Electrochemical Synthesis of Ammonia in Solid Electrolyte Cells

International Nuclear Information System (INIS)

Garagounis, Ioannis; Kyriakou, Vasileios; Skodra, Aglaia; Vasileiou, Eirini; Stoukides, Michael

2014-01-01

Developed in the early 1900s, the “Haber–Bosch” synthesis is the dominant NH 3 synthesis process. Parallel to catalyst optimization, current research efforts are also focused on the investigation of new methods for ammonia synthesis, including the electrochemical synthesis with the use of solid electrolyte cells. Since the first report on Solid State Ammonia Synthesis (SSAS), more than 30 solid electrolyte materials were tested and at least 15 catalysts were used as working electrodes. Thus far, the highest rate of ammonia formation reported is 1.13 × 10 -8 mol s -1 cm -2 , obtained at 80°C with a Nafion solid electrolyte and a mixed oxide, SmFe 0.7 Cu 0.1 Ni 0.2 O 3 , cathode. At high temperatures (>500°C), the maximum rate was 9.5 × 10 −9 mol s -1 cm -2 using Ce 0.8 Y 0.2 O 2-δ –[Ca 3 (PO 4 ) 2 –K 3 PO 4 ] as electrolyte and Ag–Pd as cathode. In this paper, the advantages and the disadvantages of SSAS vs. the conventional process and the requirements that must be met in order to promote the electrochemical process into an industrial level are discussed.

Electrochemical Synthesis of Ammonia in Solid Electrolyte Cells

Energy Technology Data Exchange (ETDEWEB)

Garagounis, Ioannis; Kyriakou, Vasileios [Department of Chemical Engineering, Aristotle University of Thessaloniki, Thessaloniki (Greece); Chemical Processes and Energy Resources Institute, Center for Research and Technology Hellas, Thessaloniki (Greece); Skodra, Aglaia [Chemical Processes and Energy Resources Institute, Center for Research and Technology Hellas, Thessaloniki (Greece); Vasileiou, Eirini; Stoukides, Michael, E-mail: stoukidi@cperi.certh.gr [Department of Chemical Engineering, Aristotle University of Thessaloniki, Thessaloniki (Greece); Chemical Processes and Energy Resources Institute, Center for Research and Technology Hellas, Thessaloniki (Greece)

2014-01-17

Developed in the early 1900s, the “Haber–Bosch” synthesis is the dominant NH{sub 3} synthesis process. Parallel to catalyst optimization, current research efforts are also focused on the investigation of new methods for ammonia synthesis, including the electrochemical synthesis with the use of solid electrolyte cells. Since the first report on Solid State Ammonia Synthesis (SSAS), more than 30 solid electrolyte materials were tested and at least 15 catalysts were used as working electrodes. Thus far, the highest rate of ammonia formation reported is 1.13 × 10{sup -8} mol s{sup -1} cm{sup -2}, obtained at 80°C with a Nafion solid electrolyte and a mixed oxide, SmFe{sub 0.7}Cu{sub 0.1}Ni{sub 0.2}O{sub 3}, cathode. At high temperatures (>500°C), the maximum rate was 9.5 × 10{sup −9} mol s{sup -1} cm{sup -2} using Ce{sub 0.8}Y{sub 0.2}O{sub 2-δ}–[Ca{sub 3}(PO{sub 4}){sub 2}–K{sub 3}PO{sub 4}] as electrolyte and Ag–Pd as cathode. In this paper, the advantages and the disadvantages of SSAS vs. the conventional process and the requirements that must be met in order to promote the electrochemical process into an industrial level are discussed.

N-Acyliminium Intermediates in Solid-Phase Synthesis

DEFF Research Database (Denmark)

Quement, Sebastian Thordal le; Petersen, Rico; Meldal, M.

2010-01-01

N-Acyliminium ions are powerful intermediates in synthetic organic chemistry. Examples of their use are numerous in solution-phase synthesis, but there are unmerited few reports on these highly reactive electrophiles in solid-phase synthesis. The present review covers the literature to date and i...

Combinatorial Solid-Phase Synthesis of Balanol Analogues

DEFF Research Database (Denmark)

Nielsen, John; Lyngsø, Lars Ole

1996-01-01

The natural product balanol has served as a template for the design and synthesis of a combinatorial library using solid-phase chemistry. Using a retrosynthetic analysis, the structural analogues have been assembled from three relatively accessible building blocks. The solid-phase chemistry inclu...

Solid-phase synthesis of protein-polymers on reversible immobilization supports.

Science.gov (United States)

Murata, Hironobu; Carmali, Sheiliza; Baker, Stefanie L; Matyjaszewski, Krzysztof; Russell, Alan J

2018-02-27

Facile automated biomacromolecule synthesis is at the heart of blending synthetic and biologic worlds. Full access to abiotic/biotic synthetic diversity first occurred when chemistry was developed to grow nucleic acids and peptides from reversibly immobilized precursors. Protein-polymer conjugates, however, have always been synthesized in solution in multi-step, multi-day processes that couple innovative chemistry with challenging purification. Here we report the generation of protein-polymer hybrids synthesized by protein-ATRP on reversible immobilization supports (PARIS). We utilized modified agarose beads to covalently and reversibly couple to proteins in amino-specific reactions. We then modified reversibly immobilized proteins with protein-reactive ATRP initiators and, after ATRP, we released and analyzed the protein polymers. The activity and stability of PARIS-synthesized and solution-synthesized conjugates demonstrated that PARIS was an effective, rapid, and simple method to generate protein-polymer conjugates. Automation of PARIS significantly reduced synthesis/purification timelines, thereby opening a path to changing how to generate protein-polymer conjugates.

Solid-phase synthesis of molecularly imprinted nanoparticles.

Science.gov (United States)

Canfarotta, Francesco; Poma, Alessandro; Guerreiro, Antonio; Piletsky, Sergey

2016-03-01

Molecularly imprinted polymers (MIPs) are synthetic materials, generally based on acrylic or methacrylic monomers, that are polymerized in the presence of a specific target molecule called the 'template' and capable of rebinding selectively to this target molecule. They have the potential to be low-cost and robust alternatives to biomolecules such as antibodies and receptors. When prepared by traditional synthetic methods (i.e., with free template in solution), their usefulness has been limited by high binding site heterogeneity, the presence of residual template and the fact that the production methods are complex and difficult to standardize. To overcome some of these limitations, we developed a method for the synthesis of MIP nanoparticles (nanoMIPs) using an innovative solid-phase approach, which relies on the covalent immobilization of the template molecules onto the surface of a solid support (glass beads). The obtained nanoMIPs are virtually free of template and demonstrate high affinity for the target molecule (e.g., melamine and trypsin in our published work). Because of an affinity separation step performed on the solid phase after polymerization, poor binders and unproductive polymer are removed, so the final product has more uniform binding characteristics. The overall protocol, starting from the immobilization of the template onto the solid phase and including the purification and characterization of the nanoparticles, takes up to 1 week.

Supporting Information Synthesis Procedure: Graphene oxide (GO ...

Indian Academy of Sciences (India)

SS

Synthesis Procedure: Graphene oxide (GO) was prepared by a modified Hummers method using expandable .... anode material for Li ion batteries, J. Solid State Electrochem. ... coupling, doping and nonadiabatic effects, Solid State Commun.

Solvent-Controlled Chemoselectivity in the Photolytic Release of Hydroxamic Acids and Carboxamides from Solid Support

DEFF Research Database (Denmark)

Qvortrup, Katrine; Petersen, Rico G; Dohn, Asmus Ougaard

2017-01-01

The synthetic utility and theoretical basis of a photolabile hydroxylamine-linker are presented. The developed protocols enable the efficient synthesis and chemoselective photolytic release of either hydroxamates or carboxamides from solid support. The bidetachable mode of the linker unit...

Visual monitoring of solid-phase extraction using chromogenic fluorous synthesis supports.

Science.gov (United States)

Blackburn, Christopher

2012-03-12

Reductive aminations and further transformations of an azo dye and fluorous tagged aldehyde are described. The intensely colored 2,4-dialkoxybenzyl protected amines undergo Fmoc-based peptide coupling, Suzuki reactions, and sulfonamide formation with product isolation facilitated by visual monitoring of fluorous solid phase extraction. Target compounds are released from the supports in high yields and purities by treatment with trifluoroacetic acid (TFA).

Solid-phase synthesis of NH-1,2,3-triazoles using 4,4′- bismethoxybenzhydryl azide

DEFF Research Database (Denmark)

Cohrt, Anders Emil O'Hanlon; Le Quement, Sebastian Thordal; Nielsen, Thomas Eiland

2014-01-01

Readily available 4,4′-bismethoxybenzhydryl azide was found to be a useful building block for the synthesis of NH-1,2,3-triazoles through copper(I)-catalyzed cycloaddition reactions with solid-supported terminal alkynes, followed by acid-mediated deprotection. Peptide-containing NH-1,2,3-triazole...

Simple automated system for simultaneous production of 11C-labeled tracers by solid supported methylation

International Nuclear Information System (INIS)

Quincoces, Gemma; Penuelas, Ivan; Valero, Marta; Serra, Patricia; Collantes, Maria; Marti-Climent, Josep; Arbizu, Javier; Jose Garcia-Velloso, Maria; Angel Richter, Jose

2006-01-01

We herein describe a simple setup for the automated simultaneous synthesis of L-[methyl- 11 C]methionine and N-[methyl- 11 C]choline by solid-supported methylation . The setup is extremely simple and easy to adapt to other automated systems and due to its versatility, the method can be utilized for the production of other radiopharmaceuticals requiring a simple [ 11 C]methylation step. Furthermore, it can be used for multiple simultaneous synthesis

Stereoselective Reduction of Imines with Trichlorosilane Using Solid-Supported Chiral Picolinamides

Directory of Open Access Journals (Sweden)

Sílvia D. Fernandes

2016-09-01

Full Text Available The stereoselective reduction of imines with trichlorosilane catalyzed by chiral Lewis bases is a well-established procedure for the synthesis of enantio-enriched amines. Five supported cinchona-based picolinamides have been prepared and their activity tested in a model reaction. The comparison of different supporting materials revealed that polystyrene gave better results than silica in terms of stereoselectivity. The applicability of the solid-supported catalyst of choice to the reduction of different imines was also demonstrated. Additionally, for the first time, a catalytic reactor containing a polymer-immobilized chiral picolinamide has been employed for the stereoselective reduction of imines with trichlorosilane under continuous flow conditions.

Linkers, resins, and general procedures for solid-phase peptide synthesis

DEFF Research Database (Denmark)

Shelton, Anne Pernille Tofteng; Jensen, Knud Jørgen

2013-01-01

and linkers for solid-phase synthesis is a key parameter for successful peptide synthesis. This chapter provides an overview of the most common and useful resins and linkers for the synthesis of peptides with C-terminal amides, carboxylic acids, and more. The chapter finishes with robust protocols for general...

Solid-phase synthesis of complex and pharmacologically interesting heterocycles

DEFF Research Database (Denmark)

Nielsen, Thomas Eiland

2009-01-01

Efficient routes for the creation of heterocycles continue to be one of the primary goals for solid-phase synthesis. Recent advances in this field rely most notably on transition-metal-catalysis and N-acyliminium chemistry to mediate a range of cyclization processes for the generation of compounds...... with significant structural complexity and diversity. This review describes some of the most systematic solid-phase approaches that are potentially suited for pharmaceutical applications, that is, the methods described are useful for the synthesis of compound collections, and exhibit tunable stereochemistry...

Methanol synthesis in a countercurrent gas-solid-solid trickle flow reactor. An experimental study

NARCIS (Netherlands)

Kuczynski, M.; Oyevaar, M.H.; Pieters, R.T.; Westerterp, K.R.

1987-01-01

The synthesis of methanol from CO and H2 was executed in a gas-solid-solid trickle flow reactor. The reactor consisted of three tubular reactor sections with cooling sections in between. The catalyst was Cu on alumina, the adsorbent was a silica-alumina powder and the experimental range 498–523 K,

Divergent solid-phase synthesis of natural product-inspired bipartite cyclodepsipeptides : total synthesis of seragamide A

NARCIS (Netherlands)

Arndt, H.-D.; Rizzo, S.; Nöcker, Chr.; Wackchaure, V.N.; Milroy, L.G.; Bieker, V.; Calderon, A.; Tran, T.T.N.; Brand, S.; Dehmelt, L.; Waldmann, H.

2015-01-01

Macrocyclic natural products (NPs) and analogues thereof often show high affinity, selectivity, and metabolic stability, and methods for the synthesis of NP-like macrocycle collections are of major current interest. We report an efficient solid-phase/cyclorelease method for the synthesis of a

SOLID-PHASE PEPTIDE SYNTHESIS OF ISOTOCIN WITH AMIDE ...

African Journals Online (AJOL)

SOLID-PHASE PEPTIDE SYNTHESIS OF ISOTOCIN WITH AMIDE OF ASPARAGINE PROTECTED WITH 1-TETRALINYL. TRIFLUOROMETHANESULPHONIC ACID (TFMSA) DEPROTECTION, CLEAVAGE AND AIR OXIDATION OF MERCAPTO GROUPS TO DISULPHIDE.

A Photolabile Linker for the Solid-Phase Synthesis of Peptide Hydrazides and Heterocycles

DEFF Research Database (Denmark)

Qvortrup, Katrine; Komnatnyy, Vitaly V.; Nielsen, Thomas Eiland

2014-01-01

A photolabile hydrazine linker for the solid-phase synthesis of peptide hydrazides and hydrazine-derived heterocycles is presented. The developed protocols enable the efficient synthesis of structurally diverse peptide hydrazides derived from the standard amino adds, including those with side......-chain protected residues at the C-terminal of the resulting peptide hydrazide, and are useful for the synthesis of dihydropyrano[2,3-c]pyrazoles. The linker is compatible with most commonly used coupling reagents and protecting groups for solid-phase peptide synthesis....

Aqueous Microwave-Assisted Solid-Phase Synthesis Using Boc-Amino Acid Nanoparticles

Directory of Open Access Journals (Sweden)

Yoshinobu Fukumori

2013-07-01

Full Text Available We have previously developed water-based microwave (MW-assisted peptide synthesis using Fmoc-amino acid nanopaticles. It is an organic solvent-free, environmentally friendly method for peptide synthesis. Here we describe water-based MW-assisted solid-phase synthesis using Boc-amino acid nanoparticles. The microwave irradiation allowed rapid solid-phase reaction of nanoparticle reactants on the resin in water. We also demonstrated the syntheses of Leu-enkephalin, Tyr-Gly-Gly-Phe-Leu-OH, and difficult sequence model peptide, Val-Ala-Val-Ala-Gly-OH, using our water-based MW-assisted protocol with Boc-amino acid nanoparticles.

Solid-phase synthesis of polyfunctional polylysine dendrons using aldehyde linkers

DEFF Research Database (Denmark)

Svenssen, Daniel K.; Mirsharghi, Sahar; Boas, Ulrik

2014-01-01

A straightforward method for the solid-phase synthesis of C-terminally modified polylysine dendrons has been developed by applying bisalkoxybenzaldehyde and trisalkoxybenzaldehyde linkers. The method has been used for the synthesis of polylysine dendrons with a variety of C-terminal ‘tail groups’...

resin as polymer-supported synthesis support

Indian Academy of Sciences (India)

Administrator

molecules since it offers advantages such as the ease of reaction work-up and automation.1 The success of a SPOS strategy depends on the properties of the solid supports in many critical ways.2 The solid sup- ports used most widely in ...

Rapid and convenient semi-automated microwave-assisted solid-phase synthesis of arylopeptoids

DEFF Research Database (Denmark)

Rasmussen, Jakob Ewald; Boccia, Marcello Massimo; Nielsen, John

2014-01-01

A facile and expedient route to the synthesis of arylopeptoid oligomers (N-alkylated aminomethyl benz-amides) using semi-automated microwave-assisted solid-phase synthesis is presented. The synthesis was optimized for the incorporation of side chains derived from sterically hindered or unreactive...

Traceless Azido Linker for the Solid-Phase Synthesis of NH-1,2,3-Triazoles via Cu-Catalyzed Azide-Alkyne Cycloaddition Reactions

DEFF Research Database (Denmark)

Cohrt, Anders Emil; Jensen, Jakob Feldthusen; Nielsen, Thomas Eiland

2010-01-01

A broadly useful acid-labile traceless azido linker for the solid-phase synthesis of NH-1,2,3-triazoles is presented. A variety of alkynes were efficiently immobilized on a range of polymeric supports by Cu(I)-mediated azide-alkyne cycloadditions. Supported triazoles showed excellent compatibility...

Semi-automated microwave assisted solid-phase peptide synthesis

DEFF Research Database (Denmark)

Pedersen, Søren Ljungberg

with microwaves for SPPS has gained in popularity as it for many syntheses has provided significant improvement in terms of speed, purity, and yields, maybe especially in the synthesis of long and "difficult" peptides. Thus, precise microwave heating has emerged as one new parameter for SPPS, in addition...... to coupling reagents, resins, solvents etc. We have previously reported on microwave heating to promote a range of solid-phase reactions in SPPS. Here we present a new, flexible semi-automated instrument for the application of precise microwave heating in solid-phase synthesis. It combines a slightly modified...... Biotage Initiator microwave instrument, which is available in many laboratories, with a modified semi-automated peptide synthesizer from MultiSynTech. A custom-made reaction vessel is placed permanently in the microwave oven, thus the reactor does not have to be moved between steps. Mixing is achieved...

