morphology of organic-inorganic hybrid foams based on alkali alumino-silicate matrix

    NASA Astrophysics Data System (ADS)

    Verdolotti, Letizia; Liguori, Barbara; Capasso, Ilaria; Caputo, Domenico; Lavorgna, Marino; Iannace, Salvatore

    2014-05-01

    Organic-inorganic hybrid foams based on an alkali alumino-silicate matrix were prepared by using different foaming methods. Initially, the synthesis of an inorganic matrix by using aluminosilicate particles, activated through a sodium silicate solution, was performed at room temperature. Subsequently the viscous paste was foamed by using three different methods. In the first method, gaseous hydrogen produced by the oxidization of Si powder in an alkaline media, was used as blowing agent to generate gas bubbles in the paste. In the second method, the porous structure was generated by mixing the paste with a "meringue" type of foam previously prepared by whipping, under vigorous stirring, a water solution containing vegetal proteins as surfactants. In the third method, a combination of these two methods was employed. The foamed systems were consolidated for 24 hours at 40°C and then characterized by FTIR, X-Ray diffraction, scanning electron microscopy (SEM) and compression tests. Low density foams (˜500 Kg/m3) with good cellular structure and mechanical properties were obtained by combining the "meringue" approach with the use of the chemical blowing agent based on Si.

  5. Direct spectrophotometric method for analysis of food supplements containing synthetic polyhydroquinones

    NASA Astrophysics Data System (ADS)

    Vasilevsky, A. M.; Konoplev, G. A.; Stepanova, O. S.; Toropov, D. K.; Zagorsky, A. L.

    2016-04-01

    A novel direct spectrophotometric method for quantitative determination of Oxiphore® drug substance (synthetic polyhydroquinone complex) in food supplements is developed. Absorption spectra of Oxiphore® water solutions in the ultraviolet region are presented. Samples preparation procedures and mathematical methods of spectra post-analytical procession are discussed. Basic characteristics of the automatic CCD-based UV spectrophotometer and special software implementing the developed method are described. The results of the trials of the developed method and software are analyzed: the error of determination for Oxiphore® concentration in water solutions of the isolated substance and singlecomponent food supplements did not exceed 15% (average error was 7…10%).

  6. Methods for preparation of concentrated graphene compositions and related composite materials

    DOEpatents

    Hersam, Mark C.; Liang, Yu Teng

    2015-07-14

    A rapid, scalable methodology for graphene dispersion with a polymer-organic solvent solution and subsequent solvent exchange, as can be utilized without centrifugation, to enhance graphene concentration.

  7. Synthesis of porphyrin nanostructures

    DOEpatents

    Fan, Hongyou; Bai, Feng

    2014-10-28

    The present disclosure generally relates to self-assembly methods for generating porphyrin nanostructures. For example, in one embodiment a method is provided that includes preparing a porphyrin solution and a surfactant solution. The porphyrin solution is then mixed with the surfactant solution at a concentration sufficient for confinement of the porphyrin molecules by the surfactant molecules. In some embodiments, the concentration of the surfactant is at or above its critical micelle concentration (CMC), which allows the surfactant to template the growth of the nanostructure over time. The size and morphology of the nanostructures may be affected by the type of porphyrin molecules used, the type of surfactant used, the concentration of the porphyrin and surfactant the pH of the mixture of the solutions, and the order of adding the reagents to the mixture, to name a few variables.

  8. Y2O3:Eu phosphor particles prepared by spray pyrolysis from a solution containing citric acid and polyethylene glycol

    NASA Astrophysics Data System (ADS)

    Roh, H. S.; Kang, Y. C.; Park, H. D.; Park, S. B.

    Y2O3:Eu phosphor particles were prepared by large-scale spray pyrolysis. The morphological control of Y2O3:Eu particles in spray pyrolysis was attempted by adding polymeric precursors to the spray solution. The effect of composition and amount of polymeric precursors on the morphology, crystallinity and photoluminescence characteristics of Y2O3:Eu particles was investigated. Particles prepared from a solution containing polyethylene glycol (PEG) with an average molecular weight of 200 had a hollow structure, while those prepared from solutions containing adequate amounts of citric acid (CA) and PEG had a spherical shape, filled morphology and clean surfaces after post-treatment at high temperature. Y2O3:Eu particles prepared from an aqueous solution with no polymeric precursors had a hollow structure and rough surfaces after post-treatment. The phosphor particles prepared from solutions with inadequate amounts of CA and/or PEG also had hollow and/or fragmented structures. The particles prepared from the solution containing 0.3 M CA and 0.3 M PEG had the highest photoluminescence emission intensity, which was 56% higher than that of the particles prepared from aqueous solution without polymeric precursors.

  9. Physical and chemical stability of proflavine contrast agent solutions for early detection of oral cancer.

    PubMed

    Kawedia, Jitesh D; Zhang, Yan-Ping; Myers, Alan L; Richards-Kortum, Rebecca R; Kramer, Mark A; Gillenwater, Ann M; Culotta, Kirk S

    2016-02-01

    Proflavine hemisulfate solution is a fluorescence contrast agent to visualize cell nuclei using high-resolution optical imaging devices such as the high-resolution microendoscope. These devices provide real-time imaging to distinguish between normal versus neoplastic tissue. These images could be helpful for early screening of oral cancer and its precursors and to determine accurate margins of malignant tissue for ablative surgery. Extemporaneous preparation of proflavine solution for these diagnostic procedures requires preparation in batches and long-term storage to improve compounding efficiency in the pharmacy. However, there is a paucity of long-term stability data for proflavine contrast solutions. The physical and chemical stability of 0.01% (10 mg/100 ml) proflavine hemisulfate solutions prepared in sterile water was determined following storage at refrigeration (4-8℃) and room temperature (23℃). Concentrations of proflavine were measured at predetermined time points up to 12 months using a validated stability-indicating high-performance liquid chromatography method. Proflavine solutions stored under refrigeration were physically and chemically stable for at least 12 months with concentrations ranging from 95% to 105% compared to initial concentration. However, in solutions stored at room temperature increased turbidity and particulates were observed in some of the tested vials at 9 months and 12 months with peak particle count reaching 17-fold increase compared to baseline. Solutions stored at room temperature were chemically stable up to six months (94-105%). Proflavine solutions at concentration of 0.01% were chemically and physically stable for at least 12 months under refrigeration. The solution was chemically stable for six months when stored at room temperature. We recommend long-term storage of proflavine solutions under refrigeration prior to diagnostic procedure. © The Author(s) 2014.

  10. PREPARATION OF OXALATES OF METALS OF ATOMIC NUMBER GREATER THAN 88

    DOEpatents

    Duffield, R.B.

    1959-02-01

    A method is presented for the preparation of oxalates of metals of atomic number greater than 88. A solid peroxide of the heavy metal is contacted with an aqueous oxalic acid solution ai a temperature of about 50 C for a period of time sufficient to form the insoluble metal oxalate which is subsequentiy recovered as a pures crystalline compound.

  11. Processable Aromatic Polyimide Thermoplastic Blends

    NASA Technical Reports Server (NTRS)

    Baucom, Robert M; Johnston, Norman J.; St. Clair, Terry L.; Nelson, James B.; Gleason, John R.; Proctor, K. Mason

    1988-01-01

    Method developed for preparing readily-processable thermoplastic polyimides by blending linear, high-molecular-weight, polyimic acid solutions in ether solvents with ultrafine, semicrystalline, thermoplastic polyimide powders. Slurries formed used to make prepregs. Consolidation of prepregs into finsihed composites characterized by excellent melt flow during processing. Applied to film, fiber, fabric, metal, polymer, or composite surfaces. Used to make various stable slurries from which prepregs prepared.

  12. Surface defects on the Gd{sub 2}Zr{sub 2}O{sub 7} oxide films grown on textured NiW technical substrates by chemical solution method

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

    Zhao, Y., E-mail: yuezhao@sjtu.edu.cn

    2017-02-15

    Epitaxial growth of oxide thin films has attracted much interest because of their broad applications in various fields. In this study, we investigated the microstructure of textured Gd{sub 2}Zr{sub 2}O{sub 7} films grown on (001)〈100〉 orientated NiW alloy substrates by a chemical solution deposition (CSD) method. The aging effect of precursor solution on defect formation was thoroughly investigated. A slight difference was observed between the as-obtained and aged precursor solutions with respect to the phase purity and global texture of films prepared using these solutions. However, the surface morphologies are different, i.e., some regular-shaped regions (mainly hexagonal or dodecagonal) weremore » observed on the film prepared using the as-obtained precursor, whereas the film prepared using the aged precursor exhibits a homogeneous structure. Electron backscatter diffraction and scanning electron microscopy analyses showed that the Gd{sub 2}Zr{sub 2}O{sub 7} grains present within the regular-shaped regions are polycrystalline, whereas those present in the surrounding are epitaxial. Some polycrystalline regions ranging from several micrometers to several tens of micrometers grew across the NiW grain boundaries underneath. To understand this phenomenon, the properties of the precursors and corresponding xerogel were studied by Fourier transform infrared spectroscopy and coupled thermogravimetry/differential thermal analysis. The results showed that both the solutions mainly contain small Gd−Zr−O clusters obtained by the reaction of zirconium acetylacetonate with propionic acid during the precursor synthesis. The regular-shaped regions were probably formed by large Gd−Zr−O frameworks with a metastable structure in the solution with limited aging time. This study demonstrates the importance of the precise control of chemical reaction path to enhance the stability and homogeneity of the precursors of the CSD route. - Highlights: •We investigate microstructure of Gd{sub 2}Zr{sub 2}O{sub 7} films grown by a chemical solution route. •The aging effect of precursor solution on formation of surface defect was thoroughly studied. •Gd−Zr−O clusters are present in the precursor solutions.« less

  13. In Situ Preparation of Biomimetic Thin Films and Their Surface-Shielding Effect for Organisms in High Vacuum

    PubMed Central

    Muranaka, Yoshinori; Shimomura, Masatsugu; Hariyama, Takahiko

    2013-01-01

    Self-standing biocompatible films have yet to be prepared by physical or chemical vapor deposition assisted by plasma polymerization because gaseous monomers have thus far been used to create only polymer membranes. Using a nongaseous monomer, we previously found a simple fabrication method for a free-standing thin film prepared from solution by plasma polymerization, and a nano-suit made by polyoxyethylene (20) sorbitan monolaurate can render multicellular organisms highly tolerant to high vacuum. Here we report thin films prepared by plasma polymerization from various monomer solutions. The films had a flat surface at the irradiated site and were similar to films produced by vapor deposition of gaseous monomers. However, they also exhibited unique characteristics, such as a pinhole-free surface, transparency, solvent stability, flexibility, and a unique out-of-plane molecular density gradient from the irradiated to the unirradiated surface of the film. Additionally, covering mosquito larvae with the films protected the shape of the organism and kept them alive under the high vacuum conditions in a field emission-scanning electron microscope. Our method will be useful for numerous applications, particularly in the biological sciences. PMID:24236023

  14. Synthesis of Bimetallic Platinum Nanoparticles for Biosensors

    PubMed Central

    Leteba, Gerard M.; Lang, Candace I.

    2013-01-01

    The use of magnetic nanomaterials in biosensing applications is growing as a consequence of their remarkable properties; but controlling the composition and shape of metallic nanoalloys is problematic when more than one precursor is required for wet chemistry synthesis. We have developed a successful simultaneous reduction method for preparation of near-spherical platinum-based nanoalloys containing magnetic solutes. We avoided particular difficulties in preparing platinum nanoalloys containing Ni, Co and Fe by the identification of appropriate synthesis temperatures and chemistry. We used transmission electron microscopy (TEM) to show that our particles have a narrow size distribution, uniform size and morphology, and good crystallinity in the as-synthesized condition. Energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD) confirms the coexistence of Pt with the magnetic solute in a face-centered cubic (FCC) solid solution. PMID:23941910

  15. Stability study of carboplatin infusion solutions in 0.9% sodium chloride in polyvinyl chloride bags.

    PubMed

    Myers, Alan L; Zhang, Yang-Ping; Kawedia, Jitesh D; Trinh, Van A; Tran, Huyentran; Smith, Judith A; Kramer, Mark A

    2016-02-01

    Carboplatin is a platinum-containing compound with efficacy against various malignancies. The physico-chemical stability of carboplatin in dextrose 5% water (D5W) has been thoroughly studied; however, there is a paucity of stability data in clinically relevant 0.9% sodium chloride infusion solutions. The manufacturer's limited stability data in sodium chloride solutions hampers the flexibility of carboplatin usage in oncology patients. Hence, the purpose of this study is to determine the physical and chemical stability of carboplatin-sodium chloride intravenous solutions under different storage conditions. The physico-chemical stability of 0.5 mg/mL, 2.0 mg/mL, and 4.0 mg/mL carboplatin-sodium chloride solutions prepared in polyvinyl chloride bags was determined following storage at room temperature under ambient fluorescent light and under refrigeration in the dark. Concentrations of carboplatin were measured at predetermined time points up to seven days using a stability-indicating high-performance liquid chromatography method. All tested solutions were found physically stable for at least seven days. The greatest chemical stability was observed under refrigerated storage conditions. At 4℃, all tested solutions were found chemically stable for at least seven days, with nominal losses of ≤6%. Following storage at room temperature exposed to normal fluorescent light, the chemical stability of 0.5 mg/mL, 2.0 mg/mL, and 4.0 mg/mL solutions was three days, five days, and seven days, respectively. The extended physico-chemical stability of carboplatin prepared in sodium chloride reported herein permits advance preparation of these admixtures, facilitating pharmacy utility and operations. Since no antibacterial preservative is contained within these carboplatin solutions, we recommend storage, when prepared under specified aseptic conditions, no greater than 24 h at room temperature or three days under refrigeration. © The Author(s) 2014.

  16. Preparation of fatty acid methyl esters for gas-liquid chromatography[S

    PubMed Central

    Ichihara, Ken'ichi; Fukubayashi, Yumeto

    2010-01-01

    A convenient method using commercial aqueous concentrated HCl (conc. HCl; 35%, w/w) as an acid catalyst was developed for preparation of fatty acid methyl esters (FAMEs) from sterol esters, triacylglycerols, phospholipids, and FFAs for gas-liquid chromatography (GC). An 8% (w/v) solution of HCl in methanol/water (85:15, v/v) was prepared by diluting 9.7 ml of conc. HCl with 41.5 ml of methanol. Toluene (0.2 ml), methanol (1.5 ml), and the 8% HCl solution (0.3 ml) were added sequentially to the lipid sample. The final HCl concentration was 1.2% (w/v). This solution (2 ml) was incubated at 45°C overnight or heated at 100°C for 1–1.5 h. The amount of FFA formed in the presence of water derived from conc. HCl was estimated to be <1.4%. The yields of FAMEs were >96% for the above lipid classes and were the same as or better than those obtained by saponification/methylation or by acid-catalyzed methanolysis/methylation using commercial anhydrous HCl/methanol. The method developed here could be successfully applied to fatty acid analysis of various lipid samples, including fish oils, vegetable oils, and blood lipids by GC. PMID:19759389

  17. n-Type Conductivity of Cu2O Thin Film Prepared in Basic Aqueous Solution Under Hydrothermal Conditions

    NASA Astrophysics Data System (ADS)

    Ursu, Daniel; Miclau, Nicolae; Miclau, Marinela

    2018-03-01

    We report for the first time in situ hydrothermal synthesis of n-type Cu2O thin film using strong alkaline solution. The use of copper foil as substrate and precursor material, low synthesis temperature and short reaction time represent the arguments of a new, simple, inexpensive and high field synthesis method for the preparation of n-type Cu2O thin film. The donor concentration of n-type Cu2O thin film obtained at 2 h of reaction time has increased two orders of magnitude than previous reported values. We have demonstrated n-type conduction in Cu2O thin film prepared in strong alkaline solution, in the contradiction with the previous works. Based on experimental results, the synthesis mechanism and the origin of n-type photo-responsive behavior of Cu2O thin film were discussed. We have proposed that the unexpected n-type character could be explained by H doping of Cu2O thin film in during of the hydrothermal synthesis that caused the p-to-n conductivity-type conversion. Also, this work raises new questions about the origin of n-type conduction in Cu2O thin film, the influence of the synthesis method on the nature of the intrinsic defects and the electrical conduction behavior.

  18. [Application of fuzzy mathematics on modifying taste of oral solution of traditional Chinese drug].

    PubMed

    Wang, Youjie; Feng, Yi; Zhang, Bo

    2009-01-01

    To apply Fuzzy mathematical methods to choose the best taste modifying prescription of oral solution of traditional Chinese drug. Jin-Fukang oral solution was used as a model drug. The oral solution was prepared in different taste modifying prescriptions, whose tastes were evaluated by the fuzzy quality synthetic evaluation system. Compound-sweeteners with Sucralose and Erythritol was the best choice. Fuzzy integrated evaluation can be used to evaluate the taste of traditional Chinese medicinal pharmaceuticals, which overcame the artificial factors and achieve more objective conclusion.

  19. Common stock solutions, buffers, and media.

    PubMed

    2001-05-01

    This collection of recipes describes the preparation of buffers and reagents used in Current Protocols in Pharmacology for cell culture, manipulation of neural tissue, molecular biological methods, and neurophysiological/neurochemical measurements. RECIPES: Acid, concentrated stock solutions Ammonium hydroxide, concentrated stock solution EDTA (ethylenediaminetetraacetic acid), 0.5 M (pH 8.0) Ethidium bromide staining solution Fetal bovine serum (FBS) Gel loading buffer, 6× LB medium (Luria broth) and LB plates Potassium phosphate buffer, 0.1 M Sodium phosphate buffer, 0.1 M TE (Tris/EDTA) buffer Tris⋅Cl, 1 M.

  20. Mercuric 5-Nitrotetrazole, a Possible Replacement for Lead Azide in Australian Ordnance. Part 1. An Assessment of Preparation Methods

    DTIC Science & Technology

    1983-08-01

    nitrotetrazole) (Cuen2 (NT)2 ) [7) A solution of sodium nitrite (26 g) and cupric sulfate pentahydrate (13.75 g) in water (75 ml) was placed in the 600 ml...pan and cooled to 50C. To this stirred solution was added a solution of 5-aminotetrazole monohydrate (12.9 g), cupric sulfate pentahydrate (1.0 g) and...stirring then a solution of cupric sulfate pentahydrate (5.25 q) and ethylenediamine (11.25 ml) in water (20 ml) was added. Stirring and heating were

  1. The low temperature synthesis, characterization and properties of ferroelectrics

    NASA Astrophysics Data System (ADS)

    Xu, Jie

    2000-10-01

    PZT 50:50 xerogels prepared by two different sol-gel routes crystallized in a similar fashion to give a mixture of tetragonal and rhombohedral at high temperature (1000°C). Both the diffraction and EXAFS data suggest that the compositional inhomogeneity of the samples prepared by the two routes is similar. The crystallization of CZT gels is complicated. Crystalline CaCO 3 was always detected in the dry gels regardless of the sample composition and preparation methods. At intermediate temperatures a fluorite related phase was always formed and it transformed to perovskite at higher temperatures. The EXAFS data suggest that perovskite CZT samples prepared using alkoxide sol-gel chemistry may not be random solid solutions. All the solution processed ZrTiO4 materials crystallized in the range 600--700°C. The KTN samples prepared using a conventional alkoxide sol-gel route crystallized completely to perovskite at lower temperatures than those prepared using prehydrolyzed precursors. The EXAFS data for the KTN samples prepared using a conventional alkoxide sol-gel route are consistent with a random distribution of tantalum and niobium in the solid solution. However, materials prepared using the inhomogeneous sol-gel route and by the direct reaction of mixed oxides were shown to be compositionally inhomogeneous. The heterogeneity could not be removed by regrinding and heating the mixed oxide samples several times. K2Ta4-xNbxO11 (x = 0, 2, 4) samples were prepared using alkoxide sol-gel chemistry and their crystallization was examined by powder X-ray diffraction. A Rietveld structure analysis of the pyrochlore formed from a gel with bulk composition K2Ta 2Nb2O11 indicated that it was rich in potassium relative to the bulk sample. On heating to high temperatures tetragonal tungsten bronzes were formed. A Rietveld analysis was also performed for K2Ta 2Nb2O11 with tetragonal tungsten bronze structure. The defect pyrochlores "AgTaO3" and GaTaO 3 were synthesized by ion-exchange using pyrochlore KTaO3 as a starting material. The structures of the pyrochlores were examined using the Rietveld method. The pyrochlore-to-perovskite transformations were also explored.

  2. A novel strategy to design sustained-release poorly water-soluble drug mesoporous silica microparticles based on supercritical fluid technique.

    PubMed

    Li-Hong, Wang; Xin, Che; Hui, Xu; Li-Li, Zhou; Jing, Han; Mei-Juan, Zou; Jie, Liu; Yi, Liu; Jin-Wen, Liu; Wei, Zhang; Gang, Cheng

    2013-09-15

    The organic solvent solution immersion method was often used to achieve the loading of the drugs into mesoporous silica, but the drugs that have loaded into the pores of the mesoporous silica would inevitable migrate from the inside to the external surface or near the outside surface during the process of drying. Hence, it often leads to the pores of mesoporous materials not be fully utilized, and results in a low drug loading efficiency and a fast releasing rate. The purpose of this study was to develop a novel drug loading strategy to avoid soluble component migration during the process of drying, then, to prepare poorly water-soluble drug mesoporous silica microparticles with higher drug loading efficiency and longer sustained-release time. Ibuprofen was used as model drug. The microparticles were prepared by a novel method based on mesoporous silica and supercritical fluid (SCF) technique. The drug-loaded mesoporous silica microparticles prepared by SCF technique were analyzed by thermogravimetric analysis (TGA), N2 adsorption/desorption, scanning electron microscopy (SEM), powder X-ray diffraction (XRD) and differential scanning calorimetry (DSC). In vitro releasing study was used to evaluate the sustained-release effect of the drug-loaded microparticles. By virtue of the high diffusibility and the high dissolving capacity of the supercritical carbon dioxide (SCF-CO2), the poorly water-soluble drugs, ibuprofen, entered the pores of the mesoporous silica. The amount and the depth of ibuprofen entered the pores of the mesoporous silica by SCF technique were both larger than those by the solution immersion method. It was found that ibuprofen loaded into the mesoporous silica by SCF technique was amorphous and the largest amount of the ibuprofen loaded into the mesoporous silica by SCF technique could reach 386 mg/g (w/w, ibuprofen/SiO2), it was more than that by the solution immersion method. In vitro releasing study showed that the sustained-release effect of ibuprofen in the samples prepared by SCF technique was 50% in 15 min and 90% in 60 min. It was longer than that prepared by the solution immersion method. Present study showed that sustained-release poorly water-soluble drug mesoporous silica microparticle based on SCF technique has twofold advantages. One is the larger drug loading amount in internal pores of the mesoporous silica, the other is the longer drug releasing time. Copyright © 2013 Elsevier B.V. All rights reserved.

  3. Preparation and characterization of progesterone dispersions using supercritical carbon dioxide.

    PubMed

    Falconer, James R; Wen, Jingyuan; Zargar-Shoshtari, Sara; Chen, John J; Farid, Mohammed; Tallon, Stephen J; Alany, Raid G

    2014-04-01

    Supercritical fluid methods offer an alternative to conventional mixing methods, particularly for heat sensitive drugs and where an organic solvent is undesirable. To design, develop and construct a unit for the particles from a gas-saturated suspension/solution (PGSS) method and form endogenous progesterone (PGN) dispersion systems using SC-CO2. The PGN dispersions were manufactured using three selected excipients: polyethylene glycol (PEG) 400/4000 (50:50), Gelucire 44/14 and D-α-tocopheryl PEG 1000 succinate (TPGS). Semisolid dispersions of PGN prepared by PGSS method were compared to the conventional methods; comelting (CM), cosolvent (CS) and physical mixing (PM). The dispersion systems made were characterized by Raman and Fourier transform infrared (FTIR) spectroscopies, X-ray powder diffraction (XRPD), scanning electron microscopy (SEM), PGN recovery, uniformity and in vitro dissolution, analyzed by high-performance liquid chromatography (HPLC). Raman spectra revealed no changes in the crystalline structure of PGN treated with SC-CO2 compared to that of untreated PGN. XRPD and FTIR showed the presence of peaks and bands for PGN confirming that PGN has been incorporated well with each individual excipient. All PGN dispersions prepared by the PGSS method resulted in the improvement of PGN dissolution rates compared to that prepared by the conventional methods and untreated PGN after 60 min (p value < 0.05). The novel PGN dispersions prepared by the PGSS method offer the great potential to enhance PGN dissolution rate, reduce preparation time and form stable crystalline dispersion systems over those prepared by conventional methods.

  4. Feasible way of Human Solid and Liquid Wastes' Inclusion Into Intersystem Mass Exchange of Biological-Technical Life Support Systems

    NASA Astrophysics Data System (ADS)

    Ushakova, Sofya; Tikhomirov, Alexander A.; Tikhomirova, Natalia; Kudenko, Yurii; Griboskaya, Illiada; Gros, Jean-Bernard; Lasseur, Christophe

    The basic objective arising at use of mineralized human solid and liquid wastes serving as the source of mineral elements for plants cultivation in biological-technical life support systems appears to be NaCl presence in them. The given work is aimed at feasibility study of mineralized human metabolites' utilization for nutrient solutions' preparation for their further employment at a long-term cultivation of uneven-aged wheat and Salicornia europaea L. cenosis in a conveyer regime. Human solid and liquid wastes were mineralized by the "wet incineration" method developed by Yu. Kudenko. On their base the solutions were prepared which were used for cultivation of 5-aged wheat conveyer with the time step-interval of 14 days. Wheat was cultivated by hydroponics method on expanded clay aggregate. For partial demineralization of nutrient solution every two weeks after regular wheat harvesting 12 L of solution was withdrawn from the wheat irrigation tank and used for Salicornia europaea cultivation by the water culture method in a conveyer regime. The Salicornia europaea conveyer was represented by 2 ages with the time step-interval of 14 days. Resulting from repeating withdrawal of the solution used for wheat cultivation, sodium concentration in the wheat irrigation solution did not exceed 400 mg/l, and mineral elements contained in the taken solution were used for Salicornia europaea cultivation. The experiment lasted 7 months. Total wheat biomass productivity averaged 30.1 g*m-2*day-1 at harvest index equal to 36.8The work was carried out under support of SB RAS grant 132 and INTAS 05-1000008-8010

  5. New Tools to Prepare ACE Cross-section Files for MCNP Analytic Test Problems

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

    Brown, Forrest B.

    Monte Carlo calculations using one-group cross sections, multigroup cross sections, or simple continuous energy cross sections are often used to: (1) verify production codes against known analytical solutions, (2) verify new methods and algorithms that do not involve detailed collision physics, (3) compare Monte Carlo calculation methods with deterministic methods, and (4) teach fundamentals to students. In this work we describe 2 new tools for preparing the ACE cross-section files to be used by MCNP ® for these analytic test problems, simple_ace.pl and simple_ace_mg.pl.

  6. Study of viscous flow about airfoils by the integro-differential method

    NASA Technical Reports Server (NTRS)

    Wu, J. C.; Sampath, S.

    1975-01-01

    An integro-differential method was used for numerically solving unsteady incompressible viscous flow problems. A computer program was prepared to solve the problem of an impulsively started 9% thick symmetric Joukowski airfoil at an angle of attack of 15 deg and a Reynolds number of 1000. Some of the results obtained for this problem were discussed and compared with related work completed previously. Two numerical procedures were used, an Alternating Direction Implicit (ADI) method and a Successive Line Relaxation (SLR) method. Generally, the ADI solution agrees well with the SLR solution and with previous results are stations away from the trailing edge. At the trailing edge station, the ADI solution differs substantially from previous results, while the vorticity profiles obtained from the SLR method there are in good qualitative agreement with previous results.

  7. Investigation of solvent-free MALDI-TOFMS sample preparation methods for the analysis of organometallic and coordination compounds.

    PubMed

    Hughes, Laura; Wyatt, Mark F; Stein, Bridget K; Brenton, A Gareth

    2009-01-15

    An investigation of various solvent-free matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS) sample preparation methods for the characterization of organometallic and coordination compounds is described. Such methods are desirable for insoluble materials, compounds that are only soluble in disadvantageous solvents, or complexes that dissociate in solution, all of which present a major "difficulty" to most mass spectrometry techniques. First-row transition metal acetylacetonate complexes, which have been characterized previously by solution preparation MALDI-TOFMS, were used to evaluate the various solvent-free procedures. These procedures comprise two distinct steps: the first being the efficient "solids mixing" (the mixing of sample and matrix), and the second being the effective transfer of the sample/matrix mixture to the MALDI target plate. This investigation shows that vortex mixing is the most efficient first step and that smearing using a microspatula is the most effective second step. In addition, the second step is shown to be much more critical than the first step in obtaining high-quality data. Case studies of truly insoluble materials highlight the importance of these techniques for the wider chemistry community.

  8. Waters of Hydration of Cupric Hydrates: A Comparison between Heating and Absorbance Methods

    ERIC Educational Resources Information Center

    Barlag, Rebecca; Nyasulu, Frazier

    2011-01-01

    The empirical formulas of four cupric hydrates are determined by measuring the absorbance in aqueous solution. The Beer-Lambert Law is verified by constructing a calibration curve of absorbance versus known Cu[superscript 2+](aq) concentration. A solution of the unknown hydrate is prepared by using 0.2-0.3 g of hydrate, and water is added such…

  9. TBARs distillation method: revision to minimize the interference from yellow pigments in meat products.

    PubMed

    Díaz, P; Linares, M B; Egea, M; Auqui, S M; Garrido, M D

    2014-12-01

    The aim was to study the effect of the incubation method and TBA reagent (concentration/solvent) on yellow pigment interference in meat products. Distillates from red sausage, sucrose, malondialdehyde and a mixture of sucrose-malondialdehyde were reacted with four different TBA solutions at five different temperature/time relations. Two TBA solutions were prepared at 20mM using 90% glacial acetic acid or 3.86% perchloric acid. In addition, an 80mM TBA solution was prepared using distilled water adjusted to pH4 and another using 0.8% TBA in distilled water. The temperature/time relations were: (1) 35min in a boiling water bath; (2) 70°C/30min; (3) 40°C/90min; (4) room temperature (r.t.) (24°C) in dark conditions for 20h; and (5) 60min in a boiling water bath. The results showed that aqueous or diluted acid solutions of TBA reagent and the application of 100°C for less than 1h provided the best conditions to minimize the presence of yellow pigments and maximize pink pigment formation in meat products. Copyright © 2014 Elsevier Ltd. All rights reserved.

  10. Synthesis of non-hydrazine solution processed Cu2(ZnSn)S4 thin films for solar cells applications

    NASA Astrophysics Data System (ADS)

    Gupta, Indu; Gupta, Preeti; Mohanty, Bhaskar Chandra

    2017-05-01

    Solution processing provides a versatile and inexpensive means to prepare Cu2ZnSnS4 (CZTS) thin films for photovoltaic applications. Differently with the reported growth of CZTS films from hydrazine based toxic solutions, we demonstrate a simple non-toxic ethanol based solution approach to synthesize the films. Using the chemical bath deposition (CBD) method, the CZTS thin films were grown from metal salts (copper chloride, zinc chloride, and tin chloride) in ethanol and monoethanol amine (MEA) and thioacetamide in ethanol as sulfur source in a single dip followed by sulfurization. The structure, composition, morphology and optical properties of the CZTS film were studied by X-ray diffraction, scanning electron microscopy and UV-vis spectroscopy. The results revealed that a post-deposition sulfurization is necessary to the phase formation and among all, sulfurization at 450°C for 60 min yielded phase pure CZTS films having kesterite structure, relatively compact morphology and an optical band gap of ˜1.52 eV indicating its suitability for solar cell applications. The results clearly validate the CBD method as a potential scalable route of preparation of CZTS thin films.

  11. Preparation of κ-carra-oligosaccharides with microwave assisted acid hydrolysis method

    NASA Astrophysics Data System (ADS)

    Li, Guangsheng; Zhao, Xia; Lv, Youjing; Li, Miaomiao; Yu, Guangli

    2015-04-01

    A rapid method of microwave assisted acid hydrolysis was established to prepare κ-carra-oligosaccharides. The optimal hydrolysis condition was determined by an orthogonal test. The degree of polymerization (DP) of oligosaccharides was detected by high performance thin layer chromatography (HPTLC) and polyacrylamide gel electrophoresis (PAGE). Considering the results of HPTLC and PAGE, the optimum condition of microwave assisted acid hydrolysis was determined. The concentration of κ-carrageenan was 5 mg mL-1; the reaction solution was adjusted to pH 3 with diluted hydrochloric acid; the solution was hydrolyzed under microwave irradiation at 100 for 15 °C min. Oligosaccharides were separated by a Superdex 30 column (2.6 cm × 90 cm) using AKTA Purifier UPC100 and detected with an online refractive index detector. Each fraction was characterized by electrospray ionization mass spectrometry (ESI-MS). The data showed that odd-numbered κ-carra-oligosaccharides with DP ranging from 3 to 21 could be obtained with this method, and the structures of the oligosaccharides were consistent with those obtained by traditional mild acid hydrolysis. The new method was more convenient, efficient and environment-friendly than traditional mild acid hydrolysis. Our results provided a useful reference for the preparation of oligosaccharides from other polysaccharides.

  12. Physicochemical characterization of atorvastatin calcium/ezetimibe amorphous nano-solid dispersions prepared by electrospraying method.

    PubMed

    Jahangiri, Azin; Barzegar-Jalali, Mohammad; Javadzadeh, Yousef; Hamishehkar, Hamed; Adibkia, Khosro

    2017-09-01

    In the present study, electrospraying was applied as a novel method for the fabrication of amorphous nano-solid dispersions (N-SDs) of atorvastatin calcium (ATV), ezetimibe (EZT), and ATV/EZT combination as poorly water-soluble drugs. N-SDs were prepared using polyvinylpyrrolidone K30 as an amorphous carrier in 1:1 and 1:5 drug to polymer ratios and the total solid (including drug and polymer) concentrations of 10 and 20% (w/v). The prepared formulations were further investigated for their morphological, physicochemical, and dissolution properties. Scanning electron microscopy studies indicated that the morphology and diameter of the electrosprayed samples (ESs) were influenced by the solution concentration and drug:polymer ratio, so that an increase in the solution concentration resulted in fiber formation while an increase in the polymer ratio led to enhancement of the particle diameter. Differential scanning calorimetry and X-ray powder diffraction studies together with in vitro dissolution test revealed that the ESs were present in an amorphous form with improved dissolution properties. Infrared spectroscopic studies showed hydrogen-bonding interaction between the drug and polymer in ESs. Since the electrospraying method benefits from the both amorphization and nanosizing effect, this novel approach seems to be an efficient method for the fabrication of N-SDs of poorly water-soluble drugs.

  13. Experimental Analysis of Temperature Differences During Implant Site Preparation: Continuous Drilling Technique Versus Intermittent Drilling Technique.

    PubMed

    Di Fiore, Adolfo; Sivolella, Stefano; Stocco, Elena; Favero, Vittorio; Stellini, Edoardo

    2018-02-01

    Implant site preparation through drilling procedures may cause bone thermonecrosis. The aim of this in vitro study was to evaluate, using a thermal probe, overheating at implant sites during osteotomies through 2 different drilling methods (continuous drilling technique versus intermittent drilling technique) using irrigation at different temperatures. Five implant sites 13 mm in length were performed on 16 blocks (fresh bovine ribs), for a total of 80 implant sites. The PT-100 thermal probe was positioned 5 mm from each site. Two physiological refrigerant solutions were used: one at 23.7°C and one at 6.0°C. Four experimental groups were considered: group A (continuous drilling with physiological solution at 23.7°C), group B (intermittent drilling with physiological solution at 23.7°C), group C (continuous drilling with physiological solution at 6.0°C), and group D (intermittent drilling with physiological solution at 6.0°C). The Wilcoxon rank-sum test (2-tailed) was used to compare groups. While there was no difference between group A and group B (W = 86; P = .45), statistically significant differences were observed between experimental groups A and C (W = 0; P =.0001), B and D (W = 45; P =.0005), and C and D (W = 41; P = .003). Implant site preparation did not affect the overheating of the bone. Statistically significant differences were found with the refrigerant solutions. Using both irrigating solutions, bone temperature did not exceed 47°C.

  14. Preparation of Fish Skin Gelatin-Based Nanofibers Incorporating Cinnamaldehyde by Solution Blow Spinning.

    PubMed

    Liu, Fei; Türker Saricaoglu, Furkan; Avena-Bustillos, Roberto J; Bridges, David F; Takeoka, Gary R; Wu, Vivian C H; Chiou, Bor-Sen; Wood, Delilah F; McHugh, Tara H; Zhong, Fang

    2018-02-22

    Cinnamaldehyde, a natural preservative that can non-specifically deactivate foodborne pathogens, was successfully incorporated into fish skin gelatin (FSG) solutions and blow spun into uniform nanofibers. The effects of cinnamaldehyde ratios (5-30%, w / w FSG) on physicochemical properties of fiber-forming emulsions (FFEs) and their nanofibers were investigated. Higher ratios resulted in higher values in particle size and viscosity of FFEs, as well as higher values in diameter of nanofibers. Loss of cinnamaldehyde was observed during solution blow spinning (SBS) process and cinnamaldehyde was mainly located on the surface of resultant nanofibers. Nanofibers all showed antibacterial activity by direct diffusion and vapor release against Escherichia coli O157:H7 , Salmonella typhimurium , and Listeria monocytogenes . Inhibition zones increased as cinnamaldehyde ratio increased. Nanofibers showed larger inhibition effects than films prepared by casting method when S . typhimurium was exposed to the released cinnamaldehyde vapor, although films had higher remaining cinnamaldehyde than nanofibers after preparation. Lower temperature was favorable for cinnamaldehyde retention, and nanofibers added with 10% cinnamaldehyde ratio showed the highest retention over eight-weeks of storage. Results suggest that FSG nanofibers can be prepared by SBS as carriers for antimicrobials.

  15. Preparation of Fish Skin Gelatin-Based Nanofibers Incorporating Cinnamaldehyde by Solution Blow Spinning

    PubMed Central

    Liu, Fei; Avena-Bustillos, Roberto J.; Bridges, David F.; Takeoka, Gary R.; Wu, Vivian C. H.; Chiou, Bor-Sen; McHugh, Tara H.; Zhong, Fang

    2018-01-01

    Cinnamaldehyde, a natural preservative that can non-specifically deactivate foodborne pathogens, was successfully incorporated into fish skin gelatin (FSG) solutions and blow spun into uniform nanofibers. The effects of cinnamaldehyde ratios (5–30%, w/w FSG) on physicochemical properties of fiber-forming emulsions (FFEs) and their nanofibers were investigated. Higher ratios resulted in higher values in particle size and viscosity of FFEs, as well as higher values in diameter of nanofibers. Loss of cinnamaldehyde was observed during solution blow spinning (SBS) process and cinnamaldehyde was mainly located on the surface of resultant nanofibers. Nanofibers all showed antibacterial activity by direct diffusion and vapor release against Escherichia coli O157:H7, Salmonella typhimurium, and Listeria monocytogenes. Inhibition zones increased as cinnamaldehyde ratio increased. Nanofibers showed larger inhibition effects than films prepared by casting method when S. typhimurium was exposed to the released cinnamaldehyde vapor, although films had higher remaining cinnamaldehyde than nanofibers after preparation. Lower temperature was favorable for cinnamaldehyde retention, and nanofibers added with 10% cinnamaldehyde ratio showed the highest retention over eight-weeks of storage. Results suggest that FSG nanofibers can be prepared by SBS as carriers for antimicrobials. PMID:29470390

  16. Low density microcellular carbon foams and method of preparation

    DOEpatents

    Arnold, C. Jr.; Aubert, J.H.; Clough, R.L.; Rand, P.B.; Sylwester, A.P.

    1988-06-20

    A low density, open-celled microcellular carbon foam is disclosed which is prepared by dissolving a carbonizable polymer or copolymer in a solvent, pouring the solution into a mold, cooling the solution, removing the solvent, and then carbonizing the polymer or copolymer in a high temperature oven to produce the foam. If desired, an additive can be introduced in order to produce a doped carbon foam, and the foams can be made isotropic by selection of a suitable solvent. The low density, microcellular foams produced by this process are particularly useful in the fabrication of inertial confinement fusion targets, but can also be used as catalysts, absorbents, and electrodes.

  17. Low density microcellular carbon foams and method of preparation

    DOEpatents

    Arnold, Jr., Charles; Aubert, James H.; Clough, Roger L.; Rand, Peter B.; Sylwester, Alan P.

    1989-01-01

    A low density, open-celled microcellular carbon foam is disclosed which is prepared by dissolving a carbonizable polymer or copolymer in a solvent, pouring the solution into a mold, cooling the solution, removing the solvent, and then carbonizing the polymer or copolymer in a high temperature oven to produce the foam. If desired, an additive can be introduced in order to produce a doped carbon foam, and the foams can be made isotropic by selection of a suitable solvent. The low density, microcellular foams produced by this process are particularly useful in the fabrication of inertial confinement fusion targets, but can also be used as catalysts, absorbents, and electrodes.

  18. A potentiometric titration method for the crystallization of drug-like organic molecules.

    PubMed

    Du-Cuny, Lei; Huwyler, Jörg; Fischer, Holger; Kansy, Manfred

    2007-09-05

    It is generally accepted, that crystalline solids representing a low energy polymorph should be selected for development of oral dosage forms. As a consequence, efficient and robust procedures are needed at an early stage during drug discovery to prepare crystals from drug-like organic molecules. In contrast to the use of supersaturated solutions, we present a potentiometric crystallization procedure where saturated solutions are prepared in a controlled manner by pH-titration. Crystallization is carried out under defined conditions using the sample concentration and experimental pK(a) values as input parameters. Crystals of high quality were obtained for 11 drugs selected to demonstrate the efficiency and applicability of the new method. Technical improvements are suggested to overcome practical limitations and to enhance the possibility of obtaining crystals from molecules in their uncharged form.

  19. Physical Compatibility of Magnesium Sulfate and Sodium Bicarbonate in a Pharmacy-compounded Bicarbonate-buffered Hemofiltration Solution

    PubMed Central

    Moriyama, Brad; Henning, Stacey A.; Jin, Haksong; Kolf, Mike; Rehak, Nadja N.; Danner, Robert L.; Walsh, Thomas J.; Grimes, George J.

    2011-01-01

    PURPOSE To assess the physical compatibility of magnesium sulfate and sodium bicarbonate in a pharmacy-compounded bicarbonate-buffered hemofiltration solution used at the National Institutes of Health Clinical Center (http://www.cc.nih.gov). METHODS Two hemofiltration fluid formulations with a bicarbonate of 50 mEq/L and a magnesium of 1.5 mEq/L or 15 mEq/L were prepared in triplicate with an automated compounding device. The hemofiltration solution with a bicarbonate of 50 mEq/L and a magnesium of 1.5 mEq/L contains the maximum concentration of additives that we use in clinical practice. The hemofiltration solution of 15 mEq/L of magnesium and 50 mEq/L of bicarbonate was used to study the physicochemical properties of this interaction. The solutions were stored without light protection at 22 to 25 °C for 48 hours. Physical compatibility was assessed by visual inspection and microscopy. The pH of the solutions was assayed at 3 to 4 hours and 52 to 53 hours after compounding. In addition, electrolyte and glucose concentrations in the solutions were assayed at two time points after preparation: 3 to 4 hours and 50 to 51 hours. RESULTS No particulate matter was observed by visual and microscopic inspection in the compounded hemofiltration solutions at 48 hours. Electrolyte and glucose concentrations and pH were similar at both time points after solution preparation. CONCLUSION Magnesium sulfate (1.5 mEq/L) and sodium bicarbonate (50 mEq/L) were physically compatible in a pharmacy-compounded bicarbonate-buffered hemofiltration solution at room temperature without light protection at 48 hours. PMID:20237384

  20. Photocatalytic properties of h-WO3 nanoparticles obtained by annealing and h-WO3 nanorods prepared by hydrothermal method

    NASA Astrophysics Data System (ADS)

    Boyadjiev, Stefan I.; Nagy-Kovács, Teodóra; Lukács, István; Szilágyi, Imre M.

    2016-03-01

    In the present study, two different methods for preparing hexagonal WO3 (h-WO3) photocatalysts were used - controlled thermal decomposition and hydrothermal synthesis. WO3 nanoparticles with hexagonal structure were obtained by annealing (NH4)xWO3-y at 500 °C in air. WO3 nanorods were prepared by a hydrothermal method using sodium tungstate Na2WO4, HCl, (COOH)2 and NaSO4 precursors at 200 °C. The formation, morphology, structure and composition of the as-prepared nanoparticles and nanorods were studied by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy combined with energy-dispersive X-ray spectroscopy (SEM-EDX). The photocatalytic activity of the h-WO3 nanoparticles and nanorods was studied by decomposing methyl orange in aqueous solution under UV light irradiation.

  1. Evaluation of preparation methods for suspended nano-objects on substrates for dimensional measurements by atomic force microscopy

    PubMed Central

    Göhler, Daniel; Wessely, Benno; Stintz, Michael; Lazzerini, Giovanni Mattia; Yacoot, Andrew

    2017-01-01

    Dimensional measurements on nano-objects by atomic force microscopy (AFM) require samples of safely fixed and well individualized particles with a suitable surface-specific particle number on flat and clean substrates. Several known and proven particle preparation methods, i.e., membrane filtration, drying, rinsing, dip coating as well as electrostatic and thermal precipitation, were performed by means of scanning electron microscopy to examine their suitability for preparing samples for dimensional AFM measurements. Different suspensions of nano-objects (with varying material, size and shape) stabilized in aqueous solutions were prepared therefore on different flat substrates. The drop-drying method was found to be the most suitable one for the analysed suspensions, because it does not require expensive dedicated equipment and led to a uniform local distribution of individualized nano-objects. Traceable AFM measurements based on Si and SiO2 coated substrates confirmed the suitability of this technique. PMID:28904839

  2. Evaluation of preparation methods for suspended nano-objects on substrates for dimensional measurements by atomic force microscopy.

    PubMed

    Fiala, Petra; Göhler, Daniel; Wessely, Benno; Stintz, Michael; Lazzerini, Giovanni Mattia; Yacoot, Andrew

    2017-01-01

    Dimensional measurements on nano-objects by atomic force microscopy (AFM) require samples of safely fixed and well individualized particles with a suitable surface-specific particle number on flat and clean substrates. Several known and proven particle preparation methods, i.e., membrane filtration, drying, rinsing, dip coating as well as electrostatic and thermal precipitation, were performed by means of scanning electron microscopy to examine their suitability for preparing samples for dimensional AFM measurements. Different suspensions of nano-objects (with varying material, size and shape) stabilized in aqueous solutions were prepared therefore on different flat substrates. The drop-drying method was found to be the most suitable one for the analysed suspensions, because it does not require expensive dedicated equipment and led to a uniform local distribution of individualized nano-objects. Traceable AFM measurements based on Si and SiO 2 coated substrates confirmed the suitability of this technique.

  3. Proposed correlation of modern processing principles for Ayurvedic herbal drug manufacturing: A systematic review.

    PubMed

    Jain, Rahi; Venkatasubramanian, Padma

    2014-01-01

    Quality Ayurvedic herbal medicines are potential, low-cost solutions for addressing contemporary healthcare needs of both Indian and global community. Correlating Ayurvedic herbal preparations with modern processing principles (MPPs) can help develop new and use appropriate technology for scaling up production of the medicines, which is necessary to meet the growing demand. Understanding the fundamental Ayurvedic principles behind formulation and processing is also important for improving the dosage forms. Even though Ayurvedic industry has adopted technologies from food, chemical and pharmaceutical industries, there is no systematic study to correlate the traditional and modern processing methods. This study is an attempt to provide a possible correlation between the Ayurvedic processing methods and MPPs. A systematic literature review was performed to identify the Ayurvedic processing methods by collecting information from English editions of classical Ayurveda texts on medicine preparation methods. Correlation between traditional and MPPs was done based on the techniques used in Ayurvedic drug processing. It was observed that in Ayurvedic medicine preparations there were two major types of processes, namely extraction, and separation. Extraction uses membrane rupturing and solute diffusion principles, while separation uses volatility, adsorption, and size-exclusion principles. The study provides systematic documentation of methods used in Ayurveda for herbal drug preparation along with its interpretation in terms of MPPs. This is the first step which can enable improving or replacing traditional techniques. New technologies or use of existing technologies can be used to improve the dosage forms and scaling up while maintaining the Ayurvedic principles similar to traditional techniques.

  4. Development and characterization of a mucoadhesive sublingual formulation for pain control: extemporaneous oxycodone films in personalized therapy.

    PubMed

    Parodi, Brunella; Russo, Eleonora; Baldassari, Sara; Zuccari, Guendalina; Pastorino, Sara; Yan, Mengying; Neduri, Karthik; Caviglioli, Gabriele

    2017-06-01

    The aim of this work was the development of mucoadhesive sublingual films, prepared using a casting method, for the administration of oxycodone. A solvent casting method was employed to prepare the mucoadhesive films. A calibrated pipette was used to deposit single aliquots of different polymeric solutions on a polystyrene plate lid. Among the various tested polymers, hydroxypropylcellulose at low and medium molecular weight (HPC) and pectin at two different degrees of esterification (PC) were chosen for preparing solutions with good casting properties, capable of producing films suitable for mucosal application. The obtained films showed excellent drug content uniformity and stability and rapid drug release, which, at 8 min, ranged from 60% to 80%. All films presented satisfactory mucoadhesive and mechanical properties, also confirmed by a test on healthy volunteers, who did not experience irritation or mucosa damages. Pectin films based on pectin at lower degrees of esterification have been further evaluated to study the influence of two different amounts of drug on the physicochemical properties of the formulation. A slight reduction in elasticity has been observed in films containing a higher drug dose; nevertheless, the formulation maintained satisfactory flexibility and resistance to elongation. HPC and PC sublingual films, obtained by a simple casting method, could be proposed to realize personalized hospital pharmacy preparations on a small scale.

  5. Effect of small bowel preparation with simethicone on capsule endoscopy*

    PubMed Central

    Fang, You-hong; Chen, Chun-xiao; Zhang, Bing-ling

    2009-01-01

    Background: Capsule endoscopy is a novel non-invasive method for visualization of the entire small bowel. The diagnostic yield of capsule endoscopy depends on the quality of visualization of the small bowel mucosa and its complete passage through the small bowel. To date, there is no standardized protocol for bowel preparation before capsule endoscopy. The addition of simethicone in the bowel preparation for the purpose of reducing air bubbles in the intestinal lumen had only been studied by a few investigators. Methods: Sixty-four participants were randomly divided into two groups to receive a bowel preparation of polyethylene glycol (PEG) solution (Group 1) and both PEG solution and simethicone (Group 2). The PEG solution and simethicone were taken the night before and 20 min prior to capsule endoscopy, respectively. Frames taken in the small intestine were examined and scored for luminal bubbles by two professional capsule endoscopists. Gastric emptying time and small bowel transit time were also recorded. Results: Simethicone significantly reduced luminal bubbles both in the proximal and distal small intestines. The mean time proportions with slight bubbles in the proximal and distal intestines in Group 2 were 97.1% and 99.0%, respectively, compared with 67.2% (P<0.001) and 68.8% (P<0.001) in Group 1. Simethicone had no effect on mean gastric emptying time, 32.08 min in Group 2 compared with 30.88 min in Group 1 (P=0.868), but it did increase mean small intestinal transit time from 227.28 to 281.84 min (P=0.003). Conclusion: Bowel preparation with both PEG and simethicone significantly reduced bubbles in the intestinal lumen and improved the visualization of the small bowel by capsule endoscopy without any side effects observed. PMID:19198022

  6. Activity measurements of 55Fe by two different methods

    NASA Astrophysics Data System (ADS)

    da Cruz, Paulo A. L.; Iwahara, Akira; da Silva, Carlos J.; Poledna, Roberto; Loureiro, Jamir S.; da Silva, Monica A. L.; Ruzzarin, Anelise

    2018-03-01

    A calibrated germanium detector and CIEMAT/NIST liquid scintillation method were used in the standardization of solution of 55Fe coming from a key-comparison BIPM. Commercial cocktails were used in source preparation for activity measurements in CIEMAT/NIST method. Measurements were performed in Liquid Scintillation Counter. In the germanium counting method standard point sources were prepared for obtaining atomic number versus efficiency curve of the detector in order to obtain the efficiency of 5.9 keV KX-ray of 55Fe by interpolation. The activity concentrations obtained were 508.17 ± 3.56 and 509.95 ± 16.20 kBq/g for CIEMAT/NIST and germanium methods, respectively.

  7. MANGANESE DIOXIDE METHOD FOR PREPARATION OF PROTACTINIUM

    DOEpatents

    Katzin, L.I.

    1958-08-12

    A method of obtaining U/sup 233/ is described. An aqueous solution of neutriln irradiated thoriunn is treated by forming tberein a precipitate of manganese dioxide which carries and thus separates the Pa/sup 233/ from the solution. The carrier precipitate so formed is then dissolved in an acidic solution containing a reducing agent sufficiently electronegative to reduce the tetravalent manganese to the divalent state. Further purification of the Pa/sup 233/ may be obtained by forming another manganese dioxide carrier precipitate and subsequently dissolving it. Ater a sufficient number of such cycles have brought the Pa/sup 233/ to the desired purity, the solution is aged, allowing the formation ot U/sup 233/ by radioaetive decay. A manganese dioxide precipitate is then formed in the U/sup 233/ containing solution. This precipitate carries down any remaining Pa/sup 233/ thus leaving the separated U/sup 233/solution, from whieh it may be easily recovered.

  8. Stability of antimycobacterial drugs in susceptibility testing.

    PubMed Central

    Griffith, M E; Bodily, H L

    1992-01-01

    Aqueous solutions of 0.02% isoniazid, 0.2% streptomycin, 0.2% para-aminosalicylate, and 0.5% ethambutol and ethylene glycol solutions of 0.5% ethionamide stored at 3 to 7 degrees C remained stable for 1 year, as did aqueous solutions of 0.05% ethionamide hydrochloride, 0.05% kanamycin, 0.05% viomycin, and 0.1% capreomycin stored at -20 degrees C. The ethambutol and capreomycin solutions were tested by microbiologic methods; the other solutions were tested by both spectrophotometric and microbiologic methods. Prepared susceptibility testing media made with cycloserine, rifampin, and the above solutions incorporated into Middlebrook 7H10 medium showed acceptable stability when stored at 3 to 7 degrees C for 1 month. During incubation of the test medium at 37 degrees C, approximately half of the activity of isoniazid, ethionamide, ethambutol, cycloserine, and rifampin was lost after periods ranging from 2 to 4 days for ethambutol to 2 weeks for rifampin. PMID:1489183

  9. Current Technical Approaches for the Early Detection of Foodborne Pathogens: Challenges and Opportunities.

    PubMed

    Cho, Il-Hoon; Ku, Seockmo

    2017-09-30

    The development of novel and high-tech solutions for rapid, accurate, and non-laborious microbial detection methods is imperative to improve the global food supply. Such solutions have begun to address the need for microbial detection that is faster and more sensitive than existing methodologies (e.g., classic culture enrichment methods). Multiple reviews report the technical functions and structures of conventional microbial detection tools. These tools, used to detect pathogens in food and food homogenates, were designed via qualitative analysis methods. The inherent disadvantage of these analytical methods is the necessity for specimen preparation, which is a time-consuming process. While some literature describes the challenges and opportunities to overcome the technical issues related to food industry legal guidelines, there is a lack of reviews of the current trials to overcome technological limitations related to sample preparation and microbial detection via nano and micro technologies. In this review, we primarily explore current analytical technologies, including metallic and magnetic nanomaterials, optics, electrochemistry, and spectroscopy. These techniques rely on the early detection of pathogens via enhanced analytical sensitivity and specificity. In order to introduce the potential combination and comparative analysis of various advanced methods, we also reference a novel sample preparation protocol that uses microbial concentration and recovery technologies. This technology has the potential to expedite the pre-enrichment step that precedes the detection process.

  10. An Improved Method for Generating Consistent Soluble Amyloid-beta Oligomer Preparations for In Vitro Neurotoxicity Studies

    PubMed Central

    Ryan, Deborah A.; Narrow, Wade C.; Federoff, Howard J.; Bowers, William J.

    2010-01-01

    Soluble Aβ oligomers are recognized as playing a key role in Alzheimer’s disease (AD) pathophysiology. Despite their significance, many investigators encounter difficulty generating reliable preparations for in vitro and in vivo experiments. Solutions of Aβ are often unstable and soluble conformer profiles inconsistent. In this study we describe detailed methods for preparing Aβ oligomers that are stable for several weeks and are enriched for low and high molecular weight oligomeric forms, including the 56-kDa form, a conformer implicated in AD-related cognitive impairment. We characterize their structural and functional properties using Western blot, dot blot, atomic force microscopy, Thioflavine T fluorescence, and primary neuronal culture toxicity assays. These synthetic preparations should prove valuable to many studying Aβ-mediated mechanisms underlying AD. PMID:20452375

  11. Multicenter, randomized study to optimize bowel preparation for colon capsule endoscopy

    PubMed Central

    Kastenberg, David; Jr, Wilmot C Burch; Romeo, David P; Kashyap, Pankaj K; Pound, David C; Papageorgiou, Neophytos; Sainz, Ignacio Fernández-Urien; Sokach, Carly E; Rex, Douglas K

    2017-01-01

    AIM To assess the cleansing efficacy and safety of a new Colon capsule endoscopy (CCE) bowel preparation regimen. METHODS This was a multicenter, prospective, randomized, controlled study comparing two CCE regimens. Subjects were asymptomatic and average risk for colorectal cancer. The second generation CCE system (PillCam® COLON 2; Medtronic, Yoqneam, Israel) was utilized. Preparation regimens differed in the 1st and 2nd boosts with the Study regimen using oral sulfate solution (89 mL) with diatrizoate meglumine and diatrizoate sodium solution (“diatrizoate solution”) (boost 1 = 60 mL, boost 2 = 30 mL) and the Control regimen oral sulfate solution (89 mL) alone. The primary outcome was overall and segmental colon cleansing. Secondary outcomes included safety, polyp detection, colonic transit, CCE completion and capsule excretion ≤ 12 h. RESULTS Both regimens had similar cleansing efficacy for the whole colon (Adequate: Study = 75.9%, Control = 77.3%; P = 0.88) and individual segments. In the Study group, CCE completion was superior (Study = 90.9%, Control = 76.9%; P = 0.048) and colonic transit was more often < 40 min (Study = 21.8%, Control = 4%; P = 0.0073). More Study regimen subjects experienced adverse events (Study = 19.4%, Control = 3.4%; P = 0.0061), and this difference did not appear related to diatrizoate solution. Adverse events were primarily gastrointestinal in nature and no serious adverse events related either to the bowel preparation regimen or the capsule were observed. There was a trend toward higher polyp detection with the Study regimen, but this did not achieve statistical significance for any size category. Mean transit time through the entire gastrointestinal tract, from ingestion to excretion, was shorter with the Study regimen while mean colonic transit times were similar for both study groups. CONCLUSION A CCE bowel preparation regimen using oral sulfate solution and diatrizoate solution as a boost agent is effective, safe, and achieved superior CCE completion. PMID:29358870

  12. A Simple Surface-Enhanced Raman Spectroscopic Method for on-Site Screening of Tetracycline Residue in Whole Milk

    PubMed Central

    Dhakal, Sagar; Chao, Kuanglin; Huang, Qing; Kim, Moon; Schmidt, Walter; Qin, Jianwei; Broadhurst, C. Leigh

    2018-01-01

    Therapeutic and subtherapeutic use of veterinary drugs has increased the risk of residue contamination in animal food products. Antibiotics such as tetracycline are used for mastitis treatment of lactating cows. Milk expressed from treated cows before the withdrawal period has elapsed may contain tetracycline residue. This study developed a simple surface-enhanced Raman spectroscopic (SERS) method for on-site screening of tetracycline residue in milk and water. Six batches of silver colloid nanoparticles were prepared for surface enhancement measurement. Milk-tetracycline and water-tetracycline solutions were prepared at seven concentration levels (1000, 500, 100, 10, 1, 0.1, and 0.01 ppm) and spiked with silver colloid nanoparticles. A 785 nm Raman spectroscopic system was used for spectral measurement. Tetracycline vibrational modes were observed at 1285, 1317 and 1632 cm−1 in water-tetracycline solutions and 1322 and 1621 cm−1 (shifted from 1317 and 1632 cm−1, respectively) in milk-tetracycline solutions. Tetracycline residue concentration as low as 0.01 ppm was detected in both the solutions. The peak intensities at 1285 and 1322 cm−1 were used to estimate the tetracycline concentrations in water and milk with correlation coefficients of 0.92 for water and 0.88 for milk. Results indicate that this SERS method is a potential tool that can be used on-site at field production for qualitative and quantitative detection of tetracycline residues. PMID:29389871

  13. A Simple Surface-Enhanced Raman Spectroscopic Method for on-Site Screening of Tetracycline Residue in Whole Milk.

    PubMed

    Dhakal, Sagar; Chao, Kuanglin; Huang, Qing; Kim, Moon; Schmidt, Walter; Qin, Jianwei; Broadhurst, C Leigh

    2018-02-01

    Therapeutic and subtherapeutic use of veterinary drugs has increased the risk of residue contamination in animal food products. Antibiotics such as tetracycline are used for mastitis treatment of lactating cows. Milk expressed from treated cows before the withdrawal period has elapsed may contain tetracycline residue. This study developed a simple surface-enhanced Raman spectroscopic (SERS) method for on-site screening of tetracycline residue in milk and water. Six batches of silver colloid nanoparticles were prepared for surface enhancement measurement. Milk-tetracycline and water-tetracycline solutions were prepared at seven concentration levels (1000, 500, 100, 10, 1, 0.1, and 0.01 ppm) and spiked with silver colloid nanoparticles. A 785 nm Raman spectroscopic system was used for spectral measurement. Tetracycline vibrational modes were observed at 1285, 1317 and 1632 cm -1 in water-tetracycline solutions and 1322 and 1621 cm -1 (shifted from 1317 and 1632 cm -1 , respectively) in milk-tetracycline solutions. Tetracycline residue concentration as low as 0.01 ppm was detected in both the solutions. The peak intensities at 1285 and 1322 cm -1 were used to estimate the tetracycline concentrations in water and milk with correlation coefficients of 0.92 for water and 0.88 for milk. Results indicate that this SERS method is a potential tool that can be used on-site at field production for qualitative and quantitative detection of tetracycline residues.

  14. Enhanced photocatalytic degradation of 2-propanol over macroporous GaN/ZnO solid solution prepared by a novel sol-gel method

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

    Wang, Lizhong; Ouyang, Shuxin; Ren, Bofan

    2015-10-01

    Macroporous GaN/ZnO solid solution photocatalyst is synthesized through a novel sol-gel method under mild conditions. The performance of as-synthesized solid solution photocatalyst is evaluated for decomposition of gaseous 2-propanol (IPA). It is found that due to enhancement in both the adsorption to gaseous IPA and the absorbance to visible light, the porous GaN/ZnO solid solution exhibits a good photocatalytic performance for IPA decomposition. Moreover, the mechanism for photocatalytic degradation IPA over porous GaN/ZnO solid solution is also investigated in comparison with those for the two end materials ZnO and GaN. The trapping effects with different scavengers prove that both themore » photoexcited electrons and holes affect the IPA photodegradation process, simultaneously.« less

  15. Antiscalant properties of Spergularia rubra and Parietaria officinalis aqueous solutions

    NASA Astrophysics Data System (ADS)

    Cheap-Charpentier, Hélène; Gelus, Dominique; Pécoul, Nathalie; Perrot, Hubert; Lédion, Jean; Horner, Olivier; Sadoun, Jonathan; Cachet, Xavier; Litaudon, Marc; Roussi, Fanny

    2016-06-01

    The formation of calcium carbonate in water has important implications in industry. Chemical antiscalant is usually used to control scale depositions. Plant extracts have been recently used as new green antiscalant agents, as they can be easily prepared and are environmentally friendly. In this study, stock aqueous solutions of Spergularia rubra and Parietaria officinalis, two plants used in traditional medicine to treat or prevent urolithiasis, were obtained by infusion. The antiscaling properties of these extracts towards CaCO3 formation were tested by using chronoamperometry and Fast Controlled Precipitation methods. The aqueous solution of S. rubra was further fractionated to isolate compounds of lower polarity. Their efficiency towards CaCO3 precipitation was characterized by Fast Controlled Precipitation method. The inhibiting efficiency of this fractionated solution was greater than that of the stock aqueous solution.

  16. Crystallization from high temperature solutions of Si in copper

    DOEpatents

    Ciszek, Theodore F.

    1994-01-01

    A liquid phase epitaxy method for forming thin crystalline layers of device quality silicon having less than 5X10.sup.16 Cu atoms/cc impurity, comprising: preparing a saturated liquid solution melt of Si in Cu at about 16% to about 90% wt. Si at a temperature range of about 800.degree. C. to about 1400.degree. C. in an inert gas; immersing a substrate in the saturated solution melt; supersaturating the solution by lowering the temperature of the saturated solution melt and holding the substrate immersed in the solution melt for a period of time sufficient to cause growing Si to precipitate out of the solution to form a crystalline layer of Si on the substrate; and withdrawing the substrate from the solution.

  17. Common stock solutions, buffers, and media.

    PubMed

    2001-05-01

    This section describes the preparation of buffers and reagents used in this manual for cell culture, manipulation of tissue, and cell biological methods. Also discussed are special considerations for PCR experiments and for working with RNA.

  18. METHOD OF PREPARING RADIOACTIVE CESIUM SOURCES

    DOEpatents

    Quinby, T.C.

    1963-12-17

    A method of preparing a cesium-containing radiation source with physical and chemical properties suitable for high-level use is presented. Finely divided silica is suspended in a solution containing cesium, normally the fission-product isotope cesium 137. Sodium tetraphenyl boron is then added to quantitatively precipitate the cesium. The cesium-containing precipitate is converted to borosilicate glass by heating to the melting point and cooling. Up to 60 weight percent cesium, with a resulting source activity of up to 21 curies per gram, is incorporated in the glass. (AEC)

  19. SEVERAL METHODS FOR PREPARING RADIOACTIVE STANDARDS FOR ALPHA AND BETA URANIUM SOURCES (in Serbo-Croatian)

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

    Nemoda, D.

    1963-03-01

    Electrolytic methods for obtaining U radiation sources are described. The radiochemical and electrochemical characteristics of U are described which permit the preparation of a thin or a thick oxide saturation layer on the cathode. Experiments are described representing the deposit of U on metallic surfaces by acido-suifuric solutions with adapted acidity. The influence of acidity, temperature, concentration, reaction period, and surface size was studied. Under the optimal (NH/sub 4/)2CO/sub 3/ acidity, Fe, Al, and Cu are receptive in that order. (OID)

  20. SERS spectra of pyridine adsorbed on nickel film prepared by magnetron sputtering

    NASA Astrophysics Data System (ADS)

    Li, Daoyong; Ouyang, Yu; Chen, Li; Cao, Weiran; Shi, Shaohua

    2011-02-01

    As a repeating well and cheaper enhancement substrate, the nickel film was fabricated with magnetron sputtering coating instrument. Surface enhanced Raman spectra (SERS) of pyridine adsorbed on this nickel film are compared with the experimental values of gaseous pyridine, the theoretical value of pyridine solution listed in other literatures and our method is better than electro-chemical etching electrode method for large scale preparation. The enhancement factor of the nickel film is calculated and the result indicates that magnetron sputtering coating technology is feasible for obtaining good SERS active surface.

  1. METHOD FOR PREPARATION OF UO$sub 2$ PARTICLES

    DOEpatents

    Johnson, J.R.; Taylor, A.J.

    1959-09-22

    A method is described for the preparation of highdensity UO/sub 2/ particles within the size range of 40 to 100 microns. In accordance with the invention UO/sub 2/ particles are autoclaved with an aqueous solution of uranyl ions. The resulting crystals are reduced to UO/sub 2/ and the UO/sub 2/ is heated to at least 1000 deg C to effect densification. The resulting UO/sub 2/ particles are screened, and oversize particles are crushed and screened to recover the particles within the desired size range.

  2. Micro- and macrostructural characterization of polyvinylpirrolidone rotary-spun fibers.

    PubMed

    Sebe, István; Kállai-Szabó, Barnabás; Kovács, Krisztián Norbert; Szabadi, Enikő; Zelkó, Romána

    2015-01-01

    The application of high-speed rotary spinning can offer a useful mean for either preparation of fibrous intermediate for conventional dosage forms or drug delivery systems. Polyvinylpyrrolidone (PVP) and poly(vinylpyrrolidone-vinylacetate) (PVP VA) micro- and nanofibers of different polymer concentrations and solvent ratios were prepared with a high-speed rotary spinning technique. In order to study the influence of parameters that enable successful fiber production from polymeric viscous solutions, a complex micro- and macrostructural screening method was implemented. The obtained fiber mats were subjected to detailed morphological analysis using scanning electron microscope (SEM), and rheological measurements while the microstructural changes of fiber samples, based on the free volume changes, was analyzed by positron annihilation lifetime spectroscopy (PALS) and compared with their mechanical characteristics. The plasticizing effect of water tracked by ortho-positronium lifetime changes in relation to the mechanical properties of fibers. A concentration range of polyvinylpyrrolidone solutions was defined for the preparation of fibers of optimum fiber morphology and mechanical properties. The method enabled fiber formulation of advantageous functionality-related properties for further formulation of solid dosage forms.

  3. Synthesis of nanocrystalline CeO{sub 2} particles by different emulsion methods

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

    Supakanapitak, Sunisa; Boonamnuayvitaya, Virote; Jarudilokkul, Somnuk, E-mail: somnuk.jar@kmutt.ac.th

    2012-05-15

    Cerium oxide nanoparticles were synthesized using three different methods of emulsion: (1) reversed micelle (RM); (2) emulsion liquid membrane (ELM); and (3) colloidal emulsion aphrons (CEAs). Ammonium cerium nitrate and polyoxyethylene-4-lauryl ether (PE4LE) were used as cerium and surfactant sources in this study. The powder was calcined at 500 Degree-Sign C to obtain CeO{sub 2}. The effect of the preparation procedure on the particle size, surface area, and the morphology of the prepared powders were investigated. The obtained powders are highly crystalline, and nearly spherical in shape. The average particle size and the specific surface area of the powders frommore » the three methods were in the range of 4-10 nm and 5.32-145.73 m{sup 2}/g, respectively. The CeO{sub 2} powders synthesized by the CEAs are the smallest average particle size, and the highest surface area. Finally, the CeO{sub 2} prepared by the CEAs using different cerium sources and surfactant types were studied. It was found that the surface tensions of cerium solution and the type of surfactant affect the particle size of CeO{sub 2}. - Graphical Abstract: The emulsion droplet size distribution and the TEM images of CeO{sub 2} prepared by different methods: reversed micelle (RM), emulsion liquid membrane (ELM) and colloidal emulsion aphrons (CEAs). Highlights: Black-Right-Pointing-Pointer Nano-sized CeO{sub 2} was successfully prepared by three different emulsion methods. Black-Right-Pointing-Pointer The colloidal emulsion aphrons method producing CeO{sub 2} with the highest surface area. Black-Right-Pointing-Pointer The surface tensions of a cerium solution have slightly effect on the particle size. Black-Right-Pointing-Pointer The size control could be interpreted in terms of the adsorption of the surfactant.« less

  4. Synthesis and Characterization of BaFe12O19 Thin Films Using Suspension of Nano Powders

    NASA Astrophysics Data System (ADS)

    Salemizadeh, Saman; Seyyed Ebrahimi, S. A.