CSBB-ConeExclusion, adapting structure based solution virtual screening to libraries on solid support.

Science.gov (United States)

Shave, Steven; Auer, Manfred

2013-12-23

Combinatorial chemical libraries produced on solid support offer fast and cost-effective access to a large number of unique compounds. If such libraries are screened directly on-bead, the speed at which chemical space can be explored by chemists is much greater than that addressable using solution based synthesis and screening methods. Solution based screening has a large supporting body of software such as structure-based virtual screening tools which enable the prediction of protein-ligand complexes. Use of these techniques to predict the protein bound complexes of compounds synthesized on solid support neglects to take into account the conjugation site on the small molecule ligand. This may invalidate predicted binding modes, the linker may be clashing with protein atoms. We present CSBB-ConeExclusion, a methodology and computer program which provides a measure of the applicability of solution dockings to solid support. Output is given in the form of statistics for each docking pose, a unique 2D visualization method which can be used to determine applicability at a glance, and automatically generated PyMol scripts allowing visualization of protein atom incursion into a defined exclusion volume. CSBB-ConeExclusion is then exemplarically used to determine the optimum attachment point for a purine library targeting cyclin-dependent kinase 2 CDK2.

Solid-Phase Synthesis of Difficult Purine-Rich PNAs through Selective Hmb Incorporation: Application to the Total Synthesis of Cell Penetrating Peptide-PNAs

Directory of Open Access Journals (Sweden)

Julien Tailhades

2017-10-01

Full Text Available Antisense oligonucleotide (ASO-based drug development is gaining significant momentum following the recent FDA approval of Eteplirsen (an ASO based on phosphorodiamidate morpholino and Spinraza (2′-O-methoxyethyl-phosphorothioate in late 2016. Their attractiveness is mainly due to the backbone modifications which have improved the in vivo characteristics of oligonucleotide drugs. Another class of ASO, based on peptide nucleic acid (PNA chemistry, is also gaining popularity as a platform for development of gene-specific therapy for various disorders. However, the chemical synthesis of long PNAs, which are more target-specific, remains an ongoing challenge. Most of the reported methodology for the solid-phase synthesis of PNA suffer from poor coupling efficiency which limits production to short PNA sequences of less than 15 residues. Here, we have studied the effect of backbone modifications with Hmb (2-hydroxy-4-methoxybenzyl and Dmb (2,4-dimethoxybenzyl to ameliorate difficult couplings and reduce “on-resin” aggregation. We firstly synthesized a library of PNA dimers incorporating either Hmb or Dmb and identified that Hmb is superior to Dmb in terms of its ease of removal. Subsequently, we used Hmb backbone modification to synthesize a 22-mer purine-rich PNA, targeting dystrophin RNA splicing, which could not be synthesized by standard coupling methodology. Hmb backbone modification allowed this difficult PNA to be synthesized as well as to be continued to include a cell-penetrating peptide on the same solid support. This approach provides a novel and straightforward strategy for facile solid-phase synthesis of difficult purine-rich PNA sequences.

Solid-phase synthesis of difficult purine-rich PNAs through selective Hmb incorporation: Application to the total synthesis of cell penetrating peptide-PNAs

Science.gov (United States)

Tailhades, Julien; Takizawa, Hotake; Gait, Michael J.; Wellings, Don A.; Wade, John D.; Aoki, Yoshitsugu; Shabanpoor, Fazel

2017-10-01

Antisense oligonucleotide (ASO)-based drug development is gaining significant momentum following the recent FDA approval of Eteplirsen (an ASO based on phosphorodiamidate morpholino) and Spinraza (2’-O-methoxyethyl-phosphorothioate) in late 2016. Their attractiveness is mainly due to the backbone modifications which have improved the in vivo characteristics of oligonucleotide drugs. Another class of ASO, based on peptide nucleic acid (PNA) chemistry, is also gaining popularity as a platform for development of gene-specific therapy for various disorders. However, the chemical synthesis of long PNAs, which are more target-specific, remains an ongoing challenge. Most of the reported methodology for the solid-phase synthesis of PNA suffer from poor coupling efficiency which limits production to short PNA sequences of less than 15 residues. Here we have studied the effect of backbone modifications with Hmb (2-hydroxy-4-methoxybenzyl) and Dmb (2,4-dimethoxybenzyl) to ameliorate difficult couplings and reduce “on-resin” aggregation. We firstly synthesized a library of PNA dimers incorporating either Hmb or Dmb and identified that Hmb is superior to Dmb in terms of its ease of removal. Subsequently, we used Hmb backbone modification to synthesize a 22-mer purine-rich PNA, targeting dystrophin RNA splicing, which could not be synthesized by standard coupling methodology. Hmb backbone modification allowed this difficult PNA to be synthesized as well as to be continued to include a cell-penetrating peptide on the same solid support. This approach provides a novel and straightforward strategy for facile solid-phase synthesis of difficult purine-rich PNA sequences.

Low-temperature synthesis of actinide tetraborides by solid-state metathesis reactions

Science.gov (United States)

Lupinetti, Anthony J [Los Alamos, NM; Garcia, Eduardo [Los Alamos, NM; Abney, Kent D [Los Alamos, NM

2004-12-14

The synthesis of actinide tetraborides including uranium tetraboride (UB.sub.4), plutonium tetraboride (PuB.sub.4) and thorium tetraboride (ThB.sub.4) by a solid-state metathesis reaction are demonstrated. The present method significantly lowers the temperature required to .ltoreq.850.degree. C. As an example, when UCl.sub.4 is reacted with an excess of MgB.sub.2, at 850.degree. C., crystalline UB.sub.4 is formed. Powder X-ray diffraction and ICP-AES data support the reduction of UCl.sub.3 as the initial step in the reaction. The UB.sub.4 product is purified by washing water and drying.

Solid-phase synthesis of 3-amino-2-pyrazolines

DEFF Research Database (Denmark)

Nielsen, John

1998-01-01

The development of a solid-phase synthesis of 3-amino-2-pyrazolines is described. Conjugate addition of hydrazines to alpha,beta-unsaturated nitriles followed by cyclization yields 3-amino-2-pyrazolines. Acylation or sulfonation of the free amino-group yields a 24 member library of 3-amino-2...

Combinatorial Libraries on Rigid Scaffolds: Solid Phase Synthesis of Variably Substituted Pyrazoles and Isoxazoles

Directory of Open Access Journals (Sweden)

Eduard R. Felder

1997-01-01

Full Text Available The synthesis of combinatorial compound libraries has become a powerful lead finding tool in modern drug discovery. The ability to synthesize rapidly, in high yield, new chemical entities with low molecular weight on a solid support has a recognized strategic relevance (“small molecule libraries”. We designed and validated a novel solid phase synthesis scheme, suitable to generate diversity on small heterocycles of the pyrazole and isoxazole type. Appropriate conditions were worked out for each reaction, and a variety of more or less reactive agents (building blocks was utilized for discrete conversions, in order to exploit the system’s breadth of applicability. Four sequential reaction steps were validated, including the loading of the support with an acetyl bearing moiety, a Claisen condensation, an a-alkylation and a cyclization of a b-diketone with monosubstituted hydrazines. In a second stage, the reaction sequence was applied in a split and mix approach, in order to prepare a combinatorial library built-up from 4 acetyl carboxylic acids (R1, 35 carboxylic esters (R2 and 41 hydrazines (R4 (and 1 hydroxylamine to yield a total of 11,760 compounds divided into 41 pyrazole sublibraries with 140 pairs of regioisomers and 1 isoxazole sublibrary of equal size.

Solid-Phase Synthesis of Smac Peptidomimetics Incorporating Triazoloprolines and Biarylalanines

DEFF Research Database (Denmark)

Le Quement, Sebastian T.; Ishoey, Mette; Petersen, Mette T.

2011-01-01

by deactivating proteolytic caspases. The Smac protein has an antagonistic effect on IAPs, thus providing structural clues for the synthesis of new pro-apoptotic compounds. Herein, we report a solid-phase approach for the synthesis of Smac-derived tetrapeptide libraries. On the basis of a common (N......-Me)AVPF sequence, peptides incorporating triazoloprolines and biarylalanines were synthesized by means of Cu(I)-catalyzed azide–alkyne cycloaddition and Pd-catalyzed Suzuki cross-coupling reactions. Solid-phase procedures were optimized to high efficiency, thus accessing all products in excellent crude purities...... and yields (both typically above 90%). The peptides were subjected to biological evaluation in a live/dead cellular assay which revealed that structural decorations on the AVPF sequence indeed are highly important for cytotoxicity toward HeLa cells....

Smectite clays as solid supports for immobilization of beta-glucosidase : Synthesis, characterization, and biochemical properties

NARCIS (Netherlands)

Serefoglou, Evangelia; Litina, Kiriaki; Gournis, Dimitrios; Kalogeris, Emmanuel; Tzialla, Aikaterini A.; Pavlidis, Ioannis V.; Stamatis, Haralambos; Maccallini, Enrico; Lubomska, Monika; Rudolf, Petra

2008-01-01

Nanomaterials as solid supports can improve the efficiency of immobilized enzymes by reducing diffusional limitation as well as by increasing the surface area per mass unit and therefore improving enzyme loading. In this work, beta-glucosidase from almonds was immobilized on two smectite nanoclays.

Solid-phase synthesis of polynucleotides. III. Synthesis of polynucleotides with defined sequences by the block coupling phosphotriester method.

OpenAIRE

Miyoshi, K; Huang, T; Itakura, K

1980-01-01

Preparation of the three hexadecanucleotides, dGpTpApTpCpApCpGpApGpGpCpCpCpTpT, dCpGpApCpGpApGpCpGpTpGpApCpApCpC and cTpGpCpCpGpGpCpCpApCpGpApTpGpCpG, is described by a rapid and simple solid-phase method on polyacrylamide supports. The synthesis were performed by the extension of the method described in the previous paper using di and trinucleotides of defined sequences as an incoming 3'-phosphodiester unit. Although the coupling yields to form phosphotriester bonds are slightly lower than t...

A Facile Synthesis of Hollow Palladium/Copper Alloy Nanocubes Supported on N-Doped Graphene for Ethanol Electrooxidation Catalyst

OpenAIRE

Zhengyu Bai; Rumeng Huang; Lu Niu; Qing Zhang; Lin Yang; Jiujun Zhang

2015-01-01

In this paper, a catalyst of hollow PdCu alloy nanocubes supported on nitrogen-doped graphene support (H-PdCu/ppy-NG) is successfully synthesized using a simple one-pot template-free method. Two other catalyst materials such as solid PdCu alloy particles supported on this same nitrogen-doped graphene support (PdCu/ppy-NG) and hollow PdCu alloy nanocubes supported on the reduced graphene oxide support (H-PdCu/RGO) are also prepared using the similar synthesis conditions for comparison. It is f...

Solid-phase oligosaccharide and glycopeptide synthesis using glycosynthases

DEFF Research Database (Denmark)

Tolborg, Jakob Fjord; Petersen, Lars; Jensen, Knud Jørgen

2002-01-01

and the prospect of automatability. Here, we report the first application of glycosynthases to solid-phase oligosaccharide synthesis by use of the 51 kDa serine and glycine mutants of Agrobacterium sp. beta-glucosidase, Abg E358S and E358G. Acceptors were linked to PEGA resin through a backbone amide linker (BAL...

Use of the 2-chlorotrityl chloride resin for microwave-assisted solid phase peptide synthesis.

Science.gov (United States)

Ieronymaki, Matthaia; Androutsou, Maria Eleni; Pantelia, Anna; Friligou, Irene; Crisp, Molly; High, Kirsty; Penkman, Kirsty; Gatos, Dimitrios; Tselios, Theodore

2015-09-01

A fast and efficient microwave (MW)-assisted solid-phase peptide synthesis protocol using the 2-chlorotrityl chloride resin and the Fmoc/tBu methodology, has been developed. The established protocol combines the advantages of MW irradiation and the acid labile 2-chlorotrityl chloride resin. The effect of temperature during the MW irradiation, the degree of resin substitution during the coupling of the first amino acids and the rate of racemization for each amino acid were evaluated. The suggested solid phase methodology is applicable for orthogonal peptide synthesis and for the synthesis of cyclic peptides. © 2015 Wiley Periodicals, Inc.

Nanometric solid solutions of the fluorite and perovskite type crystal structures: Synthesis and properties

Directory of Open Access Journals (Sweden)

Snežana Bošković

2012-09-01

Full Text Available In this paper a short review of our results on the synthesis of nanosized CeO2, CaMnO3 and BaCeO3 solid solutions are presented. The nanopowders were prepared by two innovative methods: self propagating room temperature synthesis (SPRT and modified glycine/nitrate procedure (MGNP. Different types of solid solutions with rare earth dopants in concentrations ranging from 0–0.25 mol% were synthesized. The reactions forming solid solutions were studied. In addition, the characteristics of prepared nanopowders, phenomena during sintering and the properties of sintered samples are discussed.

Automated solid-phase peptide synthesis to obtain therapeutic peptides

Directory of Open Access Journals (Sweden)

Veronika Mäde

2014-05-01

Full Text Available The great versatility and the inherent high affinities of peptides for their respective targets have led to tremendous progress for therapeutic applications in the last years. In order to increase the drugability of these frequently unstable and rapidly cleared molecules, chemical modifications are of great interest. Automated solid-phase peptide synthesis (SPPS offers a suitable technology to produce chemically engineered peptides. This review concentrates on the application of SPPS by Fmoc/t-Bu protecting-group strategy, which is most commonly used. Critical issues and suggestions for the synthesis are covered. The development of automated methods from conventional to essentially improved microwave-assisted instruments is discussed. In order to improve pharmacokinetic properties of peptides, lipidation and PEGylation are described as covalent conjugation methods, which can be applied by a combination of automated and manual synthesis approaches. The synthesis and application of SPPS is described for neuropeptide Y receptor analogs as an example for bioactive hormones. The applied strategies represent innovative and potent methods for the development of novel peptide drug candidates that can be manufactured with optimized automated synthesis technologies.

Chemical synthesis on SU-8

DEFF Research Database (Denmark)

Qvortrup, Katrine; Taveras, Kennedy; Thastrup, Ole

2011-01-01

In this paper we describe a highly effective surface modification of SU-8 microparticles, the attachment of appropriate linkers for solid-supported synthesis, and the successful chemical modification of these particles via controlled multi-step organic synthesis leading to molecules attached...

New immobilisation protocol for the template used in solid-phase synthesis of MIP nanoparticles

Science.gov (United States)

Chen, Lu; Muhammad, Turghun; Yakup, Burabiye; Piletsky, Sergey A.

2017-06-01

As a novel imprinting method, solid-phase synthesis has proven to be a promising approach to prepare polymer nanoparticles with specific recognition sites for a template molecule. In this method, imprinted polymer nanoparticles were synthesized using template immobilized on a solid support. Herein, preparation of immobilized templates on quartz chips through homogeneous route was reported as an efficient alternative strategy to heterogeneous one. The template molecule indole-3-butyric acid (IBA) was reacted with 3-aminopropyltriethoxysilane (APTES) to produce silylated template (IBA-APTES), and it was characterized by IR, 1H NMR and GC-MS. Then, the silylated template molecule was grafted onto the activated surfaces of quartz chip to prepare immobilized template (SiO2@IBA-APTES). The immobilization was confirmed by contact angle, XPS, UV and fluorescence measurement. Immobilization protocol has shown good reproducibility and stability of the immobilized template. MIP nanoparticles were prepared with high selectivity toward the molecule immobilized onto the solid surface. This provides a new approach for the development of molecularly imprinted nanoparticles.

Facile solid-state synthesis of oxidation-resistant metal nanoparticles at ambient conditions

Science.gov (United States)

Lee, Kyu Hyung; Jung, Hyuk Joon; Lee, Ju Hee; Kim, Kyungtae; Lee, Byeongno; Nam, Dohyun; Kim, Chung Man; Jung, Myung-Hwa; Hur, Nam Hwi

2018-05-01

A simple and scalable method for the synthesis of metal nanoparticles in the solid-state was developed, which can produce nanoparticles in the absence of solvents. Nanoparticles of coinage metals were synthesized by grinding solid hydrazine and the metal precursors in their acetates and oxides at 25 °C. The silver and gold acetates converted completely within 6 min into Ag and Au nanoparticles, respectively, while complete conversion of the copper acetate to the Cu sub-micrometer particles took about 2 h. Metal oxide precursors were also converted into metal nanoparticles by grinding alone. The resulting particles exhibit distinctive crystalline lattice fringes, indicating the formation of highly crystalline phases. The Cu sub-micrometer particles are better resistant to oxidation and exhibit higher conductivity compared to conventional Cu nanoparticles. This solid-state method was also applied for the synthesis of platinum group metals and intermetallic Cu3Au, which can be further extended to synthesize other metal nanoparticles.