    BaM thin films have been synthesized by dispersing the dried gel nano powders prepared by Sol-Gel method. The solution was made by dissolving iron nitrate Fe(NO3).9H2O, barium nitrate Ba(NO3)2 and citric acid in deyonized water and methanol. This sol was slowly evaporated until a dried gel was formed. This dried gel was then added to ethylene glycol. The final solution was vigorously shaken and mixed in ultrasonic cleaner for 30 min to disperse particles sufficiently. Then the prepared solution spin coated on Si(110) substrate. The obtained thin films were dried at 120 °C and then calcined at 900 °C for 1 h. The films were characterized using X-ray diffraction (XRD) and vibrating sample magnetometer (VSM).

  5. Preparation of Husk-Based Porous Carbon-TiO2 Composites for Adsorption-Photocatalytic Degradation of Toluene in Aqueous Solution

    NASA Astrophysics Data System (ADS)

    Shi, Ning; Zhao, Lei; Liang, Shuran; Guo, Fengnan; Zhang, Dan; Liu, Xue; Li, Menghan; Peng, Xiao; Wu, Yan

    2017-12-01

    In this study, PC-nanoTiO2 and PC-P25 were prepared via chemical-deposition and mixture-calcination methods, respectively. Both of PC-nanoTiO2 and PC-P25 were employed to adsorb and photocatalytic degrade toluene in aqueous solution. The characterization results show that distribution of TiO2 nanoparticles in PC-nanoTiO2 and PC-P25 were different, but their binding force between PC and TiO2 were both chemical bonds. Due to synergy of adsorption and photocatalytic degradation, both PC-nanoTiO2 and PC-P25 exhibit good effect in removing toluene in aqueous solution, and both PC-nanoTiO2 and PC-P25 could be utilized for treating wastewater generated from hazardous chemicals leakage accidents emergency.

  6. Preparation and characterization of chitosan-clay nanocomposites for the removal of Cu(II) from aqueous solution.

    PubMed

    Azzam, Eid M S; Eshaq, Gh; Rabie, A M; Bakr, A A; Abd-Elaal, Ali A; El Metwally, A E; Tawfik, Salah M

    2016-08-01

    In the present study, chitosan assembled on gold and silver nanoparticles were prepared and characterized by UV-vis, TEM, EDX and DLS techniques. The nanocomposites chitosan (Ch)/clay, chitosan (Ch)/AgNPs/clay and chitosan (Ch)/AuNPs/clay were prepared by solution mixing method and characterized by FTIR, XRD, and SEM techniques. The adsorption of copper(II) ions onto the prepared hybrid composites from an aqueous solution using batch adsorption was examined. The results showed that benefiting from the surface property of clay, the abundant amino and hydroxyl functional groups of chitosan, the adsorbent provides adequate and versatile adsorption for the Cu(II) ions under investigation. The batch adsorption experiments showed that the adsorption of the Cu(II) is considerably dependent on pH of milieu, the amount of adsorbent, and contact time. Batch adsorption studies revealed that the adsorption capacity of Cu(II) increased with increase in initial concentration and contact time with optimum pH in the range around neutral. The maximum uptake of Cu(II) ions by (Ch)/AgNPs/clay composite was found to be 181.5mg/g. The adsorption efficiency of Cu(II) ions by prepared (Ch)/AgNPs/clay and (Ch)/AuNPs/clay is bigger than that the individual chitosan (Ch)/clay composite which clarifies the role of metal nanoparticles in enhancement the adsorption characters. The study suggests that the (Ch)/AgNPs/clay hybrid composite is a promising nano-adsorbent for the removal of Cu(II) ions from aqueous solution. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Preparation of Nonionic Vesicles Using the Supercritical Carbon Dioxide Reverse Phase Evaporation Method and Analysis of Their Solution Properties.

    PubMed

    Yamaguchi, Shunsuke; Tsuchiya, Koji; Sakai, Kenichi; Abe, Masahiko; Sakai, Hideki

    2016-01-01

    We have previously reported a new preparation method for liposomes using supercritical carbon dioxide (scCO2) as a solvent, referred to as the supercritical carbon dioxide reverse phase evaporation (scRPE) method. In our previous work, addition of ethanol to scCO2 as a co-solvent was needed, because lipid molecules had to be dissolved in scCO2 to form liposomes. In this new study, niosomes (nonionic surfactant vesicles) were prepared from various nonionic surfactants using the scRPE method. Among the nonionic surfactants tested were polyoxyethylene (6) stearylether (C18EO6), polyoxyethylene (5) phytosterolether (BPS-5), polyoxyethylene (6) sorbitan stearylester (TS-106V), and polyoxyethylene (4) sorbitan stearylester (Tween 61). All these surfactants have hydrophilic-lipophilic balance values (HLBs) around 9.5 to 9.9, and they can all form niosomes using the scRPE method even in the absence of ethanol. The high solubility of these surfactants in scCO2 was shown to be an important factor in yielding niosomes without ethanol addition. The niosomes prepared with the scRPE method had higher trapping efficiencies than those prepared using the conventional Bangham method, since the scRPE method gives a large number of unilamellar vesicles while the Bangham method gives multilamellar vesicles. Polyoxyethylene-type nonionic surfactants with HLB values from 9.5 to 9.9 were shown to be optimal for the preparation of niosomes with the scRPE method.

  8. Preparation of resveratrol-loaded nanoporous silica materials with different structures

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

    Popova, Margarita, E-mail: mpopova@orgchem.bas.bg; Szegedi, Agnes; Mavrodinova, Vesselina

    2014-11-15

    Solid, nanoporous silica-based spherical mesoporous MCM-41 and KIL-2 with interparticle mesoporosity as well as nanosized zeolite BEA materials differing in morphology and pore size distribution, were used as carriers for the preparation of resveratrol-loaded delivery systems. Two preparation methods have been applied: (i) loading by mixing of resveratrol and mesoporous carrier in solid state and (ii) deposition in ethanol solution. The parent and the resveratrol loaded carriers were characterized by XRD, TEM, N2 physisorption, thermal analysis, and FT-IR spectroscopy. The influence of the support structure on the adsorption capacity and the release kinetics of this poorly soluble compound were investigated.more » Our results indicated that the chosen nanoporous silica supports are suitable for stabilization of trans-resveratrol and reveal controlled release and ability to protect the supported compound against degradation regardless of loading method. The solid-state dry mixing appears very effective for preparation of drug formulations composed of poorly soluble compound. - Graphical abstract: trans-Resveratrol was stabilized in the pores of BEA zeolite, MCM-41and KIL2 mesoporous silicas. - Highlights: • BEA, KIL-2 and MCM-41 materials were used as carriers for resveratrol loading. • Resveratrol encapsulation in ethanol solution and solid state procedure were applied. • The solid-state preparation appears very effective for stabilization of trans-resveratrol.« less

  9. Improved Understanding of In Situ Chemical Oxidation. Technical Objective 2: Soil Reactivity

    DTIC Science & Technology

    2009-05-01

    each reaction tube. The reagents ( sulfuric acid /potassium dichromate/mercury sulfate ) were prepared following standard methods (APHA, 1998). When...reaction tubes. A volume (~20 mL) of potassium dichromate digestion solution (potassium dichromate (BDH Laboratories), sulfuric acid (EM Science...and mercury sulphate (EM Science)) and a sulfuric acid reagent solution ( sulfuric acid (EM Science) and silver sulphate (Alfa Aesar)) were added to

  10. CH3NH3I treatment temperature of 70 °C in low-pressure vapor-assisted deposition for mesoscopic perovskite solar cells

    NASA Astrophysics Data System (ADS)

    Jin, Wenbin; Zou, Xiaoping; Bai, Xiao; Yang, Ying; Chen, Dan

    2018-01-01

    Herein, we report a modified vapor-assisted deposition method to fabricate CH3NH3PbI3 film at 70 °C in a vacuum drying oven. The modified method has excellent operability and expandability in preparing perovskite solar cells. The CH3NH3I treatment temperature is 130 °C or 150 °C in conventional method, but we reduced the temperature to 70 °C in the modified vapor-assisted method. Meanwhile, the quality of CH3NH3PbI3 films prepared via the modified method is superior to that of CH3NH3PbI3 films of solution-processed method.

  11. Catalytic conversion of hydrocarbons to hydrogen and high-value carbon

    DOEpatents

    Shah, Naresh; Panjala, Devadas; Huffman, Gerald P.

    2005-04-05

    The present invention provides novel catalysts for accomplishing catalytic decomposition of undiluted light hydrocarbons to a hydrogen product, and methods for preparing such catalysts. In one aspect, a method is provided for preparing a catalyst by admixing an aqueous solution of an iron salt, at least one additional catalyst metal salt, and a suitable oxide substrate support, and precipitating metal oxyhydroxides onto the substrate support. An incipient wetness method, comprising addition of aqueous solutions of metal salts to a dry oxide substrate support, extruding the resulting paste to pellet form, and calcining the pellets in air is also discloses. In yet another aspect, a process is provided for producing hydrogen from an undiluted light hydrocarbon reactant, comprising contacting the hydrocarbon reactant with a catalyst as described above in a reactor, and recovering a substantially carbon monoxide-free hydrogen product stream. In still yet another aspect, a process is provided for catalytic decomposition of an undiluted light hydrocarbon reactant to obtain hydrogen and a valuable multi-walled carbon nanotube coproduct.

  12. Corrosion resistance of premodeled wires made of stainless steel used for heart electrotherapy leaders

    NASA Astrophysics Data System (ADS)

    Przondziono, J.; Walke, W.; Młynarski, R.; Szatka, W.

    2012-05-01

    The purpose of the study is to evaluate resistance to electrochemical corrosion of wire made of X10CrNi18-8 stainless steel designed for use in cardiology treatment. The influence of strain formed in the premodeling process and methods of wire surface preparation to corrosive resistance in artificial plasma solution were analysed. Wire corrosion tests were carried out in the solution of artificial plasma. Resistance to electrochemical corrosion was evaluated on the ground of recorded curves of anodic polarization by means of potentiodynamic method. Potentiodynamic tests carried out enabled to determine how the resistance to pitting corrosion of wire changes, depending on strain formed in the premodeling process as well as on the method of wire surface preparation. For evaluation of phenomena occurring on the surface of tested steel, electrochemical impedance spectroscopy (EIS) was applied. Deterioration of corrosive properties of wire along with the increase in the formed strain hardening was observed.

  13. The study of membrane formation via phase inversion method by cloud point and light scattering experiment

    NASA Astrophysics Data System (ADS)

    Arahman, Nasrul; Maimun, Teuku; Mukramah, Syawaliah

    2017-01-01

    The composition of polymer solution and the methods of membrane preparation determine the solidification process of membrane. The formation of membrane structure prepared via non-solvent induced phase separation (NIPS) method is mostly determined by phase separation process between polymer, solvent, and non-solvent. This paper discusses the phase separation process of polymer solution containing Polyethersulfone (PES), N-methylpirrolidone (NMP), and surfactant Tetronic 1307 (Tet). Cloud point experiment is conducted to determine the amount of non-solvent needed on induced phase separation. Amount of water required as a non-solvent decreases by the addition of surfactant Tet. Kinetics of phase separation for such system is studied by the light scattering measurement. With the addition of Tet., the delayed phase separation is observed and the structure growth rate decreases. Moreover, the morphology of fabricated membrane from those polymer systems is analyzed by scanning electron microscopy (SEM). The images of both systems show the formation of finger-like macrovoids through the cross-section.

  14. Toxicity of crude oil chemically dispersed in a wave tank to embryos of Atlantic herring (Clupea harengus).

    PubMed

    Greer, Colleen D; Hodson, Peter V; Li, Zhengkai; King, Thomas; Lee, Kenneth

    2012-06-01

    Tests of crude oil toxicity to fish are often chronic, exposing embryos from fertilization to hatch to oil solutions prepared using standard mixing procedures. However, during oil spills, fish are not often exposed for long periods and the dynamic nature of the ocean is not easily replicated in the lab. Our objective was to determine if brief exposures of Atlantic herring (Clupea harengus) embryos to dispersed oil prepared by standard mixing procedures was as toxic as oil dispersed in a more realistic model system. Embryos were first exposed to chemically dispersed Alaska North Slope crude and Arabian light crude oil for 2.4 h to 14 d from fertilization to determine if exposure time affected toxicity. Toxicity increased with exposure time, but 2.4-h exposures at realistic concentrations of oil induced blue-sac disease and reduced the percentage of normal embryos at hatch; there was little difference in toxicity between the two oils. Secondly, oil was chemically dispersed in a wave tank to determine if the resultant oil solutions were as toxic to herring embryos as laboratory-derived dispersed oil using a single exposure period of 24 h. Samples taken 15 min postdispersion were more toxic than laboratory-prepared solutions, but samples taken at 5, 30, and 60 min postdispersion were less toxic. Overall, the laboratory- and wave tank-derived solutions of dispersed oil provided similar estimates of toxicity despite differences in the methods for preparing test solutions, suggesting that laboratory and wave tank data are a reliable basis for ecological risk assessments of spilled oil. Copyright © 2012 SETAC.

  15. Transient bleaching of small PbS colloids. Influence of surface properties

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

    Nenadovic, M.T.; Comor, M.I.; Vasic, V.

    1990-08-09

    Small PbS colloids with a particle diameter of 40 {angstrom} were prepared in aqueous solution, and their absorption spectra exhibit several maxima. Injection of electrons into these particles was achieved by using the pulse radiolysis technique. Excess electrons trapped on the surface lead to a blue shift in the absorption edge of colloids. The appearance of this shift depends critically on the method of colloid preparation. PbS and CdS colloids prepared at pH < 6 have long-lived bleaching, which disappears after several seconds. On the other hand, absorption bleaching does not appear after the addition of hydroxide ions to colloidalmore » solutions (pH > 8). The existence of a hydroxide ion on the particle surface most likely removes surface defects on which electrons are trapped. PbS colloids prepared in the presence of 3-mercapto-1,2-propanediol have an unstructured absorption spectrum, which is due to a wide particle size distribution (10-50 {angstrom}).« less

  16. Numerical solution of the nonlinear Schrodinger equation by feedforward neural networks

    NASA Astrophysics Data System (ADS)

    Shirvany, Yazdan; Hayati, Mohsen; Moradian, Rostam

    2008-12-01

    We present a method to solve boundary value problems using artificial neural networks (ANN). A trial solution of the differential equation is written as a feed-forward neural network containing adjustable parameters (the weights and biases). From the differential equation and its boundary conditions we prepare the energy function which is used in the back-propagation method with momentum term to update the network parameters. We improved energy function of ANN which is derived from Schrodinger equation and the boundary conditions. With this improvement of energy function we can use unsupervised training method in the ANN for solving the equation. Unsupervised training aims to minimize a non-negative energy function. We used the ANN method to solve Schrodinger equation for few quantum systems. Eigenfunctions and energy eigenvalues are calculated. Our numerical results are in agreement with their corresponding analytical solution and show the efficiency of ANN method for solving eigenvalue problems.

  17. A stability analysis on forced convection boundary layer stagnation-point slip flow in Darcy-Forchheimer porous medium towards a shrinking sheet

    NASA Astrophysics Data System (ADS)

    Bakar, Shahirah Abu; Arifin, Norihan Md; Ali, Fadzilah Md; Bachok, Norfifah; Nazar, Roslinda

    2017-08-01

    The stagnation-point flow over a shrinking sheet in Darcy-Forchheimer porous medium is numerically studied. The governing partial differential equations are transformed into ordinary differential equations using a similarity transformation, and then solved numerically by using shooting technique method with Maple implementation. Dual solutions are observed in a certain range of the shrinking parameter. Regarding on numerical solutions, we prepared stability analysis to identify which solution is stable between non-unique solutions by bvp4c solver in Matlab. Further we obtain numerical results or each solution, which enable us to discuss the features of the respective solutions.

  18. The formation of stable pH gradients with weak monovalent buffers for isoelectric focusing in free solution

    NASA Technical Reports Server (NTRS)

    Mosher, Richard A.; Thormann, Wolfgang; Graham, Aly; Bier, Milan

    1985-01-01

    Two methods which utilize simple buffers for the generation of stable pH gradients (useful for preparative isoelectric focusing) are compared and contrasted. The first employs preformed gradients comprised of two simple buffers in density-stabilized free solution. The second method utilizes neutral membranes to isolate electrolyte reservoirs of constant composition from the separation column. It is shown by computer simulation that steady-state gradients can be formed at any pH range with any number of components in such a system.

  19. Plasma-induced grafting of acrylic acid on bentonite for the removal of U(VI) from aqueous solution

    NASA Astrophysics Data System (ADS)

    Hongshan, ZHU; Shengxia, DUAN; Lei, CHEN; Ahmed, ALSAEDI; Tasawar, HAYAT; Jiaxing, LI

    2017-11-01

    Fabrication of reusable adsorbents with satisfactory adsorption capacity and using environment-friendly preparation processes is required for the environment-related applications. In this study, acrylic acid (AA) was grafted onto bentonite (BT) to generate an AA-graft-BT (AA-g-BT) composite using a plasma-induced grafting technique considered to be an environment-friendly method. The as-prepared composite was characterized by scanning electron microscopy, x-ray powder diffraction, thermal gravity analysis, Fourier transform infrared spectroscopy and Barrett-Emmett-Teller analysis, demonstrating the successful grafting of AA onto BT. In addition, the removal of uranium(VI) (U(VI)) from contaminated aqueous solutions was examined using the as-prepared composite. The influencing factors, including contact time, pH value, ionic strength, temperature, and initial concentration, for the removal of U(VI) were investigated by batch experiments. The experimental process fitted best with the pseudo-second-order kinetic and the Langmuir models. Moreover, thermodynamic investigation revealed a spontaneous and endothermic process. Compared with previous adsorbents, AA-g-BT has potential practical applications in treating U(VI)-contaminated solutions.

  20. Process for preparing fine grain silicon carbide powder

    DOEpatents

    Wei, G.C.

    Method of producing fine-grain silicon carbide powder comprises combining methyltrimethoxysilane with a solution of phenolic resin, acetone and water or sugar and water, gelling the resulting mixture, and then drying and heating the obtained gel.

  1. Photoluminescence in Sm3+ doped Ba2P2O7 phosphor prepared by solution combustion method

    NASA Astrophysics Data System (ADS)

    Ghawade, Sonal P.; Deshmukh, Kavita A.; Dhoble, S. J.; Deshmukh, Abhay D.

    2018-05-01

    In this paper, Sm3+ doped Ba2P2O7 phosphors were synthesized via a Solution combustion method. The crystal structure of the phosphor was characterized by XRD. Orange-red emission was observed from these phosphors under near-ultraviolet (UV) excitation at 404 nm. The luminescence properties of the obtained phosphors were characterized by different techniques. The Ba2P2O7:Sm3+ phosphor can be efficiently excited by near-UV and blue light, and their emission spectrum consists of three emission peaks, at 564, 602, and 646 nm, respectively. Based on the results, the as prepared Ba2P2O7:Sm3+ phosphors are promising orange-red-emitting phosphors exhibit great potential may be applicable as a spectral convertor in c-Si solar cell to enhance the efficiency of solar cell in future.

  2. Characteristics of polyaniline cobalt supported catalysts for epoxidation reactions.

    PubMed

    Kowalski, Grzegorz; Pielichowski, Jan; Grzesik, Mirosław

    2014-01-01

    A study of polyaniline (PANI) doping with various cobalt compounds, that is, cobalt(II) chloride, cobalt(II) acetate, and cobalt(II) salen, is presented. The catalysts were prepared by depositing cobalt compounds onto the polymer surface. PANI powders containing cobalt ions were obtained by one- or two-step method suspending PANI in the following acetonitrile/acetic acid solution or acetonitrile and then acetic acid solution. Moreover different ratios of Co(II) : PANI were studied. Catalysts obtained with both methods and at all ratios were investigated using various techniques including AAS and XPS spectroscopy. The optimum conditions for preparation of PANI/Co catalysts were established. Catalytic activity of polyaniline cobalt(II) supported catalysts was tested in dec-1-ene epoxidation with molecular oxygen at room temperature. The relationship between the amount of cobalt species, measured with both AAS and XPS techniques, and the activity of PANI-Co catalysts has been established.

  3. Characteristics of Polyaniline Cobalt Supported Catalysts for Epoxidation Reactions

    PubMed Central

    Kowalski, Grzegorz; Pielichowski, Jan; Grzesik, Mirosław

    2014-01-01

    A study of polyaniline (PANI) doping with various cobalt compounds, that is, cobalt(II) chloride, cobalt(II) acetate, and cobalt(II) salen, is presented. The catalysts were prepared by depositing cobalt compounds onto the polymer surface. PANI powders containing cobalt ions were obtained by one- or two-step method suspending PANI in the following acetonitrile/acetic acid solution or acetonitrile and then acetic acid solution. Moreover different ratios of Co(II) : PANI were studied. Catalysts obtained with both methods and at all ratios were investigated using various techniques including AAS and XPS spectroscopy. The optimum conditions for preparation of PANI/Co catalysts were established. Catalytic activity of polyaniline cobalt(II) supported catalysts was tested in dec-1-ene epoxidation with molecular oxygen at room temperature. The relationship between the amount of cobalt species, measured with both AAS and XPS techniques, and the activity of PANI-Co catalysts has been established. PMID:24701183

  4. High quality thin films of thermoelectric misfit cobalt oxides prepared by a chemical solution method

    PubMed Central

    Rivas-Murias, Beatriz; Manuel Vila-Fungueiriño, José; Rivadulla, Francisco

    2015-01-01

    Misfit cobaltates ([Bi/Ba/Sr/Ca/CoO]nRS[CoO2]q) constitute the most promising family of thermoelectric oxides for high temperature energy harvesting. However, their complex structure and chemical composition makes extremely challenging their deposition by high-vacuum physical techniques. Therefore, many of them have not been prepared as thin films until now. Here we report the synthesis of high-quality epitaxial thin films of the most representative members of this family of compounds by a water-based chemical solution deposition method. The films show an exceptional crystalline quality, with an electrical conductivity and thermopower comparable to single crystals. These properties are linked to the epitaxial matching of the rock-salt layers of the structure to the substrate, producing clean interfaces free of amorphous phases. This is an important step forward for the integration of these materials with complementary n-type thermoelectric oxides in multilayer nanostructures. PMID:26153533

  5. Preparation of poly(N-vinylpyrrolidone)-stabilized ZnO colloid nanoparticles

    PubMed Central

    Gutul, Tatyana; Condur, Nadejda; Ursaki, Veaceslav; Goncearenco, Evgenii; Vlazan, Paulina

    2014-01-01

    Summary We propose a method for the synthesis of a colloidal ZnO solution with poly(N-vinylpyrrolidone) (PVP) as stabilizer. Stable colloidal solutions with good luminescence properties are obtained by using PVP as stabilizer in the synthesis of ZnO nanoparticles by a sol–gel method assisted by ultrasound. Nanoparticles with sizes of 30–40 nm in a PVP matrix are produced as a solid product. The colloidal ZnO/PVP/methanol solution, apart from the most intense PL band at 356 nm coming from the PVP, exhibits a strong PL band at 376 nm (3.30 eV) which corresponds to the emission of the free exciton recombination in ZnO nanoparticles. PMID:24778966

  6. ELECTROLYTIC PREPARATION OF UF$sub 4$

    DOEpatents

    Allen, A.L.; Anderson, R.W.; Powell, E.W.

    1958-11-01

    A method is presented for converting hexavalent aranium to uranium tetrafluoride. The method consists of electrolyzing a solution of uranyl fluoride in hydrofluoric acld at about 90 icient laborato C. The uranyl ions are reduced at the cathode and a hydrated uranium tetrafluoride precipitates. The precipitate is separated and subsequently dehydrated to UF/sub 4/.

  7. Determination of Bosentan in Pharmaceutical Preparations by Linear Sweep, Square Wave and Differential Pulse Voltammetry Methods

    PubMed Central

    Atila, Alptug; Yilmaz, Bilal

    2015-01-01

    In this study, simple, fast and reliable cyclic voltammetry (CV), linear sweep voltammetry (LSV), square wave voltammetry (SWV) and differential pulse voltammetry (DPV) methods were developed and validated for determination of bosentan in pharmaceutical preparations. The proposed methods were based on electrochemical oxidation of bosentan at platinum electrode in acetonitrile solution containing 0.1 M TBACIO4. The well-defined oxidation peak was observed at 1.21 V. The calibration curves were linear for bosentan at the concentration range of 5-40 µg/mL for LSV and 5-35 µg/mL for SWV and DPV methods, respectively. Intra- and inter-day precision values for bosentan were less than 4.92, and accuracy (relative error) was better than 6.29%. The mean recovery of bosentan was 100.7% for pharmaceutical preparations. No interference was found from two tablet excipients at the selected assay conditions. Developed methods in this study are accurate, precise and can be easily applied to Tracleer and Diamond tablets as pharmaceutical preparation. PMID:25901151

  8. Determination of bosentan in pharmaceutical preparations by linear sweep, square wave and differential pulse voltammetry methods.

    PubMed

    Atila, Alptug; Yilmaz, Bilal

    2015-01-01

    In this study, simple, fast and reliable cyclic voltammetry (CV), linear sweep voltammetry (LSV), square wave voltammetry (SWV) and differential pulse voltammetry (DPV) methods were developed and validated for determination of bosentan in pharmaceutical preparations. The proposed methods were based on electrochemical oxidation of bosentan at platinum electrode in acetonitrile solution containing 0.1 M TBACIO4. The well-defined oxidation peak was observed at 1.21 V. The calibration curves were linear for bosentan at the concentration range of 5-40 µg/mL for LSV and 5-35 µg/mL for SWV and DPV methods, respectively. Intra- and inter-day precision values for bosentan were less than 4.92, and accuracy (relative error) was better than 6.29%. The mean recovery of bosentan was 100.7% for pharmaceutical preparations. No interference was found from two tablet excipients at the selected assay conditions. Developed methods in this study are accurate, precise and can be easily applied to Tracleer and Diamond tablets as pharmaceutical preparation.

  9. Preparation of nitrogen-doped carbon tubes

    DOEpatents

    Chung, Hoon Taek; Zelenay, Piotr

    2015-12-22

    A method for synthesizing nitrogen-doped carbon tubes involves preparing a solution of cyanamide and a suitable transition metal-containing salt in a solvent, evaporating the solvent to form a solid, and pyrolyzing the solid under an inert atmosphere under conditions suitable for the production of nitrogen-doped carbon tubes from the solid. Pyrolyzing for a shorter period of time followed by rapid cooling resulted in a tubes with a narrower average diameter.

  10. WET METHOD OF PREPARING PLUTONIUM TRIBROMIDE

    DOEpatents

    Davidson, N.R.; Hyde, E.K.

    1958-11-11

    S> The preparation of anhydrous plutonium tribromide from an aqueous acid solution of plutonium tetrabromide is described, consisting of adding a water-soluble volatile bromide to the tetrabromide to provide additional bromide ions sufficient to furnish an oxidation-reduction potential substantially more positive than --0.966 volt, evaporating the resultant plutonium tribromides to dryness in the presence of HBr, and dehydrating at an elevated temperature also in the presence of HBr.

  11. One-pot ultrasonic-assisted method for preparation of Ag/AgCl sensitized ZnO nanostructures as visible-light-driven photocatalysts

    NASA Astrophysics Data System (ADS)

    Naghizadeh-Alamdari, Sara; Habibi-Yangjeh, Aziz; Pirhashemi, Mahsa

    2015-02-01

    Ultrasonic-assisted method was applied for preparation of Ag/AgCl sensitized ZnO nanostructures by one-pot procedure in water without using any post preparation treatments. The resultant nanocomposites were characterized by XRD, EDX, SEM, DRS, XPS, BET, and PL techniques. In the nanocomposites, ZnO and AgCl have wurtzite hexagonal and cubic crystalline phases, respectively and their surface morphologies remarkably change with increasing mole fraction of silver chloride. The EDX and XPS techniques show that the prepared samples are extremely pure. Ability of the nanocomposites for absorption of visible-light irradiation enhanced with increasing AgCl content. Photocatalytic examination of the nanocomposites was carried out using aqueous solution of methylene blue under visible-light irradiation. The degradation rate constant on the nancomposite rapidly increases with mole fraction of silver chloride up to 0.237. Enhancing activity of the nanocomposite was attributed to its ability for absorbing visible light and separation of electron-hole pairs. Furthermore, influence of ultrasonic irradiation time, calcination temperature, catalyst weight, pH of solution, and scavengers of reactive species on the degradation activity was investigated and the results were discussed. Finally, the photocatalyst has good activity after five successive cycles.

  12. Hydrogen production from water-glucose solution over NiO/La-NaTaO3 photocatalyst

    NASA Astrophysics Data System (ADS)

    Mardian, R.; Husin, H.; Pontas, K.; Zaki, M.; Asnawi, T. M.; Ahmadi

    2018-03-01

    This paper reports the evaluation of La-NaTaO3 photocatalyst performance in producing hydrogen from water-glucose solution. The main goal of the studies is to investigate the influence of glucose as a sacrificial reagent on the photocatalytic efficiency in water splitting reactions under ultraviolet (UV) irradiation. Photocatalyst has been fabricated via sol-gel method and being confirmed using x-ray diffraction (XRD) and scanning electron microscopy (SEM). Nickel loaded La-NaTaO3 photocatalyst are prepared by impregnation method. It was observed that the prepared photocatalysts displayed particle sizes in the 30-250 nm range with orthorhombic structure. Their photocatalytic activity for hydrogen production via water splitting was conducted in a Pyrex glass reactor under UV light irradiation. The aqueous solution contained glucose employed as a renewable organic scavenger. A significant improvement in hydrogen production was observed in glucose-water mixtures and NiO loaded photocatalyst. The prepared La-NaTaO3 showed that the highest activity for hydrogen generation of 35.1 mmol h-1.g-1 was obtained at 0.10 mol.L-1 glucose and 0.3 wt.% NiO. This suggests the important role played by the glucose as electron donor and loading nickel on La-NaTaO3 as a cocatalyst increasing electron storage and suppressing electron-hole recombination.

  13. Effect of mixing techniques on bacterial attachment and disinfection time of polyether impression material

    PubMed Central

    Guler, Umut; Budak, Yasemin; Ruh, Emrah; Ocal, Yesim; Canay, Senay; Akyon, Yakut

    2013-01-01

    Objective: The aim of this study was 2-fold. The first aim was to evaluate the effects of mixing technique (hand-mixing or auto-mixing) on bacterial attachment to polyether impression materials. The second aim was to determine whether bacterial attachment to these materials was affected by length of exposure to disinfection solutions. Materials and Methods: Polyether impression material samples (n = 144) were prepared by hand-mixing or auto-mixing. Escherichia coli, Staphylococcus aureus and Pseudomonas aeruginosa were used in testing. After incubation, the bacterial colonies were counted and then disinfectant solution was applied. The effect of disinfection solution was evaluated just after the polymerization of impression material and 30 min after polymerization. Differences in adherence of bacteria to the samples prepared by hand-mixing and to those prepared by auto-mixing were assessed by Kruskal-Wallis and Mann-Whitney U-tests. For evaluating the efficiency of the disinfectant, Kruskal-Wallis multiple comparisons test was used. Results: E. coli counts were higher in hand-mixed materials (P < 0.05); no other statistically significant differences were found between hand- and auto-mixed materials. According to the Kruskal-Wallis test, significant differences were found between the disinfection procedures (Z > 2.394). Conclusion: The methods used for mixing polyether impression material did not affect bacterial attachment to impression surfaces. In contrast, the disinfection procedure greatly affects decontamination of the impression surface. PMID:24966729

  14. Preparation of anatase TiO2 thin film by low temperature annealing as an electron transport layer in inverted polymer solar cells

    NASA Astrophysics Data System (ADS)

    Noh, Hongche; Oh, Seong-Geun; Im, Seung Soon

    2015-04-01

    To prepare the anatase TiO2 thin films on ITO glass, amorphous TiO2 colloidal solution was synthesized through the simple sol-gel method by using titanium (IV) isopropoxide as a precursor. This amorphous TiO2 colloidal solution was spread on ITO glass by spin-coating, then treated at 450 °C to obtain anatase TiO2 film (for device A). For other TiO2 films, amorphous TiO2 colloidal solution was treated through solvothermal process at 180 °C to obtain anatase TiO2 colloidal solution. This anatase TiO2 colloidal solution was spread on ITO glass by spin coating, and then annealed at 200 °C (for device B) and 130 °C (for device C), respectively. The average particle size of amorphous TiO2 colloidal solution was about 1.0 nm and that of anatase TiO2 colloidal solution was 10 nm. The thickness of TiO2 films was about 15 nm for all cases. When inverted polymer solar cells were fabricated by using these TiO2 films as an electron transport layer, the device C showed the highest PCE (2.6%) due to the lack of defect, uniformness and high light absorbance of TiO2 films. The result of this study can be applied for the preparation of inverted polymer solar cell using TiO2 films as a buffer layer at low temperature on plastic substrate by roll-to roll process.

  15. Enhanced oral bioavailability of silymarin using liposomes containing a bile salt: preparation by supercritical fluid technology and evaluation in vitro and in vivo

    PubMed Central

    Yang, Gang; Zhao, Yaping; Zhang, Yongtai; Dang, Beilei; Liu, Ying; Feng, Nianping

    2015-01-01

    The aim of this investigation was to develop a procedure to improve the dissolution and bioavailability of silymarin (SM) by using bile salt-containing liposomes that were prepared by supercritical fluid technology (ie, solution-enhanced dispersion by supercritical fluids [SEDS]). The process for the preparation of SM-loaded liposomes containing a bile salt (SM-Lip-SEDS) was optimized using a central composite design of response surface methodology with the ratio of SM to phospholipids (w/w), flow rate of solution (mL/min), and pressure (MPa) as independent variables. Particle size, entrapment efficiency (EE), and drug loading (DL) were dependent variables for optimization of the process and formulation variables. The particle size, zeta potential, EE, and DL of the optimized SM-Lip-SEDS were 160.5 nm, −62.3 mV, 91.4%, and 4.73%, respectively. Two other methods to produce SM liposomes were compared to the SEDS method. The liposomes obtained by the SEDS method exhibited the highest EE and DL, smallest particle size, and best stability compared to liposomes produced by the thin-film dispersion and reversed-phase evaporation methods. Compared to the SM powder, SM-Lip-SEDS showed increased in vitro drug release. The in vivo AUC0−t of SM-Lip-SEDS was 4.8-fold higher than that of the SM powder. These results illustrate that liposomes containing a bile salt can be used to enhance the oral bioavailability of SM and that supercritical fluid technology is suitable for the preparation of liposomes. PMID:26543366

  16. Solid-gel precursor solutions and methods for the fabrication of polymetallicsiloxane coating films

    DOEpatents

    Sugama, Toshifumi

    1992-01-01

    Solutions and preparation methods necessary for the fabrication of metal oxide cross-linked polysiloxane coating films are disclosed. The films are useful in provide heat resistance against oxidation, wear resistance, thermal insulation, and corrosion resistance of substrates. The sol-gel precursor solution comprises a mixture of a monomeric organoalkoxysilane, a metal alkoxide M(OR).sub.n (wherein M is Ti, Zr, Ge or Al; R is CH.sub.3, C.sub.2 H.sub.5 or C.sub.3 H.sub.7 ; and n is 3 or 4), methanol, water, HCl and NaOH. The invention provides a sol-gel solution, and a method of use thereof, which can be applied and processed at low temperatures (i.e., <1000.degree. C.). The substrate can be coated by immersing it in the above mentioned solution at ambient temperature. The substrate is then withdrawn from the solution. Next, the coated substrate is heated for a time sufficient and at a temperature sufficient to yield a solid coating. The coated substrate is then heated for a time sufficient, and temperature sufficient to produce a polymetallicsiloxane coating.

  17. Solid-gel precursor solutions and methods for the fabrication of polymetallicsiloxane coating films

    DOEpatents

    Sugama, Toshifumi

    1993-01-01

    Solutions and preparation methods necessary for the fabrication of metal oxide cross-linked polysiloxane coating films are disclosed. The films are useful in provide heat resistance against oxidation, wear resistance, thermal insulation, and corrosion resistance of substrates. The sol-gel precursor solution comprises a mixture of a monomeric organoalkoxysilane, a metal alkoxide M(OR).sub.n (wherein M is Ti, Zr, Ge or Al; R is CH.sub.3, C.sub.2 H.sub.5 or C.sub.3 H.sub.7 ; and n is 3 or 4), methanol, water, HCl and NaOH. The invention provides a sol-gel solution, and a method of use thereof, which can be applied and processed at low temperatures (i.e., <1000.degree. C.). The substrate can be coated by immersing it in the above mentioned solution at ambient temperature. The substrate is then withdrawn from the solution. Next, the coated substrate is heated for a time sufficient and at a temperature sufficient to yield a solid coating. The coated substrate is then heated for a time sufficient, and temperature sufficient to produce a polymetallicsiloxane coating.

  18. Solid-gel precursor solutions and methods for the fabrication of polymetallicsiloxane coating films

    DOEpatents

    Toshifumi Sugama.

    1993-04-06

    Solutions and preparation methods necessary for the fabrication of metal oxide cross-linked polysiloxane coating films are disclosed. The films are useful in provide heat resistance against oxidation, wear resistance, thermal insulation, and corrosion resistance of substrates. The sol-gel precursor solution comprises a mixture of a monomeric organoalkoxysilane, a metal alkoxide M(OR)[sub n] (wherein M is Ti, Zr, Ge or Al; R is CH[sub 3], C[sub 2]H[sub 5] or C[sub 3]H[sub 7]; and n is 3 or 4), methanol, water, HCl and NaOH. The invention provides a sol-gel solution, and a method of use thereof, which can be applied and processed at low temperatures (i.e., < 1,000 C.). The substrate can be coated by immersing it in the above mentioned solution at ambient temperature. The substrate is then withdrawn from the solution. Next, the coated substrate is heated for a time sufficient and at a temperature sufficient to yield a solid coating. The coated substrate is then heated for a time sufficient, and temperature sufficient to produce a polymetallicsiloxane coating.

  19. A sample preparation method for recovering suppressed analyte ions in MALDI TOF MS.

    PubMed

    Lou, Xianwen; de Waal, Bas F M; Milroy, Lech-Gustav; van Dongen, Joost L J

    2015-05-01

    In matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI TOF MS), analyte signals can be substantially suppressed by other compounds in the sample. In this technical note, we describe a modified thin-layer sample preparation method that significantly reduces the analyte suppression effect (ASE). In our method, analytes are deposited on top of the surface of matrix preloaded on the MALDI plate. To prevent embedding of analyte into the matrix crystals, the sample solution were prepared without matrix and efforts were taken not to re-dissolve the preloaded matrix. The results with model mixtures of peptides, synthetic polymers and lipids show that detection of analyte ions, which were completely suppressed using the conventional dried-droplet method, could be effectively recovered by using our method. Our findings suggest that the incorporation of analytes in the matrix crystals has an important contributory effect on ASE. By reducing ASE, our method should be useful for the direct MALDI MS analysis of multicomponent mixtures. Copyright © 2015 John Wiley & Sons, Ltd.

  20. Carbohydrate crops as a renewable resource for fuels production. Volume III. Juice preservation

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

    Fink, D.J.; Allen, B.R.; Litchfield, J.H.

    1980-01-29

    The objective of this study was to evaluate a process to preserve sugar crop juices. The process is energy conserving in that concentrated sugar solutions are produced with little evaporation of water. A preliminary investigation was conducted of polysaccharide hydrolysis as a means for preserving mixed sugar solutions obtained from crops such as sweet sorghum. Four subtasks have been addressed during this report period: I. Concentration of Pure Sugar Solutions by Hydrolysis of Purified Starch; II. Concentration of Genuine Sugar Crop Juice by Hydrolysis of Purified Starch; III. Concentration of Pure Sugar Solutions by Hydrolysis of Genuine Biomass Starch; andmore » IV. Concentration of Pure Sugar Solutions by Hydrolysis of Cellulosic Materials. The results obtained from the experiments conducted in Subtasks I and II included the following: (1) Concentrated sucrose-glucose-fructose solutions (greater than 50 percent) can be prepared from simulated or actual sweet sorghum juice using enzymatic thinning and saccharification of pure starch-sugar solution mixtures. (2) Enzymatic saccharification of corn meal and cracked wheat in simulated sorghum juice was also demonstrated. (3) Concentration of sugar solutions also can be accomplished by saccharification of cellulosic materials. In our experiments, inhibition of the cellobiase component of the cellulase preparation was observed. The hydrolysis studies were directed to the demonstration of the feasibility of one approach to the preparation of concentrated, microbiologically stable sugar syrups starting with sweet sorghum juice. Future work on Subtask V of this program will continue the investigations already underway and will consider other approaches to the stabilization of juices. Subtask VI of this program will consider the process economics of the Subtask I to IV approaches, or combinations of two or more methods, that are considered to be most feasible for juice preservation.« less

  1. Fabrication of a Microbial Biosensor Based on QD-MWNT Supports by a One-Step Radiation Reaction and Detection of Phenolic Compounds in Red Wines

    PubMed Central

    Kim, Seul-Ki; Kwen, Hai-Doo; Choi, Seong-Ho

    2011-01-01

    An Acaligense sp.-immobilized biosensor was fabricated based on QD-MWNT composites as an electron transfer mediator and a microbe immobilization support by a one-step radiation reaction and used for sensing phenolic compounds in commercial red wines. First, a quantum dot-modified multi-wall carbon nanotube (QD-MWNT) composite was prepared in the presence of MWNT by a one-step radiation reaction in an aqueous solution at room temperature. The successful preparation of the QD-MWNT composite was confirmed by XPS, TEM, and elemental analysis. Second, the microbial biosensor was fabricated by immobilization of Acaligense sp. on the surface of the composite thin film of a glassy carbon (GC) electrode, which was prepared by a hand casting method with a mixture of the previously obtained composite and Nafion solution. The sensing ranges of the microbial biosensor based on CdS-MWNT and Cu2S-MWNT supports were 0.5–5.0 mM and 0.7–10 mM for phenol in a phosphate buffer solution, respectively. Total concentration of phenolic compounds contained in commercial red wines was also determined using the prepared microbial immobilized biosensor. PMID:22319395

  2. Patterned forests of vertically-aligned multiwalled carbon nanotubes using metal salt catalyst solutions.

    PubMed

    Garrett, David J; Flavel, Benjamin S; Baronian, Keith H R; Downard, Alison J

    2013-01-01

    A simple method for producing patterned forests of multiwalled carbon nanotubes (MWCNTs) is described. An aqueous metal salt solution is spin-coated onto a substrate patterned with photoresist by standard methods. The photoresist is removed by acetone washing leaving the acetone-insoluble catalyst pattern on the substrate. Dense forests of vertically aligned (VA) MWCNTs are grown on the patterned catalyst layers by chemical vapour deposition. The procedures have been demonstrated by growing MWCNT forests on two substrates: silicon and conducting graphitic carbon films. The forests adhere strongly to the substrates and when grown directly on carbon film, offer a simple method of preparing MWCNT electrodes.

  3. Visible Light Responsive Liquid Crystal Polymers Containing Reactive Moieties with Good Processability.

    PubMed

    Liu, Yuyun; Wu, Wei; Wei, Jia; Yu, Yanlei

    2017-01-11

    Two types of novel reactive linear liquid crystal polymers (LLCPs) with different azotolene concentrations have been synthesized and processed into films and fibers by solution and melting processing methods. Then, the LLCPs in the obtained monodomain fiber and polydomain film were easily cross-linked with difunctional primary amines. The resulted cross-linked liquid crystal polymers (CLCPs) underwent reversible photoinduced bending and unbending behaviors in response to 445 and 530 nm visible light at room temperature, respectively. The post-cross-linking method provides a facile way to prepare the CLCP films and fibers with different shapes from LLCPs, which can be processed by traditional melting and solution methods.

  4. Photoprecursor approach as an effective means for preparing multilayer organic semiconducting thin films by solution processes

    PubMed Central

    Yamaguchi, Yuji; Suzuki, Mitsuharu; Motoyama, Takao; Sugii, Shuhei; Katagiri, Chiho; Takahira, Katsuya; Ikeda, Shinya; Yamada, Hiroko; Nakayama, Ken-ichi

    2014-01-01

    The vertical composition profile of active layer has a major effect on the performance of organic photovoltaic devices (OPVs). While stepwise deposition of different materials is a conceptually straightforward method for controlled preparation of multi-component active layers, it is practically challenging for solution processes because of dissolution of the lower layer. Herein, we overcome this difficulty by employing the photoprecursor approach, in which a soluble photoprecursor is solution-deposited then photoconverted in situ to a poorly soluble organic semiconductor. This approach enables solution-processing of the p-i-n triple-layer architecture that has been suggested to be effective in obtaining efficient OPVs. We show that, when 2,6-dithienylanthracene and a fullerene derivative PC71BM are used as donor and acceptor, respectively, the best p-i-n OPV affords a higher photovoltaic efficiency than the corresponding p-n device by 24% and bulk-heterojunction device by 67%. The photoprecursor approach is also applied to preparation of three-component p-i-n films containing another donor 2,6-bis(5′-(2-ethylhexyl)-(2,2′-bithiophen)-5-yl)anthracene in the i-layer to provide a nearly doubled efficiency as compared to the original two-component p-i-n system. These results indicate that the present approach can serve as an effective means for controlled preparation of well-performing multi-component active layers in OPVs and related organic electronic devices. PMID:25413952

  5. Self-assembled phytosterol-fructose-chitosan nanoparticles as a carrier of anticancer drug.

    PubMed

    Qiu, Yeyan; Zhu, Jun; Wang, Jianting; Gong, Renmin; Zheng, Mingming; Huang, Fenghong

    2013-08-01

    Self-assembled nanoparticles were synthesized from water-soluble fructose-chitosan, substituted by succinyl linkages with phytosterols as hydrophobic moieties for self-assembly. The physicochemical properties of the prepared self-assembled nanoparticles were characterized by Fourier transform infrared spectroscopy, fluorescence spectroscopy, and transmission electron microscopy. Doxorubicin (DOX), as a model anticancer drug, was physically entrapped inside prepared self-assembled nanoparticles by the dialysis method. With increasing initial levels of the drug, the drug loading content increased, but the encapsulation efficiency decreased. The release profiles in vitro demonstrated that the DOX showed slow sustained released over 48 h, and the release rate in phosphate buffered saline (PBS) solution (pH 7.4) was much slower than in PBS solution (pH 5.5 and pH 6.5), indicating the prepared self-assembled nanoparticles had the potential to be used as a carrier for targeted delivery of hydrophobic anticancer drugs with declined cytotoxicity to normal tissues.

  6. Substitution effects on the ferroelectric properties of BiFeO3 thin films prepared by chemical solution deposition

    NASA Astrophysics Data System (ADS)

    Kim, Jong Kuk; Kim, Sang Su; Kim, Won-Jeong; Bhalla, Amar S.

    2007-01-01

    Ferroelectric properties of Cr-substituted BiFeO3 (BFCr) and Pb-cosubstituted BFCr films prepared by a chemical solution deposition method and annealed at 550°C in nitrogen have been studied. X-ray diffraction measurements revealed that the thin films were composed of a rhombohedrally distorted perovskite structure without secondary phases. The 5mol% Pb-cosubstituted BFCr films appeared to have superior ferroelectric properties to those of other BFCr films prepared by the same conditions. The remanent polarization (Pr) and the coercive field (Ec) of the 5mol% Pb-cosubstituted BFCr film were 62μC /cm2 and 235kV/cm, respectively, with a maximum applied field of 712kV/cm. In addition, the film exhibited a fatigue-free behavior up to 1.45×1010 read/write cycles.

  7. Preparation of iron oxide-impregnated spherical granular activated carbon-carbon composite and its photocatalytic removal of methylene blue in the presence of oxalic acid.

    PubMed

    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.

  8. Crystallization from high temperature solutions of Si in Cu/Al solvent

    DOEpatents

    Ciszek, Theodore F.; Wang, Tihu

    1996-01-01

    A liquid phase epitaxy method for forming thin crystalline layers of device quality silicon having less than 3.times.10.sup.16 Cu atoms/cc impurity, comprising: preparing a saturated liquid solution of Si in a Cu/Al solvent at about 20 to about 40 at. % Si at a temperature range of about 850.degree. to about 1100.degree. C. in an inert gas; immersing or partially immersing a substrate in the saturated liquid solution; super saturating the solution by lowering the temperature of the saturated solution; holding the substrate in the saturated solution for a period of time sufficient to cause Si to precipitate out of solution and form a crystalline layer of Si on the substrate; and withdrawing the substrate from the solution.

  9. Crystallization from high temperature solutions of Si in Cu/Al solvent

    DOEpatents

    Ciszek, T.F.; Wang, T.

    1996-08-13

    A liquid phase epitaxy method is disclosed for forming thin crystalline layers of device quality silicon having less than 3{times}10{sup 16} Cu atoms/cc impurity, comprising: preparing a saturated liquid solution of Si in a Cu/Al solvent at about 20 to about 40 at. % Si at a temperature range of about 850 to about 1100 C in an inert gas; immersing or partially immersing a substrate in the saturated liquid solution; super saturating the solution by lowering the temperature of the saturated solution; holding the substrate in the saturated solution for a period of time sufficient to cause Si to precipitate out of solution and form a crystalline layer of Si on the substrate; and withdrawing the substrate from the solution. 3 figs.

  10. Uniform manganese hexacyanoferrate hydrate nanocubes featuring superior performance for low-cost supercapacitors and nonenzymatic electrochemical sensors

    NASA Astrophysics Data System (ADS)

    Pang, Huan; Zhang, Yizhou; Cheng, Tao; Lai, Wen-Yong; Huang, Wei

    2015-09-01

    Uniform manganese hexacyanoferrate hydrate nanocubes are prepared via a simple chemical precipitation method at room temperature. Due to both micro/mesopores of the Prussian blue analogue and nanocubic structures, the manganese hexacyanoferrate hydrate nanocubes allow the efficient charge transfer and mass transport for electrolyte solution and chemical species. Thus, the manganese hexacyanoferrate hydrate nanocube electrode shows a good rate capability and cycling stability for electrochemical capacitors. Furthermore, electrodes modified with manganese hexacyanoferrate hydrate nanocubes demonstrate a sensitive electrochemical response to hydrogen peroxide (H2O2) in buffer solutions with a high selectivity.Uniform manganese hexacyanoferrate hydrate nanocubes are prepared via a simple chemical precipitation method at room temperature. Due to both micro/mesopores of the Prussian blue analogue and nanocubic structures, the manganese hexacyanoferrate hydrate nanocubes allow the efficient charge transfer and mass transport for electrolyte solution and chemical species. Thus, the manganese hexacyanoferrate hydrate nanocube electrode shows a good rate capability and cycling stability for electrochemical capacitors. Furthermore, electrodes modified with manganese hexacyanoferrate hydrate nanocubes demonstrate a sensitive electrochemical response to hydrogen peroxide (H2O2) in buffer solutions with a high selectivity. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr04322k

  11. Ferrofluid of magnetic clay and menthol based deep eutectic solvent: Application in directly suspended droplet microextraction for enrichment of some emerging contaminant explosives in water and soil samples.

    PubMed

    Zarei, Ali Reza; Nedaei, Maryam; Ghorbanian, Sohrab Ali

    2018-06-08

    In this work, for the first time, ferrofluid of magnetic montmorillonite nanoclay and deep eutectic solvent was prepared and coupled with directly suspended droplet microextraction. Incorporation of ferrofluid in a miniaturized sample preparation technique resulted in achieving high extraction efficiency while developing a green analytical method. The prepared ferrofluid has strong sorbing properties and hydrophobic characteristics. In this method, a micro-droplet of ferrofluid was suspended into the vortex of a stirring aqueous solution and after completing the extraction process, was easily separated from the solution by a magnetic rod without any operational problems. The predominant experimental variables affecting the extraction efficiency of explosives were evaluated. Under optimal conditions, the limits of detection were in the range 0.22-0.91 μg L -1 . The enrichment factors were between 23 and 93 and the relative standard deviations were <10%. The relative recoveries were ranged from 88 to 104%. This method was successfully applied for the extraction and preconcentration of explosives in water and soil samples, followed their determination by high performance liquid chromatography with ultraviolet detection (HPLC-UV). Copyright © 2018 Elsevier B.V. All rights reserved.

  12. TRIZ theory in NEA photocathode preparation system

    NASA Astrophysics Data System (ADS)

    Qiao, Jianliang; Huang, Dayong; Li, Xiangjiang; Gao, Youtang

    2016-09-01

    The solutions to the engineering problems were provided according to the innovation principle based on the theory of TRIZ. The ultra high vacuum test and evaluation system for the preparation of negative electron affinity (NEA) photocathode has the characteristics of complex structure and powerful functions. Segmentation principle, advance function principle, curved surface principle, dynamic characteristics principle and nested principle adopted by the design of ultra high vacuum test and evaluation system for cathode preparation were analyzed. The applications of the physical contradiction and the substance-field analysis method of the theory of TRIZ in the cathode preparation ultra high vacuum test and evaluation system were discussed.

  13. Shape control VO2 nanorods prepared by soft chemistry and electrochemical method

    NASA Astrophysics Data System (ADS)

    Simo, A.; Sibanyoni, J.; Fuku, X.; Numan, N.; Omorogbe, S.; Maaza, M.

    2018-07-01

    "Bottom up" approach is of primary interest for chemistry and materials science because the fundamental building blocks are atoms. Thus colloidal chemical synthetic methods can be utilized to prepare uniform nanocrystals with controlled particle size. In the following work of study, thermochromic VO2 nanostructures were prepared by hydrothermal technique soft chemistry. We concentrate on solution phase synthetic methods that enable a proper shape and size control of metal oxide nanocrystals. Their structural properties were studied by Scanning Electron Microscopy (SEM), Fourier Transform IR (FTIR) and Differential Scanning Calorimetry (DSC). It is demonstrated that the surfactant assistance (NaOH) has great influence on the morphology-control of the material. Electrochemical properties of the nanospheres show good stability after 20 cycles and the surface diffusion coefficient was calculated to be 5 × 10-6 cm2 s-1.

  14. Recent advances in f-element separations based on a new method for the production of pentavalent americium in acidic solution

    DOE PAGES

    Mincher, Bruce J.; Schmitt, Nicholas C.; Schuetz, Brian K.; ...

    2015-03-11

    The peroxydisulfate anion has long been used for the preparation of hexavalent americium (Am VI) from the normally stable Am III valence state in mildly acidic solutions. However, there has been no satisfactory means to directly prepare the pentavalent state (Am V) in that medium. Some early literature reports indicated that the peroxydisulfate oxidation was incomplete, and silver ion catalysis in conjunction with peroxydisulfate became accepted as the means to ensure quantitative generation of Am VI. Incomplete oxidation would be expected to leave residual Am III, or to produce Am V in treated solutions. However, until recently, the use ofmore » peroxydisulfate as an Am V reagent has not been reported. Here, parameters influencing the oxidation were investigated, including peroxydisulfate and acid concentration, temperature, duration of oxidative treatment, and the presence of higher concentrations of other redox active metals such as plutonium. Using optimized conditions determined here, quantitative Am V was prepared in an acidic solution and the UV/Vis extinction coefficients of the Am V 513 nm peak were measured over a range of nitric acid concentrations. Furthermore, the utility of Am V for separations from the lanthanides and curium by solvent extraction, organic column chromatography and inorganic ion exchangers was also investigated.« less

  15. Preparation of Si and O co-solution strengthened Ti alloys by using rice husks as SiO2 resource and quantitative descriptions on their strengthening effects

    NASA Astrophysics Data System (ADS)

    Jia, Lei; Chen, Jiang-xian; Lu, Zhen-lin; Li, Shu-feng; Umeda, Junko; Kondoh, Katsuyoshi

    2018-04-01

    Ti alloys strengthened by both Si and O solutes were prepared by powder metallurgy method from pure Ti and amorphous SiO2 powder obtained by combusting rice husks. At the same time, Ti alloys singly strengthened by Si or O were also prepared for studying the strengthening effect of Si and O solutes. Results showed that amorphous SiO2 powder originated from rice husks could almost fully dissolve into pure Ti matrix when the content was not higher than 1.0 wt%, while higher content of SiO2 addition resulted in the formation of Ti5Si3 intermetallics. Si and O elements leaded to negative and positive distortion of Ti lattice, and the influencing degrees were ‑0.02 and +0.014 Å/wt% for lattice constant a, while ‑0.05 and +0.046 Å/wt% for constant c, respectively. Solid solution of Si and O would also result in the increase of hardness, which was 98.5 and 209.43 HV/wt%, respectively. When Si and O were co-exsited in Ti matrix, the negative and positive distortion cancelled each other, while the strengthening effect did not cancel but enhance each other.

  16. THE PREPARATION AND PROPERTIES OF HIGHLY PURIFIED ASCORBIC ACID OXIDASE

    PubMed Central

    Powers, Wendell H.; Lewis, Stanley; Dawson, Charles R.

    1944-01-01

    1. A method is described for the preparation of a highly purified ascorbic acid oxidase containing 0.24 per cent copper. 2. Using comparable activity measurements, this oxidase is about one and a half times as active on a dry weight basis as the hitherto most highly purified preparation described by Lovett-Janison and Nelson. The latter contained 0.15 per cent copper. 3. The oxidase activity is proportional to the copper content and the proportionality factor is the same as that reported by Lovett-Janison and Nelson. 4. When dialyzed free of salt, the blue concentrated oxidase solutions precipitate a dark green-blue protein which carries the activity. This may be prevented by keeping the concentrated solutions about 0.1 M in Na2HPO4. 5. When highly diluted for activity measurements the oxidase rapidly loses activity (irreversibly) previous to the measurement, unless the dilution is made with a dilute inert protein (gelatin) solution. Therefore activity values obtained using such gelatin-stabilized dilute solutions of the oxidase run considerably higher than values obtained by the Lovett-Janison and Nelson technique. 6. The effect of pH and substrate concentration on the activity of the purified oxidase in the presence and absence of inert protein was studied. PMID:19873382

  17. Preparation of crotaline F-ab antivenom (CroFab) with automated mixing methods: in vitro observations.

    PubMed

    Vohra, Rais; Kelner, Michael; Clark, Richard F

    2009-01-01

    Crotaline Polyvalent Ovine Fab antivenom (CroFab, Savage Laboratories and Protherics Inc., Brentwood, TN, USA) preparation requires that the lyophilized powder be manually reconstituted before use. We compared automated methods for driving the product into solution with the standard manual method of reconstitution, and the effect of repeated rinsing of the product vial, on the per-vial availability of antivenom. Normal saline (NS, 10 mL) was added to 12 vials of expired CroFab. Vials were assigned in pairs to each of six mixing methods, including one pair mixed manually as recommended by the product package insert. Each vial's contents were diluted to a final volume of 75 mL of normal saline. Protein concentration was measured with a colorimetric assay. The fluid left in each vial was removed and the vial was washed with 10 mL NS. Total protein yield from each step was calculated. There was no significant change in protein yield among three of five automated mixing methods when compared to manual reconstitution. Repeat rinsing of the product vial with an additional 10 mLs of fluid added to the protein yield regardless of the mixing method used. We found slightly higher protein yields with all automated methods compared to manual mixing, but only two of five comparisons with the standard mixing method demonstrated statistical significance. However, for all methods tested, the addition of a second rinsing and recovery step increased the amount of protein recovered considerably, presumably by allowing solution of protein trapped in the foamy residues. Automated mixing methods and repeat rinsing of the product vial may allow higher protein yields in the preparation of CroFab antivenom.

  18. The Underpotential Deposition of Copper on Pt(311): Site Selective Deposition and Anion Effects

    DTIC Science & Technology

    1994-03-14

    water (18 MOhms Millipore Milli-Q water). Aqueous acid solutions were prepared from high-purity (ULTREX) sulfuric acid . Copper ion solutions were...prepared by dissolution of CuSO 4 .5H 2 0 (Aldrich Gold Label 5N5) in sulfuric acid solutions. Chloride and bromide containing solutions were prepared by...Voltammetric characteristics of a Pt(311) electrode in acidic solutions containing chloride and bromide. Fig. 1 shows cyclic voltammograxns for the

  19. Comparison of ozone-specific (OZAC) and oxygen radical (ORAC) antioxidant capacity assays for use with nasal lavage fluid.

    PubMed

    Rutkowski, Joseph M; Santiag, Lizzie Y; Ben-Jebria, Abdellaziz; Ultman, James S

    2011-10-01

    Antioxidants in respiratory mucus protect the underlying airway epithelium from damage by ozone (O(3)), a common outdoor air pollutant. To understand O(3)-antioxidant interactions and the variation of these interactions among individuals, in vitro assays are needed to measure the total antioxidant capacity of airway lavage fluid, a convenient source of (diluted) mucous samples. Here, we compare the oxygen radical absorbance capacity (ORAC), a general method that uses peroxyl radicals as a reactive substance, to the recently developed ozone specific antioxidant capacity (OZAC), a procedure that directly employs O(3). For prepared model mucous antioxidant solutions containing uric acid, ascorbic acid or glutathione, the ORAC and OZAC methods yielded comparable antioxidant capacities. The addition of EDTA or DETAPAC, necessary to prevent auto-oxidation of test solutions during the ORAC assay, unpredictably altered ORAC measurements. EDTA did not have a significant effect on OZAC measurements in either prepared uric acid or ascorbic acid solutions. When assessing antioxidant capacities of nasal lavage samples, the ORAC and OZAC assays were no longer comparable. Because the OZAC of nasal lavage samples was positively related to measured uric acid concentrations whereas the ORAC data were not, the OZAC method appears to provide more realistic mucous antioxidant capacities than the ORAC method. Copyright © 2011 Elsevier Ltd. All rights reserved.

  20. Scalable hydrothermal synthesis of free-standing VO₂ nanowires in the M1 phase.

    PubMed

    Horrocks, Gregory A; Singh, Sujay; Likely, Maliek F; Sambandamurthy, G; Banerjee, Sarbajit

    2014-09-24

    VO2 nanostructures derived from solution-phase methods are often plagued by broadened and relatively diminished metal-insulator transitions and adventitious doping due to imperfect control of stoichiometry. Here, we demonstrate a stepwise scalable hydrothermal and annealing route for obtaining VO2 nanowires exhibiting almost 4 orders of magnitude abrupt (within 1 °C) metal-insulator transitions. The prepared nanowires have been characterized across their structural and electronic phase transitions using single-nanowire Raman microprobe analysis, ensemble differential scanning calorimetry, and single-nanowire electrical transport measurements. The electrical band gap is determined to be 600 meV and is consistent with the optical band gap of VO2, and the narrowness of differential scanning calorimetry profiles indicates homogeneity of stoichiometry. The preparation of high-quality free-standing nanowires exhibiting pronounced metal-insulator transitions by a solution-phase process allows for scalability, further solution-phase processing, incorporation within nanocomposites, and integration onto arbitrary substrates.

  1. Properties of alginate fiber spun-dyed with fluorescent pigment dispersion.

    PubMed

    Wang, Ping; Tawiah, Benjamin; Tian, Anli; Wang, Chunxia; Zhang, Liping; Fu, Shaohai

    2015-03-15

    Spun-dyed alginate fiber was prepared by the spun-dyeing method with the mixture of fluorescent pigment dispersion and sodium alginate fiber spinning solution, and its properties were characterized by SEM, TGA, DSC, and XRD. The results indicate that fluorescent pigment dispersion prepared with esterified poly (styrene-alt maleic acid) had excellent compatibility with sodium alginate fiber spinning solution, and small amount of fluorescent pigment could reduce the viscosity of spun-dyed spinning solutions. SEM photo of spun-dyed alginate fiber indicated that fewer pigment particles deposited on its surface. TGA, DSC, and XRD results suggested that thermal properties and crystal phase of spun-dyed alginate fibers had slight changes compared to the original alginate fibers. The fluorescence intensity of spun-dyed alginate fiber reached its maximum when the content of fluorescent pigment was 4%. The spun-dyed alginate fiber showed excellent rubbing and washing fastness. Copyright © 2014 Elsevier Ltd. All rights reserved.

  2. Physical characteristics of commercial and home-made nasal lavage solutions.

    PubMed

    Lilic, N; Waldvogel-Thurlow, S; Douglas, R G

    2014-01-01

    Nasal saline lavage forms a cornerstone of chronic rhinosinusitis management. A number of saline lavage recipes and products are currently available but little is known of their relative physical characteristics. To determine the osmolarity and pH of nasal lavage solutions, both commercial preparations and home-made recipes, and to determine the reproducibility of saline solution preparation. Five home-made recipes and two commercial products were prepared in triplicate and analysed. Eight consecutive clinic patients prepared a commercial product and 11 prepared a home-made recipe, and the osmolarity and pH were measured. The osmolarity of the solutions varied widely, from 140 to 788 mmol/l and the pH varied from 7.88 to 8.50. The commercial and home-made solutions had similar reproducibility when prepared by patients. Some recipes were markedly hypo-osmolar and some were hyper-osmolar. All were slightly alkaline. The home-made recipes had similar physical characteristics and reproducibility to commercial preparations.

  3. Method for the preparation of high surface area high permeability carbons

    DOEpatents

    Lagasse, Robert R.; Schroeder, John L.

    1999-05-11

    A method for preparing carbon materials having high surface area and high macropore volume to provide high permeability. These carbon materials are prepared by dissolving a carbonizable polymer precursor, in a solvent. The solution is cooled to form a gel. The solvent is extracted from the gel by employing a non-solvent for the polymer. The non-solvent is removed by critical point drying in CO.sub.2 at an elevated pressure and temperature or evaporation in a vacuum oven. The dried product is heated in an inert atmosphere in a first heating step to a first temperature and maintained there for a time sufficient to substantially cross-link the polymer material. The cross-linked polymer material is then carbonized in an inert atmosphere.

  4. A green and facile preparation approach, licochalcone A capped on hollow gold nanoparticles, for improving the solubility and dissolution of anticancer natural product.

    PubMed

    Sun, Yi-Wei; Wang, Li-Hong; Meng, Da-Li; Che, Xin

    2017-12-01

    This study described a valuable drug delivery system for poorly water-soluble anticancer naturalproduct, licochalcone A, isolated from Glycyrrhiza inflata , loaded on hollow gold nanoparticles by green method to improve solubility and dissolution and maintain its natural pharmacological property. Briefly, the formation of hollow gold nanoparticles involves three steps: preparing of silica nanospheres by Stober method, forming of a thick gold shell around the silica templates and etching of silica particles by HF solution. Hollow gold nanoparticles (HGNPs) and drug loaded hollow gold nanoparticles (L-HGNPs) displayed spherical structure and approximately 200nm in size observed by SEM, XRD, EDS and DSC analysis showed that HGNPs were gold hollow structure and crystalline form. The solubility in aqueous solution of licochalcone A was increased obviously to 488.9 μg/ml, compared with free drugs of 136.1 μg/ml. Another interesting finding is that near-infrared (NIR) irradiation increased the speed of solubility of licochalcone A in aqueous solutions, rather than quantity. In short, the method of nano-delivery system combined with poorly water-soluble drug to improve its solubility and dissolution is worth applying to other natural products in order to increase their opportunities in clinical applications.

  5. In situ molecular elucidation of drug supersaturation achieved by nano-sizing and amorphization of poorly water-soluble drug.

    PubMed

    Ueda, Keisuke; Higashi, Kenjirou; Yamamoto, Keiji; Moribe, Kunikazu

    2015-09-18

    Quantitative evaluation of drug supersaturation and nanoparticle formation was conducted using in situ evaluation techniques, including nuclear magnetic resonance (NMR) spectroscopy. We prepared a ternary complex of carbamazepine (CBZ) with hydroxypropyl methylcellulose (HPMC) and sodium dodecyl sulfate (SDS) to improve the drug concentration. Different preparation methods, including grinding and spray drying, were performed to prepare the ternary component products, ground mixture (GM) and spray-dried sample (SD), respectively. Although CBZ was completely amorphized in the ternary SD, CBZ was partially amorphized with the remaining CBZ crystals in the ternary GM. Aqueous dispersion of the ternary GM formed nanoparticles of around 150 nm, originating from the CBZ crystals in the ternary GM. In contrast, the ternary SD formed transparent solutions without a precipitate. The molecular-level evaluation using NMR measurements revealed that approximately half a dose of CBZ in the ternary GM dispersion was present as nanoparticles; however, CBZ in the ternary SD was completely dissolved in the aqueous solution. The characteristic difference between the solid states, followed by different preparation methods, induced different solution characteristics in the ternary GM and SD. The permeation study, using a dialysis membrane, showed that the CBZ concentration dissolved in the bulk water phase rapidly reduced in the ternary SD dispersion compared to the ternary GM dispersion; this demonstrated the advantage of ternary GM dispersion in the maintenance of CBZ supersaturation. Long-term maintenance of a supersaturated state of CBZ observed in the ternary GM dispersion rather than in the ternary SD dispersion was achieved by the inhibition of CBZ crystallization owing to the existence of CBZ nanoparticles in the ternary GM dispersion. Nanoparticle formation, combined with drug amorphization, could be a promising approach to improve drug concentrations. The detailed elucidation of solution characteristics using in situ evaluation techniques will lead to the formation of useful solid dispersion and nanoparticle formulations, resulting in improved drug absorption. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Inverse supercritical fluid extraction as a sample preparation method for the analysis of the nanoparticle content in sunscreen agents.

    PubMed

    Müller, David; Cattaneo, Stefano; Meier, Florian; Welz, Roland; de Vries, Tjerk; Portugal-Cohen, Meital; Antonio, Diana C; Cascio, Claudia; Calzolai, Luigi; Gilliland, Douglas; de Mello, Andrew

    2016-04-01

    We demonstrate the use of inverse supercritical carbon dioxide (scCO2) extraction as a novel method of sample preparation for the analysis of complex nanoparticle-containing samples, in our case a model sunscreen agent with titanium dioxide nanoparticles. The sample was prepared for analysis in a simplified process using a lab scale supercritical fluid extraction system. The residual material was easily dispersed in an aqueous solution and analyzed by Asymmetrical Flow Field-Flow Fractionation (AF4) hyphenated with UV- and Multi-Angle Light Scattering detection. The obtained results allowed an unambiguous determination of the presence of nanoparticles within the sample, with almost no background from the matrix itself, and showed that the size distribution of the nanoparticles is essentially maintained. These results are especially relevant in view of recently introduced regulatory requirements concerning the labeling of nanoparticle-containing products. The novel sample preparation method is potentially applicable to commercial sunscreens or other emulsion-based cosmetic products and has important ecological advantages over currently used sample preparation techniques involving organic solvents. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. NC-AFM observation of atomic scale structure of rutile-type TiO2(110) surface prepared by wet chemical process.

    PubMed

    Namai, Yoshimichi; Matsuoka, Osamu

    2006-04-06

    We succeeded in observing the atomic scale structure of a rutile-type TiO2(110) single-crystal surface prepared by the wet chemical method of chemical etching in an acid solution and surface annealing in air. Ultrahigh vacuum noncontact atomic force microscopy (UHV-NC-AFM) was used for observing the atomic scale structures of the surface. The UHV-NC-AFM measurements at 450 K, which is above a desorption temperature of molecularly adsorbed water on the TiO2(110) surface, enabled us to observe the atomic scale structure of the TiO2(110) surface prepared by the wet chemical method. In the UHV-NC-AFM measurements at room temperature (RT), however, the atomic scale structure of the TiO2(110) surface was not observed. The TiO2(110) surface may be covered with molecularly adsorbed water after the surface was prepared by the wet chemical method. The structure of the TiO2(110) surface that was prepared by the wet chemical method was consistent with the (1 x 1) bulk-terminated model of the TiO2(110) surface.

  8. Modified Pechini's method to prepare LaAlO3:RE thermoluminescent materials

    NASA Astrophysics Data System (ADS)

    Rivera-Montalvo, T.; Morales-Hernandez, A.; Barrera-Angeles, A. A.; Alvarez-Romero, R.; Falcony, C.; Zarate-Medina, J.