Synthesis of CdS hollow/solid nanospheres and their chain-structures by membrane technique

International Nuclear Information System (INIS)

Duan Shumin; Wu Qingsheng; Jia Runping; Liu Xinbo

2008-01-01

CdS hollow/solid nanospheres and their chain-structures were successfully synthesized through supporting liquid membrane (SLM) system with bio-membrane. X-ray powder diffraction (XRD), transmission electron microscopy (TEM), UV-Vis spectroscopy, and photoluminescence (PL) spectroscopy have been used for the characterization of the products. The average diameters of CdS solid/hollow spheres are about 10, 40 nm, respectively. The wall of the hollow spheres is about 5 nm. CdS products are all cubic face-centered structure with the cell constant a = 5.830 A. We also explore the morphology, structure and possible synthesis mechanism. A possible template mechanism has been proposed for the production of the hollow CdS nanocrystals, that is, CdS nanoparticles grow along the non-soakage interface between CHCl3 and reactant solution. During this process, the organic functional groups were crucial to the control of crystal morphologies

Construction of 1,3,4-Oxadiazole and 1,3,4-Thiadiazole Library with a High Level of Skeletal Diversity Based on Branching Diversity-Oriented Synthesis on Solid-Phase Supports.

Science.gov (United States)

Ha, Ji-Eun; Yang, Seung-Ju; Gong, Young-Dae

2018-02-12

An efficient solid-phase synthetic route for the construction of 1,3,4-oxadiazole and 1,3,4-thiadiazole libraries based on branching diversity-oriented synthesis (DOS) has been developed in this study. The core skeleton resins, 1,3,4-oxadiazole and 1,3,4-thiadiazole, were obtained through desulfurative and dehydrative cyclizations of thiosemicarbazide resin, respectively. Various functional groups have been introduced to the core skeleton resins, such as aryl, amine, amide, urea, thiourea, and an amino acid. Most of the libraries were purified by simple trituration without extraction or column chromatography after cleavage of the products from the solid-supported resin. As a result, we obtained high yields of pure 1,3,4-oxadiazole and 1,3,4-thiadiazole derivatives (total numbers = 128). Finally, we confirmed the drug-like properties of our library by calculation of physicochemical properties, displays of the skeletal diversities of the library in 3D-space, and occupation of a broad range of areas by their functional groups.

Solid-phase Synthesis of Combinatorial 2,4-Disubstituted-1,3,5-Triazine via Amine Nucleophilic Reaction

Energy Technology Data Exchange (ETDEWEB)

Moon, Sung Won [KIST Gangneung Institute, Gangneung (Korea, Republic of); Ham, Jungyeob [Gangneung-Wonju National University, Gangneung (Korea, Republic of); Chang, Young-Tae [National University of Singapore, Singapore (Singapore); Lee, Jae Wook [University of Science and Technology, Daejon (Korea, Republic of)

2015-01-15

In combinatorial chemistry, solid-phase synthesis is a popular approach formass production of small molecules. Compared to solution-phase synthesis, it is easy to prepare and purify a large number of heterocyclic small molecules via solid-phase chemistry; the overall reaction time is decreased as well. 1,3,5-Triazine is a nitrogen-containing heterocyclic aromatic scaffold that was shown to be a druggable scaffold in recent studies. These structures have been reported as anticancer, antimicrobial, and antiretroviral compounds, as CDKs and p38 MAP kinase inhibitors, as estrogen receptor modulators, and as inosine monophosphate dehydrogenase inhibitors. we designed and synthesized disubstituted triazine compounds as an analog of disubstituted pyrimidine compounds. These disubstituted triazine compounds possess a linear structure which may have biological activity similar to that of disubstituted pyrimidine. Here we report the solid-phase synthesis of disubstituted triazine compounds.

Solid-phase Synthesis of Combinatorial 2,4-Disubstituted-1,3,5-Triazine via Amine Nucleophilic Reaction

International Nuclear Information System (INIS)

Moon, Sung Won; Ham, Jungyeob; Chang, Young-Tae; Lee, Jae Wook

2015-01-01

In combinatorial chemistry, solid-phase synthesis is a popular approach formass production of small molecules. Compared to solution-phase synthesis, it is easy to prepare and purify a large number of heterocyclic small molecules via solid-phase chemistry; the overall reaction time is decreased as well. 1,3,5-Triazine is a nitrogen-containing heterocyclic aromatic scaffold that was shown to be a druggable scaffold in recent studies. These structures have been reported as anticancer, antimicrobial, and antiretroviral compounds, as CDKs and p38 MAP kinase inhibitors, as estrogen receptor modulators, and as inosine monophosphate dehydrogenase inhibitors. we designed and synthesized disubstituted triazine compounds as an analog of disubstituted pyrimidine compounds. These disubstituted triazine compounds possess a linear structure which may have biological activity similar to that of disubstituted pyrimidine. Here we report the solid-phase synthesis of disubstituted triazine compounds

Preparation of peptide thioesters through fmoc-based solid-phase peptide synthesis by using amino thioesters

DEFF Research Database (Denmark)

Stuhr-Hansen, N.; Wilbek, T.S.; Strømgaard, K.

2013-01-01

protected peptide thioester, which was globally deprotected to afford the desired unprotected peptide thioester. The method is compatible with labile groups such as phosphoryl and glycosyl moieties. The synthesis of peptide alkyl thioesters by 9-fluorenylmethoxycarbonyl (Fmoc) solid-phase peptide synthesis...

Solid-phase synthesis of head and tail bis-acridinylated peptides

Czech Academy of Sciences Publication Activity Database

Šebestík, Jaroslav; Matějka, P.; Hlaváček, Jan; Stibor, I.

2004-01-01

Roč. 45, č. 6 (2004), s. 1203-1205 ISSN 0040-4039 R&D Projects: GA ČR GA203/02/1379 Institutional research plan: CEZ:AV0Z4055905 Keywords : 9-amino acridine * solid phase synthesis * head and tail peptide conjugates Subject RIV: CC - Organic Chemistry Impact factor: 2.484, year: 2004

Solid-solid synthesis and structural phase transition process of SmF3

Science.gov (United States)

Yan, Qi-Cao; Guo, Xing-Min

2018-04-01

Mazes of contradictory conclusions have been obtained by previous researches about structural phase transition process of SmF3. In this paper, the single crystals of SmF3 (hexagonal and orthorhombic) were prepared by solid-solid synthesis, which have shown gradual changes in crystal growth modes with the increase temperature and holding time. Furthermore, we propose the phase transition process of in SmF3. Hexagonal symmetry of SmF3 (space group Pnma) was prepared firstly by heating Sm2O3 and NH4HF2 over 40 min at 270 °C. And then orthorhombic symmetry of SmF3 (space group P63mc) was obtained by heating hexagonal symmetry over 10 h at 650 °C. The reaction of SmF3 (hexagonal) = SmF3 (orthorhombic) is extremely sluggish at a low temperature (less than 650 °C), which was seen as a Mixed Grown Region.

Investigation into process of solid-phase synthesis of calcium vanadates

International Nuclear Information System (INIS)

Fotiev, A.A.; Krasnenko, T.I.; Slobodin, B.V.

1983-01-01

Processes of solid-phase synthesis of calcium vanadates by Toubandt method, measuring electric conductivity and Ca 45 and V 48 radioactive indicators are investigated. It is shown that reaction diffusion during calcium vanadates production from oxides is ensured by calcium and oxygen ions or calcium ions and electrons through the product layer, as to oxygen - through the gas phase

Modern methods for the synthesis of peptide-oligonucleotide conjugates

International Nuclear Information System (INIS)

Zubin, Evgenii M; Oretskaya, Tat'yana S; Romanova, Elena A

2002-01-01

The published data on the methods of chemical solution and solid-phase synthesis of peptide-oligonucleotide conjugates are reviewed. The known methods are systematised and their advantages and disadvantages are considered. The approaches to the solution synthesis of peptide-oligonucleotide conjugates are systematised according to the type of chemical bonds between the fragments, whereas those to the solid-phase synthesis are classified according to the procedure used for the preparation of conjugates, viz., stepwise elongation of oligonucleotide and peptide chains on the same polymeric support or solid-phase condensation of two presynthesised fragments. The bibliography includes 141 references.

Paraffin scintillator for radioassay of solid support samples

International Nuclear Information System (INIS)

Fujii, Haruo; Takiue, Makoto

1989-01-01

A new paraffin scintillator used for solid support sample counting has been proposed, and its composition and various characteristics are described. The solid support sample treated with this scintillator can be easily handled because of rigid sample conditions. This technique provides great advantages such as the elimination of a large volume of scintillator and little radioactive waste material by using an economical polyethylene bag instead of the conventional counting vial. (author)

Solid polymer electrolyte composite membrane comprising plasma etched porous support

Science.gov (United States)

Liu, Han; LaConti, Anthony B.

2010-10-05

A solid polymer electrolyte composite membrane and method of manufacturing the same. According to one embodiment, the composite membrane comprises a rigid, non-electrically-conducting support, the support preferably being a sheet of polyimide having a thickness of about 7.5 to 15 microns. The support has a plurality of cylindrical pores extending perpendicularly between opposing top and bottom surfaces of the support. The pores, which preferably have a diameter of about 0.1 to 5 microns, are made by plasma etching and preferably are arranged in a defined pattern, for example, with fewer pores located in areas of high membrane stress and more pores located in areas of low membrane stress. The pores are filled with a first solid polymer electrolyte, such as a perfluorosulfonic acid (PFSA) polymer. A second solid polymer electrolyte, which may be the same as or different than the first solid polymer electrolyte, may be deposited over the top and/or bottom of the first solid polymer electrolyte.

Solid polymer electrolyte composite membrane comprising laser micromachined porous support

Science.gov (United States)

Liu, Han [Waltham, MA; LaConti, Anthony B [Lynnfield, MA; Mittelsteadt, Cortney K [Natick, MA; McCallum, Thomas J [Ashland, MA

2011-01-11

A solid polymer electrolyte composite membrane and method of manufacturing the same. According to one embodiment, the composite membrane comprises a rigid, non-electrically-conducting support, the support preferably being a sheet of polyimide having a thickness of about 7.5 to 15 microns. The support has a plurality of cylindrical pores extending perpendicularly between opposing top and bottom surfaces of the support. The pores, which preferably have a diameter of about 5 microns, are made by laser micromachining and preferably are arranged in a defined pattern, for example, with fewer pores located in areas of high membrane stress and more pores located in areas of low membrane stress. The pores are filled with a first solid polymer electrolyte, such as a perfluorosulfonic acid (PFSA) polymer. A second solid polymer electrolyte, which may be the same as or different than the first solid polymer electrolyte, may be deposited over the top and/or bottom of the first solid polymer electrolyte.

Silica-Supported Polyphosphoric Acid in the Synthesis of 4-Substituted Tetrahydroisoquinoline Derivatives

Directory of Open Access Journals (Sweden)

Iliyan Ivanov

2013-02-01

Full Text Available We report herein an application of an α-amidoalkylation reaction, as an alternative efficient synthesis of 4-aryl- and 4-methyl-1,2,3,4-tetrahydroisoquinoline derivatives. The amides required for this purpose would result from reaction of aminoacetaldehyde dimethylacetal with different substituted benzenes in polyphosphoric acid, followed by acylation of the obtained amines with different acid chlorides or sulfochlorides. We compared the cyclisation step using conventional (milieu of acetic-trifluoracetic acid = 4:1 and solid supported reagents (SiO2/PPA, as recovered, regenerated and reused without loss of its activity catalyst. We found that in comparison to conventional methods, the yields of the reaction are greater and the reaction time is shorter.

Production of fungal antibiotics using polymeric solid supports in solid-state and liquid fermentation.

Science.gov (United States)

Bigelis, Ramunas; He, Haiyin; Yang, Hui Y; Chang, Li-Ping; Greenstein, Michael

2006-10-01

The use of inert absorbent polymeric supports for cellular attachment in solid-state fungal fermentation influenced growth, morphology, and production of bioactive secondary metabolites. Two filamentous fungi exemplified the utility of this approach to facilitate the discovery of new antimicrobial compounds. Cylindrocarpon sp. LL-Cyan426 produced pyrrocidines A and B and Acremonium sp. LL-Cyan416 produced acremonidins A-E when grown on agar bearing moist polyester-cellulose paper and generated distinctly different metabolite profiles than the conventional shaken or stationary liquid fermentations. Differences were also apparent when tenfold concentrated methanol extracts from these fermentations were tested against antibiotic-susceptible and antibiotic-resistant Gram-positive bacteria, and zones of inhibition were compared. Shaken broth cultures of Acremonium sp. or Cylindrocarpon sp. showed complex HPLC patterns, lower levels of target compounds, and high levels of unwanted compounds and medium components, while agar/solid support cultures showed significantly increased yields of pyrrocidines A and B and acremonidins A-E, respectively. This method, mixed-phase fermentation (fermentation with an inert solid support bearing liquid medium), exploited the increase in surface area available for fungal growth on the supports and the tendency of some microorganisms to adhere to solid surfaces, possibly mimicking their natural growth habits. The production of dimeric anthraquinones by Penicillium sp. LL-WF159 was investigated in liquid fermentation using various inert polymeric immobilization supports composed of polypropylene, polypropylene cellulose, polyester-cellulose, or polyurethane. This culture produced rugulosin, skyrin, flavomannin, and a new bisanthracene, WF159-A, after fermentation in the presence and absence of polymeric supports for mycelial attachment. The physical nature of the different support systems influenced culture morphology and relative

A photolabile linker for the solid-phase synthesis of 4-substituted NH-1,2,3-triazoles

DEFF Research Database (Denmark)

Qvortrup, Katrine; Nielsen, Thomas Eiland

2011-01-01

A novel photolabile linker for solid-phase synthesis is presented. The linker displays an azido handle for copper-catalyzed azide–alkyne cycloaddition reactions with a variety of alkynes, remains intact under typical solid-phase reaction conditions, and enables a mild photolytic release of 4...

Solid-phase synthesis of an apoptosis-inducing tetrapeptide mimicking the Smac protein

DEFF Research Database (Denmark)

Le Quement, Sebastian Thordal; Ishøy, Mette; Petersen, Mette Terp

2011-01-01

An approach for the solid-phase synthesis of apoptosis-inducing Smac peptidomimetics is presented. Using a Rink linker strategy, tetrapeptides mimicking the N-4-terminal residue of the Smac protein [(N-Me)AVPF sequence] were synthesized on PEGA resin in excellent purities and yields. Following two...

Pyrolysis-GCMS Analysis of Solid Organic Products from Catalytic Fischer-Tropsch Synthesis Experiments

Science.gov (United States)

Locke, Darren R.; Yazzie, Cyriah A.; Burton, Aaron S.; Niles, Paul B.; Johnson, Natasha M.

2015-01-01

Abiotic synthesis of complex organic compounds in the early solar nebula that formed our solar system is hypothesized to occur via a Fischer-Tropsch type (FTT) synthesis involving the reaction of hydrogen and carbon monoxide gases over metal and metal oxide catalysts. In general, at low temperatures (less than 200 C), FTT synthesis is expected to form abundant alkane compounds while at higher temperatures (greater than 200 C) it is expected to product lesser amounts of n-alkanes and greater amounts of alkene, alcohol, and polycyclic aromatic hydrocarbons (PAHs). Experiments utilizing a closed-gas circulation system to study the effects of FTT reaction temperature, catalysts, and number of experimental cycles on the resulting solid insoluble organic products are being performed in the laboratory at NASA Goddard Space Flight Center. These experiments aim to determine whether or not FTT reactions on grain surfaces in the protosolar nebula could be the source of the insoluble organic matter observed in meteorites. The resulting solid organic products are being analyzed at NASA Johnson Space Center by pyrolysis gas chromatography mass spectrometry (PY-GCMS). PY-GCMS yields the types and distribution of organic compounds released from the insoluble organic matter generated from the FTT reactions. Previously, exploratory work utilizing PY-GCMS to characterize the deposited organic materials from these reactions has been reported. Presented here are new organic analyses using magnetite catalyst to produce solid insoluble organic FTT products with varying reaction temperatures and number of experimental cycles.

Solid-supported enzymatic synthesis of pectic oligogalacturonides and their analysis by MALDI-TOF mass spectrometry

DEFF Research Database (Denmark)

Guillaumie, Fanny; Sterling, J.D.; Jensen, K.J.

2003-01-01

Solid-phase biosynthetic reactions, followed by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry analysis (MALDI-TOF), was used to gain insight into the biosynthesis of pectin oligomers. Sepharose supports bearing long pectic oligogalacturonides (OGAs) anchored through...... into the liquid phases by MALDI-TOF mass spectrometry. In time course studies conducted with an immobilized (alpha-D-GalA)(14) and limiting amounts of the glycosyl donor, the predominant product was an OGA extended by one GalA residue at the non-reducing end (i.e., (GalA)(15)). When UDP-GalA was added...

Molecular phospholipid films on solid supports

DEFF Research Database (Denmark)

Czolkos, Ilja; Jesorka, Aldo; Orwar, Owe

2011-01-01

Phospholipid membranes are versatile structures for mimicking biological surfaces. Bilayer and monolayer membranes can be formed on solid supports, leading to enhanced stability and accessibility of the biomimetic molecular film. This has facilitated functional studies of membrane proteins and ai...