    2017-11-01

    This work presents an alternative method to prepare rare-earth doped lanthanum aluminates materials for thermoluminescent (TL) dosimetry applications. Modified Pechini´s method was using to prepare praseodymium doped LaAlO3 powders. LaAlO3:Pr3+ powders were prepared using La(NO3)3·6H2O, Al(NO3)3·6H2O, Pr(NO3)3·6H2O, citric acid, and ethylene glycol. The solution was heated to 80 °C for its polyesterification reaction. The obtained powders were submitted at different thermal treatment from 700 up to 1600 °C. The structural and morphological characterizations were carried out using X-ray diffraction (XRD) and scanning electron microscopy techniques. TL glow curves of the X-ray irradiated samples showed one peak for europium and praseodymium dopants, meanwhile for powders doped with dysprosium ion showed two peaks. The technique is low cost, faster and it produces homogeneous particles can be used as thermoluminescent phosphors.

  9. Hydrazine-Free Solution-Deposited CuIn(S,Se)2 Solar Cells by Spray Deposition of Metal Chalcogenides.

    PubMed

    Arnou, Panagiota; van Hest, Maikel F A M; Cooper, Carl S; Malkov, Andrei V; Walls, John M; Bowers, Jake W

    2016-05-18

    Solution processing of semiconductors, such as CuInSe2 and its alloys (CIGS), can significantly reduce the manufacturing costs of thin film solar cells. Despite the recent success of solution deposition approaches for CIGS, toxic reagents such as hydrazine are usually involved, which introduce health and safety concerns. Here, we present a simple and safer methodology for the preparation of high-quality CuIn(S, Se)2 absorbers from metal sulfide solutions in a diamine/dithiol mixture. The solutions are sprayed in air, using a chromatography atomizer, followed by a postdeposition selenization step. Two different selenization methods are explored resulting in power conversion efficiencies of up to 8%.

  10. Phase transformation of TiO2 powder prepared by TiCl4 hydrolysis-electrolysis

    NASA Astrophysics Data System (ADS)

    Nur, Adrian; Purwanto, Agus; Jumari, Arif; Dyartanti, Endah R.; A. N., Richard Leonardo; Gultom, Barry Januari

    2017-01-01

    Metal oxide combined with graphite becomes an interesting composition. TiO2 is a good candidate for Li ion battery anode because of low cost, availability sufficient, and environmentally friendly. The form of TiO2 crystals is highly depended on the synthesis method used. The electrochemical method is beginning to emerge as a valuable option for preparing TiO2 powders. Using the electrochemical method, the particle phase can easily be controlled by simply adjusting the imposed current or potential to the system. The present work aims to investigate the effects of electrode distance in the electrolysis of TiCl4 solution to the phase transformation of anatase to rutile. The homogeneous solution for the electro-synthesis of TiO2 powders was TiCl4 in ethanol solution. The electrolysis was carried out in an electrochemical cell consisting of two carbon electrodes with dimensions of (5×2) cm. The electrodes were set parallel with various distances of 2.6 cm, 3 cm, and 4 cm between the electrodes and were immersed in the electrolytic solution at a depth of 2 cm. The electrodes were connected to the positive and negative terminals of a DC power supply (Zhaoxin PS-3005D). The electro-synthesis was performed galvanostatically at 2.5 hours and a voltage 10 V under constant stirring at room temperature. Phase transformation from anatase to rutile occurred at 2.6 cm to 3 cm electrode distance.

  11. a New Method to Prepare the Novel Anatase TiO2

    NASA Astrophysics Data System (ADS)

    Cui, Guanjun; Xu, Zhanxia; Wang, Yan; Zhang, Min; Yang, Jianjun

    In this paper, a kind of novel anatase TiO2 nanoparticle with single-electron-trapped oxygen vacancies was prepared by hydrothermal treated nanotube titanic acid. The morphology, structure, and properties of the products were characterized by transmission electron microscope, X-ray diffraction, electron spin resonance, and photoluminescence. Photocatalytic decolorization of the Methylene Blue solution was carried out in the visible light region and showed a high photocatalytic activity.

  12. Organic inorganic hybrid coating (poly(methyl methacrylate)/monodisperse silica)

    NASA Astrophysics Data System (ADS)

    Rubio, E.; Almaral, J.; Ramírez-Bon, R.; Castaño, V.; Rodríguez, V.

    2005-04-01

    Polymethylmethacrylate-silica hybrid coatings were prepared from methyl methacrylate and monodisperse colloidal silica prepared by the Stöber method. The surfaces of the spheres were successfully modified by chemical reaction with 3-(trimethoxysilyl) propyl methacrylate (TMSPM) to compatibilise the organic and inorganic components of the precursor solution mixture. The coatings were deposited by dip-coating on glass substrates. They result with good properties of homogeneity, optical transparence, hardness and adhesion.

  13. METHOD FOR THE PREPARATION OF STABLE ACTINIDE METAL OXIDE-CONTAINING SLURRIES AND OF THE OXIDES THEREFOR

    DOEpatents

    Hansen, R.S.; Minturn, R.E.

    1958-02-25

    This patent deals with a method of preparing actinide metal oxides of a very fine particle size and of forming stable suspensions therefrom. The process consists of dissolving the nitrate of the actinide element in a combustible organic solvent, converting the solution obtained into a spray, and igniting the spray whereby an oxide powder is obtained. The oxide powder is then slurried in an aqueous soiution of a substance which is adsorbable by said oxides, dspersed in a colloid mill whereby a suspension is obtained, and electrodialyzed until a low spectiic conductance is reached.

  14. Evaluation of transport parameters for PVC based polyvinyl alcohol Ce(IV) phosphate composite membrane.

    PubMed

    Khan, Mohammad Mujahid Ali; Rafiuddin; Inamuddin

    2013-05-01

    The aim of this study was to investigate the preparation of novel membrane and the characterization of their properties. A new class of polyvinyl chloride (PVC) based polyvinyl alcohol Ce(IV) phosphate composite membrane was successfully prepared by solution casting method. The structural formation was confirmed by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy and morphological studies. The thermal property was investigated by thermogravimetry analysis (TGA) method. The order of surface charge density for various electrolytes was found to be LiCl

  15. Preparation method and quality control of multigamma volume sources with different matrices.

    PubMed

    Listkowska, A; Lech, E; Saganowski, P; Tymiński, Z; Dziel, T; Cacko, D; Ziemek, T; Kołakowska, E; Broda, R

    2018-04-01

    The aim of the work was to develop new radioactive standard sources based on epoxy resins. The optimal proportions of the components and the homogeneity of the matrices were determined. The activity of multigamma sources prepared in Marinelli beakers was determined with reference to the National Standard of Radionuclides Activity in Poland. The difference of radionuclides activity values determined using calibrated gamma spectrometer and the activity of standard solutions used are in most cases significantly lower than measurement uncertainty limits. Sources production method and quality control procedure have been developed. Copyright © 2017 Elsevier Ltd. All rights reserved.

  16. Method for the preparation of thin-skinned asymmetric reverse osmosis membranes and products thereof

    NASA Technical Reports Server (NTRS)

    Wydeven, T. J. (Inventor); Katz, M. G.

    1984-01-01

    A method for preparing water insoluble asymmetric membranes from water soluble polymers is discussed. The process involves casting a film of the polymer, partially drying it, and then contacting it with a concentrated solution of a transition metal salt. The transition metal ions render the polymer insoluable and are believed to form a complex with it. Optionally, the polymer is crosslinked with heat or radiation. The most preferred polymer is poly(vinyl alcohol). The most preferred complexing salt is copper sulfate. The process and the metal ion linked membranes are discussed. The membranes are reverse osmosis membranes.

  17. Cryochemical method for forming spherical metal oxide particles from metal salt solutions

    DOEpatents

    Tinkle, M.C.

    1973-12-01

    A method is described of preparing small metal oxide spheres cryochemically utilizing metal salts (e.g., nitrates) that cannot readily be dried and calcined without loss of sphericity of the particles. Such metal salts are cryochemically formed into small spheres, partially or completely converted to an insoluble salt, and dried and calcined. (Official Gazette)

  18. DEVELOPMENT AND APPLICATION OF IMMUNOAFFINITY COLUMN CHROMATOGRAPHY AS A CLEANUP METHOD FOR THE DETERMINATION OF ATRAZINE IN COMPLEX ENVIRONMENTAL SAMPLE MEDIA

    EPA Science Inventory

    A rabbit antibody immunoaffinity (IA) column procedure was evaluated as a cleanup method for the determination of atrazine in soil, sediment, and food. Four IA columns were prepared by immobilizing a polyclonal rabbit anti-atrazine antibody solution to HiTrap Sepharose columns. A...

  19. A new method for long-term storage of titred microbial standard solutions suitable for microbiologic quality control activities of pharmaceutical companies.

    PubMed

    Chiellini, Carolina; Mocali, Stefano; Fani, Renato; Ferro, Iolanda; Bruschi, Serenella; Pinzani, Alessandro

    2016-08-01

    Commercially available lyophilized microbial standards are expensive and subject to reduction in cell viability due to freeze-drying stress. Here we introduce an inexpensive and straightforward method for in-house microbial standard preparation and cryoconservation that preserves constant cell titre and cell viability over 14 months.

  20. Barriers and Solutions to Fieldwork Education in Hand Therapy.

    PubMed

    Short, Nathan; Sample, Shelby; Murphy, Malachi; Austin, Brittany; Glass, Jillian

    2017-08-09

    Survey. Fieldwork education is a vital component of training the next generation of CHTs. Barriers and solutions to fieldwork rotations in hand therapy are examined, as well as proposed solutions, including recommendations for student preparation. This descriptive study examined barriers for certified hand therapist clinicians to accept students for clinical rotations and clinicians' preferences for student preparation before a rotation in a hand setting. A survey was developed, peer reviewed, and distributed using the electronic mailing list of the Hand Therapy Certification Commission via SurveyMonkey. Aggregate responses were analyzed to identify trends including barriers to student clinical rotations and recommendations for students to prepare for hand rotations. A total of 2080 participants responded to the survey, representing a 37% response rate. Common logistical barriers were identified for accepting students such as limited clinical time and space. Many clinicians (32% agree and 8% strongly agree) also felt that the students lack the clinical knowledge to be successful. Areas of knowledge, skill set, and experience were surveyed for development before a clinical rotation in a hand setting. Most respondents (74%) reported increased likelihood of accepting a student with the recommended preparation. Novel qualitative responses to improve clinical experiences are presented as well. Student preparation before a clinical rotation in a hand setting appears to be a significant barrier based on the survey results. Areas of recommended knowledge, skill set, and experience may serve to guide both formal and informal methods of student preparation before a hand-specific clinical rotation to facilitate knowledge translation from experienced certified hand therapists to the next generation. Although logistical barriers may be difficult to overcome, hand-specific preparation based on clinician' recommendations may facilitate student acceptance and success in hand specialty clinical rotations. N/A. Copyright © 2017 Hanley & Belfus. Published by Elsevier Inc. All rights reserved.

  1. Preparation and evaluation of thermosensitive liposomal hydrogel for enhanced transcorneal permeation of ofloxacin.

    PubMed

    Hosny, Khaled Mohamed

    2009-01-01

    Ofloxacin, available as ophthalmic solution, has two major problems: first, it needs frequent administration every 4 hours or even every 1 hour to treat severe eye infection; second, there is formation of white crystalline deposit on cornea due to its pH-dependent solubility, which is very low at pH of corneal fluid. In order to provide a solution to previous problems, ofloxacin in this study is prepared as topically effective in situ thermosensitive prolonged release liposomal hydrogel. Two preparation procedures were carried out, leading to the formation of multilamellar vesicles (MLVs) and reverse-phase evaporation vesicles (REVs) at pH 7.4. Effects of method of preparation, lipid content, and charge inducers on encapsulation efficiency were studied. For the preparation of in situ thermosensitive hydrogel, chitosan/beta-glycerophosphate system was synthesized and used as carrier for ofloxacin liposomes. The effect of addition of liposomes on gelation temperature, gelation time, and rheological behaviors of the hydrogel were evaluated. In vitro transcorneal permeation was also determined. MLVs entrapped greater amount of ofloxacin than REVs liposomes at pH 7.4; drug loading was increased by including charge-inducing agent and by increasing cholesterol content until a certain limit. The gelation time was decreased by the addition of liposomes into the hydrogel. The prepared liposomal hydrogel enhances the transcorneal permeation sevenfold more than the aqueous solution. These results suggested that the in situ thermosensitive ofloxacin liposomal hydrogel ensures steady and prolonged transcorneal permeation, which improves the ocular bioavailability, minimizes the need for frequent administration, and decreases the ocular side effect of ofloxacin.

  2. Taste intensities of ten vegetables commonly consumed in the Netherlands.

    PubMed

    van Stokkom, V L; Teo, P S; Mars, M; de Graaf, C; van Kooten, O; Stieger, M

    2016-09-01

    Bitterness has been suggested to be the main reason for the limited palatability of several vegetables. Vegetable acceptance has been associated with preparation method. However, the taste intensity of a variety of vegetables prepared by different methods has not been studied yet. The objective of this study is to assess the intensity of the five basic tastes and fattiness of ten vegetables commonly consumed in the Netherlands prepared by different methods using the modified Spectrum method. Intensities of sweetness, sourness, bitterness, umami, saltiness and fattiness were assessed for ten vegetables (cauliflower, broccoli, leek, carrot, onion, red bell pepper, French beans, tomato, cucumber and iceberg lettuce) by a panel (n=9) trained in a modified Spectrum method. Each vegetable was assessed prepared by different methods (raw, cooked, mashed and as a cold pressed juice). Spectrum based reference solutions were available with fixed reference points at 13.3mm (R1), 33.3mm (R2) and 66.7mm (R3) for each taste modality on a 100mm line scale. For saltiness, R1 and R3 differed (16.7mm and 56.7mm). Mean intensities of all taste modalities and fattiness for all vegetables were mostly below R1 (13.3mm). Significant differences (p<0.05) within vegetables between preparation methods were found. Sweetness was the most intensive taste, followed by sourness, bitterness, fattiness, umami and saltiness. In conclusion, all ten vegetables prepared by different methods showed low mean intensities of all taste modalities and fattiness. Preparation method affected taste and fattiness intensity and the effect differed by vegetable type. Copyright © 2016 Elsevier Ltd. All rights reserved.

  3. Performance improvement for solution-processed high-mobility ZnO thin-film transistors

    NASA Astrophysics Data System (ADS)

    Sha Li, Chen; Li, Yu Ning; Wu, Yi Liang; Ong, Beng S.; Loutfy, Rafik O.

    2008-06-01

    The fabrication technology of stable, non-toxic, transparent, high performance zinc oxide (ZnO) thin-film semiconductors via the solution process was investigated. Two methods, which were, respectively, annealing a spin-coated precursor solution and annealing a drop-coated precursor solution, were compared. The prepared ZnO thin-film semiconductor transistors have well-controlled, preferential crystal orientation and exhibit superior field-effect performance characteristics. But the ZnO thin-film transistor (TFT) fabricated by annealing a drop-coated precursor solution has a distinctly elevated linear mobility, which further approaches the saturated mobility, compared with that fabricated by annealing a spin-coated precursor solution. The performance of the solution-processed ZnO TFT was further improved when substituting the spin-coating process by the drop-coating process.

  4. Preparation and Characterization of Nano Gold Supported over Montmorillonite Clays

    NASA Astrophysics Data System (ADS)

    Suraja, P. V.; Binitha, N. N.; Yaakob, Z.; Silija, P. P.

    2011-02-01

    The use of montmorillonite clays as a matrix, or as a host, for obtaining intercalated/supported metal particles has potential applications in catalysis and other areas. The gold nanoparticles were obtained from the most common anionic gold precursor HAuCl4·3H2O by deposition-precipitation (DP) methods. However, it is difficult to prepare nanoscale gold catalysts supported on silica surfaces with lower isoelectric point (IEP). Homogeneous precipitation method using urea also fails on silica surfaces. Reasons for the inefficiency of these methods are the negative charge of the metal precursor as well as the support surface and the high pH required for depositing gold nanoparticles. In the present work, we use glucose as the reductant in the presence of stabilizer for preparation of nano gold supported on montmorillonite clay. There is no need of increasing the pH of the solution to reduce the Au3+ ions. The prepared systems are characterized using various techniques such as using X-ray fluorescence (XRF), UV-VIS Diffuse reflectance spectra (DRS) and Fourier Transform infra red spectra (FTIR) to prove the efficiency of the present method.

  5. Determination of green tea catechins in human plasma using liquid chromatography-electrospray ionization mass spectrometry.

    PubMed

    Masukawa, Yoshinori; Matsui, Yuji; Shimizu, Namii; Kondou, Naoki; Endou, Hidenori; Kuzukawa, Michiya; Hase, Tadashi

    2006-04-13

    A method for the sensitive and specific determination of eight green tea catechins, consisting of catechin (C), epicatechin (EC), gallocatechin (GC), epigallocatechin (EGC), catechin-3-gallate (CG), epicatechin-3-gallate (ECG), gallocatechin-3-gallate (GCG) and epigallocatechin-3-gallate (EGCG), in human plasma was established. For optimization of conditions for LC-ESIMS, the separation of the eight catechins was achieved chromatographically using Inertsil ODS-2 column combined with a gradient elution system of 0.1M aqueous acetic acid and 0.1M acetic acid in acetonitrile. Detection using a mass spectrometer was performed with selected ion monitoring at m/z=289 for E and EC, 305 for GC and EGC, 441 for CG and ECG, and 457 for GCG and EGCG under negative ESI. A preparative procedure, consisting of the addition of perchloric acid and acetonitrile to the plasma for deproteinizing and the subsequent addition of potassium carbonate solution to remove excess acid, was developed. In six different plasma with the eight catechins spiked at two different concentrations, the average recoveries were in the range between 72.7 and 84.1%, which resulted from the matrix effect and preparative loss, with coefficients of variance being 8.2-19.8% among individuals. The levels of the catechins in prepared plasma solutions that were kept at 5 degrees C within 24h were stable, which allows us to simply analyze many prepared plasma solutions using an autosampler overnight. When using this method to analyze the eight catechins in human plasma after oral ingestion of a commercial green tea beverage, we detected all the catechins absorbed into human blood for the first time. This also suggested that extremely small amounts of the eight catechins orally ingested may be absorbed based on each absorptive property for the catechins. The method should enable pharmacokinetic studies of green tea catechins in humans.

  6. Fabrication of quantum dot/silica core-shell particles immobilizing Au nanoparticles and their dual imaging functions

    NASA Astrophysics Data System (ADS)

    Kobayashi, Yoshio; Matsudo, Hiromu; Li, Ting-ting; Shibuya, Kyosuke; Kubota, Yohsuke; Oikawa, Takahiro; Nakagawa, Tomohiko; Gonda, Kohsuke

    2016-03-01

    The present work proposes preparation methods for quantum dot/silica (QD/SiO2) core-shell particles that immobilize Au nanoparticles (QD/SiO2/Au). A colloid solution of QD/SiO2 core-shell particles with an average size of 47.0 ± 6.1 nm was prepared by a sol-gel reaction of tetraethyl orthosilicate in the presence of the QDs with an average size of 10.3 ± 2.1 nm. A colloid solution of Au nanoparticles with an average size of 17.9 ± 1.3 nm was prepared by reducing Au3+ ions with sodium citrate in water at 80 °C. Introduction of amino groups to QD/SiO2 particle surfaces was performed using (3-aminopropyl)-triethoxysilane (QD/SiO2-NH2). The QD/SiO2/Au particles were fabricated by mixing the Au particle colloid solution and the QD/SiO2-NH2 particle colloid solution. Values of radiant efficiency and computed tomography for the QD/SiO2/Au particle colloid solution were 2.23 × 107 (p/s/cm2/sr)/(μW/cm2) at a QD concentration of 8 × 10-7 M and 1180 ± 314 Hounsfield units and an Au concentration of 5.4 × 10-2 M. The QD/SiO2/Au particle colloid solution was injected into a mouse chest wall. Fluorescence emitted from the colloid solution could be detected on the skin covering the chest wall. The colloid solution could also be X-ray-imaged in the chest wall. Consequently, the QD/SiO2/Au particle colloid solution was found to have dual functions, i.e., fluorescence emission and X-ray absorption in vivo, which makes the colloid solution suitable to function as a contrast agent for dual imaging processes.

  7. Synthesis and characterization of amorphous yttrium oxide layers by metal organic chemical solution deposition

    NASA Astrophysics Data System (ADS)

    Martynova, I.; Tsymbarenko, D.; Kamenev, A.; Kuzmina, N.; Kaul, A.

    2014-02-01

    The Solution Deposition Planarization method was successfully used for smoothing Ni-alloy tapes with initial surface roughness of 26.7 nm (on 40×40 μm2 area) and 12.6 nm (on 5×5 μm2 area). New precursor solutions were prepared from yttrium acetate and diethylenetriamine or ethylenediamine in MeOH and i-PrOH-alcohols with different viscosities. Using those solutions yttria films with the residual roughness Sa=0.4 nm (on 5×5 μm2 area) and Sa=7.6 nm (on 40×40 μm2 area) were deposited on the Ni-alloy tapes.

  8. In situ polymerization of monomers for polyphenylquinoxaline/graphite

    NASA Technical Reports Server (NTRS)

    Serafini, T. T.; Delvigs, P.; Vannucci, R. D.

    1973-01-01

    Methods currently used to prepare fiber reinforced, high temperature resistant polyphenylquinoxaline (PPQ) composites employ extremely viscous, low solids content solutions of high molecular weight PPQ polymers. An improved approach, described in this report, consists of impregnating the fiber with a solution of the appropriate monomers instead of a solution of previously synthesized high molecular weight polymer. Polymerization of the monomers occurs in situ on the fiber during the solvent removal and curing stages. The in situ polymerization approach greatly simplifies the fabrication of PPQ graphite fiber composites. The use of low viscosity monomeric type solutions facilitates fiber wetting, permits a high solids content, and eliminates the need for prior polymer synthesis.

  9. Cryoradiation sterilization—Contemporary state and outlook

    NASA Astrophysics Data System (ADS)

    Talrose, V. L.; Trofimov, V. I.

    1995-02-01

    The new approach of radiation sterilization — cryoradiosterilization with programmed freezing — was developed for pharmaceutical solutions. Both scientific and technical problems are solved, the results are discussed. Programmed freezing of vials with the drug's solutions provides the high stability of soluted components with biological activity at sterilizing irradiation without significant change of sterilization doses. Physical, chemical, biological and pharmacological properties of a lot of drug solutions for injection satisfy official requirements after cryoradiation sterilization treatment. This method seems to be especially important for the protein systems which could be infected by dangerous viruses (VIH, hepatitis B): blood plasma, diagnostic sera, protein preparations manufactured from donor's blood, etc.

  10. Manipulation of surface morphology of flower-like Ag/ZnO nanorods to enhance photocatalytic performance

    NASA Astrophysics Data System (ADS)

    U-thaipan, Kasira; Tedsree, Karaked

    2018-06-01

    The surface morphology of flower-like Ag/ZnO nanorod can be manipulated by adopting different synthetic routes and also loading different levels of Ag in order to alter their surface structures to achieve the maximum photocatalytic efficiency. In a single-step preparation method Ag/ZnO was prepared by heating directly a mixture of Zn2+ and Ag+ precursors in an aqueous NaOH-ethylene glycol solution, while in the two-step preparation method an intermediate of flower-shaped ZnO nanorod was obtained by a hydrothermal process before depositing Ag particles on the ZnO surfaces by chemical reduction. The structure, morphology and optical properties of the synthesized samples were characterized using TEM, SEM, XRD, DRS and PL techniques. The sample prepared by single-step method are characterized with agglomeration of Ag atoms as clusters on the surface of ZnO, whereas in the sample prepared by two-step method Ag atoms are found uniformly dispersed and deposited as discrete Ag nanoparticles on the surface of ZnO. A significant enhancement in the adsorption of visible light was evident for Ag/ZnO samples prepared by two-step method especially with low Ag content (0.5 mol%). The flower-like Ag/ZnO nanorod prepared with 0.5 mol% Ag by two-step process was found to be the most efficient photocatalyst for the degradation of phenol, which can decompose 90% of phenol within 120 min.

  11. Solution-phase parallel synthesis of aryloxyimino amides via a novel multicomponent reaction among aromatic (Z)-chlorooximes, isocyanides, and electron-deficient phenols.

    PubMed

    Mercalli, Valentina; Giustiniano, Mariateresa; Del Grosso, Erika; Varese, Monica; Cassese, Hilde; Massarotti, Alberto; Novellino, Ettore; Tron, Gian Cesare

    2014-11-10

    A library of 41 aryloxyimino amides was prepared via solution phase parallel synthesis by extending the multicomponent reaction of (Z)-chlorooximes and isocyanides to the use of electron-deficient phenols. The resulting aryloxyiminoamide derivatives can be used as intermediates for the synthesis of benzo[d]isoxazole-3-carboxamides, dramatically reducing the number of synthetic steps required by other methods reported in literature.

  12. Synthesis of Perfluorinated Ethers by Solution Phase Direct Fluorination: An Adaptation of the La-Mar Technique

    DTIC Science & Technology

    1990-08-22

    Six of the 3 perfluorinated ethers prepared have been previously synthesized by other methods: perfluoro -5,5-bis(ethoxy- f methyl) -3,7-dioxanonane...from partially fluorinated starting material [34]. Third, as with perfluoroalkanes and simple perfluoroethers , Clark’s experimental results indicated 3...a highly branched perfluoroether ) by direct fluorination 3 in solution. Second, since some of these perfluorinated compounds had been previously

  13. Dense protective coatings, methods for their preparation and coated articles

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

    Tulyani, Sonia; Bhatia, Tania; Smeggil, John G.

    A method for depositing a protective coating on a complex shaped substrate includes the steps of: (1) dipping a complex shaped substrate into a slurry to form a base coat thereon, the slurry comprising an aqueous solution, at least one refractory metal oxide, and at least one transient fluid additive present in an amount of about 0.1 percent to 10 percent by weight of the slurry; (2) curing the dipped substrate; (3) dipping the substrate into a precursor solution to form a top barrier coat thereon; and (4) heat treating the dipped, cured substrate to form a protective coating.

  14. Porous Chromatographic Materials as Substrates for Preparing Synthetic Nuclear Explosion Debris Particles

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

    Harvey, Scott D.; Liezers, Martin; Antolick, Kathryn C.

    2013-06-13

    In this study, we investigated several porous chromatographic materials as synthetic substrates for preparing surrogate nuclear explosion debris particles. The resulting synthetic debris materials are of interest for use in developing analytical methods. Eighteen metals, including some of forensic interest, were loaded onto materials by immersing them in metal solutions (556 mg/L of each metal) to fill the pores, applying gentle heat (110°C) to drive off water, and then treating them at high temperatures (up to 800°C) in air to form less soluble metal species. High-boiling-point metals were uniformly loaded on spherical controlled-pore glass to emulate early fallout, whereas low-boiling-pointmore » metals were loaded on core-shell silica to represent coated particles formed later in the nuclear fallout-formation process. Analytical studies were applied to characterize solubility, material balance, and formation of recalcitrant species. Dissolution experiments indicated loading was 1.5 to 3 times higher than expected from the pore volume alone, a result attributed to surface coating. Analysis of load solutions before and after filling the material pores revealed that most metals were passively loaded; that is, solutions filled the pores without active metal discrimination. However, niobium and tin concentrations were lower in solutions after pore filling, and were found in elevated concentrations in the final products, indicating some metals were selectively loaded. High-temperature treatments caused reduced solubility of several metal species, and loss of some metals (rhenium and tellurium) because volatile species were formed. Sample preparation reproducibility was high (the inter-batch relative standard deviation was 7.8%, and the intra-batch relative standard deviation was 0.84%) indicating that this material is suitable for use as a working standard for analytical methods development. We anticipate future standardized radionuclide-loaded materials will find use in radioanalytical methods development and/or serve as a starting material for the synthesis of more complex forms of nuclear explosion debris (e.g., Trinitite).« less

  15. Antimicrobial activity of TiO2 nanostructures synthesized by hydrothermal method

    NASA Astrophysics Data System (ADS)

    Surah, Shivani Singh; Sirohi, Siddharth; Nain, Ratyakshi; Kumar, Gulshan

    2018-02-01

    Titania nanostructures were synthesized by hydrothermal method. Titanium tetrachloride was used as a precursor, sodium hydroxide was used as a solvent. Effect on their morphology by variation of parameters like temperature (110°C, 160°C and 180°C), time (15h,18h, 20h, 22h, 24h) and concentration of the solvent NaOH (5M, 8M, 10 M, 12M) were studied. The obtained TiO2 nanostructures were washed with deionized water. The structure, size, morphology of the prepared nanostructures were analyzed by SEM (scanning electron microscope), DLS (dynamic light scattering), TEM (transmission electron microscope). SEM and TEM revealed the shape, size of the nanostructures. DLS reported the particle size of prepared TiO2 nanoparticles. Polymeric films based on polyvinyl alcohol (PVA) doped with titanium dioxide nanostructures at different weight percentage (0.5, 0.75, 1,2 TiO2/PVA) were prepared using the ultra sonication and solution casting techniques. The appropriate weight of PVA was dissolved in deionized water. The mixture was magnetically stirred continuously and heated (80°C) for 4 hours, until the solution mixture becomes homogenous. Different weight percentage of TiO2 nanostructures were added to deionized water and sonicated for 3 hours to prevent the nanostructures agglomeration. The mixture was mixed with the PVA solution and magnetically stirred for 1 hour to get good dispersion without agglomeration. The final PVA /TiO2 mixture were casted in glass Petridish, were left until dry. Ultrasonication was used as a major factor for preparation in order to get better dispersion. Nanocomposite films were characterized using SEM and were found to exhibit antimicrobial properties when treated with E.coli and pseudomonas.

  16. Method of preparing mercury with an arbitrary isotopic distribution

    DOEpatents

    Grossman, Mark W.; George, William A.

    1986-01-01

    This invention provides for a process for preparing mercury with a predetermined, arbitrary, isotopic distribution. In one embodiment, different isotopic types of Hg.sub.2 Cl.sub.2, corresponding to the predetermined isotopic distribution of Hg desired, are placed in an electrolyte solution of HCl and H.sub.2 O. The resulting mercurous ions are then electrolytically plated onto a cathode wire producing mercury containing the predetermined isotopic distribution. In a similar fashion, Hg with a predetermined isotopic distribution is obtained from different isotopic types of HgO. In this embodiment, the HgO is dissolved in an electrolytic solution of glacial acetic acid and H.sub.2 O. The isotopic specific Hg is then electrolytically plated onto a cathode and then recovered.

  17. Step-reduced synthesis of starch-silver nanoparticles.

    PubMed

    Raghavendra, Gownolla Malegowd; Jung, Jeyoung; Kim, Dowan; Seo, Jongchul

    2016-05-01

    In the present process, silver nanoparticles were directly synthesized in a single step by microwave irradiation of a mixture of starch, silver nitrate, and deionized water. This is different from the commonly adopted procedure for starch-silver nanoparticle synthesis in which silver nanoparticles are synthesized by preparing a starch solution as a reaction medium first. Thus, the additional step associated with the preparation of the starch solution was eliminated. In addition, no additional reducing agent was utilized. The adopted method was facile and straight forward, affording spherical silver nanoparticles with diameter below 10nm that exhibited good antibacterial activity. Further, influence of starch on the size of the silver nanoparticles was noticed. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Facile synthesis of stable superhydrophobic nanocomposite based on multi-walled carbon nanotubes

    NASA Astrophysics Data System (ADS)

    Mokarian, Zahra; Rasuli, Reza; Abedini, Yousefali

    2016-04-01

    A facile approach to fabricate a stable superhydrophobic composite comprising multi-walled carbon nanotubes and silicone rubber has been reported. Contact angle of de-ionized water droplets on the prepared surface was measured with the value of near 159°; while water droplets easily rolled off and bounced on it. Surface free energy of the superhydrophobic coating was examined by three methods about 26 mJ/m2. The prepared film shows good stability under high stress conditions such as ultraviolet exposure, heating, pencil hardness test, attacking with different pH value and ionic-strength solutions. In addition, remarkable stability of the coating was observed after soaking in condensed hydrochloric acid, 5 wt.% NaCl aqueous solution, boiling water and tape test.

  19. Method of preparing mercury with an arbitrary isotopic distribution

    DOEpatents

    Grossman, M.W.; George, W.A.

    1986-12-16

    This invention provides for a process for preparing mercury with a predetermined, arbitrary, isotopic distribution. In one embodiment, different isotopic types of Hg[sub 2]Cl[sub 2], corresponding to the predetermined isotopic distribution of Hg desired, are placed in an electrolyte solution of HCl and H[sub 2]O. The resulting mercurous ions are then electrolytically plated onto a cathode wire producing mercury containing the predetermined isotopic distribution. In a similar fashion, Hg with a predetermined isotopic distribution is obtained from different isotopic types of HgO. In this embodiment, the HgO is dissolved in an electrolytic solution of glacial acetic acid and H[sub 2]O. The isotopic specific Hg is then electrolytically plated onto a cathode and then recovered. 1 fig.

  20. Preparation of core-shell Ag@CeO2 nanocomposite by LSPR photothermal induced interface reaction

    NASA Astrophysics Data System (ADS)

    Zhong, H. X.; Wei, Y.; Yue, Y. Z.; Zhang, L. H.; Liu, Y.

    2016-04-01

    The core-shell structure of Ag@CeO2 was prepared by a novel and facile method, which was based on the photothermal effect of localized surface plasmon resonance (LSPR). Nanoparticles (NPs) of Ag were dispersed in a solution containing citric acid, ethylene glycol and cerium nitrate, then under irradiation, Ag NPs generated heat from LSPR and the heat-induced polymerization reaction in the interface between Ag and the sol resulted in cerium gel formation only on the surface of the Ag NPs. After calcination, Ag@CeO2 was successfully obtained, then Ag@CeO2/SiO2 was prepared by loading Ag@CeO2 on SiO2. The resultant catalyst exhibited favorable activity and stability for CO oxidation. The preparation method proposed here should be extendable to other composites with metallic cores and oxide shells in which the metallic nanoparticle possesses LSPR properties.

  1. Preparation of superhydrophobic titanium surfaces via electrochemical etching and fluorosilane modification

    NASA Astrophysics Data System (ADS)

    Lu, Yao; Xu, Wenji; Song, Jinlong; Liu, Xin; Xing, Yingjie; Sun, Jing

    2012-12-01

    The preparation of superhydrophobic surfaces on hydrophilic metal substrates depends on both surface microstructures and low surface energy modification. In this study, a simple and inexpensive electrochemical method for preparing robust superhydrophobic titanium surfaces is reported. The neutral sodium chloride solution is used as electrolyte. Fluoroalkylsilane (FAS) was used to reduce the surface energy of the electrochemically etched surface. Scanning electron microscopy (SEM) images, energy-dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FTIR) spectra, and contact angle measurement are performed to characterize the morphological features, chemical composition, and wettability of the titanium surfaces. Stability and friction tests indicate that the prepared titanium surfaces are robust. The analysis of electrolyte, reaction process, and products demonstrates that the electrochemical processing is very inexpensive and environment-friendly. This method is believed to be easily adaptable for use in large-scale industry productions to promote the application of superhydrophobic titanium surfaces in aviation, aerospace, shipbuilding, and the military industry.

  2. Preparation of resveratrol-loaded nanoporous silica materials with different structures

    NASA Astrophysics Data System (ADS)

    Popova, Margarita; Szegedi, Agnes; Mavrodinova, Vesselina; Novak Tušar, Natasa; Mihály, Judith; Klébert, Szilvia; Benbassat, Niko; Yoncheva, Krassimira

    2014-11-01

    Solid, nanoporous silica-based spherical mesoporous MCM-41 and KIL-2 with interparticle mesoporosity as well as nanosized zeolite BEA materials differing in morphology and pore size distribution, were used as carriers for the preparation of resveratrol-loaded delivery systems. Two preparation methods have been applied: (i) loading by mixing of resveratrol and mesoporous carrier in solid state and (ii) deposition in ethanol solution. The parent and the resveratrol loaded carriers were characterized by XRD, TEM, N2 physisorption, thermal analysis, and FT-IR spectroscopy. The influence of the support structure on the adsorption capacity and the release kinetics of this poorly soluble compound were investigated. Our results indicated that the chosen nanoporous silica supports are suitable for stabilization of trans-resveratrol and reveal controlled release and ability to protect the supported compound against degradation regardless of loading method. The solid-state dry mixing appears very effective for preparation of drug formulations composed of poorly soluble compound.

  3. Preparation and characterization of novel biocompatible cryogels of poly (vinyl alcohol) and egg-albumin and their water sorption study.

    PubMed

    Bajpai, A K; Saini, Rajesh

    2006-01-01

    Polyvinyl alcohol (PVA) and egg albumin are water-soluble, biocompatible and biodegradable polymers and have been widely employed in biomedical fields. In this paper, novel physically cross-linked hydrogels composed of poly (vinyl alcohol) and egg albumin were prepared by cyclic freezing/thawing processes of aqueous solutions containing PVA and egg albumin. The FTIR analysis of prepared cryogels indicated that egg albumin was successfully introduced into the formed hydrogel possibly via hydrogen bonds among hydroxyl groups, amide groups and amino groups present in PVA and egg albumin. The gels were also characterized thermally and morphologically by DSC and SEM-techniques, respectively. The prepared so called 'cryogels' were evaluated for their water uptake potential and influence of various factors such as chemical architecture of the spongy hydrogels, pH and temperature of the swelling bath were investigated on the degree of water sorption by the cryogels. The effect of salt solution and various simulated biological fluids on the swelling of cryogel was also studied. The in vitro biocompatibility of the prepared cryogel was also judged by methods such as protein (BSA) adsorption, blood clot formation and percentage hemolysis measurements.

  4. CuInSe₂ thin-film solar cells with 7.72 % efficiency prepared via direct coating of a metal salts/alcohol-based precursor solution.

    PubMed

    Ahn, Sejin; Son, Tae Hwa; Cho, Ara; Gwak, Jihye; Yun, Jae Ho; Shin, Keeshik; Ahn, Seoung Kyu; Park, Sang Hyun; Yoon, Kyunghoon

    2012-09-01

    A simple direct solution coating process for forming CuInSe₂ (CIS) thin films was described, employing a low-cost and environmentally friendly precursor solution. The precursor solution was prepared by mixing metal acetates, ethanol, and ethanolamine. The facile formation of a precursor solution without the need to prefabricate nanoparticles enables a rapid and easy processing, and the high stability of the solution in air further ensures the precursor preparation and the film deposition in ambient conditions without a glove box. The thin film solar cell fabricated with the absorber film prepared by this route showed an initial conversion efficiency of as high as 7.72 %. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. A simple method to prepare magnetic modified beer yeast and its application for cationic dye adsorption.

    PubMed

    Yu, Jun-Xia; Wang, Li-Yan; Chi, Ru-An; Zhang, Yue-Fei; Xu, Zhi-Gao; Guo, Jia

    2013-01-01

    The purpose of this research is to use a simple method to prepare magnetic modified biomass with good adsorption performances for cationic ions. The magnetic modified biomass was prepared by two steps: (1) preparation of pyromellitic dianhydride (PMDA) modified biomass in N, N-dimethylacetamide solution and (2) preparation of magnetic PMDA modified biomass by a situ co-precipitation method under the assistance of ultrasound irradiation in ammonia water. The adsorption potential of the as-prepared magnetic modified biomass was analyzed by using cationic dyes: methylene blue and basic magenta as model dyes. Optical micrograph and x-ray diffraction analyses showed that Fe(3)O(4) particles were precipitated on the modified biomass surface. The as-prepared biosorbent could be recycled easily by using an applied magnetic field. Titration analysis showed that the total concentration of the functional groups on the magnetic PMDA modified biomass was calculated to be 0.75 mmol g(-1) by using the first derivative method. The adsorption capacities (q(m)) of the magnetic PMDA modified biomass for methylene blue and basic magenta were 609.0 and 520.9 mg g(-1), respectively, according to the Langmuir equation. Kinetics experiment showed that adsorption could be completed within 150 min for both dyes. The desorption experiment showed that the magnetic sorbent could be used repeatedly after regeneration. The as-prepared magnetic modified sorbent had a potential in the dyeing industry wastewater treatment.

  6. Method for determining the three-dimensional structure of a protein

    NASA Technical Reports Server (NTRS)

    Morrison, Dennis R. (Inventor); Mosier, Benjamin (Inventor)

    2004-01-01

    Microcapsules prepared by encapsulating an aqueous solution of a protein, drug or other bioactive substance inside a semi-permeable membrane by are disclosed. The microcapsules are formed by interfacial coacervation under conditions where the shear forces are limited to 0-100 dynes/cm.sup.2 at the interface. By placing the microcapsules in a high osmotic dewatering solution, the protein solution is gradually made saturated and then supersaturated, and the controlled nucleation and crystallization of the protein is achieved. The crystal-filled microcapsules prepared by this method can be conveniently harvested and stored while keeping the encapsulated crystals in essentially pristine condition due to the rugged, protective membrane. Because the membrane components themselves are x-ray transparent, large crystal-containing microcapsules can be individually selected, mounted in x-ray capillary tubes and subjected to high energy x-ray diffraction studies to determine the 3-D structure of the protein molecules. Certain embodiments of the microcapsules of the invention have composite polymeric outer membranes which are somewhat elastic, water insoluble, permeable only to water, salts, and low molecular weight molecules and are structurally stable in fluid shear forces typically encountered in the human vascular system.

  7. Quantitative Detection of Trace Explosive Vapors by Programmed Temperature Desorption Gas Chromatography-Electron Capture Detector

    PubMed Central

    Field, Christopher R.; Lubrano, Adam; Woytowitz, Morgan; Giordano, Braden C.; Rose-Pehrsson, Susan L.

    2014-01-01

    The direct liquid deposition of solution standards onto sorbent-filled thermal desorption tubes is used for the quantitative analysis of trace explosive vapor samples. The direct liquid deposition method yields a higher fidelity between the analysis of vapor samples and the analysis of solution standards than using separate injection methods for vapors and solutions, i.e., samples collected on vapor collection tubes and standards prepared in solution vials. Additionally, the method can account for instrumentation losses, which makes it ideal for minimizing variability and quantitative trace chemical detection. Gas chromatography with an electron capture detector is an instrumentation configuration sensitive to nitro-energetics, such as TNT and RDX, due to their relatively high electron affinity. However, vapor quantitation of these compounds is difficult without viable vapor standards. Thus, we eliminate the requirement for vapor standards by combining the sensitivity of the instrumentation with a direct liquid deposition protocol to analyze trace explosive vapor samples. PMID:25145416

  8. Quantitative detection of trace explosive vapors by programmed temperature desorption gas chromatography-electron capture detector.

    PubMed

    Field, Christopher R; Lubrano, Adam; Woytowitz, Morgan; Giordano, Braden C; Rose-Pehrsson, Susan L

    2014-07-25

    The direct liquid deposition of solution standards onto sorbent-filled thermal desorption tubes is used for the quantitative analysis of trace explosive vapor samples. The direct liquid deposition method yields a higher fidelity between the analysis of vapor samples and the analysis of solution standards than using separate injection methods for vapors and solutions, i.e., samples collected on vapor collection tubes and standards prepared in solution vials. Additionally, the method can account for instrumentation losses, which makes it ideal for minimizing variability and quantitative trace chemical detection. Gas chromatography with an electron capture detector is an instrumentation configuration sensitive to nitro-energetics, such as TNT and RDX, due to their relatively high electron affinity. However, vapor quantitation of these compounds is difficult without viable vapor standards. Thus, we eliminate the requirement for vapor standards by combining the sensitivity of the instrumentation with a direct liquid deposition protocol to analyze trace explosive vapor samples.

  9. Structural and Spectral Characterization of Co2+- and Ni2+-DOPED CdO Powder Prepared From Solution at Room Temperature

    NASA Astrophysics Data System (ADS)

    Reddy, C. V.; Rao, L. V. Krishna; Satish, D. V.; Shim, J.; Ravikumar, R. V. S. S. N.

    2015-11-01

    The mild and simple solution method was used for the synthesis of Co2+- and Ni2+-doped CdO powders at room temperature. The prepared powders were characterized using powder X-ray diffraction, scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS), optical absorption, and Fourier transform infrared spectroscopy (FTIR). From the powder X-ray diffraction patterns, it has been observed that the prepared Co2+ and Ni2+ ion-doped CdO powders belong to the cubic phase, and the evaluated average crystalline sizes of the powders are 20 and 14 nm, respectively. The SEM images and the EDS spectra show that the prepared powders are distributed over different sizes in the grain boundaries. Optical absorption studies allow determination of site symmetry of the metal ion with its ligands. The crystal field (Dq) and inter-electronic repulsion (B and C) parameters have been evaluated from the optical absorption spectra. The FTIR spectra show the characteristic fundamental vibrations of the metal oxide and CdO.

  10. Fabrication of a novel superhydrophobic and superoleophilic surface by one-step electrodeposition method for continuous oil/water separation

    NASA Astrophysics Data System (ADS)

    Xiang, Meisu; Jiang, Meihuizi; Zhang, Yanzong; Liu, Yan; Shen, Fei; Yang, Gang; He, Yan; Wang, Lilin; Zhang, Xiaohong; Deng, Shihuai

    2018-03-01

    A novel superhydrophobic and superoleophilic surface was fabricated by one-step electrodeposition on stainless steel meshes, and the durability and oil/water separation properties were assessed. Field emission scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), fourier transform infrared spectroscopy (FT-IR) and optical contact angle measurements were used to characterize surface morphologies, chemical compositions, and wettabilities, respectively. The results indicated that the as-prepared mesh preformed excellent superhydrophobicity and superoleophilicity with a high water contact angle (WCA) of 162 ± 1° and oil contact angle of (OCA) 0°. Meanwhile, the as-prepared mesh also exhibited continuous separation capacity of many kinds of oil/water mixtures, and the separation efficiency for lubrication oil/water mixture was about 98.6%. In addition, after 10 separation cycles, the as-prepared mesh possessed the WCAs of 155 ± 2°, the OCAs of 0° and the separation efficiency of 97.8% for lubrication oil/water mixtures. The as-prepared mesh also retained superhydrophobic and superoleophilic properties after abrading, immersing in salt solutions and different pH solutions.

  11. Preparation and validation of gross alpha/beta samples used in EML`s quality assessment program

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

    Scarpitta, S.C.

    1997-10-01

    A set of water and filter samples have been incorporated into the existing Environmental Measurements Laboratory`s (EML) Quality Assessment Program (QAP) for gross alpha/beta determinations by participating DOE laboratories. The participating laboratories are evaluated by comparing their results with the EML value. The preferred EML method for measuring water and filter samples, described in this report, uses gas flow proportional counters with 2 in. detectors. Procedures for sample preparation, quality control and instrument calibration are presented. Liquid scintillation (LS) counting is an alternative technique that is suitable for quantifying both the alpha ({sup 241}Am, {sup 230}Th and {sup 238}Pu) andmore » beta ({sup 90}Sr/{sup 90}Y) activity concentrations in the solutions used to prepare the QAP water and air filter samples. Three LS counting techniques (Cerenkov, dual dpm and full spectrum analysis) are compared. These techniques may be used to validate the activity concentrations of each component in the alpha/beta solution before the QAP samples are actually prepared.« less

  12. Large scale synthesis of nanostructured zirconia-based compounds from freeze-dried precursors

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

    Gomez, A.; Villanueva, R.; Vie, D.

    2013-01-15

    Nanocrystalline zirconia powders have been obtained at the multigram scale by thermal decomposition of precursors resulting from the freeze-drying of aqueous acetic solutions. This technique has equally made possible to synthesize a variety of nanostructured yttria or scandia doped zirconia compositions. SEM images, as well as the analysis of the XRD patterns, show the nanoparticulated character of those solids obtained at low temperature, with typical particle size in the 10-15 nm range when prepared at 673 K. The presence of the monoclinic, the tetragonal or both phases depends on the temperature of the thermal treatment, the doping concentration and themore » nature of the dopant. In addition, Rietveld refinement of the XRD profiles of selected samples allows detecting the coexistence of the tetragonal and the cubic phases for high doping concentration and high thermal treatment temperatures. Raman experiments suggest the presence of both phases also at relatively low treatment temperatures. - Graphical abstract: Zr{sub 1-x}A{sub x}O{sub 2-x/2} (A=Y, Sc; 0{<=}x{<=}0.12) solid solutions have been prepared as nanostructured powders by thermal decomposition of precursors obtained by freeze-drying, and this synthetic procedure has been scaled up to the 100 g scale. Highlights: Black-Right-Pointing-Pointer Zr{sub 1-x}A{sub x}O{sub 2-x/2} (A=Y, Sc; 0{<=}x{<=}0.12) solid solutions have been prepared as nanostructured powders. Black-Right-Pointing-Pointer The synthetic method involves the thermal decomposition of precursors obtained by freeze-drying. Black-Right-Pointing-Pointer The temperature of the thermal treatment controls particle sizes. Black-Right-Pointing-Pointer The preparation procedure has been scaled up to the 100 g scale. Black-Right-Pointing-Pointer This method is appropriate for the large-scale industrial preparation of multimetallic systems.« less

  13. Stability of a novel corticosteroid nasal irrigation solution: betamethasone 17-valerate added to extemporaneously prepared nasal irrigation solutions.

    PubMed

    Ong, Kheng Yong; Lim, Wei Ching; Ooi, Shing Ming; Loh, Zhi Hui; Kong, Ming Chai; Chan, Lai Wah; Heng, Paul Wan Sia

    2017-05-01

    There are no commercially available nasal irrigation solutions containing corticosteroids. Instead, such preparations are extemporaneously prepared by adding existing corticosteroid formulations to nasal irrigation solutions. The stability of the corticosteroid betamethasone 17-valerate (B17V), in nasal irrigation solutions of different compositions and pH and stored under different temperatures, was studied to determine the optimal choice of solution and storage conditions. Triplicate extemporaneous preparations made with B17V were prepared by adding a predetermined volume of B17V lotion to each nasal irrigation solution: normal saline (NS), sodium bicarbonate (NaHCO 3 ) powder dissolved in tap water, and a commercially available powder mixture (FLO Sinus Care Powder), dissolved in tap water or pre-boiled tap water. Preparations were stored at 30°C and 4°C. Sampling was carried out at 0, 1, 2, 6, and 24 hours. The concentrations of B17V and its degradation compound, betamethasone 21-valerate (B21V), were determined by high-performance liquid chromatography. Preparations stored at 30°C contained a lower amount of B17V and higher amount of B21V than those stored at 4°C. B17V stability in nasal irrigation solutions decreased in the following order: NS, FLO in fresh tap water, FLO in pre-boiled tap water, and NaHCO 3 . The degradation rate of B17V increased with higher storage temperature and higher pH. B17V is most stable when added to NS and least stable in NaHCO 3 solution. FLO solution prepared with either cooled boiled water or tap water is an alternative if administered immediately. Storage at 4°C can better preserve stability of B17V, over a period of 24 hours. © 2017 ARS-AAOA, LLC.

  14. Refractive index-based determination of detergent concentration and its application to the study of membrane proteins

    PubMed Central

    Strop, Pavel; Brunger, Axel T.

    2005-01-01

    The concentration of detergent in membrane protein preparations can have a critical role on protein stability, function, and the potential for crystallization. Unfortunately, dialysis or protein concentration can lead to an unknown amount of detergent in the final membrane protein preparations. Here we present a method for the determination of detergent concentration based on refractive index of the detergent solution. This method was applied to quantitate the amount of detergent remaining in solution after concentration in various concentrators. We found that the ability of the tested detergents to pass through the molecular weight cutoff membrane correlates well with detergent micelle size. Therefore, the micelle size can be used as a rough guide to estimate the retention of a given detergent in various molecular weight cutoff concentrators. The refractive index method is exceptionally informative when coupled with size exclusion chromatography and light scattering, and can be used to determine the oligomeric state of the membrane protein, the size of a protein-associated micelle, as well as the amount and size of the unbound detergent micelle. PMID:16046633

  15. Refractive index-based determination of detergent concentration and its application to the study of membrane proteins.

    PubMed

    Strop, Pavel; Brunger, Axel T

    2005-08-01

    The concentration of detergent in membrane protein preparations can have a critical role on protein stability, function, and the potential for crystallization. Unfortunately, dialysis or protein concentration can lead to an unknown amount of detergent in the final membrane protein preparations. Here we present a method for the determination of detergent concentration based on refractive index of the detergent solution. This method was applied to quantitate the amount of detergent remaining in solution after concentration in various concentrators. We found that the ability of the tested detergents to pass through the molecular weight cutoff membrane correlates well with detergent micelle size. Therefore, the micelle size can be used as a rough guide to estimate the retention of a given detergent in various molecular weight cutoff concentrators. The refractive index method is exceptionally informative when coupled with size exclusion chromatography and light scattering, and can be used to determine the oligomeric state of the membrane protein, the size of a protein-associated micelle, as well as the amount and size of the unbound detergent micelle.

  16. Solution based approach for the fabrication of photonic devices in chalcogenide glasses

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

    Prince,, E-mail: princevish2@gmail.com; Raman, Swati; Dwivedi, Prabhat K.

    2015-06-24

    In this report, we describe the solution preparation conditions of various chalcogenide glasses. The dissolution mechanism of (As{sub 2}S{sub 3}){sub 60}Ge{sub 40}, (As{sub 2}S{sub 3}){sub 60}Se{sub 40} in ethanolamine is studied. Dynamic light scattering (DLS)measurements confirms that the particles in suspension are <10 nm in all the solutions.Prepared solutions are shown to possess similar molecular structure to the parent bulk glasses. Optical properties of the prepared solution are also discussed.

  17. Evaluation of the flow properties of xanthan gum solution

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

    Duda, J.L.; Klaus, E.E.; Leung, W.C.

    1981-02-01

    In this study, the solution properties of two forms of xanthan gum, a powder and a broth, which are commercially available were evaluated. As previous studies have shown, the solutions prepared from the broth do exhibit better injectivity properties. However, this investigation also shows that other properties of these solutions are not equivalent. In its natural state, xanthane gum exists as a multistranded helix. This ordered confirmation can be destroyed and in a denatured state, the xanthan gum exhibits a more random configuration and consequently higher viscosity. One of the major conclusions of this study is that the xanthan powdermore » is partially denatured when compared to the xanthan molecules which exist in the broth. This denaturing may occur during the drying process in which the xanthan solids are removed from the broth. Solutions prepared from the broth in the absence of the added salt show a transition in the viscosity-temperature relationship at approximately 40 to 50/sup 0/C. This is consistent with the behavior of native xanthan gum solutions. At approximately 50/sup 0/C, the molecules in solution go into a more random state and consequently, an abrupt rise in the viscosity is observed. However, solutions prepared from the polymer powder do not show any evidence of such a transition. The solutions prepared from the broth can be thermally denatured, and this denaturing results in viscosities which are equivalent to the viscosities realized with the powdered polymer. Before denaturing, the broth solution showed a lower viscosity. Further, intrinsic viscosity measurements indicate that the hydrodynamic volume of the polymer solutions prepared from the borth are smaller than the hydrodynamic volumes of solutions prepared from the powder.« less

  18. Protoplasts Obtained from Candida tropicalis Grown on Alkanes

    PubMed Central

    Lebeault, J. M.; Roche, B.; Duvnjak, Z.; Azoulay, E.

    1969-01-01

    A method for the preparation of protoplasts from Candida tropicalis cultivated on n-tetradecane is described. This essentially consists of replacing the mannitol-sorbitol solution of the classical helicase technique by 1 m magnesium sulfate and lowering the pH to 4.1 during incubation in the presence of helicase. The protoplasts thus prepared behave like intact cells and are capable of consuming oxygen in the presence of n-tetradecane, n-decane, 1-decanol, and glucose. Images PMID:5361212

  19. Formulation, Characterization and Physicochemical Evaluation of Potassium Citrate Effervescent Tablets

    PubMed Central

    Aslani, Abolfazl; Fattahi, Fatemeh

    2013-01-01

    Purpose: The aim of this study was to design and formulation of potassium citrate effervescent tablet for reduction of calcium oxalate and urate kidney stones in patients suffering from kidney stones. Methods: In this study, 13 formulations were prepared from potassium citrate and effervescent base in different concentration. The flowability of powders and granules was studied. Then effervescent tablets were prepared by direct compression, fusion and wet granulation methods. The prepared tablets were evaluated for hardness, friability, effervescent time, pH, content uniformity. To amend taste of formulations, different flavoring agents were used and then panel test was done by using Latin Square method by 30 volunteers. Results: Formulations obtained from direct compression and fusion methods had good flow but low hardness. Wet granulation improves flowability and other physicochemical properties such as acceptable hardness, effervescence time ≤3 minutes, pH<6, friability < 1%, water percentage < 0.5% and accurate content uniformity. In panel test, both of combination flavors; (orange - lemon) and (strawberry - raspberry) had good acceptability. Conclusion: The prepared tablets by wet granulation method using PVP solution had more tablet hardness. It is a reproducible process and suitable to produce granules that are compressed into effervescent tablets due to larger agglomerates. PMID:24312839

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

    Ma, Xi; Blue Sky Technology Corporation, Beijing 100083; Ma, Hongwen, E-mail: mahw@cugb.edu.cn

    Highlights: • We use the anti-drop precipitation method for synthesis of magnesium hydroxide. • Boron mud which is solid waste from a borax factory is used as the magnesium source. • The magnesium hydroxide nanoflowers are prepared in a short time. • The as-prepared magnesium hydroxide can be used as an effective flame retardant. - Abstract: Using boron mud as the starting material, the flower-like magnesium hydroxide (MH) has been successfully prepared via anti-drop precipitation method. The effect of NH{sub 3}·H{sub 2}O concentration, aging time, and surfactant on the morphology of MH was investigated. The optimum precipitation conditions are droppingmore » MgSO{sub 4} solution in 5% NH{sub 3}·H{sub 2}O solution, with 3% polyethylene glycol as surfactant, aging for 30 min. XRD, SEM, FI-IR, and TG/DTA have been employed to characterize the as-prepared samples. XRD reveals that MH with high purity has the brucite structure. SEM images show that the flower-like MH exists in the form of mono-disperse well uniform spherical aggregation with diameter of 3–5 μm. TG/DTA shows a total percentage of weight loss 33.6% with a well-defined endothermic peak near 381.3 °C corresponding to the decomposition of MH. Furthermore, it reports that the extremely fast primary nucleation is of significance for crystal growth of MH.« less

  1. Characterization of film-forming solutions and films incorporating free and nanoencapsulated tea polyphenol prepared by gelatins with different Bloom values

    USDA-ARS?s Scientific Manuscript database

    Gelatin film-forming solutions and their films incorporating tea polyphenol (TP) and chitosan nanoparticles (CSNs) were prepared from gelatins with different Bloom values (100, 150 and 225). Blank gelatin film-forming solutions and films were prepared as controls. Gelatins with higher Bloom values h...

  2. Oromucosal film preparations: points to consider for patient centricity and manufacturing processes.

    PubMed

    Krampe, Raphael; Visser, J Carolina; Frijlink, Henderik W; Breitkreutz, Jörg; Woerdenbag, Herman J; Preis, Maren

    2016-01-01

    According to the European Pharmacopoeia, oromucosal films comprise mucoadhesive buccal films and orodispersible films. Both oral dosage forms receive considerable interest in the recent years as commercially available pharmaceutical products and as small scale personalized extemporaneous preparations. In this review, technological issues such as viscosity of the casting liquid, mechanical properties of the film, upscaling and the stability of the casting solution and produced films will be discussed. Furthermore, patient-related problems like appearance, mucosal irritation, taste, drug load, safety and biopharmaceutics are described. Current knowledge and directions for solutions are summarized. The viscosity of the casting solution is a key factor for producing suitable films. This parameter is amongst others dependent on the polymer and active pharmaceutical ingredient, and the further excipients that are used. For optimal patient compliance, an acceptable taste and palatability are desirable. Safe and inert excipients should be used and appropriate packaging should be provided to produced films. Absorption through the oral mucosa will vary for each active compound, formulation and patient, which gives rise to pharmacokinetic questions. Finally, the European Pharmacopoeia needs to specify methods, requirement and definitions for oromucosal film preparations based on bio-relevant data.

  3. Aqueous Plasma Pharmacy: Preparation Methods, Chemistry, and Therapeutic Applications

    PubMed Central

    Joslin, Jessica M.; McCall, James R.; Bzdek, Justin P.; Johnson, Derek C.; Hybertson, Brooks M.

    2017-01-01

    Plasma pharmacy is a subset of the broader field of plasma medicine. Although not strictly defined, the term aqueous plasma pharmacy (APP) is used to refer to the generation and distribution of reactive plasma-generated species in an aqueous solution followed by subsequent administration for therapeutic benefits. APP attempts to harness the therapeutic effects of plasma-generated oxidant species within aqueous solution in various applications, such as disinfectant solutions, cell proliferation related to wound healing, and cancer treatment. The subsequent use of plasma-generated solutions in the APP approach facilitates the delivery of reactive plasma species to internal locations within the body. Although significant efforts in the field of plasma medicine have concentrated on employing direct plasma plume exposure to cells or tissues, here we focus specifically on plasma discharge in aqueous solution to render the solution biologically active for subsequent application. Methods of plasma discharge in solution are reviewed, along with aqueous plasma chemistry and the applications for APP. The future of the field also is discussed regarding necessary research efforts that will enable commercialization for clinical deployment. PMID:28428835

  4. Thermal Conductivity of a Nanoscale Yttrium Iron Garnet Thin-Film Prepared by the Sol-Gel Process

    PubMed Central

    2017-01-01

    The thermal conductivity of a nanoscale yttrium iron garnet (Y3Fe5O12, YIG) thin-film prepared by a sol-gel method was evaluated using the ultrafast pump-probe technique in the present study. The thermoreflectance change on the surface of a 250 nm thick YIG film, induced by the irradiation of femtosecond laser pulses, was measured, and curve fitting of a numerical solution for the transient heat conduction equation to the experimental data was performed using the finite difference method in order to extract the thermal property. Results show that the film’s thermal conductivity is 22–83% higher than the properties of bulk YIG materials prepared by different fabrication techniques, reflecting the microstructural characteristics and quality of the film. PMID:28858249

  5. Analysis and comparison of methods for the preparation of domestic hot water from district heating system, selected renewable and non-renewable sources in low-energy buildings

    NASA Astrophysics Data System (ADS)

    Knapik, Maciej

    2018-02-01

    The article presents an economic analysis and comparison of selected (district heating, natural gas, heat pump with renewable energy sources) methods for the preparation of domestic hot water in a building with low energy demand. In buildings of this type increased demand of energy for domestic hot water preparation in relation to the total energy demand can be observed. As a result, the proposed solutions allow to further lower energy demand by using the renewable energy sources. This article presents the results of numerical analysis and calculations performed mainly in MATLAB software, based on typical meteorological years. The results showed that system with heat pump and renewable energy sources Is comparable with district heating system.

  6. Method for the preparation of high surface area high permeability carbons

    DOEpatents

    Lagasse, R.R.; Schroeder, J.L.

    1999-05-11

    A method for preparing carbon materials having high surface area and high macropore volume to provide high permeability. These carbon materials are prepared by dissolving a carbonizable polymer precursor, in a solvent. The solution is cooled to form a gel. The solvent is extracted from the gel by employing a non-solvent for the polymer. The non-solvent is removed by critical point drying in CO{sub 2} at an elevated pressure and temperature or evaporation in a vacuum oven. The dried product is heated in an inert atmosphere in a first heating step to a first temperature and maintained there for a time sufficient to substantially cross-link the polymer material. The cross-linked polymer material is then carbonized in an inert atmosphere. 3 figs.

  7. Fabrication of Controllable Pore and Particle Size of Mesoporous Silica Nanoparticles via a Liquid-phase Synthesis Method and Its Absorption Characteristics

    NASA Astrophysics Data System (ADS)

    Nandiyanto, Asep Bayu Dani; Iskandar, Ferry; Okuyama, Kikuo

    2011-12-01

    Monodisperse spherical mesoporous silica nanoparticles were successfully synthesized using a liquid-phase synthesis method. The result showed particles with controllable pore size from several to tens nanometers with outer diameter of several tens nanometers. The ability in the control of pore size and outer diameter was altered by adjusting the precursor solution ratios. In addition, we have conducted the adsorption ability of the prepared particles. The result showed that large organic molecules were well-absorbed to the prepared silica porous particles, in which this result was not obtained when using commercial dense silica particle and/or hollow silica particle. With this result, the prepared mesoporous silica particles may be used efficiently in various applications, such as sensors, pharmaceuticals, environmentally sensitive pursuits, etc.

  8. Characterization of Non-Newtonian Fluids for Environmental Applications

    NASA Astrophysics Data System (ADS)

    Espinoza, I.; Hauswirth, S.; Cerda, C. C.; Sadeghi, S.

    2017-12-01

    Non-Newtonian fluids are fluids that exhibit viscosity changes with time, stress, or changing shear rates. This distinctive quality is advantageous to a number of applications, such as hydraulic fracturing and contaminant remediation. The use of non-Newtonian fluids in contaminant remediation has recently increased as a method of improving delivery of chemical oxidants and surfactants in hard-to-reach, low permeability zones within the subsurface. As the application of these fluids continues to increase, a need to improve upon the basic understanding of non-Newtonian fluid rheology becomes increasingly important. This study investigates the characteristics of guar gum and xanthan gum, two common non-Newtonian polymers, and how factors such as composition, preparation method, and chemical and biological degradation impact the rheology of the fluids. Because the polymers are semi-hydrophobic, preparation of solutions requires blending, heating, pre-dissolution in alcohol, addition of surfactant, or stirring for extended time periods. Additionally, fluids are commonly filtered to remove undissolved material and gels, and subsequently stored under a variety of conditions. We investigated the effect of these processes on the fluids' rheology by producing solutions at a range of concentrations with a variety of preparation and storage methods. The rheological properties of the solutions were then measured over a period of months with a rotational rheometer. The experimental data were fit to standard rheological models, and the parameters of these models were used to quantitatively assess the effect of chemical composition, physical processing, and storage on the fluid rheology. The results of this study provide an improved basis with which to predict physical, chemical, and temporal alterations of guar and xanthan gum rheology, and thereby allow for improved design of experimental, modeling, and field applications utilizing non-Newtonian fluids.

  9. Synergetic analgesic effect of the combination of arnica and hydroxyethyl salicylate in ethanolic solution following cutaneous application by transcutaneous electrostimulation.

    PubMed

    Kucera, Miroslav; Horácek, Ondrej; Kálal, Jan; Kolár, Pavel; Korbelar, Peter; Polesná, Zora

    2003-01-01

    A combination of the active agents arnica and hydroxyethyl salicylate (HES) in ethanolic solution (Sportino Acute Spray) is cutaneously applied for the treatment of sports injuries and diseases of the locomotor apparatus. The aim was to examine the efficacy and synergism of the single substances and the combination with regard to the analgesic effect after cutaneous application as well as to validate the method of transcutaneous electronic stimulation as a method of measuring the analgesic effect. In the present article, the method of transcutaneous electrostimulation was used in a randomized, controlled, single-blind trial on healthy volunteers to provide objective evidence that the combination of active agents displays a significantly greater analgesic effect than the individual active agents. Thus there is synergy between the active agents arnica and hydroxyethyl salicylate in the combination preparation. In addition, the effect of the vehicle ethanol and the reference substance water could be determined within the framework of these comparative experiments and the difference between the combination preparation and the individual substances arnica and HES could be shown. The method of transcutaneous electrostimulation used for the objective measurement of the analgesic effect was validated.

  10. Fabrication of Cu2SnS3 thin films by ethanol-ammonium solution process by doctor-blade technique

    NASA Astrophysics Data System (ADS)

    Wang, Yaguang; Li, Jianmin; Xue, Cong; Zhang, Yan; Jiang, Guoshun; Liu, Weifeng; Zhu, Changfei

    2017-11-01

    In the present study, a low-cost and simple method is applied to fabricate Cu2SnS3 (CTS) thin films. Namely CTS thin films are prepared by a doctor-blade method with a slurry dissolving the Cu2O and SnS powders obtained from CBD reaction solution into ethanol-ammonium solvents. Series of characterization methods including XRD, Raman spectra, SEM and UV-Vis analyses are introduced to investigate the phase structure, morphology and optical properties of CTS thin films. As a result, monoclinic CTS films have been obtained with the disappearance of binary phases CuS and SnS2 while increasing the annealing temperature and time, high quality monoclinic CTS thin films consisting of compact and large grains have been successfully prepared by this ethanol-ammonium method. Moreover, the secondary phase Cu2Sn3S7 is also observed during the annealing process. In addition, the post-annealed CTS film with a band-gap about 0.89 eV shows excellent absorbance between 400 and 1200 nm, which is proper for the bottom layer in multi-junction thin film solar cells.[Figure not available: see fulltext.

  11. The influence of the use of viscosifying agents as dispersion media on the drug release properties from PLGA nanoparticles.

    PubMed

    Dillen, Kathleen; Weyenberg, Wim; Vandervoort, Jo; Ludwig, Annick

    2004-11-01

    Poly(lactide-co-glycolide) nanoparticles incorporating ciprofloxacin HCl were prepared by means of a W/O/W emulsification solvent evaporation method. The physicochemical properties of these particles were evaluated by measuring particle size, zeta potential and drug loading efficiency. Gamma-sterilised nanoparticles were dispersed in different isoviscous polymer solutions, commonly used as vehicles in eye drops. The influence of gamma-irradiation of the viscosifying agents on the drug release properties of the dispersed nanoparticles was evaluated with respect to release in mannitol solution. The viscosity of the polymer solutions prepared was measured by flow rheometry and thereby the influence of temperature and sterilisation by autoclaving on viscosity was examined. Before and after freeze-drying and subsequent sterilisation by gamma-irradiation, the polymer solutions were also characterised by dynamic stress sweep and dynamic frequency sweep oscillation measurements to deduce possible structural changes. A possible relationship between the differences in ciprofloxacin release from the nanoparticles suspended in the various media and the network structure or rheological behaviour of the polymers was investigated.

  12. A novel pretreatment method combining sealing technique with direct injection technique applied for improving biosafety.

    PubMed

    Wang, Xinyu; Gao, Jing-Lin; Du, Chaohui; An, Jing; Li, MengJiao; Ma, Haiyan; Zhang, Lina; Jiang, Ye

    2017-01-01

    People today have a stronger interest in the risk of biosafety in clinical bioanalysis. A safe, simple, effective method of preparation is needed urgently. To improve biosafety of clinical analysis, we used antiviral drugs of adefovir and tenofovir as model drugs and developed a safe pretreatment method combining sealing technique with direct injection technique. The inter- and intraday precision (RSD %) of the method were <4%, and the extraction recoveries ranged from 99.4 to 100.7%. Meanwhile, the results showed that standard solution could be used to prepare calibration curve instead of spiking plasma, acquiring more accuracy result. Compared with traditional methods, the novel method not only improved biosecurity of the pretreatment method significantly, but also achieved several advantages including higher precision, favorable sensitivity and satisfactory recovery. With these highly practical and desirable characteristics, the novel method may become a feasible platform in bioanalysis.

  13. Stability of extemporaneously prepared preservative-free prochlorperazine nasal spray.

    PubMed

    Yellepeddi, Venkata K

    2018-01-01

    The stability of an extemporaneously prepared preservative-free prochlorperazine 5-mg/mL nasal spray was evaluated. The preservative-free prochlorperazine nasal spray was prepared by adding 250 mg of prochlorperazine edisylate to 50 mL of citrate buffer in a low-density polyethylene nasal spray bottle. A stability-indicating high-performance liquid chromatography (HPLC) method was developed and validated using the major degradant prochlorperazine sulfoxide and by performing forced-degradation studies. For chemical stability studies, 3 100-μL samples of the preservative-free prochlorperazine from 5 nasal spray bottles stored at room temperature were collected at days 0, 20, 30, 45, and 60 and were assayed in triplicate using the stability-indicating HPLC method. Microbiological testing involved antimicrobial effectiveness testing based on United States Pharmacopeia ( USP ) chapter 51 and quantitative microbiological enumeration of aerobic bacteria, yeasts, and mold based on USP chapter 61. Samples for microbiological testing were collected at days 0, 30, and 60. The stability-indicating HPLC method clearly identified the degradation product prochlorperazine sulfoxide without interference from prochlorperazine. All tested solutions retained over 90% of the initial prochlorperazine concentration for the 60-day study period. There were no detectable changes in color, pH, and viscosity in any sample. There was no growth of bacteria, yeast, and mold for 60 days in all samples tested. An extemporaneously prepared preservative-free nasal spray solution of prochlorperazine edisylate 5 mg/mL was physically, chemically, and microbiologically stable for 60 days when stored at room temperature in low-density polyethylene bottles. Copyright © 2018 by the American Society of Health-System Pharmacists, Inc. All rights reserved.