Synthesis and characterization of solid solutions in ABCO 4 system

Science.gov (United States)

Novoselov, A.; Zimina, G.; Komissarova, L.; Pajaczkowska, A.

2006-01-01

Formation of continuous solid solutions with a tetragonal structure of K 2NiF 4-type was investigated by direct solid-state synthesis, carbonate precipitations, the freeze-drying method and the Czochralski crystal growth technique. In the systems of SrLaAlO 4-CaLaAlO 4, SrNdAlO 4-CaNdAlO 4, SrPrAlO 4-CaPrAlO 4, SrLaAlO 4-SrLaGaO 4 and SrLaAlO 4-SrLaFeO 4 solid solutions are formed in the whole concentration range (0.0⩽ x⩽1.0) and in the systems of SrLaAlO 4-SrLaMnO 4 and SrLaAlO 4-SrLaCrO 4 in the limited compositional interval of (0.0⩽ x⩽0.20) and (0.0⩽ x⩽0.25), respectively, with composition dependency of lattice constants following Vegard's law.

Synthesis and comparison of the activities of a catalyst supported on two silicate materials

Energy Technology Data Exchange (ETDEWEB)

Vieira, Eduardo G., E-mail: eduardogv5007@gmail.com [Departamento de Física e Química, Unesp-Univ Estadual Paulista, Av. Brasil, 56-Centro, Caixa Postal 31, CEP 15385-000, Ilha Solteira, São Paulo (Brazil); Silva, Rafael O.; Carmo, Devaney R. do [Departamento de Física e Química, Unesp-Univ Estadual Paulista, Av. Brasil, 56-Centro, Caixa Postal 31, CEP 15385-000, Ilha Solteira, São Paulo (Brazil); Junior, Enes F. [Departamento de Fitotecnia, Tecnologia de Alimentos e Sócio Economia, Faculdade de Engenharia de Ilha Solteira, Universidade Estadual Paulista, Ilha Solteira, São Paulo (Brazil); Dias Filho, Newton L., E-mail: nldias@unesc.net [Departamento de Física e Química, Unesp-Univ Estadual Paulista, Av. Brasil, 56-Centro, Caixa Postal 31, CEP 15385-000, Ilha Solteira, São Paulo (Brazil); Universidade do Extremo Sul Catarinense, Av. Universitaria, 1105, CP 3167, CEP 88806-000, Criciúma, SC (Brazil)

2017-04-15

The focus of this work is inspecting the synthesis and comparison of the activities of a catalyst supported on two silicate materials in the epoxidation of 1-octene. The two new catalyst materials were characterized by infrared spectroscopy, elemental analysis, solid-state {sup 29}Si and {sup 13}C nuclear magnetic resonance, scanning electronic microscope (SEM) and analysis of nitrogen. Lastly, the two new catalysts, Silsesq-TCA-[(W(CO){sub 3}I{sub 2}){sub 3}] and Silica-TCA-[W(CO){sub 3}I{sub 2}] were tested as catalysts in reactions of epoxidation of 1-octene and compared with their analogue not supported [W(CO){sub 3}I{sub 2}(thiocarbamide)]. After an extensive literature search, we verified that our work is the first that has reported the immobilization process of [W(CO){sub 3}I{sub 2}(NCCH{sub 3}){sub 2}] on silsesquioxane and silica gel functionalized with propyl-thiocarbamide groups and their applications as catalysts of reactions of catalytic epoxidation of 1-octene. - Highlights: • Immobilization of [W(CO){sub 3}I{sub 2}(NCCH{sub 3}){sub 2}] complex onto mesoporous supports. • Synthesis and characterization of new mesoporous catalysts. • The new catalysts exhibit great catalytic activity in the epoxidation of 1-octene. • Recyclable catalysts with excellent reusability and stability.

Silica sulfuric acid: a reusable solid catalyst for one pot synthesis of densely substituted pyrrole-fused isocoumarins under solvent-free conditions

Directory of Open Access Journals (Sweden)

Sudipta Pathak

2013-11-01

Full Text Available A convenient and efficient methodology for the synthesis of densely substituted pyrrole-fused isocoumarins, which employs solid-supported silica sulfuric acid (SSA as catalyst, has been developed. When the mixture of ninhydrin adducts of acetylacetone/ethyl acetoacetate and primary amines was heated on the solid surface of SSA under solvent-free conditions, the pyrrole-fused isocoumarins were formed in good yields. This synthetic method has several advantages such as the employment of solvent-free reaction conditions without the use of any toxic reagents and metal catalysts, the ease of product isolation, the use of a recyclable catalyst, the low cost, the easy availability of the starting materials, and the excellent yields of products.

Polymer-Induced Swelling of Solid-Supported Lipid Membranes

Directory of Open Access Journals (Sweden)

Martin Kreuzer

2015-12-01

Full Text Available In this paper, we study the interaction of charged polymers with solid-supported 1,2-dimyristoyl-sn-glycero-3-phosphocholine (DMPC membranes by in-situ neutron reflectivity. We observe an enormous swelling of the oligolamellar lipid bilayer stacks after incubation in solutions of poly(allylamine hydrochloride (PAH in D2O. The positively charged polyelectrolyte molecules interact with the lipid bilayers and induce a drastic increase in their d-spacing by a factor of ~4. Temperature, time, and pH influence the swollen interfacial lipid linings. From our study, we conclude that electrostatic interactions introduced by the adsorbed PAH are the main cause for the drastic swelling of the lipid coatings. The DMPC membrane stacks do not detach from their solid support at T > Tm. Steric interactions, also introduced by the PAH molecules, are held responsible for the stabilizing effect. We believe that this novel system offers great potential for fundamental studies of biomembrane properties, keeping the membrane’s natural fluidity and freedom, decoupled from a solid support at physiological conditions.

Direct Synthesis of Co-doped Graphene on Dielectric Substrates Using Solid Carbon Sources

Institute of Scientific and Technical Information of China (English)

Qi Wang; Pingping Zhang; Qiqi Zhuo; Xiaoxin Lv; Jiwei Wang; Xuhui Sun

2015-01-01

Direct synthesis of high-quality doped graphene on dielectric substrates without transfer is highly desired for simplified device processing in electronic applications.However,graphene synthesis directly on substrates suitable for device applications,though highly demanded,remains unattainable and challenging.Here,a simple and transfer-free synthesis of high-quality doped graphene on the dielectric substrate has been developed using a thin Cu layer as the top catalyst and polycyclic aromatic hydrocarbons as both carbon precursors and doping sources.N-doped and N,F-co-doped graphene have been achieved using TPB and F16Cu Pc as solid carbon sources,respectively.The growth conditions were systematically optimized and the as-grown doped graphene were well characterized.The growth strategy provides a controllable transfer-free route for high-quality doped graphene synthesis,which will facilitate the practical applications of graphene.

Nanocrystal conversion chemistry: A unified and materials-general strategy for the template-based synthesis of nanocrystalline solids

International Nuclear Information System (INIS)

Vasquez, Yolanda; Henkes, Amanda E.; Chris Bauer, J.; Schaak, Raymond E.

2008-01-01

The concept of nanocrystal conversion chemistry, which involves the use of pre-formed nanoparticles as templates for chemical transformation into derivative solids, has emerged as a powerful approach for designing the synthesis of complex nanocrystalline solids. The general strategy exploits established synthetic capabilities in simple nanocrystal systems and uses these nanocrystals as templates that help to define the composition, crystal structure, and morphology of product nanocrystals. This article highlights key examples of 'conversion chemistry' approaches to the synthesis of nanocrystalline solids using a variety of techniques, including galvanic replacement, diffusion, oxidation, and ion exchange. The discussion is organized according to classes of solids, highlighting the diverse target systems that are accessible using similar chemical concepts: metals, oxides, chalcogenides, phosphides, alloys, intermetallic compounds, sulfides, and nitrides. - Graphical abstract: Nanocrystal conversion chemistry uses pre-formed nanoparticles as templates for chemical transformation into derivative solids, helping to define the composition, crystal structure, and morphology of product nanocrystals that have more complex features than their precursor templates. This article highlights the application of this concept to diverse classes of solids, including metals, oxides, chalcogenides, phosphides, alloys, intermetallics, sulfides, and nitrides

Synthesis and microstructural characterization of Sr- and Mg-substituted LaGaO3 solid electrolyte

International Nuclear Information System (INIS)

Datta, Pradyot; Majewski, Peter; Aldinger, Fritz

2007-01-01

Sr and Mg substituted LaGaO 3 is a solid electrolyte for intermediate temperature solid oxide fuel cell. Phase purity of this material is a concern for the researchers for a long time. In this contribution the secondary phases that are evolved during the synthesis of Sr and Mg doped LaGaO 3 are reported. For that purpose, a series of La 1-x Sr x Ga 1-y Mg y O 3-δ (LSGM) was prepared by solid state synthesis route. Scanning electron microscopic photographs showed secondary phases namely La 4 Ga 2 O 9 , LaSrGa 3 O 7 , LaSrGaO 4 along with the parent perovskite LSGM depending upon the amount of dopant. Amount of secondary phases was estimated from the peak positions of room temperature X-ray diffraction. It was observed that for a fixed amount of Mg dopant increasing the amount of Sr content also increased the amount of secondary phases whereas the reverse was found to be true when Sr content was fixed and Mg content was increased. This behaviour was attributed to the increase in solid solubility of Sr in presence of Mg

Synthesis, Anticonvulsant Activity and In silco Studies of Schiff ...

African Journals Online (AJOL)

Georgette M, Castanedo, Daniel PS. Synthesis of tetrasubstituted thiophenes on solid support using the Gewald reaction.Tetrahedron lett 2001; 42: 7181-7184. 11. Pushyamitra M, Hardesh K, Maurya, Brijesh K, Vishnu. K, Tandon, Vishnu JR. synthesis of thiophenes and pyranone fused thiophenes by base induced inter.

An efficient method for the synthesis of phenacyl ester-protected dipeptides using neutral alumina-supported sodium carbonate 'Na2 CO3 /n-Al2 O3 '.

Science.gov (United States)

Hashimoto, Chikao; Sugimoto, Kazuhiro; Takahashi, Youhei; Kodomari, Mitsuo

2013-10-01

In the synthesis of dipeptides (Boc-AA(1)-AA(2)-OPac: AA(1) and AA(2) represent amino acids) protected by phenacyl (Pac) ester, amines and solid bases as the base for the conversion of the trifluoroacetic acid (TFA) salt of the amino component (TFA·H-AA(2)-OPac) into the corresponding free amino component (H-AA(2)-OPac) were examined. The synthesis of a dipeptide (Boc-Ala-Gly-OPac) using amines for the conversion afforded an unsatisfactory yield with by-products. On the other hand, the use of neutral alumina-supported Na(2) CO(3) (Na(2)CO(3) /n-Al(2)O(3)) as a solid base for the conversion provided the dipeptide in a quantitative yield without by-products. The application of Na(2)CO(3) /n-Al2 O3 to the synthesis of some dipeptides protected by Pac ester gave the desired peptides in excellent yields. Copyright © 2013 European Peptide Society and John Wiley & Sons, Ltd.

Solid-State NMR and DFT Studies on the Formation of Well-Defined Silica-Supported Tantallaaziridines: From Synthesis to Catalytic Application

KAUST Repository

Hamzaoui, Bilel; Pelletier, Jeremie; Abou-Hamad, Edy; Chen, Yin; El Eter, Mohamad; Chermak, Edrisse; Cavallo, Luigi; Basset, Jean-Marie

2016-01-01

spectroscopy, elemental analysis, and 1H,13C HETCOR and DQ TQ solid-state (SS) NMR spectroscopy. The formation mechanism, by β-H abstraction, was investigated by SS NMR spectroscopy and supported by DFT calculations. The C-H activation of the dimethylamide

A convenient procedure for the solid-phase synthesis of hydroxamic acids on PEGA resins

DEFF Research Database (Denmark)

Nandurkar, Nitin Subhash; Petersen, Rico; Qvortrup, Katrine

2011-01-01

An efficient method for the solid-phase synthesis of hydroxamic acids is described. The method comprises the nucleophilic displacement of esters immobilized on PEGA resins with hydroxylamine/sodium hydroxide in isopropanol. The hydroxyaminolysis protocol is compatible with a broad range of PEGA...

Low Temperature Solid-State Synthesis and Characterization of LaBO3

Directory of Open Access Journals (Sweden)

Azmi Seyhun KIPÇAK

2016-11-01

Full Text Available Rare earth (lanthanide series borates, possess high vacuum ultraviolet (VUV transparency, large electronic band gaps, chemical and environmental stability and exceptionally large optical damage thresholds and used in the development of plasma display panels (PDPs. In this study the synthesis of lanthanum borates via solid-state method is studied. For this purpose, lanthanum oxide (La2O3 and boric acid (H3BO3 are used for as lanthanum and boron sources, respectively. Different elemental molar ratios of La to B (between 3:1 to 1:6 as La2O3:H3BO3 were reacted by solid-state method at the reaction temperatures between 500°C - 700°C with the constant reaction time of 4 h. Following the synthesis, characterizations of the synthesized products are conducted by X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FT-IR, Raman spectroscopy and scanning electron microscope (SEM. From the results of the experiments, three types of lanthanum borates of; La3BO6, LaBO3 and La(BO23 were observed at different reaction parameters. Among these three types of lanthanum borates LaBO3 phase were obtained as a major phase.

Synthesis and characterization of a homogeneous and silica supported homoleptic cationic tungsten(vi) methyl complex: application in olefin metathesis

KAUST Repository

Dey, Raju

2016-08-19

A method for the synthesis of a homogeneous cationic tungsten(VI)penta-methyl complex [(WMe5)(+)(C6F5)(3)BMe-] from neutral tungstenhexamethyl (WMe6) and a silica supported cationic tungstentetramethyl complex [( Si-O-)WMe4+ (C6F5)(3)BMe-] from a neutral silica supported tungstenpentamethyl complex [( Si-O-)WMe5] is described. In both cases a direct demethylation using the B(C6F5)(3) reagent was used. The aforesaid complexes were characterized by liquid or solid state NMR spectroscopy. Interestingly, the homogeneous cationic complex [(WMe5)(+)(C6F5)(3)BMe-] shows moderate activity whereas the supported cationic complex [( Si-O-)WMe4+(C6F5)(3)BMe-] exhibits good activity in olefin metathesis reactions.

Synthesis and characterization of a homogeneous and silica supported homoleptic cationic tungsten(vi) methyl complex: application in olefin metathesis

KAUST Repository

Dey, Raju; Samantaray, Manoja; Poater, Albert; Hamieh, Ali Imad Ali; Kavitake, Santosh Giridhar; Abou-Hamad, Edy; Callens, Emmanuel; Emwas, Abdul-Hamid M.; Cavallo, Luigi; Basset, Jean-Marie

2016-01-01

A method for the synthesis of a homogeneous cationic tungsten(VI)penta-methyl complex [(WMe5)(+)(C6F5)(3)BMe-] from neutral tungstenhexamethyl (WMe6) and a silica supported cationic tungstentetramethyl complex [( Si-O-)WMe4+ (C6F5)(3)BMe-] from a neutral silica supported tungstenpentamethyl complex [( Si-O-)WMe5] is described. In both cases a direct demethylation using the B(C6F5)(3) reagent was used. The aforesaid complexes were characterized by liquid or solid state NMR spectroscopy. Interestingly, the homogeneous cationic complex [(WMe5)(+)(C6F5)(3)BMe-] shows moderate activity whereas the supported cationic complex [( Si-O-)WMe4+(C6F5)(3)BMe-] exhibits good activity in olefin metathesis reactions.

The complex synthesis and solid state chemistry of ceria-lanthana solid solutions prepared via a hexamethylenetetramine precipitation

International Nuclear Information System (INIS)

Fleming, P.G.; Holmes, J.D.; Otway, D.J.; Morris, M.A.

2011-01-01

Mixed oxide solid solutions are becoming ever more commercially important across a range of applications. However, their synthesis can be problematical. Here, we show that ceria-lanthana solid solutions can be readily prepared via simple precipitation using hexamethylenetetramine. However, the solution chemistry can be complex, which results in the precipitated particles having a complex structure and morphology. Great care must be taken in both the synthesis and characterisation to quantify the complexity of the product. Even very high heat treatments were not able to produce highly homogeneous materials and X-ray diffractions reveals the non-equilibrium form of particles prepared in this way. Unexpected crystal structures are revealed including a new metastable cubic La 2 O 3 phase. - Graphical abstract: The suggested mechanism for the formation of dual fluorite phase particles, where Step 1 corresponds to room temperature aging, Step 2; heating the solution to 90 deg. C, Step 3; cooling of the solution to room temperature, Step 4; calcination to 500 deg. C, Step 5; calcination to 700 deg. C and Step 6; calcination to 1300 deg. C. The terminology of e.g. La 1-x Ce x (OH) 3 is used to indicate the formation of a mixed oxy-hydroxy participate rather than a definitive assignment of stoichiometry. Similarly, La 1-y Ce y O 2 only implies a mixed solid solution. Highlights: → Mol% of prepared Ce-La oxides did not follow that of reactant mol%. → Complex reaction pathway found to be dependent on metal solution concentrations. → At certain concentrations core shell particles were found to form. → A reaction model was produced based on cationic solubility. → Report lanthana solubility higher than previously reported in CeO 2 .