  14. A Simplified Extemporaneously Prepared Potassium Chloride Oral Solution.

    PubMed

    Tannous, Elias; Tal, Yana; Amarny, Kamal

    2016-01-01

    Although commercial preparations of oral potassium supplements are usually available, there are times when our Medical Center is faced with situations in which the oral solution of potassium chloride is not available. This solution is necessary for our pediatric outpatients who cannot swallow tablets and need an oral solution. Moreover, there are no studies available which describe an extemporaneously prepared potassium chloride oral solution on which we can rely for assigning a beyond-use date. The aim of this study was to formulate an extemporaneous pediatric oral solution of potassium chloride and to determine the physical and chemical stability of this preparation. We prepared 1 mMoL/mL by withdrawing 25 mL of potassium chloride 14.9%. Ora-Sweet SF was added to 50 mL in a metered flask. The solution was kept refrigerated (2°C to 8°C). Samples were withdrawn to measure potassium concentration, pH, and microbial overgrowth. The test was performed by our biochemical laboratory. The oral solution of potassium chloride 1 mMoL/mL stored at 2°C to 8°C maintained at least 91% of the initial concentration for 28 days. There were no notable changes in pH, and the solution remained physically stable with no visual microbial growth. The oral solution of potassium chloride 1 mMoL/mL prepared in Ora-Sweet and stored at 2°C to 8°C in amber glass bottles is expected to remain stable for 28 days. Copyright© by International Journal of Pharmaceutical Compounding, Inc.

  15. METHOD OF PREPARING PROTACTINIUM VALUES

    DOEpatents

    Katzin, L.I.; Larson, R.G.; Thompson, R.C.; Van Winkle, Q.

    1959-05-19

    Separation and purification from initial acid leaches of pitchblende of Pa is described. This supernatant acid solution is treated with alkali metal carbonates to precipitate Pa. Silica is removed from the precipitate by hydroxide treatment. The Pa residue is dissolved in HNO/sub 3/ and Pa is concentrated by cyclic precipitations with MnO/sub 2/. The last solution is hydrolyzed to precipitate Pa. The Pa precipitate contains Ti and Zr which are removed by ion exchange. (T.R.H.)

  16. Directed spatial organization of zinc oxide nanostructures

    DOEpatents

    Hsu, Julia [Albuquerque, NM; Liu, Jun [Richland, WA

    2009-02-17

    A method for controllably forming zinc oxide nanostructures on a surface via an organic template, which is formed using a stamp prepared from pre-defined relief structures, inking the stamp with a solution comprising self-assembled monolayer (SAM) molecules, contacting the stamp to the surface, such as Ag sputtered on Si, and immersing the surface with the patterned SAM molecules with a zinc-containing solution with pH control to form zinc oxide nanostructures on the bare Ag surface.

  17. Human serum albumin crystals and method of preparation

    NASA Technical Reports Server (NTRS)

    Carter, Daniel C. (Inventor)

    1989-01-01

    Human serum albumin (HSA) crystals are provided in the form of tetragonal plates having the space groups P42(sub 1)2, the crystals being grown to sizes in excess of 0.5 mm in two dimensions and a thickness of 0.1 mm. Growth of the crystals is carried out by a hanging drop method wherein a precipitant solution containing polyethylene glycol (PEG) and a phosphate buffer is mixed with an HSA solution, and a droplet of mixed solution is suspended over a well of precipitant solution. Crystals grow to the desired size in 3 to 7 days. Concentration of reagents, pH and other parameters are controlled within prescribed limits. The resulting crystals exhibit a size and quality such as to allow performance of x ray diffraction studies and enable the conduct of drug binding studies as well as genetic engineering studies.

  18. Method of determining the extent to which a nickel structure has been attached by a fluorine-containing gas

    DOEpatents

    Brusie, James P.

    2004-07-13

    The method of determining the extent to which a nickel structure has been attacked by a halogen containing gas to which it has been exposed which comprises preparing a quantity of water substantially free from dissolved oxygen, passing ammonia gas through a cuprammonium solution to produce ammonia substantially free from oxygen, dissolving said oxygen-free ammonia in said water to produce a saturated aqueous ammonia solution free from uncombined oxygen, treating at least a portion of said nickel structure of predetermined weight with said solution to dissolve nickel compounds from the surface of said structure without dissolving an appreciable amount of said nickel and analyzing the resulting solution to determine the quantity of said nickel compounds that was associated with said said portion of said structure to determine the proportion of combined nickel in said nickel structure.

  19. On particle track detectors

    NASA Technical Reports Server (NTRS)

    Benton, E. V.; Gruhn, T. A.; Andrus, C. H.

    1973-01-01

    Aqueous sodium hydroxide is widely used to develop charged particle tracks in polycarbonate film, particularly Lexan. The chemical nature of the etching process for this system has been determined. A method employing ultra-violet absorbance was developed for monitoring the concentration of the etch products in solution. Using this method it was possible to study the formation of the etching solution saturated in etch products. It was found that the system super-saturates to a significant extent before precipitation occurs. It was also learned that the system approaches its equilibrium state rather slowly. It is felt that both these phenomena may be due to the presence of surfactant in the solution. In light of these findings, suggestions are given regarding the preparation and maintenance of the saturated etch solution. Two additional research projects, involving automated techniques for particle track analysis and particle identification using AgCl crystals, are briefly summarized.

  20. Anodic Oxidation of Etodolac and its Linear Sweep, Square Wave and Differential Pulse Voltammetric Determination in Pharmaceuticals

    PubMed Central

    Yilmaz, B.; Kaban, S.; Akcay, B. K.

    2015-01-01

    In this study, simple, fast and reliable cyclic voltammetry, linear sweep voltammetry, square wave voltammetry and differential pulse voltammetry methods were developed and validated for determination of etodolac in pharmaceutical preparations. The proposed methods were based on electrochemical oxidation of etodolac at platinum electrode in acetonitrile solution containing 0.1 M lithium perchlorate. The well-defined oxidation peak was observed at 1.03 V. The calibration curves were linear for etodolac at the concentration range of 2.5-50 μg/ml for linear sweep, square wave and differential pulse voltammetry methods, respectively. Intra- and inter-day precision values for etodolac were less than 4.69, and accuracy (relative error) was better than 2.00%. The mean recovery of etodolac was 100.6% for pharmaceutical preparations. No interference was found from three tablet excipients at the selected assay conditions. Developed methods in this study are accurate, precise and can be easily applied to Etol, Tadolak and Etodin tablets as pharmaceutical preparation. PMID:26664057

  1. L-Cysteine capped CdTe-CdS core-shell quantum dots: preparation, characterization and immuno-labeling of HeLa cells.

    PubMed

    Zhang, Hongyan; Sun, Pan; Liu, Chang; Gao, Huanyu; Xu, Linru; Fang, Jin; Wang, Meng; Liu, Jinling; Xu, Shukun

    2011-01-01

    Functionalized CdTe-CdS core-shell quantum dots (QDs) were synthesized in aqueous solution via water-bathing combined hydrothermal method using L-cysteine (L-Cys) as a stabilizer. This method possesses both the advantages of water-bathing and hydrothermal methods for preparing high-quality QDs with markedly reduced synthesis time, and better stability than a lone hydrothermal method. The QDs were characterized by transmission electronic microscopy and powder X-ray diffraction and X-ray photoelectron spectroscopy. The CdTe-CdS QDs with core-shell structure showed both enhanced fluorescence and better photo stability than nude CdTe QDs. After conjugating with antibody rabbit anti-CEACAM8 (CD67), the as-prepared l-Cys capped CdTe-CdS QDs were successfully used as fluorescent probes for the direct immuno-labeling and imaging of HeLa cells. It was indicated that this kind of QD would have application potential in bio-labeling and cell imaging. Copyright © 2009 John Wiley & Sons, Ltd.

  2. Gravimetric method for the determination of diclofenac in pharmaceutical preparations.

    PubMed

    Tubino, Matthieu; De Souza, Rafael L

    2005-01-01

    A gravimetric method for the determination of diclofenac in pharmaceutical preparations was developed. Diclofenac is precipitated from aqueous solution with copper(II) acetate in pH 5.3 (acetic acid/acetate buffer). Sample aliquots had approximately the same quantity of the drug content in tablets (50 mg) or in ampules (75 mg). The observed standard deviation was about +/- 2 mg; therefore, the relative standard deviation (RSD) was approximately 4% for tablet and 3% for ampule preparations. The results were compared with those obtained with the liquid chromatography method recommended in the United States Pharmacopoeia using the statistical Student's t-test. Complete agreement was observed. It is possible to obtain more precise results using higher aliquots, for example 200 mg, in which case the RSD falls to 1%. This gravimetric method, contrary to what is expected for this kind of procedure, is relatively fast and simple to perform. The main advantage is the absolute character of the gravimetric analysis.

  3. Facile combustion synthesis of ZnO nanoparticles using Cajanus cajan (L.) and its multidisciplinary applications

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

    Manjunath, K.; Ravishankar, T.N.; Kumar, Dhanith

    Graphical abstract: Facile combustion synthesis of ZnO nanoparticles using Cajanuscajan (L.) and its multidisciplinary applications.Zinc oxide nanoparticles were successfully synthesized by solution combustion method (SCM) using pigeon pea as a combustible fuel for the first time. The as-prepared product shows good photocatalytic, dielectric, antibacterial, electrochemical properties. - Highlights: • ZnO Nps were synthesized via combustion method using pigeon pea as a fuel. • The structure of the product was confirmed by XRD technique. • The morphology was confirmed by SEM and TEM images. • The as-prepared product shown good photocatalytic activity, dielectric property. • It has also shown good antibacterialmore » and electrochemical properties. - Abstract: Zinc oxide nanoparticles (ZnO Nps) were successfully synthesized by solution combustion method (SCM) using pigeon pea as a fuel for the first time. X-Ray diffraction pattern reveals that the product belongs to hexagonal system. FTIR spectrum of ZnO Nps shows the band at 420 cm{sup −1} associated with the characteristic vibration of Zn–O. TEM images show that the nanoparticles are found to be ∼40–80 nm. Furthermore, the as-prepared ZnO Nps exhibits good photocatalytic activity for the photodegradation of methylene blue (MB), indicating that they are indeed a promising photocatalytic semiconductor. The antibacterial properties of ZnO nanopowders were investigated by their bactericidal activity against four bacterial strains.« less

  4. Functionalized graphene oxide quantum dot-PVA hydrogel: a colorimetric sensor for Fe2+, Co2+ and Cu2+ ions

    NASA Astrophysics Data System (ADS)

    Baruah, Upama; Chowdhury, Devasish

    2016-04-01

    Functionalized graphene oxide quantum dots (GOQDs)-poly(vinyl alcohol) (PVA) hybrid hydrogels were prepared using a simple, facile and cost-effective strategy. GOQDs bearing different surface functional groups were introduced as the cross-linking agent into the PVA matrix thereby resulting in gelation. The four different types of hybrid hydrogels were prepared using graphene oxide, reduced graphene oxide, ester functionalized graphene oxide and amine functionalized GOQDs as cross-linking agents. It was observed that the hybrid hydrogel prepared with amine functionalized GOQDs was the most stable. The potential applicability of using this solid sensing platform has been subsequently explored in an easy, simple, effective and sensitive method for optical detection of M2+ (Fe2+, Co2+ and Cu2+) in aqueous media involving colorimetric detection. Amine functionalized GOQDs-PVA hybrid hydrogel when put into the corresponding solution of Fe2+, Co2+ and Cu2+ renders brown, orange and blue coloration respectively of the solution detecting the presence of Fe2+, Co2+ and Cu2+ ions in the solution. The minimum detection limit observed was 1 × 10-7 M using UV-visible spectroscopy. Further, the applicability of the sensing material was also tested for a mixture of co-existing ions in solution to demonstrate the practical applicability of the system. Insight into the probable mechanistic pathway involved in the detection process is also being discussed.

  5. Synthesis and characterization of magnetic of Ni/ABS nanocomposites by electrical explosion of wire in liquid and solution blending methods

    NASA Astrophysics Data System (ADS)

    Thuyet-Nguyen, Minh; Hai-Nguyen, Hong; Kim, Won Joo; Kim, Ho Yoon; Kim, Jin-Chun

    2017-03-01

    Nanomaterials have attracted great attention from chemists, physicists and materials scientists because of their application benefits and special properties. Thermoplastics have been used in many applications such as molding of non-electrical components, conducting, magnetic field and 3D printing. Nanocomposites are known as a material which blends the best properties of components, a high performance material exhibits unusual property combinations and unique design possibilities. In this research, we focused to investigate and report primary results in the synthesis of magnetic nanocomposites based on acrylonitrile butadiene styrene (ABS), which are useful and important thermoplastics. Nickel nanopowder was prepared by electrical explosion of wire in a liquid were used as magnetic component. The composites were prepared by following steps, first the obtained Ni nanopowders were incorporated into the ABS matrix via a solution blending method (drop-casting), and then the solvent was evaporated. The characterizations of obtaining composites were analyzed by field emission scanning electron microscopy, X-Ray Diffraction analysis and vibrating sample magnetometer.

  6. Influence of fuel-nitrate ratio on the structural and magnetic properties of Fe and Cr based spinels prepared by solution self combustion method

    NASA Astrophysics Data System (ADS)

    Sijo, A. K.

    2017-11-01

    In this study, we report the synthesis of nano-sized CoCrFeO4 and NiCrFeO4 using the solution self combustion method and the variation in the magnetic and structural properties with different fuel to nitrate ratios-fuel lean, fuel rich and stoichiometric. Citric acid is used as the fuel. XRD analysis of the samples confirms the formation of pure spinel phased nanoparticles in fuel rich and stoichiometric cases. But CoCrFeO4 and NiCrFeO4 samples prepared under the fuel lean condition show the presence of a small amount of impurity phases: α-Ni in fuel lean NiCrFeO4 and α-Co in fuel lean CoCrFeO4. Fuel lean samples possess high magnetic saturation. The stoichiometric ratio results in finest nano-particles and structural and magnetic properties are very critically dependent on fuel to nitrate ratio.

  7. The ototoxic effect of boric acid solutions applied into the middle ear of guinea pigs.

    PubMed

    Oztürkcan, Sedat; Dündar, Riza; Katilmis, Hüseyin; Ilknur, Ali Ekber; Aktaş, Sinem; Haciömeroğlu, Senem

    2009-05-01

    This study analyzed the ototoxic effects of boric acid solutions. Boric acid solutions have been used as otologic preparations for many years. Boric acid is commonly found in solutions prepared with alcohol or distilled water but can also be found in a powder form. These preparations are used for both their antiseptic and acidic qualities in external and middle ear infections. We investigated the ototoxic effect of boric acid solutions on guinea pigs. We are unaware of any similar, previously published study of this subject in English. The study was conducted on 28 young albino guinea pigs. Prior to application of the boric acid solution under general anesthesia, an Auditory Brainstem Response (ABRs) test was applied to the right ear of the guinea pigs. Following the test, a perforation was created on the tympanic membrane of the right ear of each guinea pig and small gelfoam pieces were inserted into the perforated area. Test solutions were administered to the middle ear for 10 days by means of a transcanal route. Fifteen days after inserting the gelfoams in all of the guinea pigs, we anasthesized the guinea pigs and removed the gelfoams from the perforated region of the ear and then performed an ABRs on each guinea pig. The ABRs were within the normal range before the applications. After the application, no significant changes were detected in the ABRs thresholds in neither the saline group nor the group administered boric acid and distilled water solution; however, significant changes were detected in the ABRs thresholds of the Gentamicine and boric acid and alcohol solution groups. We believe that a 4% boric acid solution prepared with distilled water can be a more reliable preparation than a 4% boric acid solution prepared with alcohol.

  8. DMF as an Additive in a Two-Step Spin-Coating Method for 20% Conversion Efficiency in Perovskite Solar Cells.

    PubMed

    Wu, Jionghua; Xu, Xin; Zhao, Yanhong; Shi, Jiangjian; Xu, Yuzhuan; Luo, Yanhong; Li, Dongmei; Wu, Huijue; Meng, Qingbo

    2017-08-16

    DMF as an additive has been employed in FAI/MAI/IPA (FA= CH 2 (NH 2 ) 2 , MA = CH 3 NH 3 , IPA = isopropanol) solution for a two-step multicycle spin-coating method in order to prepare high-quality FA x MA 1-x PbI 2.55 Br 0.45 perovskite films. Further investigation reveals that the existence of DMF in the FAI/MAI/IPA solution can facilitate perovskite conversion, improve the film morphology, and reduce crystal defects, thus enhancing charge-transfer efficiency. By optimization of the DMF amount and spin-coating cycles, compact, pinhole-free perovskite films are obtained. The nucleation mechanisms of perovskite films in our multicycle spin-coating process are suggested; that is, the introduction of DMF in the spin-coating FAI/MAI/IPA solution can lead to the formation of an amorphous phase PbX 2 -AI-DMSO-DMF (X = I, Br; A = FA, MA) instead of intermediate phase (MA) 2 Pb 3 I 8 ·2DMSO. This amorphous phase, similar to that in the one-step method, can help FAI/MAI penetrate into the PbI 2 framework to completely convert into the perovskite. As high as 20.1% power conversion efficiency (PCE) has been achieved with a steady-state PCE of 19.1%. Our work offers a simple repeatable method to prepare high-quality perovskite films for high-performance PSCs and also help further understand the perovskite-crystallization process.

  9. Method of electroplating a conversion electron emitting source on implant

    DOEpatents

    Srivastava, Suresh C [Setauket, NY; Gonzales, Gilbert R [New York, NY; Adzic, Radoslav [East Setauket, NY; Meinken, George E [Middle Island, NY

    2012-02-14

    Methods for preparing an implant coated with a conversion electron emitting source (CEES) are disclosed. The typical method includes cleaning the surface of the implant; placing the implant in an activating solution comprising hydrochloric acid to activate the surface; reducing the surface by H.sub.2 evolution in H.sub.2SO.sub.4 solution; and placing the implant in an electroplating solution that includes ions of the CEES, HCl, H.sub.2SO.sub.4, and resorcinol, gelatin, or a combination thereof. Alternatively, before tin plating, a seed layer is formed on the surface. The electroplated CEES coating can be further protected and stabilized by annealing in a heated oven, by passivation, or by being covered with a protective film. The invention also relates to a holding device for holding an implant, wherein the device selectively prevents electrodeposition on the portions of the implant contacting the device.

  10. Structure, optical and phonon properties of bulk and nanocrystalline Al2-xScx(WO4)3 solid solutions doped with Cr3+

    NASA Astrophysics Data System (ADS)

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

    2014-01-01

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

  11. Method of preparing graphene-sulfur nanocomposites for rechargeable lithium-sulfur battery electrodes

    DOEpatents

    Liu, Jun; Lemmon, John P; Yang, Zhenguo; Cao, Yuliang; Li, Xiaolin

    2015-04-07

    A method of preparing a graphene-sulfur nanocomposite for a cathode in a rechargeable lithium-sulfur battery comprising thermally expanding graphite oxide to yield graphene layers, mixing the graphene layers with a first solution comprising sulfur and carbon disulfide, evaporating the carbon disulfide to yield a solid nanocomposite, and grinding the solid nanocomposite to yield the graphene-sulfur nanocomposite. Rechargeable-lithium-sulfur batteries having a cathode that includes a graphene-sulfur nanocomposite can exhibit improved characteristics. The graphene-sulfur nanocomposite can be characterized by graphene sheets with particles of sulfur adsorbed to the graphene sheets. The sulfur particles have an average diameter of less than 50 nm.

  12. Development of a method for detecting trace metals in aqueous solutions based on the coordination chemistry of hexahydrotriazines.

    PubMed

    Wojtecki, Rudy J; Yuen, Alexander Y; Zimmerman, Thomas G; Jones, Gavin O; Horn, Hans W; Boday, Dylan J; Hedrick, James L; García, Jeannette M

    2015-08-07

    The detection of trace amounts (<10 ppb) of heavy metals in aqueous solutions is described using 1,3,5-hexahydro-1,3,5-triazines (HTs) as chemical indicators and a low cost fluorimeter-based detection system. This method takes advantage of the inherent properties of HTs to coordinate strongly with metal ions in solution, a fundamental property that was studied using a combination of analytical tools (UV-Vis titrations, (1)H-NMR titrations and computational modeling). Based on these fundamental studies that show significant changes in the HT UV signature when a metal ion is present, HT compounds were used to prepare indicator strips that resulted in significant fluorescence changes when a metal was present. A portable and economical approach was adopted to test the concept of utilizing HTs to detect heavy metals using a fluorimeter system that consisted of a low-pressure mercury lamp, a photo-detector, a monolithic photodiode and an amplifier, which produces a voltage proportional to the magnitude of the visible fluorescence emission. Readings of the prepared HT test strips were evaluated by exposure to two different heavy metals at the safe threshold concentration described by the U.S. Environmental Protection Agency (EPA) for Cr(3+) and Ag(2+) (100 μg L(-1) and 6.25, respectively). This method of detection could be used to the presence of either metal at these threshold concentrations.

  13. Studying Some of Electrical and Mechanical Properties for Kevlar Fiber Reinforced Epoxy

    NASA Astrophysics Data System (ADS)

    Rafeeq, Sewench N.; Hussein, Samah M.

    2011-12-01

    As ordinary known the ability of synthesizing electrical conducting polymer composites is possible but with poor mechanical properties, for the solution of this problem, we carried out this study in order to obtain that both properties. Three methods were applied for preparing the conductive polyaniline (PANI) composites using Kevlar fiber fabric as substrate for the deposition of the PANI at one time and the prepared composite (EP/Kevlar fiber) at others. The chemical oxidative method was adopted for polymerization of the aniline and simultaneously protonated of PANI with a hydrochloric acid at concentration (1M). Two kinds of oxidation agents (FeCl3.6H2O) and ((NH4)2S2O8) were used. The electrical measurements indicate the effect of each preparation method, kind of oxidant agent and the kind of mat erial which PANI deposited on the electrical results. The conductivity results showed that the prepared composites lie within semiconductors region. Temperature—dependence of electric conductivity results showed semiconductors and conductors behavior of this material within the applied temperature ranges. The mechan ical property (tensile strength) was studied. X-ray diffraction study showed the crystalline structure for EP/Kevlar fiber/PANI composites prepared by the three methods. These results gave optimism to the synthesis of conductive polymer composites with excellent mechanical properties..

  14. Stability of core-shell nanowires in selected model solutions

    NASA Astrophysics Data System (ADS)

    Kalska-Szostko, B.; Wykowska, U.; Basa, A.; Zambrzycka, E.

    2015-03-01

    This paper presents the studies of stability of magnetic core-shell nanowires prepared by electrochemical deposition from an acidic solution containing iron in the core and modified surface layer. The obtained nanowires were tested according to their durability in distilled water, 0.01 M citric acid, 0.9% NaCl, and commercial white wine (12% alcohol). The proposed solutions were chosen in such a way as to mimic food related environment due to a possible application of nanowires as additives to, for example, packages. After 1, 2 and 3 weeks wetting in the solutions, nanoparticles were tested by Infrared Spectroscopy, Atomic Absorption Spectroscopy, Transmission Electron Microscopy and X-ray diffraction methods.

  15. In situ polymerization of monomers for polyphenylquinoxaline/graphite fiber composites

    NASA Technical Reports Server (NTRS)

    Serafini, T. T.; Delvigs, P.; Vannucci, R. D.

    1974-01-01

    Methods currently used to prepare fiber reinforced, high temperature resistant polyphenylquinoxaline (PPQ) composites employ extremely viscous, low solids content solutions of high molecular weight PPQ polymers. An improved approach, described in this report, consists of impregnating the fiber with a solution of the appropriate monomers instead of a solution of previously synthesized high molecular weight polymer. Polymerization of the monomers occurs in situ on the fiber during the solvent removal and curing stages. The in situ polymerization approach greatly simplifies the fabrication of PPQ graphite fiber composites. The use of low viscosity monomeric type solutions facilitates fiber wetting, permits a high solids content, and eliminates the need for prior polymer synthesis.

  16. Optical characterization of pure and Al-doped ZnO prepared by sol-gel method

    NASA Astrophysics Data System (ADS)

    Belka, Radosław; Keczkowska, Justyna; Kasińska, Justyna

    2016-09-01

    In this paper the preparation process and optical characterization of pure and Al3+ doped zinc oxide (Al:ZnO) coatings will be presented. ZnO based materials have been studied extensively due to their potential applications in optoelectronic devices as conductive gas sensors, transparent conductive, electrodes, solar cell windows, varistors, UVfilters or photovoltaic cells. It is II-VI semiconductor with wide-band gap of 3.37 eV and large exciton binding energy of 60meV. It is possible to improve the conductivity of ZnO coating by intentionally doping ZnO with aluminium ions during preparation process. Such transparent and conducting thin films, known as AZO (Aluminium Zinc Oxide) films, are very good candidate for application as transparent conducting materials in many optoelectronic devices. The well-known sol-gel method is used for preparation of solution, coated on glass substrates by dip coating process. Prepared samples were investigated by Raman and UV-VIS spectroscopy. Transmittance as well as specular and diffuse reflectance spectroscopy methods were used for studies of optical parameters. We found that Al admixture influences on optical bandgap of ZnO.

  17. Ionic liquid as a potential solvent for preparation of collagen-alginate-hydroxyapatite beads as bone filler.

    PubMed

    Iqbal, Bushra; Sarfaraz, Zenab; Muhammad, Nawshad; Ahmad, Pervaiz; Iqbal, Jibran; Khan, Zia Ul Haq; Gonfa, Girma; Iqbal, Farasat; Jamal, Arshad; Rahim, Abdur

    2018-07-01

    In this study, collagen/alginate/hydroxyapatite beads having different proportions were prepared as bone fillers for the restoration of osteological defects. Ionic liquid was used to dissolve the collagen and subsequently the solution was mixed with sodium alginate solution. Hydroxyapatite was added in different proportions, with the rationale to enhance mechanical as well as biological properties. The prepared solutions were given characteristic bead shapes by dropwise addition into calcium chloride solution. The prepared beads were characterized using FTIR, XRD, TGA and SEM analysis. Microhardness testing was used to evaluate the mechanical properties. The prepared beads were investigated for water adsorption behavior to ascertain its ability for body fluid uptake and adjusted accordingly to the bone cavity. Drug loading and subsequently the antibacterial activity was investigated for the prepared beads. The biocompatibility was assessed using the hemolysis testing and cell proliferation assay. The prepared collagen-alginate-HA beads, having biocompatibility and good mechanical properties, have showed an option of promising biologically active bone fillers for bone regeneration.

  18. Validation of an automated fluorescein method for determining bromide in water

    USGS Publications Warehouse

    Fishman, M. J.; Schroder, L.J.; Friedman, L.C.

    1985-01-01

    Surface, atmospheric precipitation and deionized water samples were spiked with ??g l-1 concentrations of bromide, and the solutions stored in polyethylene and polytetrafluoroethylene bottles. Bromide was determined periodically for 30 days. Automated fluorescein and ion chromatography methods were used to determine bromide in these prepared samples. Analysis of the data by the paired t-test indicates that the two methods are not significantly different at a probability of 95% for samples containing from 0.015 to 0.5 mg l-1 of bromide. The correlation coefficient for the same sets of paired data is 0.9987. Recovery data, except for the surface water samples to which 0.005 mg l-1 of bromide was added, range from 89 to 112%. There appears to be no loss of bromide from solution in either type of container.Surface, atmospheric precipitation and deionized water samples were spiked with mu g l** minus **1 concentrations of bromide, and the solutions stored in polyethylene and polytetrafluoroethylene bottles. Bromide was determined periodically for 30 days. Automated fluorescein and ion chromatography methods were used to determine bromide in these prepared samples. Analysis of the data by the paired t-test indicates that the two methods are not significantly different at a probability of 95% for samples containing from 0. 015 to 0. 5 mg l** minus **1 of bromide. The correlation coefficient for the same sets of paired data is 0. 9987. Recovery data, except for the surface water samples to which 0. 005 mg l** minus **1 of bromide was added, range from 89 to 112%. Refs.

  19. Performance characteristics of an ion chromatographic method for the quantitation of citrate and phosphate in pharmaceutical solutions.

    PubMed

    Jenke, Dennis; Sadain, Salma; Nunez, Karen; Byrne, Frances

    2007-01-01

    The performance of an ion chromatographic method for measuring citrate and phosphate in pharmaceutical solutions is evaluated. Performance characteristics examined include accuracy, precision, specificity, response linearity, robustness, and the ability to meet system suitability criteria. In general, the method is found to be robust within reasonable deviations from its specified operating conditions. Analytical accuracy is typically 100 +/- 3%, and short-term precision is not more than 1.5% relative standard deviation. The instrument response is linear over a range of 50% to 150% of the standard preparation target concentrations (12 mg/L for phosphate and 20 mg/L for citrate), and the results obtained using a single-point standard versus a calibration curve are essentially equivalent. A small analytical bias is observed and ascribed to the relative purity of the differing salts, used as raw materials in tested finished products and as reference standards in the analytical method. The assay is specific in that no phosphate or citrate peaks are observed in a variety of method-related solutions and matrix blanks (with and without autoclaving). The assay with manual preparation of the eluents is sensitive to the composition of the eluent in the sense that the eluent must be effectively degassed and protected from CO(2) ingress during use. In order for the assay to perform effectively, extensive system equilibration and conditioning is required. However, a properly conditioned and equilibrated system can be used to test a number of samples via chromatographic runs that include many (> 50) injections.

  20. Structural mechanical and antibacterial properties of HPMC/SF-AgNPs nanocomposite films

    NASA Astrophysics Data System (ADS)

    Harish, K. V.; Rao, B. Lakshmeesha; Asha, S.; Vipin, C.; Sangappa, Y.

    2018-04-01

    In the present study, Hydroxypropyl Methylcellulose (HPMC) pure and HPMC/SF-AgNPs biopolymer nanocomposite films were prepared by simple solution casting method. The prepared nanocomposite films were characterized using UV-Visible spectroscopy(UV-Vis), X-ray diffraction (XRD) measurements. The mechanical properties of HPMC/SF-AgNPs nanocomposites were found to be decrease with increase in the AgNP's concentrations. The HPMC/SF-AgNPs nanocomposites showed very good antibacterial activity against human pathogens P. aeruginosa, E.coli, and S.aureus.

  1. Process for preparing silicon carbide foam

    DOEpatents

    Whinnery, LeRoy Louis; Nichols, Monte Carl; Wheeler, David Roger; Loy, Douglas Anson

    1997-01-01

    A method of preparing near net shape, monolithic, porous SiC foams is disclosed. Organosilicon precursors are used to produce polymeric gels by thermally induced phase separation, wherein, a sufficiently concentrated solution of an organosilicon polymer is cooled below its solidification temperature to form a gel. Following solvent removal from the gel, the polymer foam is pretreated in an oxygen plasma in order to raise its glass transition temperature. The pretreated foam is then pyrolized in an inert atmosphere to form a SiC foam.

  2. Process for preparing silicon carbide foam

    DOEpatents

    Whinnery, L.L.; Nichols, M.C.; Wheeler, D.R.; Loy, D.A.

    1997-09-16

    A method of preparing near net shape, monolithic, porous SiC foams is disclosed. Organosilicon precursors are used to produce polymeric gels by thermally induced phase separation, wherein, a sufficiently concentrated solution of an organosilicon polymer is cooled below its solidification temperature to form a gel. Following solvent removal from the gel, the polymer foam is pretreated in an oxygen plasma in order to raise its glass transition temperature. The pretreated foam is then pyrolyzed in an inert atmosphere to form a SiC foam. 9 figs.

  3. Preparation of osmium targets with carbon backing

    NASA Astrophysics Data System (ADS)

    Fremont, Georges; Ngono-Ravache, Yvette; Schmitt, Christelle; Stodel, Christelle

    2018-05-01

    For nuclear reaction studies, thin metallic osmium targets, either natural or isotopically enriched (Os-192) of 200-300 µg/cm2 thicknesses deposited on a thin carbon backing are required. A challenging method was successfully performed at GANIL involving firstly the preparation of an aqueous solution of osmium tetrachloride, then its electro-deposition onto a thick copper backing (100 µm); this process was followed by the evaporation of a thin carbon layer (≈40 µg/cm²) and finally the dissolution of the copper material.

  4. A Forensic Workshop Report Concerning (1) The Measurement and Analysis of Energetic Materials and (2) Databasing

    DTIC Science & Technology

    1999-01-01

    contaminating the surface. Research efforts to develop an improved sampling method have previously been limited to deposits made from solutions of explosives...explosive per fingerprint calculated in this way has too much variation to allow determination of sampling efficiency or to use this method to prepare...crystals is put into suspension, the actual amount is determined by usual methods including high-performance liquid chromatography (HPLC), gas

  5. A simple and novel method for RNA-seq library preparation of single cell cDNA analysis by hyperactive Tn5 transposase.

    PubMed

    Brouilette, Scott; Kuersten, Scott; Mein, Charles; Bozek, Monika; Terry, Anna; Dias, Kerith-Rae; Bhaw-Rosun, Leena; Shintani, Yasunori; Coppen, Steven; Ikebe, Chiho; Sawhney, Vinit; Campbell, Niall; Kaneko, Masahiro; Tano, Nobuko; Ishida, Hidekazu; Suzuki, Ken; Yashiro, Kenta

    2012-10-01

    Deep sequencing of single cell-derived cDNAs offers novel insights into oncogenesis and embryogenesis. However, traditional library preparation for RNA-seq analysis requires multiple steps with consequent sample loss and stochastic variation at each step significantly affecting output. Thus, a simpler and better protocol is desirable. The recently developed hyperactive Tn5-mediated library preparation, which brings high quality libraries, is likely one of the solutions. Here, we tested the applicability of hyperactive Tn5-mediated library preparation to deep sequencing of single cell cDNA, optimized the protocol, and compared it with the conventional method based on sonication. This new technique does not require any expensive or special equipment, which secures wider availability. A library was constructed from only 100 ng of cDNA, which enables the saving of precious specimens. Only a few steps of robust enzymatic reaction resulted in saved time, enabling more specimens to be prepared at once, and with a more reproducible size distribution among the different specimens. The obtained RNA-seq results were comparable to the conventional method. Thus, this Tn5-mediated preparation is applicable for anyone who aims to carry out deep sequencing for single cell cDNAs. Copyright © 2012 Wiley Periodicals, Inc.

  6. Establishment and performance assessment of preparation technology of internal quality control products for blood transfusion compatibility testing.

    PubMed

    Yu, Yang; Ma, Chunya; Feng, Qian; Chen, Xin; Guan, Xiaozhen; Zhang, Xiaojuan; Chen, Linfeng; Lin, Zilin; Pan, Jichun; Zhang, Ting; Luo, Qun; Wang, Deqing

    2013-05-01

    The aim of this study was to establish and to optimize the preparation technology of whole blood internal quality control (IQC) products for blood transfusion compatibility testing. Several B-type RhD-negative blood samples collected from healthy donors were mixed. Two groups of whole blood IQC products, namely, the preservative solution group (PS group) and the saline group, were prepared. The agglutination intensity of IQC sample red cells and anti-B antibody, IgM anti-A antibody and reverse-typing A cell, IgG anti-D and O-type RhD-positive red cells, as well as free hemoglobin concentration in the supernatant of the two groups were detected. The erythrocytes in both groups were damaged to a certain extent during storage, but no evident (above moderate) hemolysis was observed in the stored sample within 42 days. The red cells remained structurally complete and the reaction activity of IgG anti-D reagent remained generally unchanged (P>0.05). Although the reaction activity oscillation of IgM anti-A reagent was observed, the agglutination intensity varied within an acceptable range of 1+. No difference was observed between the preparation methods of the samples, i.e., between the erythrocyte washed with saline and the one washed with red cell preservative solution (P>0.05). The long shelf life, low variance between tubes and stable antigen-antibody reaction activity of the whole blood IQC products prepared using the proposed method can meet the requirements of blood transfusion compatibility testing.