Synthesis of Dimethyl Glutarate from Cyclobutanone and Dimethyl Carbonate over Solid Base Catalysts

International Nuclear Information System (INIS)

Zhi, Chen; Dudu, Wu

2012-01-01

A facile route for the synthesis of dimethyl glutarate (DMG) from cyclobutanone and dimethyl carbonate (DMC) in the presence of solid base catalysts has been developed. It was found that the intermediate carbomethoxycyclobutanone (CMCB) was produced from cyclobutanone with DMC in the first step, and then CMCB was further converted to DMG by reacting with a methoxide group. The role of the basic catalysts can be mainly ascribed to the activation of cyclobutanone via the abstraction of a proton in the α-position by base sites, and solid bases with moderate strength, such as MgO, favor the formation of DMG

Synthesis of Dimethyl Glutarate from Cyclobutanone and Dimethyl Carbonate over Solid Base Catalysts

Energy Technology Data Exchange (ETDEWEB)

Zhi, Chen; Dudu, Wu [Guangdong Medical College, Dongguan (China)

2012-06-15

A facile route for the synthesis of dimethyl glutarate (DMG) from cyclobutanone and dimethyl carbonate (DMC) in the presence of solid base catalysts has been developed. It was found that the intermediate carbomethoxycyclobutanone (CMCB) was produced from cyclobutanone with DMC in the first step, and then CMCB was further converted to DMG by reacting with a methoxide group. The role of the basic catalysts can be mainly ascribed to the activation of cyclobutanone via the abstraction of a proton in the {alpha}-position by base sites, and solid bases with moderate strength, such as MgO, favor the formation of DMG

Solid phase synthesis and antiprotozoal evaluation of di- and trisubstituted 5'-carboxamidoadenosine analogues.

Science.gov (United States)

Rodenko, Boris; Detz, Remko J; Pinas, Victorine A; Lambertucci, Catia; Brun, Reto; Wanner, Martin J; Koomen, Gerrit-Jan

2006-03-01

The rapid increase of resistance to drugs commonly used in the treatment of tropical diseases such as malaria and African sleeping sickness calls for the prompt development of new safe and efficacious drugs. The pathogenic protozoan parasites lack the capability of synthesising purines de novo and they take up preformed purines from their host through various transmembrane transporters. Adenosine derivatives constitute a class of potential therapeutics due to their selective internalisation by these transporters. Automated solid-phase synthesis can speed up the process of lead finding and we pursued the solid-phase synthesis of di- and trisubstituted 5'-carboxamidoadenosine derivatives by using a safety-catch approach. While efforts with Kenner's sulfonamide linker remained fruitless, successful application of the hydrazide safety-catch linker allowed the construction of two representative combinatorial libraries. Their antiprotozoal evaluation identified two compounds with promising activity: N(6)-benzyl-5'-N-phenylcarboxamidoadenosine with an IC(50) value of 0.91 microM against Trypanosoma brucei rhodesiense and N(6)-diphenylethyl-5'-phenylcarboxamidoadenosine with an IC(50) value of 1.8 microM against chloroquine resistant Plasmodium falciparum.

Synthesis of 2,4-disubstituted thiazole combinatorial unit on solid-phase: microwave assisted conversion of alcohol to amine monitored by FT-IR

International Nuclear Information System (INIS)

Antonow, Dyeison; Eifler-Lima, Vera Lucia; Mahler, S. Graciela; Serra, Gloria L.; Manta, Eduardo

2005-01-01

Microwave-assisted solid-phase synthesis of the 2,4-disubstituted thiazole 3 on Merrifield Resin is described. The hydroxyl moiety was converted to amine in five steps - including coupling and cleavage - within a total reaction time of 2 hours and 26% overall yield. The entire solid-phase synthesis was efficiently monitored by FT-IR/KBr pellets and allows potential use in combinatorial chemistry. (author)

Radiolabelled neurotensin analogues. I. Solid phase synthesis and biological characterization of [Trp11]-neurotensin precursor of an ionidated ligand

International Nuclear Information System (INIS)

Labbe-Jullie, C.; Granier, C.; Van Rietschoten, J.; Kitabgi, P.; Vincent, J.P.

1983-01-01

In order to generate highly labelled neurotensin analogues, synthesis has been performed of two types of precursors, one for iodination and one for tritiation. Iodination of native neurotensin occurs on both tyrosines in position 3 and 11 and thus affects greatly its binding capacities. Synthesis and chemical characterization of [Trp 11 ]-neurotensin are described which can be iodinated without loss of activity. Synthesis was by solid phase procedure on an experimental support, Pab-resin, α-(4-chloromethylphenylacetamido)-benzyl copoly (styrene 1 per cent divinylbenzene). The homogeneity of [Trp 11 ]-neurotensin was assessed by amino acid analysis, high voltage paper electrophoresis and high pressure liquid chromatography. Iodination by the lactoperoxydase method gave iodo-[Trp 11 ]-neurotensin iodinated on the Tyr 3 . Compared to neurotensin, potency of [Trp 11 ]-neurotensin and of iodo-[Trp 11 ]-neurotensin in competitive inhibition of tritiated neurotensin binding to rat brain synaptic membranes was respectively 93 per cent and 80 per cent, but in the biological test on the contractility of isolated longitudinal smooth muscle strips of guinea pig the relative activity for the two analogues was of 10 per cent [fr

Convergent solid-phase and solution approaches in the synthesis of the cysteine-rich Mdm2 RING finger domain.

Science.gov (United States)

Vasileiou, Zoe; Barlos, Kostas; Gatos, Dimitrios

2009-12-01

The RING finger domain of the Mdm2, located at the C-terminus of the protein, is necessary for regulation of p53, a tumor suppressor protein. The 48-residues long Mdm2 peptide is an important target for studying its interaction with small anticancer drug candidates. For the chemical synthesis of the Mdm2 RING finger domain, the fragment condensation on solid-phase and the fragment condensation in solution were studied. The latter method was performed using either protected or free peptides at the C-terminus as the amino component. Best results were achieved using solution condensation where the N-component was applied with the C-terminal carboxyl group left unprotected. The developed method is well suited for large-scale synthesis of Mdm2 RING finger domain, combining the advantages of both solid-phase and solution synthesis. (c) 2009 European Peptide Society and John Wiley & Sons, Ltd.

Strength of Anode‐Supported Solid Oxide Fuel Cells

DEFF Research Database (Denmark)

Faes, A.; Frandsen, Henrik Lund; Kaiser, Andreas

2011-01-01

Nickel oxide and yttria doped zirconia composite strength is crucial for anode‐supported solid oxide fuel cells, especially during transient operation, but also for the initial stacking process, where cell curvature after sintering can cause problems. This work first compares tensile and ball....... Even though the electrolyte is to the tensile side, it is found that the anode support fails due to the thermo‐mechanical residual stresses....

Chemical cleavage reactions of DNA on solid support: application in mutation detection

Directory of Open Access Journals (Sweden)

Cotton Richard GH

2003-05-01

Full Text Available Abstract Background The conventional solution-phase Chemical Cleavage of Mismatch (CCM method is time-consuming, as the protocol requires purification of DNA after each reaction step. This paper describes a new version of CCM to overcome this problem by immobilizing DNA on silica solid supports. Results DNA test samples were loaded on to silica beads and the DNA bound to the solid supports underwent chemical modification reactions with KMnO4 (potassium permanganate and hydroxylamine in 3M TEAC (tetraethylammonium chloride solution. The resulting modified DNA was then simultaneously cleaved by piperidine and removed from the solid supports to afford DNA fragments without the requirement of DNA purification between reaction steps. Conclusions The new solid-phase version of CCM is a fast, cost-effective and sensitive method for detection of mismatches and mutations.

Solid state multinuclear NMR. A versatile tool for studying the reactivity of solid systems

Energy Technology Data Exchange (ETDEWEB)

MacKenzie, Kenneth J.D. [MacDiarmid Institute for Advanced Materials and Nanotechnology, Victoria University of Wellington, P.O. Box 600, Wellington (New Zealand)

2004-08-31

Traditionally, X-ray powder diffraction has been a favoured method for studying chemical reactions in the solid state, but the increasing importance of energy-efficient synthesis methods for solids (e.g. sol-gel synthesis, mechanochemical synthesis) has led to the need for an analytical method not dependent on long-range structural periodicity. Multinuclear solid state nuclear magnetic resonance (NMR) represents a technique which is equally applicable to amorphous or crystalline solids, and is now used in increasing numbers of solid state studies.This paper briefly outlines the principles and practical details of this powerful technique and gives examples of its use in solid-state chemistry, particularly in very recent studies of mechanochemical synthesis of advanced sialon ceramics. The temperature at which these technically important silicon aluminium oxynitride compounds are formed can be significantly lowered by high-energy grinding of their components to produce X-ray amorphous precursors. Solid-state NMR has been used to provide detailed information which could not have been obtained by any other means about the chemical environment of the Si and Al atoms in these amorphous precursors, and the various atomic movements undergone as they crystallise to the final product.

Covalent attachment of proteins to solid supports and surfaces via Sortase-mediated ligation.

Directory of Open Access Journals (Sweden)

Lilyan Chan

Full Text Available BACKGROUND: There is growing interest in the attachment of proteins to solid supports for the development of supported catalysts, affinity matrices, and micro devices as well as for the development of planar and bead based protein arrays for multiplexed assays of protein concentration, interactions, and activity. A critical requirement for these applications is the generation of a stable linkage between the solid support and the immobilized, but still functional, protein. METHODOLOGY: Solid supports including crosslinked polymer beads, beaded agarose, and planar glass surfaces, were modified to present an oligoglycine motif to solution. A range of proteins were ligated to the various surfaces using the Sortase A enzyme of S. aureus. Reactions were carried out in aqueous buffer conditions at room temperature for times between one and twelve hours. CONCLUSIONS: The Sortase A transpeptidase of S. aureus provides a general, robust, and gentle approach to the selective covalent immobilization of proteins on three very different solid supports. The proteins remain functional and accessible to solution. Sortase mediated ligation is therefore a straightforward methodology for the preparation of solid supported enzymes and bead based assays, as well as the modification of planar surfaces for microanalytical devices and protein arrays.

The combined effects of additives and supports on the synthesis of oxygenates over supported rhodium

International Nuclear Information System (INIS)

Chuang, S.C.; Tian, Y.; Goodwin, J.G. Jr.; Wender, I.

1985-01-01

There are potential advantages in the use of synthesis gas for the selective synthesis of oxygenated compounds rather than of hydrocarbons. This is due to the more versatile applications and higher value of oxygenates compared with that of hydrocarbons. Rh is known to be active in catalyzing, both heterogeneously and homogeneously, the formation of oxygenated compounds from synthesis gas. In a heterogeneous reaction system, the activity and selectivity of Rh catalysts are very sensitive to the chemical environment of Rh. By modifying its chemical environment through the use of various supports and/or with the addition of different promoters, Rh can selectively produce mostly oxygenates or mostly hydrocarbons. Studies have been carried out aimed at delineating the possible routes and intermediates involved in the formation of oxygenates and the function of additives (alkali promoters) and supports in the synthesis of oxygenates. Among the unpromoted Rh, the C/sub 2/ oxygenate selectivity decreased in the order: Rh/SiO/sub 2/ > Rh/MgO > Rh/La/sub 2/O/sub 3/ > Rh black, Rh/TiO/sub 2/ > Rh/Al/sub 2/O/sub 3/. High pressures improve selectivity to C/sub 2/ oxygenate compounds. Suppression of hydrogenation and ethanol dehydration was identified as major effects of alkali promotion. CO insertion was found to be dependent on both alkali promoters and on the supports. Results of ethanol addition indicated that the alkali species are located on both the Rh metal and on the support. The reaction network of CO hydrogenation on variously promoted catalysts is delineated, and the effect of secondary reactions on the overall product distribution is discussed

The ortho backbone amide linker (o-BAL) is an easily prepared and highly acid-labile handle for solid-phase synthesis

DEFF Research Database (Denmark)

Boas, Ulrik; Brask, Jesper; Christensen, J.B.

2002-01-01

The tris(alkoxy)benzyl backbone amide linker (BAL) has found widespread application in solid-phase synthesis. The key intermediate for preparation of para BAL (p-BAL) is 2,6-dimethoxy-4-hydroxybenzaldehyde; several reports on its synthesis have appeared. However, the ortho analogue of the handle (o...

Study of the solid-solid surface adsorption of Eu2O3 on various Al2O3 supports

International Nuclear Information System (INIS)

Liu Rongchuan; Yu Zhi; Zhou Yuan; Yoshitake Yamazaki

1997-12-01

Solid-solid surface interactions of Eu 2 O 3 on various oxide substrates are investigated with X-ray and Moessbauer experiments. The results indicate that the interaction of Eu 2 O 3 on the complex support differs from that having simple support. An incorporation model is used to explain how Eu 2 O 3 disperses onto the surface of γ-alumina or η-alumina

Decision support models for solid waste management: Review and game-theoretic approaches

International Nuclear Information System (INIS)

Karmperis, Athanasios C.; Aravossis, Konstantinos; Tatsiopoulos, Ilias P.; Sotirchos, Anastasios

2013-01-01

Highlights: ► The mainly used decision support frameworks for solid waste management are reviewed. ► The LCA, CBA and MCDM models are presented and their strengths, weaknesses, similarities and possible combinations are analyzed. ► The game-theoretic approach in a solid waste management context is presented. ► The waste management bargaining game is introduced as a specific decision support framework. ► Cooperative and non-cooperative game-theoretic approaches to decision support for solid waste management are discussed. - Abstract: This paper surveys decision support models that are commonly used in the solid waste management area. Most models are mainly developed within three decision support frameworks, which are the life-cycle assessment, the cost–benefit analysis and the multi-criteria decision-making. These frameworks are reviewed and their strengths and weaknesses as well as their critical issues are analyzed, while their possible combinations and extensions are also discussed. Furthermore, the paper presents how cooperative and non-cooperative game-theoretic approaches can be used for the purpose of modeling and analyzing decision-making in situations with multiple stakeholders. Specifically, since a waste management model is sustainable when considering not only environmental and economic but also social aspects, the waste management bargaining game is introduced as a specific decision support framework in which future models can be developed

Decision support models for solid waste management: Review and game-theoretic approaches

Energy Technology Data Exchange (ETDEWEB)

Karmperis, Athanasios C., E-mail: athkarmp@mail.ntua.gr [Sector of Industrial Management and Operational Research, School of Mechanical Engineering, National Technical University of Athens, Iroon Polytechniou 9, 15780 Athens (Greece); Army Corps of Engineers, Hellenic Army General Staff, Ministry of Defence (Greece); Aravossis, Konstantinos; Tatsiopoulos, Ilias P.; Sotirchos, Anastasios [Sector of Industrial Management and Operational Research, School of Mechanical Engineering, National Technical University of Athens, Iroon Polytechniou 9, 15780 Athens (Greece)

2013-05-15

Highlights: ► The mainly used decision support frameworks for solid waste management are reviewed. ► The LCA, CBA and MCDM models are presented and their strengths, weaknesses, similarities and possible combinations are analyzed. ► The game-theoretic approach in a solid waste management context is presented. ► The waste management bargaining game is introduced as a specific decision support framework. ► Cooperative and non-cooperative game-theoretic approaches to decision support for solid waste management are discussed. - Abstract: This paper surveys decision support models that are commonly used in the solid waste management area. Most models are mainly developed within three decision support frameworks, which are the life-cycle assessment, the cost–benefit analysis and the multi-criteria decision-making. These frameworks are reviewed and their strengths and weaknesses as well as their critical issues are analyzed, while their possible combinations and extensions are also discussed. Furthermore, the paper presents how cooperative and non-cooperative game-theoretic approaches can be used for the purpose of modeling and analyzing decision-making in situations with multiple stakeholders. Specifically, since a waste management model is sustainable when considering not only environmental and economic but also social aspects, the waste management bargaining game is introduced as a specific decision support framework in which future models can be developed.

A Facile Synthesis of Hollow Palladium/Copper Alloy Nanocubes Supported on N-Doped Graphene for Ethanol Electrooxidation Catalyst

Directory of Open Access Journals (Sweden)

Zhengyu Bai

2015-04-01

Full Text Available In this paper, a catalyst of hollow PdCu alloy nanocubes supported on nitrogen-doped graphene support (H-PdCu/ppy-NG is successfully synthesized using a simple one-pot template-free method. Two other catalyst materials such as solid PdCu alloy particles supported on this same nitrogen-doped graphene support (PdCu/ppy-NG and hollow PdCu alloy nanocubes supported on the reduced graphene oxide support (H-PdCu/RGO are also prepared using the similar synthesis conditions for comparison. It is found that, among these three catalyst materials, H-PdCu/ppy-NG gives the highest electrochemical active area and both the most uniformity and dispersibility of H-PdCu particles. Electrochemical tests show that the H-PdCu/ppy-NG catalyst can give the best electrocatalytic activity and stability towards the ethanol electrooxidation when compared to other two catalysts. Therefore, H-PdCu/ppy-NG should be a promising catalyst candidate for anodic ethanol oxidation in direct ethanol fuel cells.

A Linker for the Solid-Phase Synthesis of Hydroxamic Acids and Identification of HDAC6 Inhibitors

DEFF Research Database (Denmark)

Bang, Claus Gunnar; Jensen, Jakob Feldthusen; Cohrt, Anders Emil O'Hanlon

2017-01-01

We herein present broadly useful, readily available and nonintegral hydroxylamine linkers for the routine solid-phase synthesis of hydroxamic acids. The developed protocols enable the efficient synthesis and release of a wide range of hydroxamic acids from various resins, relying on high control...... and flexibility with respect to reagents and synthetic processes. A trityl-based hydroxylamine linker was used to synthesize a library of peptide hydroxamic acids. The inhibitory effects of the compounds were examined for seven HDAC enzyme subtypes using a chemiluminescence-based assay....

Modeling and Synthesis Support for the North American Carbon Program

Science.gov (United States)

Baskaran, L.; Cook, R. B.; Thornton, P. E.; Post, W. M.; Wilson, B. E.; Dadi, U.

2007-12-01

The Modeling and Synthesis Thematic Data Center (MAST-DC) supports the North American Carbon Program by providing data products and data management services needed for modeling and synthesis activities. The overall objective of MAST-DC is to provide advanced data management support to NACP investigators doing modeling and synthesis, thereby freeing those investigators from having to perform data management functions. MAST-DC has compiled a number of data products for North America, including sub-pixel land-water content, daily meteorological data, and soil, land cover, and elevation data. In addition, we have developed an internet-based WebGIS system that enables users to browse, query, display, subset, and download spatial data using a standard web browser. For the mid-continent intensive, MAST-DC is working with a group of data assimilation modelers to generate a consistent set of meteorological data to drive bottom-up models.

Solid polymer electrolyte composite membrane comprising a porous support and a solid polymer electrolyte including a dispersed reduced noble metal or noble metal oxide

Science.gov (United States)

Liu, Han; Mittelsteadt, Cortney K; Norman, Timothy J; Griffith, Arthur E; LaConti, Anthony B

2015-02-24

A solid polymer electrolyte composite membrane and method of manufacturing the same. According to one embodiment, the composite membrane comprises a thin, rigid, dimensionally-stable, non-electrically-conducting support, the support having a plurality of cylindrical, straight-through pores extending perpendicularly between opposing top and bottom surfaces of the support. The pores are unevenly distributed, with some or no pores located along the periphery and more pores located centrally. The pores are completely filled with a solid polymer electrolyte, the solid polymer electrolyte including a dispersed reduced noble metal or noble metal oxide. The solid polymer electrolyte may also be deposited over the top and/or bottom surfaces of the support.

Solid-State NMR and DFT Studies on the Formation of Well-Defined Silica-Supported Tantallaaziridines: From Synthesis to Catalytic Application

KAUST Repository

Hamzaoui, Bilel

2016-01-27

Single-site, well-defined, silica-supported tantallaaziridine intermediates [≡Si-O-Ta(η2-NRCH2)(NMe2)2] [R=Me (2), Ph (3)] were prepared from silica-supported tetrakis(dimethylamido)tantalum [≡Si-O-Ta(NMe2)4] (1) and fully characterized by FTIR spectroscopy, elemental analysis, and 1H,13C HETCOR and DQ TQ solid-state (SS) NMR spectroscopy. The formation mechanism, by β-H abstraction, was investigated by SS NMR spectroscopy and supported by DFT calculations. The C-H activation of the dimethylamide ligand is favored for R=Ph. The results from catalytic testing in the hydroaminoalkylation of alkenes were consistent with the N-alkyl aryl amine substrates being more efficient than N-dialkyl amines. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Automatic reactor for solid-phase synthesis of molecularly imprinted polymeric nanoparticles (MIP NPs) in water.

Science.gov (United States)

Poma, Alessandro; Guerreiro, Antonio; Caygill, Sarah; Moczko, Ewa; Piletsky, Sergey

We report the development of an automated chemical reactor for solid-phase synthesis of MIP NPs in water. Operational parameters are under computer control, requiring minimal operator intervention. In this study, "ready for use" MIP NPs with sub-nanomolar affinity are prepared against pepsin A, trypsin and α-amylase in only 4 hours.

Support Functionalization To Retard Ostwald Ripening in Copper Methanol Synthesis Catalysts

NARCIS (Netherlands)

van den Berg, Roy; Parmentier, Tanja E.; Elkjaer, Christian F.; Gommes, Cedric J.; Sehested, Jens; Helveg, Stig; de Jongh, Petra E.; de Jong, Krijn P.

A main reason for catalyst deactivation in supported catalysts for methanol synthesis is copper particle growth. We have functionalized the support surface in order to suppress the formation and/or transport of mobile copper species and thereby catalyst deactivation. A Stober silica support was

Automatic reactor for solid-phase synthesis of molecularly imprinted polymeric nanoparticles (MIP NPs) in water

OpenAIRE

Poma, Alessandro; Guerreiro, Antonio; Caygill, Sarah; Moczko, Ewa; Piletsky, Sergey

2014-01-01

We report the development of an automated chemical reactor for solid-phase synthesis of MIP NPs in water. Operational parameters are under computer control, requiring minimal operator intervention. In this study, “ready for use” MIP NPs with sub-nanomolar affinity are prepared against pepsin A, trypsin and α-amylase in only 4 hours.

Transport of Carbonate Ions by Novel Cellulose Fiber Supported Solid Membrane

Directory of Open Access Journals (Sweden)

A. G. Gaikwad

2012-06-01

Full Text Available Transport of carbonate ions was explored through fiber supported solid membrane. A novel fiber supported solid membrane was prepared by chemical modification of cellulose fiber with citric acid, 2′2-bipyridine and magnesium carbonate. The factors affecting the permeability of carbonate ions such as immobilization of citric acid-magnesium metal ion -2′2-bipyridine complex (0 to 2.5 mmol/g range over cellulose fiber, carbon-ate ion concentration in source phase and NaOH concentration in receiving phase were investigated. Ki-netic of carbonate, sulfate, and nitrate ions was investigated through fiber supported solid membrane. Transport of carbonate ions with/without bubbling of CO2 (0 to 10 ml/min in source phase was explored from source to receiving phase. The novel idea is to explore the adsorptive transport of CO2 from source to receiving phase through cellulose fiber containing magnesium metal ion organic framework. Copyright © 2012 BCREC UNDIP. All rights reserved.Received: 25th November 2011; Revised: 17th December 2011; Accepted: 19th December 2011[How to Cite: A.G. Gaikwad. (2012. Transport of Carbonate Ions by Novel Cellulose Fiber Supported Solid Membrane. Bulletin of Chemical Reaction Engineering & Catalysis, 7 (1: 49– 57.  doi:10.9767/bcrec.7.1.1225.49-57][How to Link / DOI: http://dx.doi.org/10.9767/bcrec.7.1.1225.49-57 ] | View in 

Microwave-Assisted Synthesis of Phenothiazine and Quinoline Derivatives

Science.gov (United States)

Găină, Luiza; Cristea, Castelia; Moldovan, Claudia; Porumb, Dan; Surducan, Emanoil; Deleanu, Călin; Mahamoud, Abdalah; Barbe, Jacques; Silberg, Ioan A.

2007-01-01

Application of a dynamic microwave power system in the chemical synthesis of some phenothiazine and quinoline derivatives is described. Heterocyclic ring formation, aromatic nucleophilic substitution and heterocyclic aldehydes/ketones condensation reactions were performed on solid support, or under solvent free reaction conditions. The microwave-assisted Duff formylation of phenothiazine was achieved. Comparison of microwave-assisted synthesis with the conventional synthetic methods demonstrates advantages related to shorter reaction times and in some cases better reaction yields.

Microwave-Assisted Synthesis of Phenothiazine and Qinoline Derivatives

Directory of Open Access Journals (Sweden)

Ioan A. Silberg

2007-02-01

Full Text Available Application of a dynamic microwave power system in the chemical synthesis ofsome phenothiazine and quinoline derivatives is described. Heterocyclic ring formation,aromatic nucleophilic substitution and heterocyclic aldehydes/ketones condensationreactions were performed on solid support, or under solvent free reaction conditions. Themicrowave-assisted Duff formylation of phenothiazine was achieved. Comparison ofmicrowave-assisted synthesis with the conventional synthetic methods demonstratesadvantages related to shorter reaction times and in some cases better reaction yields.

Solid state synthesis, crystal growth and optical properties of urea and p-chloronitrobenzene solid solution

Energy Technology Data Exchange (ETDEWEB)

Rai, R.N., E-mail: rn_rai@yahoo.co.in [Department of Chemistry, Centre of Advanced Study, Banaras Hindu University, Varanasi 221005 (India); Kant, Shiva; Reddi, R.S.B. [Department of Chemistry, Centre of Advanced Study, Banaras Hindu University, Varanasi 221005 (India); Ganesamoorthy, S. [Materials Science Group, Indira Gandhi Centre for Atomic Research, Kalpakkam 603102, Tamilnadu (India); Gupta, P.K. [Laser Materials Development & Devices Division, Raja Ramanna Centre for Advanced Technology, Indore 452013 (India)

2016-01-15

Urea is an attractive material for frequency conversion of high power lasers to UV (for wavelength down to 190 nm), but its usage is hindered due to its hygroscopic nature, though there is no alternative organic NLO crystal which could be transparent up to 190 nm. The hygroscopic character of urea has been modified by making the solid solution (UCNB) of urea (U) and p-chloronitrobenzene (CNB). The formation of the solid solution of CNB in U is explained on the basis of phase diagram, powder XRD, FTIR, elemental analysis and single crystal XRD studies. The solubility of U, CNB and UCNB in ethanol solution is evaluated at different temperatures. Transparent single crystals of UCNB are grown from its saturated solution in ethanol. Optical properties e.g., second harmonic generation (SHG), refractive index and the band gap for UCNB crystal were measured and their values were compared with the parent compounds. Besides modification in hygroscopic nature, UCNB has also shown the higher SHG signal and mechanical hardness in comparison to urea crystal. - Highlights: • The hygroscopic character of urea was modified by making the solid solution • Solid solution formation is support by elemental, powder- and single crystal XRD • Crystal of solid solution has higher SHG signal and mechanical stability. • Refractive index and band gap of solid solution crystal have determined.

Solid-phase synthesis of yttrium ferrites with structures of perovskite and garnet

Energy Technology Data Exchange (ETDEWEB)

Tkachenko, E V; Shapovalov, A G; Aksel' rod, N L; Pazdnikov, I P [Ural' skij Gosudarstvennyj Univ., Sverdlovsk (USSR)

1980-09-01

The solid phase synthesis of yttrium ferrites having a perovskite- and garnet-like structure has been investigated in the temperature range from 800 to 1500 deg C and temper times of up to 80 hours by reaction zone simulation and magnetic phase analysis. It is shown that for conversion degrees d<0.15 the reactions are diffusion-controlled. The rate constants and effective diffusion in the formation of YFeO/sub 3/ and Y/sub 3/Fe/sub 5/O/sub 12/ have been determined.

Mechanism of Formation of Li ₇ P ₃ S ₁₁ Solid Electrolytes through Liquid Phase Synthesis

Energy Technology Data Exchange (ETDEWEB)

Wang, Yuxing [Energy; Lu, Dongping [Energy; Bowden, Mark [Environmental; El Khoury, Patrick Z. [Environmental; Han, Kee Sung [Environmental; Deng, Zhiqun Daniel [Energy; Xiao, Jie [Energy; Zhang, Ji-Guang [Energy; Liu, Jun [Energy

2018-01-22

Crystalline Li7P3S11 is a promising solid electrolyte for all solid state lithium/lithium ion batteries. A controllable liquid phase synthesis of Li7P3S11 is more desirable compared to conventional mechanochemical synthesis, but recent attempts suffer from reduced ionic conductivities. Here we elucidate the formation mechanism of crystalline Li7P3S11 synthesized in the liquid phase (acetonitrile, or ACN). We conclude that the crystalline Li7P3S11 forms through a two-step reaction: 1) formation of solid Li3PS4∙ACN and amorphous Li2S∙P2S5 phases in the liquid phase; 2) solid-state conversion of the two phases. The implication of this two-step reaction mechanism to the morphology control and the transport properties of liquid phase synthesized Li7P3S11 is identified and discussed.

Perovskites synthesis for solid oxide fuel cells; Sintese de perovsquitas para celulas a combustivel de oxido solido

Energy Technology Data Exchange (ETDEWEB)

Soares, Sibelle F.C.X.; Melo, Dulce M.A.; Pimentel, Patricia M.; Melo, Marcus A. Freitas; Martinelli, Daniele M.H. [Universidade Federal do Rio Grande do Norte (UFRN), Natal, RN (Brazil). Dept. de Quimica]. E-mail: sibelle.cunha@gmail

2008-07-01

This work aims to study on the obtaining powders of lanthanum manganite oxides with partial substitution of La with strontium at 20% for the application as a cathode for solid oxide fuel cell, through a route of synthesis that are similar to the Pechini method, in which gelatin replaces the ethylene glycol as polymerization agent. The method highlights itself due to its simplicity, low cost and capability to obtain crystalline powders with the high purity and good stoichiometric control. The perovskite obtained were characterized by thermogravimetric analysis, X ray diffraction, electronic scanning microscopy and the superficial area by BET method. The deposition of the perovskite on electrolyte/anode system was done through the spin coating technique. The methodology used for the perovskite synthesis was very efficient, considering a monophasic material was obtained and with characteristics that were proper to the application as electrode to solid oxide fuel cells. (author)

Preparation of molybdenum borides by combustion synthesis involving solid-phase displacement reactions

International Nuclear Information System (INIS)

Yeh, C.L.; Hsu, W.S.

2008-01-01

Preparation of molybdenum borides of five different phases in the Mo-B binary system (including Mo 2 B, MoB, MoB 2 , Mo 2 B 5 , and MoB 4 ) was performed by self-propagating high-temperature synthesis (SHS) with two kinds of the reactant samples. When elemental powder compacts with an exact stoichiometry corresponding to the boride phase were employed, self-sustaining reaction was only achieved in the sample with Mo:B = 1:1 and nearly single-phase MoB was yielded. Therefore, the other four boride compounds were prepared from the reactant compacts composed of MoO 3 , Mo, and B powders, within which the displacement reaction of MoO 3 with boron was involved in combustion synthesis. Experimental evidence shows that the extent of displacement reaction in the overall reaction has a significant impact on sustainability of the synthesis reaction, combustion temperature, reaction front velocity, and composition of the end product. An increase in the solid-phase displacement reaction taking place during the SHS process contributes more heat flux to the synthesis reaction, thus resulting in the increase of combustion temperature and enhancement of the reaction front velocity. Based upon the XRD analysis, formation of Mo 2 B, MoB 2 , and Mo 2 B 5 as the dominant boride phase in the end product was successful through the SHS reaction with powder compacts under appropriate stoichiometries between MoO 3 , Mo, and B. However, a poor conversion was observed in the synthesis of MoB 4 . The powder compact prepared for the production of MoB 4 yielded mostly Mo 2 B 5

Partial Support Ventilation and Mitochondrial-Targeted Antioxidants Protect against Ventilator-Induced Decreases in Diaphragm Muscle Protein Synthesis.

Science.gov (United States)

Hudson, Matthew B; Smuder, Ashley J; Nelson, W Bradley; Wiggs, Michael P; Shimkus, Kevin L; Fluckey, James D; Szeto, Hazel H; Powers, Scott K

2015-01-01

Mechanical ventilation (MV) is a life-saving intervention in patients in respiratory failure. Unfortunately, prolonged MV results in the rapid development of diaphragm atrophy and weakness. MV-induced diaphragmatic weakness is significant because inspiratory muscle dysfunction is a risk factor for problematic weaning from MV. Therefore, developing a clinical intervention to prevent MV-induced diaphragm atrophy is important. In this regard, MV-induced diaphragmatic atrophy occurs due to both increased proteolysis and decreased protein synthesis. While efforts to impede MV-induced increased proteolysis in the diaphragm are well-documented, only one study has investigated methods of preserving diaphragmatic protein synthesis during prolonged MV. Therefore, we evaluated the efficacy of two therapeutic interventions that, conceptually, have the potential to sustain protein synthesis in the rat diaphragm during prolonged MV. Specifically, these experiments were designed to: 1) determine if partial-support MV will protect against the decrease in diaphragmatic protein synthesis that occurs during prolonged full-support MV; and 2) establish if treatment with a mitochondrial-targeted antioxidant will maintain diaphragm protein synthesis during full-support MV. Compared to spontaneously breathing animals, full support MV resulted in a significant decline in diaphragmatic protein synthesis during 12 hours of MV. In contrast, diaphragm protein synthesis rates were maintained during partial support MV at levels comparable to spontaneous breathing animals. Further, treatment of animals with a mitochondrial-targeted antioxidant prevented oxidative stress during full support MV and maintained diaphragm protein synthesis at the level of spontaneous breathing animals. We conclude that treatment with mitochondrial-targeted antioxidants or the use of partial-support MV are potential strategies to preserve diaphragm protein synthesis during prolonged MV.