  7. Novel surface modification of polymer-based separation media controlling separation selectivity, retentivity and generation of electroosmotic flow.

    PubMed

    Hosoya, Ken; Kubo, Takuya; Takahashi, Katsuo; Ikegami, Tohru; Tanaka, Nobuo

    2002-12-06

    Uniformly sized packing materials based on synthetic polymer particles for high-performance liquid chromatography (HPLC) and capillary electrochromatography (CEC) have been prepared from polymerization mixtures containing methacrylic acid (MAA) as a functional monomer and by using a novel surface modification method. This "dispersion method" affords effectively modified separation media. Both the amount of MAA utilized in the preparation and reaction time affect the selectivity of chromatographic separation in both the HPLC and the CEC mode and electroosmotic flow. This detailed study revealed that the dispersion method effectively modified internal surface of macroporous separation media and, based on the amount of MAA introduced, exclusion mechanism for the separation of certain solutes could be observed.

  8. Method for producing size selected particles

    DOEpatents

    Krumdick, Gregory K.; Shin, Young Ho; Takeya, Kaname

    2016-09-20

    The invention provides a system for preparing specific sized particles, the system comprising a continuous stir tank reactor adapted to receive reactants; a centrifugal dispenser positioned downstream from the reactor and in fluid communication with the reactor; a particle separator positioned downstream of the dispenser; and a solution stream return conduit positioned between the separator and the reactor. Also provided is a method for preparing specific sized particles, the method comprising introducing reagent into a continuous stir reaction tank and allowing the reagents to react to produce product liquor containing particles; contacting the liquor particles with a centrifugal force for a time sufficient to generate particles of a predetermined size and morphology; and returning unused reagents and particles of a non-predetermined size to the tank.

  9. Synthesis of sub-micro-flakes CrSe2 on glass and (110) Si substrates by solvothermal method

    NASA Astrophysics Data System (ADS)

    Tang, Qingkai; Liu, Changyou; Zhang, Binbin; Jie, Wanqi

    2018-06-01

    Layered structure MX2 (M = transition metal, X = S, Se and Te) chalcogenides have rich physic properties and potential applications. While it is still a challenge to prepare the chalcogenides by solvothermal method. In this work, we reported a new solution method to prepare CrSe2 sub-micro-flakes on different substrates. The surface morphologies, structures and compositions of the precursor CrSe2(en)1/2 and CrSe2 were investigated by SEM, XRD, thermogravimetric, IR and Raman spectra. The CrSe2 flakes with the sizes of 5-15 μm were obtained on both glass and (110) Si crystalline substrates. The formation mechanism of CrSe2 sub-micro-flakes is suggested.

  10. A novel ultrasonication method in the preparation of zirconium impregnated cellulose for effective fluoride adsorption.

    PubMed

    Barathi, M; Kumar, A Santhana Krishna; Rajesh, N

    2014-05-01

    In the present work, we propose for the first time a novel ultrasound assisted methodology involving the impregnation of zirconium in a cellulose matrix. Fluoride from aqueous solution interacts with the cellulose hydroxyl groups and the cationic zirconium hydroxide. Ultrasonication ensures a green and quick alternative to the conventional time intensive method of preparation. The effectiveness of this process was confirmed by comprehensive characterization of zirconium impregnated cellulose (ZrIC) adsorbent using Fourier transform infrared spectroscopy (FT-IR), energy dispersive X-ray spectrometry (EDX) and X-ray diffraction (XRD) studies. The study of various adsorption isotherm models, kinetics and thermodynamics of the interaction validated the method. Copyright © 2013 Elsevier B.V. All rights reserved.

  11. Liquid nitrogen-assisted synthesis of fluorescent carbon dots from Blueberry and their performance in Fe3+ detection

    NASA Astrophysics Data System (ADS)

    Aslandaş, Ayşe Merve; Balcı, Neslihan; Arık, Mustafa; Şakiroğlu, Halis; Onganer, Yavuz; Meral, Kadem

    2015-11-01

    Fluorescent carbon dots (C-dots) were synthesized by a facile method containing liquid N2 treatment and centrifuge processes. The photophysical properties of the C-dots in an aqueous solution were examined at various conditions such as concentration, temperature, pH and excitation wavelength by using UV-vis absorption, fluorescence and time-resolved fluorescence spectroscopies. The C-dots emitted a broad fluorescence between approximately 350-550 nm and their fluorescence was tuned by changing excitation wavelength. The as-prepared C-dots were applied to Fe3+ detection from aqueous solution. Spectroscopic data revealed that the as-prepared C-dots were used to detect Fe3+ in the range of 12.5 μM to 100 μM as a fluorescence sensor.

  12. Preparation and some properties of Cu-Li alloys containing up to 20 at. % Li

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

    Mendelsohn, M.; Krauss, A.R.; Gruen, D.M.

    1985-01-01

    Lithium strongly segregates to the surface of Cu-Li alloys, thus substantially lowering the Cu sputtering yield relative to pure Cu. Use of Cu-Li limiters or divertors in tokamaks can therefore be expected to be beneficial in limiting high-Z plasma impurity influx. A large scale (100-200g) method for the preparation of Cu-Li alloys is described. Analysis reveals that on solidification from the melt stratification occurs which leads to compositional inhomogeneity. The results are discussed in the light of the Cu-Li binary phase diagram and rationalized on the basis of large density differences between Cu and Cu-Li solid solutions. It is concludedmore » that obtaining homogeneous Cu-Li solid solutions is a nontrivial task.« less

  13. Fabrication and characterization of lead-free BaTiO3 thin film for storage device applications

    NASA Astrophysics Data System (ADS)

    Sharma, Hakikat; Negi, N. S.

    2018-05-01

    The lead-free BaTiO3 (BT) thin film solution has been prepared by sol-gel method. The prepared solution spin coated on Pt/TiO2/SiO2/ Si substrate. The fabricated thin film was analyzed by XRD and Raman spectrometer for structural conformation. Uniformity of thin film was examined by Atomic force microscope (AFM). Thickness of the film was measured by cross sectional FESEM. Activation energies for both positive and negative biasing have been calculated from temperature dependent leakage current density as a function of electric field. For ferroelectric memory devices such as FRAM the hysteresis loop plays important role. Electric filed dependent polarization of BT thin film measured at different switching voltages. With increasing voltage maximum polarization increases.

  14. Hearing loss effects of administering boric alcohol solution prepared with alcohol in various degrees on guinea pigs (an experimental study).

    PubMed

    Aktas, Sinem; Basoglu, Mehmet Sinan; Aslan, Hale; Ilknur, Ali Ekber; Dundar, Riza; Katilmis, Huseyin; Ozturkcan, Sedat

    2013-09-01

    To investigate the ototoxic effect of boric acid solution prepared with different degree of alcohol. This study was performed on 28 young albino guinea pigs. After the animals divided four groups prior to the application of the solution an auditory brainstem response (ABR) test was applied to the each animal under general anesthesia. Their tympanic membranes perforated and test solutions were administrated to the middle ear through the perforation. On 15th day, ABR measurements were carried out and comparison was made with preadministration values. The degrees of hearing loss occurring as a result of the administration of 4% boric alcohol solutions prepared with 60° and 40° alcohol differed significantly (p < 0.001). It was established that 4% boric acid solution prepared with 60 alcohol affected hearing in guinea pigs more negatively and an increase in degree of alcohol also increased the ototoxicity of the boric acid solution. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

  15. Antibacterial Efficacy of Several Surgical Hand Preparation Products Used by Veterinary Students.

    PubMed

    Chou, Po-Yen; Doyle, Aimie J; Arai, Shiori; Burke, Pierre J; Bailey, Trina R

    2016-05-01

    To compare the antibacterial efficacy of different surgical hand antisepsis protocols used by veterinary students. Prospective, randomized, controlled study. Third year veterinary students (n=45). The participants were randomly assigned to 4 of the following 12 hand preparation product/time combinations: nonabrasive hand scrub method with 4% chlorhexidine gluconate (CH); hand rub with a mixture of 30% 1-propanol and 45% 2-propanol solution (MPS), 70% 2-propanol solution (IPS), or 61% ethanol solution with 1% chlorhexidine gluconate (ES/CH), with a contact time of 1.5, 3, or 5 minutes. Antibacterial efficacy was assessed after surgical hand preparation and at the end of surgery. Log reductions of total bacterial colony forming unit (CFU)/mL and positive aerobic culture rates were compared using multivariable analysis of variance and multivariable logistic regression, respectively. After surgical hand preparation, CH and ES/CH provided significantly higher log CFU reduction and lower positive culture rate for Gram-positive and spore-forming bacteria compared to MPS and IPS. Increase in contact time did not provide significant improvement in bacterial reduction. At the end of surgery, ES/CH provided significantly higher log CFU reduction compared to IPS and lower positive culture rate for Gram-positive bacteria compared to CH, MPS, and IPS. Increase in contact time significantly improved log CFU reduction in ES/CH and MPS groups. In our population of veterinary students ES/CH hand rubs or CH scrubs were more effective in reducing bacterial CFU during surgical hand preparation than MPS or IPS. © Copyright 2016 by The American College of Veterinary Surgeons.

  16. Photocatalysis as an Effective Advanced Oxidation Process

    EPA Science Inventory

    Photocatalysis is generally referred to as the acceleration of a photoreaction by the presence of a semiconductor catalyst such as titanium dioxide (TiO2) or zinc oxide (ZnO). Photocatalytic materials can be prepared by using various methods such as a sol-gel process, solution pr...

  17. Emulsion-Assisted Polymerization-Induced Hierarchical Self-Assembly of Giant Sea Urchin-like Aggregates in a Large Scale.

    PubMed

    Xu, Qingsong; Huang, Tong; Li, Shanlong; Li, Ke; Li, Chuanlong; Liu, Yannan; Wang, Yuling; Yu, Chunyang; Zhou, Yongfeng

    2018-05-09

    Hierarchical solution self-assembly has nowadays become an important biomimetic method to prepare highly complex and multifunctional supramolecular structures. However, despites the great progress, it is still highly challenging to prepare hierarchical self-assemblies in a large scale since the self-assembly processes are generally performed at high dilution. Herein, we report an emulsion-assisted polymerization-induced self-assembly (EAPISA) method with the advantages of in-situ self-assembly process, scalable preparation and facile functionalization to prepare hierarchical multiscale sea urchin-like aggregates (SUAs). It also extends horizons of PISA in monomers and in polymerization method. The obtained SUAs from amphiphilic alternating copolymers represent a novel self-assembled structure with micron-sized rattan ball-like capsule (RBC) acting as the hollow core body and radiating nanotubes tens of micrometers in length as the hollow spines. They can effectively capture model proteins at an ultra-low concentration (≈10 nM) after functionalized with amino groups through click copolymerization. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Different preparation methods and characterization of magnetic maghemite coated with chitosan

    NASA Astrophysics Data System (ADS)

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

    2013-06-01

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

  19. One-pot synthesis of triangular Ag nanoplates with tunable edge length.

    PubMed

    Zhang, Yulan; Yang, Ping; Zhang, Lipeng

    2012-11-01

    Triangular Ag nanoplates were prepared via a one-pot synthesis method by using citrate and poly (vinyl pyrolidone) (PVP). The edge length of the nanoplates was changed from 30 nm to 100 nm with increasing the concentration of PVP and the amount of sodium borohydride in aqueous solutions during preparation. The molar ratio of PVP to Ag nitrate affected the morphologies of the nanoplates. PVP plays an important role for determining the final morphologies and edge length of resulting nanoplates because the amount of PVP affected the viscosity of solutions. The viscosity of solutions kinetically controlled the nucleation and growth of Ag nanoplates. Furthermore, Ag nanoplates were not created in the case of without PVP. After adding sodium chloride, irregular Ag nanoparticles (NPs) instead of nanoplates were fabricated because of a Cl-/O2 etching process. Stacking fault was a key for the growth of triangular nanostructures. Reaction temperature and aging time also affected the formation of Ag nanoplates.

  20. Gold nanoparticles prepared by electro-exploding wire technique in aqueous solutions

    NASA Astrophysics Data System (ADS)

    Kumar, Lalit; Kapoor, Akanksha; Meghwal, Mayank; Annapoorni, S.

    2016-05-01

    This article presents an effective approach for the synthesis of Au nanoparticles via an environmentally benevolent electro-exploding wire (EEW) technique. In this process, Au nanoparticles evolve through the plasma generated from the parent Au metal. Compared to other typical chemical methods, electro-exploding wire technique is a simple and economical technique which normally operates in water or organic liquids under ambient conditions. Efficient size control was achieved using different aqueous medium like (1mM) NaCl, deionized water and aqueous solution of sodium hydroxide (NaOH, pH 9.5) using identical electro-exploding conditions. The gold nanoparticles exhibited the UV-vis absorption spectrum with a maximum absorption band at 530 nm, similar to that of gold nanoparticles chemically prepared in a solution. The mechanism of size variation of Au nanoparticles is also proposed. The results obtained help to develop methodologies for the control of EEW based nanoparticle growth and the functionalization of nanoparticle surfaces by specific interactions.

  1. Assessment of Recovery of Milk Protein Allergens from Processed Food for Mass Spectrometry Quantification.

    PubMed

    Groves, Kate; Cryar, Adam; Walker, Michael; Quaglia, Milena

    2018-01-01

    Assessing the recovery of food allergens from solid processed matrixes is one of the most difficult steps that needs to be overcome to enable the accurate quantification of protein allergens by immunoassay and MS. A feasibility study is described herein applying International System of Units (SI)-traceably quantified milk protein solutions to assess recovery by an improved extraction method. Untargeted MS analysis suggests that this novel extraction method can be further developed to provide high recoveries for a broad range of food allergens. A solution of α-casein was traceably quantified to the SI for the content of α-S1 casein. Cookie dough was prepared by spiking a known amount of the SI-traceable quantified solution into a mixture of flour, sugar, and soya spread, followed by baking. A novel method for the extraction of protein food allergens from solid matrixes based on proteolytic digestion was developed, and its performance was compared with the performance of methods reported in the literature.

  2. Physicochemical stability of carfilzomib (Kyprolis®) containing solutions in glass vials, ready-to-administer plastic syringes and infusion bags over a 28-day storage period.

    PubMed

    Kim, Sun Hee; Krämer, Irene

    2017-01-01

    Centralized aseptic preparation of ready-to-administer carfilzomib containing parenteral solutions in plastic syringes and polyolefine (PO) infusion bags needs profound knowledge about the physicochemical stability in order to determine the beyond-use-date of the preparations. Therefore, the purpose of this study was to determine the physicochemical stability of carfilzomib solution marketed as Kyprolis® powder for solution for infusion. Reconstituted solutions and ready-to-administer preparations of Kyprolis® stored under refrigeration (2-8℃) or at room temperature (25℃) were analyzed at predetermined intervals over a maximum storage period of 28 days. Chemical stability of carfilzomib was planned to be determined with a stability-indicating reversed-phase high-performance liquid chromatography assay. Physicochemical stability was planned to be determined by visual inspection of clarity and color as well as pH measurement. The study results show that reconstituted carfilzomib containing parenteral solutions are stable in glass vials as well as diluted solutions in plastic syringes and PO infusion bags over a period of at least 28 days when stored light protected under refrigeration. When stored at room temperature, reconstituted and diluted carfilzomib solutions are physicochemically stable over 14 days and 10 days, respectively. The physicochemical stability of carfilzomib infusion solutions allows cost-saving pharmacy-based centralized preparation of ready-to-administer preparations.

  3. An assessment of cleaning and sampling methods for food-contact surfaces in premises preparing and selling high-risk foods.

    PubMed Central

    Tebbutt, G. M.

    1991-01-01

    The performance of agar-contact plates and an alginate-swab method for sampling food surfaces before and after cleaning was compared. Contact plates were more convenient, and were at least as sensitive as the swabbing method. To assess cleaning efficiency repeated sampling was carried out in selected premises, and several cleaning methods were introduced for trial periods. Some surfaces, notably wood and polypropylene, were particularly difficult to clean. For these scrubbing with a nylon brush was the best method. Other surfaces were more easily cleaned, and generally the methods introduced as part of this study were better than the original method used in the premises. Paper proved to be unpopular, and cleaning solutions applied with it did no better than those cleaned with a multiuse cloth kept soaking in a detergent and hypochlorite solution. PMID:1850362

  4. European Scientific Notes. Volume 38, Number 2.

    DTIC Science & Technology

    1984-02-01

    Two-Dimensional Systems .................. J.T. Schriempf 80 The conference focused on the quantum Hall effect and the anomalous quantum Hall effect ...Study of the Effects of tional methods occur when the aim of Teaching Algorithmic and Heuristic instruction is to develop problem-solv- Solution Methods...Sharp and Dohme already has are therefore generally unsuitable as a fairly effective vaccine prepared from vaccines. The approach used by the the

  5. Measurement of Henry's Law Constants Using Internal Standards: A Quantitative GC Experiment for the Instrumental Analysis or Environmental Chemistry Laboratory

    ERIC Educational Resources Information Center

    Ji, Chang; Boisvert, Susanne M.; Arida, Ann-Marie C.; Day, Shannon E.

    2008-01-01

    An internal standard method applicable to undergraduate instrumental analysis or environmental chemistry laboratory has been designed and tested to determine the Henry's law constants for a series of alkyl nitriles. In this method, a mixture of the analytes and an internal standard is prepared and used to make a standard solution (organic solvent)…

  6. A liquid chromatography - tandem mass spectrometry method to measure a selected panel of uremic retention solutes derived from endogenous and colonic microbial metabolism.

    PubMed

    de Loor, Henriette; Poesen, Ruben; De Leger, Wout; Dehaen, Wim; Augustijns, Patrick; Evenepoel, Pieter; Meijers, Björn

    2016-09-14

    Chronic kidney disease (CKD) is associated with an increased risk of mortality and cardiovascular disease, which is, at least partly, mediated by the accumulation of so-called uremic retention solutes. Although there has been an increasing interest in the behavior of these solutes, derived from both the endogenous and colonic microbial metabolism, methods to simultaneously and accurately measure a broad panel of relevant uremic retention solutes remain scarce. We developed a highly sensitive ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method. A high throughput sample preparation was used with extraction of analytes from 50 μl serum using Ostro plate technology. For most solutes, stable isotopes labelled metabolites were used as internal standards. Chromatography was achieved using an Acquity UPLC CSH Fluoro Phenyl column. The total run time was 8 min, the mobile phase was a gradient of 0.1% formic acid in Milli-Q water and pure methanol at a flow rate of 0.5 ml min(-1). Detection was performed using a tandem mass spectrometer with alternated positive and negative electrospray ionization. Calibration curves were linear for all solutes. Precision was assessed according to the NCCLS EP5-T guideline, being below 15% for all metabolites. Mean recoveries were between 83 and 104% for all metabolites. The validated method was successfully applied in a cohort of 488 patients with CKD. We developed and validated a sensitive and robust UPLC-MS/MS method for quantification of 15 uremic retention solutes derived from endogenous and colonic microbial metabolism. This method allows for studying the behavior and relevance of these solutes in patients with CKD. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. [Controlled release of prednisolone from suppository prepared using powder of pulverized tablet].

    PubMed

    Tatsumi, Akitoshi; Oda, Shoko; Nakamoto, Tomoko; Muraoka, Reiko; Takahashi, Yoshiko; Tanaka, Kuniyoshi; Shikata, Toshiyuki; Tatsumi, Sumiyo; Tagawa, Noriko; Kobayashi, Yoshiharu; Hamaguchi, Tsuneo; Kadobayashi, Muneo

    2008-04-01

    Prednisolone suppositories have been used successfully for the treatment of ulcerative colitis in hospital settings. However, the raw material of prednisolone suppository, JP prednisolone powder (JP Powder), was recently removed from the market. Therefore we studied the effects of raw material and suppository base on the release of prednisolone suppository for the purpose of designing a new suppository with similar effects to those of suppository prepared using JP powder (old suppository). New suppositories consisting of the powder of pulverized tablet as raw material and Witepsol H-15 and Witepsol E-75 as suppository base were prepared according to the fusion method. Suppository release test was performed by reciprocating dialysis tube method with tapping (RDT method) and dialysis tubing method (DT method). Both RDT method and DT method were performed using a suppository dissolution apparatus (modified JP disintegration apparatus) and a JP15 paddle apparatus, respectively. The test fluid was 50 mM phosphate buffer solution (pH 7.4) maintained at 37+/-0.5 degrees C. The results of release test by RDT method were similar to those of DT method. Release rate of prednisolone from the new suppository was much faster than that of old suppository. The addition of Witepsol E-75 to new suppository base markedly delayed the release of prednisolone from the new suppository. Release rate of prednisolone from the new suppository, consisting of pulverized tablet and Witepsol H-15 and Witepsol E-75 (76:24), corresponded well with that of the old suppository. It was suggested that this suppository could be used as incoming preparation of suppository prepared using JP powder.

  8. Formulation, characterization and physicochemical evaluation of potassium citrate effervescent tablets.

    PubMed

    Aslani, Abolfazl; Fattahi, Fatemeh

    2013-01-01

    The aim of this study was to design and formulation of potassium citrate effervescent tablet for reduction of calcium oxalate and urate kidney stones in patients suffering from kidney stones. In this study, 13 formulations were prepared from potassium citrate and effervescent base in different concentration. The flowability of powders and granules was studied. Then effervescent tablets were prepared by direct compression, fusion and wet granulation methods. The prepared tablets were evaluated for hardness, friability, effervescent time, pH, content uniformity. To amend taste of formulations, different flavoring agents were used and then panel test was done by using Latin Square method by 30 volunteers. Formulations obtained from direct compression and fusion methods had good flow but low hardness. Wet granulation improves flowability and other physicochemical properties such as acceptable hardness, effervescence time ≤3 minutes, pH<6, friability < 1%, water percentage < 0.5% and accurate content uniformity. In panel test, both of combination flavors; (orange - lemon) and (strawberry - raspberry) had good acceptability. The prepared tablets by wet granulation method using PVP solution had more tablet hardness. It is a reproducible process and suitable to produce granules that are compressed into effervescent tablets due to larger agglomerates.

  9. New pathway to prepare gold nanoparticles and their applications in catalysis and surface-enhanced Raman scattering.

    PubMed

    Chang, Chun-Chao; Yang, Kuang-Hsuan; Liu, Yu-Chuan; Hsu, Ting-Chu

    2012-05-01

    As shown in the literature, additional energies are necessary for the reduction of positively charged noble metal ions to prepare metal nanoparticles (NPs). In this work, we report a new green pathway to prepare Au NPs in neutral 0.1M NaCl aqueous solutions from bulk Au substrates without addition of any stabilizer and reductant just via aid of natural chitosan (Ch) at room temperature. Au- and Ch-containing complexes in aqueous solution were electrochemically prepared. The role of Ch is just an intermediate to perform electron transfer with Au NPs. The stability of these prepared Au NPs is well maintained by Au NPs themselves with slightly positively charged Au remained on the surface of Au NPs. The particle size of prepared spherical Au (111) NPs is ca. 15 nm in diameter. Moreover, increasing the pH of preparation solutions can be contributive to preparing concentrated Au NPs in solutions. The prepared Au NPs are surface-enhanced Raman scattering (SERS)-active for probe molecules of Rhodamine 6G. They also demonstrate significantly catalytic activity for decomposition of acetaldehyde in rice wine. Copyright © 2012 Elsevier B.V. All rights reserved.

  10. Multispectroscopic (FTIR, XPS, and TOFMS-TPD) Investigation of the Core-Shell Bonding in Sonochemically-Prepared Aluminum Nanoparticles Capped with Oleic Acid (Preprint)

    DTIC Science & Technology

    2010-04-01

    dimethylethylamine and a titanium (IV) isopropoxide catalyst were added to the solution. The concentrations of the alane complex and titanium catalyst in...public release 3.0 METHODS, ASSUMPTIONS, AND PROCEDURES 3.1 Materials Alane N,N-dimethylethylamine in a 0.4 M toluene solution, titanium (IV... isopropoxide (98%), oleic acid (99%), dodecane (99% and anhydrous), and oleyl alcohol (99%) were all obtained from Aldrich and used as received

  11. A Solution-Processed Transparent NiO Hole-Extraction Layer for High-Performance Inverted Perovskite Solar Cells.

    PubMed

    Tang, Li Juan; Chen, Xiao; Wen, Tian Yu; Yang, Shuang; Zhao, Jun Jie; Qiao, Hong Wei; Hou, Yu; Yang, Hua Gui

    2018-02-26

    A highly transparent NiO layer was prepared by a solution processing method with nickel(II) 2-ethylhexanoate in non-polar solvent and utilized as HTM in perovskite solar cells. Excellent optical transmittance and the matched energy level lead to the enhanced power conversion efficiency (PCE, 18.15 %) than that of conventional sol-gel-processed NiO-based device (12.98 %). © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Performance evaluation soil samples utilizing encapsulation technology

    DOEpatents

    Dahlgran, J.R.

    1999-08-17

    Performance evaluation soil samples and method of their preparation uses encapsulation technology to encapsulate analytes which are introduced into a soil matrix for analysis and evaluation by analytical laboratories. Target analytes are mixed in an appropriate solvent at predetermined concentrations. The mixture is emulsified in a solution of polymeric film forming material. The emulsified solution is polymerized to form microcapsules. The microcapsules are recovered, quantitated and introduced into a soil matrix in a predetermined ratio to form soil samples with the desired analyte concentration. 1 fig.

  13. Performance evaluation soil samples utilizing encapsulation technology

    DOEpatents

    Dahlgran, James R.

    1999-01-01

    Performance evaluation soil samples and method of their preparation using encapsulation technology to encapsulate analytes which are introduced into a soil matrix for analysis and evaluation by analytical laboratories. Target analytes are mixed in an appropriate solvent at predetermined concentrations. The mixture is emulsified in a solution of polymeric film forming material. The emulsified solution is polymerized to form microcapsules. The microcapsules are recovered, quantitated and introduced into a soil matrix in a predetermined ratio to form soil samples with the desired analyte concentration.

  14. Optical Properties and Microstructure of Barium Titanate Thin Film (BaTiO3) for Solar Cell Applications

    NASA Astrophysics Data System (ADS)

    Setyadi, A. U. L. S.; Iriani, Y.; Nurosyid, F.

    2018-03-01

    Barium Titanate thin films were prepared with variations in the number of layers and variation of the solution on a Quartz substrate using the sol-gel method with spin coating technique, at rotation speed 3000 rpm for 30 seconds. The first solution was made with heated and the second with stirred and heated. In this experiment, BaTiO3 were heated at 900°C for 2 hours. The characterization of optical properties was performed by UV-Vis spectrometer and microstructural characterization was performed by X-Ray Diffraction (XRD). Variation of layers number affects the intensity of the diffraction peaks. The more layers of the intensity are also greater. The variation of solution making process affects the intensity of diffraction peak. The process of making the solution with stirred and heated has greater intensity than the process of solution by simply heating it. When stirred at the same time heated to produce atoms diffuses more easily with other atoms so the bonds between atoms are more orderly and strong. The process of making the solution in the heated is larger in the crystallite size of than preparation of solution by stirred and heated. The stirred which the solution is produced influences the appearance of the size of the crystal. Variation number of layers influences the absorbance value of layer. The absorbance increases with increasing number of layers. The absorbance of the sample was made with heated the higher than with stirred and heated.

  15. Differential-Integral method in polymer processing: Taking melt electrospinning technique for example

    NASA Astrophysics Data System (ADS)

    Haoyi, Li; Weimin, Yang; Hongbo, Chen; Jing, Tan; Pengcheng, Xie

    2016-03-01

    A concept of Differential-Integral (DI) method applied in polymer processing and molding was proposed, which included melt DI injection molding, DI nano-composites extrusion molding and melt differential electrospinning principle and equipment. Taking the melt differential electrospinning for example to introduce the innovation research progress, two methods preparing polymer ultrafine fiber have been developed: solution electro-spinning and melt electro-spinning, between which solution electro-spinning is much simpler to realize in lab. More than 100 institutions have endeavored to conduct research on it and more than 30 thousand papers have been published. However, its industrialization was restricted to some extend because of the existence of toxic solvent during spinning process and poor mechanical strength of resultant fibers caused by small pores on fiber surface. Solvent-free melt electrospinning is environmentally friendly and highly productive. However, problems such as the high melt viscosity, thick fiber diameter and complex equipment makes it relatively under researched compared with solution electrospinning. With the purpose of solving the shortage of traditional electro-spinning equipment with needles or capillaries, a melt differential electro-spinning method without needles or capillaries was firstly proposed. Nearly 50 related patents have been applied since 2005, and systematic method innovations and experimental studies have also been conducted. The prepared fiber by this method had exhibited small diameter and smooth surface. The average fiber diameter can reach 200-800 nm, and the single nozzle can yield two orders of magnitude more than the capillaries. Based on the above principle, complete commercial techniques and equipment have been developed to produce ultra-fine non-woven fabrics for the applications in air filtration, oil spill recovery and water treatment, etc.

  16. Method and apparatus for physical separation of different sized nanostructures

    DOEpatents

    Roberts, Christopher B.; Saunders, Steven R.

    2012-07-10

    The present application provides apparatuses and methods for the size-selective fractionation of ligand-capped nanoparticles that utilizes the tunable thermophysical properties of gas-expanded liquids. The nanoparticle size separation processes are based on the controlled reduction of the solvent strength of an organic phase nanoparticle dispersion through increases in concentration of the antisolvent gas, such as CO.sub.2, via pressurization. The method of nanomaterial separation contains preparing a vessel having a solvent and dispersed nanoparticles, pressurizing the chamber with a gaseous antisolvent, and causing a first amount of the nanoparticles to precipitate, transporting the solution to a second vessel, pressurizing the second vessel with the gaseous antisolvent and causing further nanoparticles to separate from the solution.

  17. Influence of the preparation method on the physicochemical properties of indomethacin and methyl-β-cyclodextrin complexes.

    PubMed

    Rudrangi, Shashi Ravi Suman; Bhomia, Ruchir; Trivedi, Vivek; Vine, George J; Mitchell, John C; Alexander, Bruce David; Wicks, Stephen Richard

    2015-02-20

    The main objective of this study was to investigate different manufacturing processes claimed to promote inclusion complexation between indomethacin and cyclodextrins in order to enhance the apparent solubility and dissolution properties of indomethacin. Especially, the effectiveness of supercritical carbon dioxide processing for preparing solid drug-cyclodextrin inclusion complexes was investigated and compared to other preparation methods. The complexes were prepared by physical mixing, co-evaporation, freeze drying from aqueous solution, spray drying and supercritical carbon dioxide processing methods. The prepared complexes were then evaluated by scanning electron microscopy, differential scanning calorimetry, X-ray powder diffraction, solubility and dissolution studies. The method of preparation of the inclusion complexes was shown to influence the physicochemical properties of the formed complexes. Indomethacin exists in a highly crystalline solid form. Physical mixing of indomethacin and methyl-β-cyclodextrin appeared not to reduce the degree of crystallinity of the drug. The co-evaporated and freeze dried complexes had a lower degree of crystallinity than the physical mix; however the lowest degree of crystallinity was achieved in complexes prepared by spray drying and supercritical carbon dioxide processing methods. All systems based on methyl-β-cyclodextrin exhibited better dissolution properties than the drug alone. The greatest improvement in drug dissolution properties was obtained from complexes prepared using supercritical carbon dioxide processing, thereafter by spray drying, freeze drying, co-evaporation and finally by physical mixing. Supercritical carbon dioxide processing is well known as an energy efficient alternative to other pharmaceutical processes and may have application for the preparation of solid-state drug-cyclodextrin inclusion complexes. It is an effective and economic method that allows the formation of solid complexes with a high yield, without the use of organic solvents and problems associated with their residues. Copyright © 2015 Elsevier B.V. All rights reserved.

  18. Stability of admixtures of pethidine and metoclopramide in aqueous solution, 5% dextrose and 09% sodium chloride.

    PubMed

    Hor, M M; Chan, S Y; Yow, K L; Lim, L Y; Chan, E

    1997-01-01

    To study the stability of admixtures of pethidine and metoclopramide in aqueous solution, 0.9% sodium chloride and 5% dextrose preparations. Aqueous mixtures of 1 ml of 50 mg/ml pethidine with 2ml of 5 mg/ml metoclopramide were prepared in plastic syringes, while the 0.9% sodium chloride and 5% dextrose admixtures, each containing 7.35 mg/ml of pethidine and 0.15 mg/ml of metoclopramide, were prepared in infusion bags. The preparations were stored under light and dark conditions at 32 degrees C for 48 h. Samples were collected at 0, 0.5, 1, 2, 4, 6, 8, 24, 32 and 48 h. A high-performance liquid chromatographic method was developed to separate and quantify both drugs. All preparations were found to be physically and chemically stable for at least 48h, as concentration changes were within 10% of their initial level, with no development of haze, precipitate or colour. Light appeared to have a negligible effect. Although pH changes were observed, they were inconsistent and were within the ranges in which the drugs are expected to remain stable. Pethidine and metoclopramide admixtures can, therefore, on stability grounds be used for the concomitant management of pain, nausea and vomiting.

  19. Low-temperature solution route to macroscopic amounts of hydrogen terminated silicon nanoparticles.

    PubMed

    Neiner, Doinita; Chiu, Hsiang Wei; Kauzlarich, Susan M

    2006-08-30

    A new solution route for preparing gram-scale, hydrogen terminated silicon nanoparticles is presented. Dimethoxyethane and diocytl ether have been used to prepare silicon nanoparticles via a solution reaction between sodium silicide and ammonium bromide. The reaction products are isolated as a clear yellow-orange solution and a dark black powder. Both the solution and the powder have been characterized.

  20. Rapid Quantitative Analysis of Naringenin in the Fruit Bodies of Inonotus vaninii by Two-phase Acid Hydrolysis Followed by Reversed Phase-high Performance Liquid Chromatography-ultra Violet.

    PubMed

    Guohua, Xia; Pan, Ruirong; Bao, Rui; Ge, Yanru; Zhou, Cunshan; Shen, Yuping

    2017-01-01

    Sanghuang is one of mystical traditional Chinese medicines recorded earliest 2000 years ago, that included various fungi of Inonotus genus and was well-known for antitumor effect in modern medicine. Inonotus vaninii is grown in natural forest of Northeastern China merely and used as Sanghuang commercially, but it has no quality control specification until now. This study was to establish a rapid method of two-phase acid hydrolysis followed by reversed phase-high performance liquid chromatography-ultra violet (RP-HPLC-UV) to quantify naringenin in the fruit body of I. vaninii . Sample solution was prepared by pretreatment of raw material in two-phase acid hydrolysis and the hydrolysis technology was optimized. After reconstitution, analysis was performed using RP-HPLC-UV. The method validation was investigated and the naringenin content of sample and comparison were determined. The naringenin was obtained by two-phase acid hydrolysis method, namely, 10.0 g of raw material was hydrolyzed in 200 mL of 1% sulfuric acid aqueous solution (v/v) and 400 mL of chloroform in oil bath at 110°C for 2 h. Good linearity ( r = 0.9992) was achieved between concentration of analyte and peak area. The relative standard deviation (RSD) of precision was 2.47% and the RSD of naringenin contents for repeatability was 3.13%. The accuracy was supported with recoveries at 96.37%, 97.30%, and 99.31%. The sample solution prepared using the proposed method contained higher content of naringenin than conventional method and was stable for 8 h. Due to the high efficiency of sample preparation and high reliability of the HPLC method, it is feasible to use this method for routine analysis of naringenin in the fungus. A convenient two-phase acid hydrolysis was employed to produce naringenin from raw material, and then an efficient and reliable reversed phase-high performance liquid chromatography-ultra violet method was established to monitor naringenin in the fruit bodies of Inonotus vaninii . The newly established method could be used to control the quality of the herb. Abbreviations used: RP-HPLC-UV: Reversed Phase-High Performance Liquid Chromatography-Ultra Violet, RSD: Relative Standard Deviation, EtOAc: Ethyl acetate, ACN: Acetonitrile, MeOH: Methanol, RH: Relative Humility.

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