Partial Support Ventilation and Mitochondrial-Targeted Antioxidants Protect against Ventilator-Induced Decreases in Diaphragm Muscle Protein Synthesis.

Directory of Open Access Journals (Sweden)

Matthew B Hudson

Full Text Available Mechanical ventilation (MV is a life-saving intervention in patients in respiratory failure. Unfortunately, prolonged MV results in the rapid development of diaphragm atrophy and weakness. MV-induced diaphragmatic weakness is significant because inspiratory muscle dysfunction is a risk factor for problematic weaning from MV. Therefore, developing a clinical intervention to prevent MV-induced diaphragm atrophy is important. In this regard, MV-induced diaphragmatic atrophy occurs due to both increased proteolysis and decreased protein synthesis. While efforts to impede MV-induced increased proteolysis in the diaphragm are well-documented, only one study has investigated methods of preserving diaphragmatic protein synthesis during prolonged MV. Therefore, we evaluated the efficacy of two therapeutic interventions that, conceptually, have the potential to sustain protein synthesis in the rat diaphragm during prolonged MV. Specifically, these experiments were designed to: 1 determine if partial-support MV will protect against the decrease in diaphragmatic protein synthesis that occurs during prolonged full-support MV; and 2 establish if treatment with a mitochondrial-targeted antioxidant will maintain diaphragm protein synthesis during full-support MV. Compared to spontaneously breathing animals, full support MV resulted in a significant decline in diaphragmatic protein synthesis during 12 hours of MV. In contrast, diaphragm protein synthesis rates were maintained during partial support MV at levels comparable to spontaneous breathing animals. Further, treatment of animals with a mitochondrial-targeted antioxidant prevented oxidative stress during full support MV and maintained diaphragm protein synthesis at the level of spontaneous breathing animals. We conclude that treatment with mitochondrial-targeted antioxidants or the use of partial-support MV are potential strategies to preserve diaphragm protein synthesis during prolonged MV.

Solid-Binding Peptides in Biomedicine.

Science.gov (United States)

Care, Andrew; Bergquist, Peter L; Sunna, Anwar

2017-01-01

Some peptides are able to bind to inorganic materials such as silica and gold. Over the past decade, Solid-binding peptides (SBPs) have been used increasingly as molecular building blocks in nanobiotechnology. These peptides show selectivity and bind with high affinity to a diverse range of inorganic surfaces e.g. metals, metal oxides, metal compounds, magnetic materials, semiconductors, carbon materials, polymers and minerals. They can be used in applications such as protein purification and synthesis, assembly and the functionalization of nanomaterials. They offer simple and versatile bioconjugation methods that can increase biocompatibility and also direct the immobilization and orientation of nanoscale entities onto solid supports without impeding their functionality. SBPs have been employed in numerous nanobiotechnological applications such as the controlled synthesis of nanomaterials and nanostructures, formation of hybrid biomaterials, immobilization of functional proteins and improved nanomaterial biocompatibility. With advances in nanotechnology, a multitude of novel nanomaterials have been designed and synthesized for diagnostic and therapeutic applications. New approaches have been developed recently to exert a greater control over bioconjugation and eventually, over the optimal and functional display of biomolecules on the surfaces of many types of solid materials. In this chapter we describe SBPs and highlight some selected examples of their potential applications in biomedicine.

A General Solid-State Synthesis of Chemically-Doped Fluorescent Graphene Quantum Dots for Bioimaging and Optoelectronic Applications

KAUST Repository

Ma, Chong-Bo

2015-05-05

Graphene quantum dots (GQDs) have attracted increasing interest because of their excellent properties such as strong photoluminescence, excellent biocompatibility and low cost. Herein, we develop a general method for the synthesis of doped and undoped GQDs, which relies on direct carbonization of organic precursors at solid state.

A General Solid-State Synthesis of Chemically-Doped Fluorescent Graphene Quantum Dots for Bioimaging and Optoelectronic Applications

KAUST Repository

Ma, Chong-Bo; Zhu, Zhentong; Wang, Hang-Xing; Huang, Xiao; Zhang, Xiao; Qi, Xiaoying; Zhang, Haoli; Zhu, Yihan; Deng, Xia; Peng, Yong; Han, Yu; Zhang, Hua

2015-01-01

Graphene quantum dots (GQDs) have attracted increasing interest because of their excellent properties such as strong photoluminescence, excellent biocompatibility and low cost. Herein, we develop a general method for the synthesis of doped and undoped GQDs, which relies on direct carbonization of organic precursors at solid state.

Solid State Division

International Nuclear Information System (INIS)

Green, P.H.; Watson, D.M.

1989-08-01

This report contains brief discussions on work done in the Solid State Division of Oak Ridge National Laboratory. The topics covered are: Theoretical Solid State Physics; Neutron scattering; Physical properties of materials; The synthesis and characterization of materials; Ion beam and laser processing; and Structure of solids and surfaces

Solid-Phase Synthesis of Molecularly Imprinted Polymer Nanoparticles with a Reusable Template - "Plastic Antibodies".

Science.gov (United States)

Poma, Alessandro; Guerreiro, Antonio; Whitcombe, Michael J; Piletska, Elena V; Turner, Anthony P F; Piletsky, Sergey A

2013-06-13

Molecularly Imprinted Polymers (MIPs) are generic alternatives to antibodies in sensors, diagnostics and separations. To displace biomolecules without radical changes in infrastructure in device manufacture, MIPs should share their characteristics (solubility, size, specificity and affinity, localized binding domain) whilst maintaining the advantages of MIPs (low-cost, short development time and high stability) hence the interest in MIP nanoparticles. Herein we report a reusable solid-phase template approach (fully compatible with automation) for the synthesis of MIP nanoparticles and their precise manufacture using a prototype automated UV photochemical reactor. Batches of nanoparticles (30-400 nm) with narrow size distributions imprinted with: melamine (d = 60 nm, K d = 6.3 × 10 -8 m), vancomycin (d = 250 nm, K d = 3.4 × 10 -9 m), a peptide (d = 350 nm, K d = 4.8 × 10 -8 m) and proteins have been produced. Our instrument uses a column packed with glass beads, bearing the template. Process parameters are under computer control, requiring minimal manual intervention. For the first time we demonstrate the reliable re-use of molecular templates in the synthesis of MIPs (≥ 30 batches of nanoMIPs without loss of performance). NanoMIPs are produced template-free and the solid-phase acts both as template and affinity separation medium.

High-pressure synthesis of rhombohedral α-AgGaO{sub 2} via direct solid state reaction

Energy Technology Data Exchange (ETDEWEB)

Akhtar, Meysam [Department of Physics and Astronomy, University of Louisville, 102 Natural Science Building, Louisville, KY 40292 (United States); Menon, Madhu [Center for Computational Sciences, University of Kentucky, 325 McVey Hall, Lexington, KY 40506 (United States); Sunkara, Mahendra [Conn Center for Renewable Energy Research, University of Louisville, Ernst Hall Room 102A, Louisville, KY 40292 (United States); Sumanasekera, Gamini [Department of Physics and Astronomy, University of Louisville, 102 Natural Science Building, Louisville, KY 40292 (United States); Conn Center for Renewable Energy Research, University of Louisville, Ernst Hall Room 102A, Louisville, KY 40292 (United States); Durygin, Andriy [Center for the Study of Matter at Extreme Conditions, Florida International University, VH 140, University Park, Miami, FL 33199 (United States); Jasinski, Jacek B., E-mail: jacek.jasinski@louisville.edu [Conn Center for Renewable Energy Research, University of Louisville, Ernst Hall Room 102A, Louisville, KY 40292 (United States)

2015-08-25

Highlights: • Direct synthesis of α-AgGaO{sub 2} via a solid state reaction of Ag{sub 2}O and Ga{sub 2}O{sub 3} powders. • Utilizing high pressure diamond anvil cell to facilitate solid state reaction. • Experimental and theoretical study of vibrational modes for α-AgGaO{sub 2}. • Extensive characterization of synthesized α-AgGaO{sub 2} samples. • GGA + U formalism-based DFT calculations of electronic structure and band gap in α-AgGaO{sub 2}. - Abstract: In this work, we demonstrate the application of high pressure conditions to enable the direct synthesis of α-AgGaO{sub 2} via a solid state reaction of Ag{sub 2}O and Ga{sub 2}O{sub 3}. Synthesis experiments were carried out at pressures and temperatures up to ∼10 GPa and ∼600 °C, respectively, using a resistively-heated diamond anvil cell. Thus synthesized α-AgGaO{sub 2} samples were characterized and their chemical composition and crystal structure were confirmed. In particular, electron diffraction confirmed the rhombohedral delafossite crystal structure of the synthesized AgGaO{sub 2} and its corresponding lattice parameters of a = 2.99 Å and c = 18.43 Å. The vibrational modes analysis was also conducted using a combination of ab initio density functional theory (DFT) and Raman spectroscopy. This analysis yielded good agreement between the calculated Raman-active modes and experimental Raman data. Finally, the application of the GGA + U formalism-based on DFT to calculate the electronic band structure of α-AgGaO{sub 2} provided a more realistic theoretical band gap value than those reported previously.

Solid-phase polyamine synthesis using piperazine and piperidine building blocks

DEFF Research Database (Denmark)

Olsen, Christian A; Witt, Matthias; Jaroszewski, Jerzy W

2003-01-01

[reaction: see text]. Polyamines containing piperidine and piperazine moieties have been synthesized on solid support using SN2 alkylation of resin-bound secondary amines with 2-nitrobenzenesulfonates (nosylates). The effect of solvent on this alkylation was investigated. The methodology was empl...

Synthesis of solid catalyst from egg shell waste and clay for biodiesel production

Science.gov (United States)

Setiadji, S.; Sundari, C. D. D.; Munir, M.; Fitriyah, S.

2018-05-01

Until now, energy consumption in Indonesia is almost entirely fulfilled by fossil fuels, thus, its availability will be limited and continue to decrease. To overcome these problems, development and utilization of renewable energy are required, one of which is biodiesel. Biodiesel can be prepared through transesterification reaction of vegetable oil using catalyst. In this research, a solid catalyst for biodiesel synthesis was prepared from chicken egg shell waste and clay. Optimization of the transesterification reaction of coconut (Cocos nucifera) oil to obtain biodiesel was also carried out. The formation of CaO/kaolin catalyst was confirmed based on the results of XRD and SEM-EDS. This catalyst is suitable for biodiesel synthesis from vegetable oils with lower FFA (free fatty acid) levels, i.e. coconut oil with FFA level of 0.18%. Based on FTIR result, FFA level and flame tests, it was found that biodiesel was successfully formed. Synthesis of biodiesel has the optimum conditions on reaction time of 16 hours and temperature of 64 °C, with oil: methanol ratio of 1: 15 and CaO/kaolin catalyst concentration of 0.9% in a reflux system.

Fully automated synthesis of 11C-acetate as tumor PET tracer by simple modified solid-phase extraction purification

International Nuclear Information System (INIS)

Tang, Xiaolan; Tang, Ganghua; Nie, Dahong

2013-01-01

Introduction: Automated synthesis of 11 C-acetate ( 11 C-AC) as the most commonly used radioactive fatty acid tracer is performed by a simple, rapid, and modified solid-phase extraction (SPE) purification. Methods: Automated synthesis of 11 C-AC was implemented by carboxylation reaction of MeMgBr on a polyethylene Teflon loop ring with 11 C-CO 2 , followed by acidic hydrolysis with acid and SCX cartridge, and purification on SCX, AG11A8 and C18 SPE cartridges using a commercially available 11 C-tracer synthesizer. Quality control test and animals positron emission tomography (PET) imaging were also carried out. Results: A high and reproducible decay-uncorrected radiochemical yield of (41.0±4.6)% (n=10) was obtained from 11 C-CO 2 within the whole synthesis time about 8 min. The radiochemical purity of 11 C-AC was over 95% by high-performance liquid chromatography (HPLC) analysis. Quality control test and PET imaging showed that 11 C-AC injection produced by the simple SPE procedure was safe and efficient, and was in agreement with the current Chinese radiopharmaceutical quality control guidelines. Conclusion: The novel, simple, and rapid method is readily adapted to the fully automated synthesis of 11 C-AC on several existing commercial synthesis module. The method can be used routinely to produce 11 C-AC for preclinical and clinical studies with PET imaging. - Highlights: • A fully automated synthesis of 11 C-acetate by simple modified solid-phase extraction purification has been developed. • Typical non-decay-corrected yields were (41.0±4.6)% (n=10) • Radiochemical purity was determined by radio-HPLC analysis on a C18 column using the gradient program, instead of expensive organic acid column or anion column. • QC testing (RCP>99%)

Solid State Division

Energy Technology Data Exchange (ETDEWEB)

Green, P.H.; Watson, D.M. (eds.)

1989-08-01

This report contains brief discussions on work done in the Solid State Division of Oak Ridge National Laboratory. The topics covered are: Theoretical Solid State Physics; Neutron scattering; Physical properties of materials; The synthesis and characterization of materials; Ion beam and laser processing; and Structure of solids and surfaces. (LSP)

Analytic webs support the synthesis of ecological data sets.

Science.gov (United States)

Ellison, Aaron M; Osterweil, Leon J; Clarke, Lori; Hadley, Julian L; Wise, Alexander; Boose, Emery; Foster, David R; Hanson, Allen; Jensen, David; Kuzeja, Paul; Riseman, Edward; Schultz, Howard

2006-06-01

A wide variety of data sets produced by individual investigators are now synthesized to address ecological questions that span a range of spatial and temporal scales. It is important to facilitate such syntheses so that "consumers" of data sets can be confident that both input data sets and synthetic products are reliable. Necessary documentation to ensure the reliability and validation of data sets includes both familiar descriptive metadata and formal documentation of the scientific processes used (i.e., process metadata) to produce usable data sets from collections of raw data. Such documentation is complex and difficult to construct, so it is important to help "producers" create reliable data sets and to facilitate their creation of required metadata. We describe a formal representation, an "analytic web," that aids both producers and consumers of data sets by providing complete and precise definitions of scientific processes used to process raw and derived data sets. The formalisms used to define analytic webs are adaptations of those used in software engineering, and they provide a novel and effective support system for both the synthesis and the validation of ecological data sets. We illustrate the utility of an analytic web as an aid to producing synthetic data sets through a worked example: the synthesis of long-term measurements of whole-ecosystem carbon exchange. Analytic webs are also useful validation aids for consumers because they support the concurrent construction of a complete, Internet-accessible audit trail of the analytic processes used in the synthesis of the data sets. Finally we describe our early efforts to evaluate these ideas through the use of a prototype software tool, SciWalker. We indicate how this tool has been used to create analytic webs tailored to specific data-set synthesis and validation activities, and suggest extensions to it that will support additional forms of validation. The process metadata created by SciWalker is

Hollow nanoporous covalent triazine frameworks via acid vapor-assisted solid phase synthesis for enhanced visible light photoactivity

KAUST Repository

Huang, Wei

2016-04-11

Herein, we report a novel trifluoromethanesulfonic acid vapor-assisted solid phase synthetic method to construct nanoporous covalent triazine frameworks with highly ordered hollow interconnected pores under mild reaction conditions. This unique solid state synthetic route allows not only the avoidance of undesired side reactions caused by traditional high temperature synthesis, but also the maintaining of defined and precise optical and electronic properties of the nonporous triazine frameworks. Promising photocatalytic activity of the polytriazine networks was demonstrated in the photoreduction reaction of 4-nitrophenol into 4-aminophenol under visible light irradiation.

Hollow nanoporous covalent triazine frameworks via acid vapor-assisted solid phase synthesis for enhanced visible light photoactivity

KAUST Repository

Huang, Wei; Wang, Zi Jun; Ma, Beatriz Chiyin; Ghasimi, Saman; Gehrig, Dominik; Laquai, Fré dé ric; Landfester, Katharina; Zhang, Kai A. I.

2016-01-01

Herein, we report a novel trifluoromethanesulfonic acid vapor-assisted solid phase synthetic method to construct nanoporous covalent triazine frameworks with highly ordered hollow interconnected pores under mild reaction conditions. This unique solid state synthetic route allows not only the avoidance of undesired side reactions caused by traditional high temperature synthesis, but also the maintaining of defined and precise optical and electronic properties of the nonporous triazine frameworks. Promising photocatalytic activity of the polytriazine networks was demonstrated in the photoreduction reaction of 4-nitrophenol into 4-aminophenol under visible light irradiation.

Template synthesis of two new supramolecular zinc(II) complexes containing pentadentate N.sub.3./sub.O.sub.2./sub. semicarbazone ligand: Nanostructure synthesis, Hirshfeld surface analysis, and DFT studies

Czech Academy of Sciences Publication Activity Database

Tyula, Y.A.; Zabardasti, A.; Goudarziafshar, H.; Roudsari, M.S.; Dušek, Michal; Eigner, Václav

2017-01-01

Roč. 1150, Dec (2017), s. 383-394 ISSN 0022-2860 R&D Projects: GA ČR(CZ) GA14-03276S Institutional support: RVO:68378271 Keywords : sonochemical synthesis * Hirshfeld surface analysis * DFT calculations * bis(semicarbazone) * pentagonal-bipyramidal Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 1.753, year: 2016

Combinatorial chemistry on solid support in the search for central nervous system agents.

Science.gov (United States)

Zajdel, Paweł; Pawłowski, Maciej; Martinez, Jean; Subra, Gilles

2009-08-01

The advent of combinatorial chemistry was one of the most important developments, that has significantly contributed to the drug discovery process. Within just a few years, its initial concept aimed at production of libraries containing huge number of compounds (thousands to millions), so called screening libraries, has shifted towards preparation of small and medium-sized rationally designed libraries. When applicable, the use of solid supports for the generation of libraries has been a real breakthrough in enhancing productivity. With a limited amount of resin and simple manual workups, the split/mix procedure may generate thousands of bead-tethered compounds. Beads can be chemically or physically encoded to facilitate the identification of a hit after the biological assay. Compartmentalization of solid supports using small reactors like teabags, kans or pellicular discrete supports like Lanterns resulted in powerful sort and combine technologies, relying on codes 'written' on the reactor, and thus reducing the need for automation and improving the number of compounds synthesized. These methods of solid-phase combinatorial chemistry have been recently supported by introduction of solid-supported reagents and scavenger resins. The first part of this review discusses the general premises of combinatorial chemistry and some methods used in the design of primary and focused combinatorial libraries. The aim of the second part is to present combinatorial chemistry methodologies aimed at discovering bioactive compounds acting on diverse GPCR involved in central nervous system disorders.

Solid-Phase Synthesis of RNA Analogs Containing Phosphorodithioate Linkages.

Science.gov (United States)

Yang, Xianbin

2017-09-18

The oligoribonucleotide phosphorodithioate (PS2-RNA) modification uses two sulfur atoms to replace two non-bridging oxygen atoms at an internucleotide phosphorodiester backbone linkage. Like a natural phosphodiester RNA backbone linkage, a PS2-modified backbone linkage is achiral at phosphorus. PS2-RNAs are highly stable to nucleases and several in vitro assays have demonstrated their biological activity. For example, PS2-RNAs silenced mRNA in vitro and bound to protein targets in the form of PS2-aptamers (thioaptamers). Thus, the interest in and promise of PS2-RNAs has drawn attention to synthesizing, isolating, and characterizing these compounds. RNA-thiophosphoramidite monomers are commercially available from AM Biotechnologies and this unit describes an effective methodology for solid-phase synthesis, deprotection, and purification of RNAs having PS2 internucleotide linkages. © 2017 by John Wiley & Sons, Inc. Copyright © 2017 John Wiley & Sons, Inc.

Hydrothermal synthesis of pollucite, analcime and their solid solutions and analysis of their properties

Energy Technology Data Exchange (ETDEWEB)

Jing, Zhenzi, E-mail: zzjing@tongji.edu.cn [Key Laboratory of Advanced Civil Engineering Materials, Ministry of Education, Tongji University, 4800 Cao' an Road, Shanghai 201804 (China); Cai, Kunchuan; Li, Yan; Fan, Junjie; Zhang, Yi; Miao, Jiajun; Chen, Yuqian [Key Laboratory of Advanced Civil Engineering Materials, Ministry of Education, Tongji University, 4800 Cao' an Road, Shanghai 201804 (China); Jin, Fangming [School of Environmental Science and Engineering, Shanghai Jiao Tong University, 800 Dongchuan Road, Shanghai 200240 (China)

2017-05-15

Pollucite, as a perfect long-term potential host for radioactive Cs immobilization, barely exists in pure form naturally but in an isomorphism form between pollucite and analcime due to coexistence of Cs and Na. Pollucite could be hydrothermally synthesized with Cs-polluted soil or clay minerals which contain Cs and Na, and it is necessary to study the properties of the synthesis if Cs and Na contained. Pure pollucite, analcime and their solid solutions were hydrothermally synthesized with chemicals, and it was found that the most formed pollucite analcime solid solutions with Cs/(Cs + Na) ratios of 2/6–5/6 had very similar properties in mineral composition, morphology and size, structural water (Cs cations) and coordination environment to pollucite. This also suggests that even coexistence of Cs and Na in nature, pollucite favors to form due to site preference for Cs over Na, which leads to the property and the structure of the most solid solutions similar to that of pollucite. - Highlights: •Pure pollucite barely exists in nature due to coexistence of Cs and Na. •Pollucite, analcime and their solid solutions could be hydrothermally synthesized. •Most formed solid solutions were found to have similar properties to pollucite. •Even coexistence in nature, pollucite favors to form due to site preference for Cs over Na.

Synthesis of carbon nanotubes by pyrolysis of solid Ni(dmg)2

International Nuclear Information System (INIS)

Kordatos, K.; Vlasopoulos, A.D.; Strikos, S.; Ntziouni, A.; Gavela, S.; Trasobares, S.; Kasselouri-Rigopoulou, V.

2009-01-01

We describe the high yield synthesis of multi-walled carbon nanotubes (MWCNTs) and the determination of the optimum production conditions. The method involves the catalytic pyrolysis of solid Ni(dmg) 2 under an Ar atmosphere. The obtained materials were characterized by scanning electron microscopy (SEM), energy dispersive X-ray (EDX) analysis, high resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), Raman spectroscopy and thermogravimetry analysis (TGA). The data revealed the formation of MWCNTs surrounded by a varying quantity of byproducts such as amorphous carbon and metallic particles, depending mainly on the reaction temperature. Pyrolysis of Ni(dmg) 2 at 900 deg. C results in the production of nanotube material with the highest degree of crystallinity

Solid-state synthesis and electrical properties of polyaniline/Cu-montmorillonite nanocomposite

International Nuclear Information System (INIS)

Bekri-Abbes, Imene; Srasra, Ezzeddine

2010-01-01

In this paper, the solid-state synthesis of polyaniline/Cu-montmorillonite nanocomposite is reported. Mixture of anilinium chlorure and Cu exchanged montmorillonite was grinded at room temperature while we vary the molar rate of aniline to interlayer Cu 2+ cations (R) from 0.5 to 6. The properties of the hybrid compounds are characterized by X-ray diffraction, thermogravimetric analysis, SEM, FTIR and impedance spectroscopy. The results showed that the structure and the conductivity of PANI in hybrid materials depend on R. The ac conduction showed a regime of constant dc conductivity at low frequencies and a crossover to a frequency-dependent regime of the type A ω s at high frequencies.

Supported zirconium sulfate on carbon nanotubes as water-tolerant solid acid catalyst

International Nuclear Information System (INIS)

Juan, Joon Ching; Jiang Yajie; Meng Xiujuan; Cao Weiliang; Yarmo, Mohd Ambar; Zhang Jingchang

2007-01-01

A new solid acid of zirconium sulfate (CZ) was successfully supported on carbon nanotube (CNT) for esterification reaction. Preparation conditions of the supported CZ have been investigated, to obtain highest catalytic activity for esterification reaction. XRD, TEM, BET, X-ray photoelectron spectra (XPS) and in situ FTIR analysis has also been carried out to understand the characteristics of the catalyst. In the esterification of acrylic acid with n-octanol, the supported CZ exhibited high catalytic activity and stability. The catalytic activity was nearly unchanged during four times of reuse. XRD and TEM analysis indicated that CZ was finely dispersed on CNT. XPS analysis shows that the CZ species was preserved and the chemical environment of the CZ has changed after loaded on CNT. This finding show that CNT as CZ support is an efficient water-tolerant solid acid

Mitochondrial nucleoid interacting proteins support mitochondrial protein synthesis.

Science.gov (United States)

He, J; Cooper, H M; Reyes, A; Di Re, M; Sembongi, H; Litwin, T R; Gao, J; Neuman, K C; Fearnley, I M; Spinazzola, A; Walker, J E; Holt, I J

2012-07-01

Mitochondrial ribosomes and translation factors co-purify with mitochondrial nucleoids of human cells, based on affinity protein purification of tagged mitochondrial DNA binding proteins. Among the most frequently identified proteins were ATAD3 and prohibitin, which have been identified previously as nucleoid components, using a variety of methods. Both proteins are demonstrated to be required for mitochondrial protein synthesis in human cultured cells, and the major binding partner of ATAD3 is the mitochondrial ribosome. Altered ATAD3 expression also perturbs mtDNA maintenance and replication. These findings suggest an intimate association between nucleoids and the machinery of protein synthesis in mitochondria. ATAD3 and prohibitin are tightly associated with the mitochondrial membranes and so we propose that they support nucleic acid complexes at the inner membrane of the mitochondrion.

Hairy foam" : carbon nanofibers grown on solid foam. A fully accessible, high surface area, graphitic catalyst support

NARCIS (Netherlands)

Wenmakers, P.W.A.M.; Schaaf, van der J.; Kuster, B.F.M.; Schouten, J.C.

2008-01-01

This paper describes the synthesis of carbon nanofibers (CNFs) on solid carbon foam ("Hairy Foam") by catalytic decompn. of ethylene. The effect of nickel loading on fiber diam. and morphol., CNF coverage, and fiber layer thickness is studied using SEM and N2/Kr-physisorption. The surface area

Solid State Division progress report for period ending March 31, 1997

Energy Technology Data Exchange (ETDEWEB)

Green, P.H.; Hinton, L.W. [eds.

1997-12-01

This report covers research progress in the Solid State Division from April 1, 1995, through March 31, 1997. During this period, the division conducted a broad, interdisciplinary materials research program in support of Department of Energy science and technology missions. The report includes brief summaries of research activities in condensed matter theory, neutron scattering, synthesis and characterization of materials, ion beam and laser processing, and the structure of solids and surfaces. An addendum includes listings of division publications and professional activities.

Ammonia synthesis with barium-promoted iron–cobalt alloys supported on carbon

DEFF Research Database (Denmark)

Hagen, Stefan; Barfod, Rasmus; Fehrmann, Rasmus

2003-01-01

Iron–cobalt alloys supported on carbon were investigated as ammonia synthesis catalysts. Barium was found to have a promoting effect for Fe with an optimum atomic ratio Ba/Fe of 0.35. At this Ba loading, a local maximum for the NH3 synthesis activity was found at 4 wt% Co by varying the Fe/Co ratio....... Samples containing only Co and no Fe, however, yielded by far the most active catalysts (7.0 μmol (NH3) g−1 s−1, 673 K, 10 bar). Barium was a very efficient promoter for Co, increasing the NH3 synthesis activity by more than two orders of magnitude compared to the unpromoted Co samples, while...

Robot-performed synthesis of [11C]CH3-methionine with isolation by means of solid-phase extraction

International Nuclear Information System (INIS)

Vasil'ev, D.A.; Kiselev, M.Yu.; Korsakov, M.V.; Khorti, A.G.

1992-01-01

Robot-performed technology of synthesizing radiopharmaceutical preparation 11 CH 3 -methionine, used in positron-emission tomography of brain to evaluate the rate of protein biosynthesis was developed. The technology is based on the synthesis of 11 CH 3 -methionine from[ 11 C]-CH I and DL-homocysteinethiolactone with subsequent isolation of the preparation by the method of solid-phase extraction. Activity of the preparation synthesized is 0.13-0.17 Ci, specific activity -325-850 Ci/mmol, total duration of the synthesis from the moment of irradiation end is 16-19 min, radiochemical yield, as regards 11 CH 3 I corrected for carbon-11 decay, is 60 %

Solid amine sorbents for CO2 capture by chemical adsorption: A review

Directory of Open Access Journals (Sweden)

Elif Erdal Ünveren

2017-03-01

Full Text Available Amines are well-known for their reversible reactions with CO2, which make them ideal for CO2 capture from several gas streams, including flue gas. In this respect, selective CO2 absorption by aqueous alkanolamines is the most mature technology but the process is energy intensive and has also corrosion problems. Both disadvantages can be diminished to a certain extent by chemical adsorption of CO2 selectively. The most important element of the chemical adsorption of CO2 involves the design and development of a suitable adsorbent which consist of a porous support onto which an amine is attached or immobilized. Such an adsorbent is often called as solid amine sorbent. This review covers solid amine-based studies which are developed and published in recent years. First, the review examines several different types of porous support materials, namely, three mesoporous silica (MCM-41, SBA-15 and KIT-6 and two polymeric supports (PMMA and PS for CO2 adsorption. Emphasis is given to the synthesis, modifications and characterizations -such as BET and PXRD data-of them. Amination of these supports to obtain a solid amine sorbent through impregnation or grafting is reviewed comparatively. Focus is given to the adsorption mechanisms, material characteristics, and synthesis methods which are discussed in detail. Significant amount of original data are also presented which makes this review unique. Finally, relevant CO2 adsorption (or equilibrium capacity data, and cyclic adsorption/desorption performance and stability of important classes of solid amine sorbents are critically reviewed. These include severa PEI or TEPA impregnated adsorbents and APTES-grafted systems.

Solid oxide electrochemical reactor science.

Energy Technology Data Exchange (ETDEWEB)

Sullivan, Neal P. (Colorado School of Mines, Golden, CO); Stechel, Ellen Beth; Moyer, Connor J. (Colorado School of Mines, Golden, CO); Ambrosini, Andrea; Key, Robert J. (Colorado School of Mines, Golden, CO)

2010-09-01

Solid-oxide electrochemical cells are an exciting new technology. Development of solid-oxide cells (SOCs) has advanced considerable in recent years and continues to progress rapidly. This thesis studies several aspects of SOCs and contributes useful information to their continued development. This LDRD involved a collaboration between Sandia and the Colorado School of Mines (CSM) ins solid-oxide electrochemical reactors targeted at solid oxide electrolyzer cells (SOEC), which are the reverse of solid-oxide fuel cells (SOFC). SOECs complement Sandia's efforts in thermochemical production of alternative fuels. An SOEC technology would co-electrolyze carbon dioxide (CO{sub 2}) with steam at temperatures around 800 C to form synthesis gas (H{sub 2} and CO), which forms the building blocks for a petrochemical substitutes that can be used to power vehicles or in distributed energy platforms. The effort described here concentrates on research concerning catalytic chemistry, charge-transfer chemistry, and optimal cell-architecture. technical scope included computational modeling, materials development, and experimental evaluation. The project engaged the Colorado Fuel Cell Center at CSM through the support of a graduate student (Connor Moyer) at CSM and his advisors (Profs. Robert Kee and Neal Sullivan) in collaboration with Sandia.

Recovery of Terephthalic Acid by employing magnetic nanoparticles as a solid support

Directory of Open Access Journals (Sweden)

Elmira Ghamary

2018-03-01

Full Text Available Abstract The aim of this research work is focused on the improvement of Terephthalic acid recovery from PET wastes by using organically modified nano-Fe3O4@Cyanuric Chloride as the solid support. The performance of organically modified nano magnetic was examined in detail and the obtained results were compared with the unsupported reaction data. Required reaction time for complete glycolysis of the wastes, consumption of the solvent as well as catalyst decreases up 99%, 37.5% and 40% respectively. Result showed that nano-Fe 3O4@Cyanuric Chloride delivered good performance as solid support in depolymerizing of PET to the terephthalic acid.

Tubular solid oxide fuel cells with porous metal supports and ceramic interconnections

Science.gov (United States)

Huang, Kevin [Export, PA; Ruka, Roswell J [Pittsburgh, PA

2012-05-08

An intermediate temperature solid oxide fuel cell structure capable of operating at from 600.degree. C. to 800.degree. C. having a very thin porous hollow elongated metallic support tube having a thickness from 0.10 mm to 1.0 mm, preferably 0.10 mm to 0.35 mm, a porosity of from 25 vol. % to 50 vol. % and a tensile strength from 700 GPa to 900 GPa, which metallic tube supports a reduced thickness air electrode having a thickness from 0.010 mm to 0.2 mm, a solid oxide electrolyte, a cermet fuel electrode, a ceramic interconnection and an electrically conductive cell to cell contact layer.

A Convergent Solid-Phase Synthesis of Actinomycin Analogues - Towards Implementation of Double-Combinatorial Chemistry

DEFF Research Database (Denmark)

Tong, Glenn; Nielsen, John

1996-01-01

The actinomycin antibiotics bind to nucleic acids via both intercalation and hydrogen bonding. We found this 'double-action attack' mechanism very attractive in our search for a novel class of nucleic acid binders. A highly convergent, solid-phase synthetic strategy has been developed for a class...... with the requirements for combinatorial synthesis and furthermore, the final segment condensation allows, for the first time, double-combinatorial chemistry to be performed where two combinatorial libraries can be reacted with each other. Copyright (C) 1996 Elsevier Science Ltd....

Solid-phase synthesis and biological evaluation of Joro spider toxin-4 from Nephila clavata

DEFF Research Database (Denmark)

Barslund, Anne Fuglsang; Poulsen, Mette Homann; Bach, Tinna Brøbech

2011-01-01

Polyamine toxins from orb weaver spiders are attractive pharmacological tools particularly for studies of ionotropic glutamate (iGlu) receptors in the brain. These polyamine toxins are biosynthesized in a combinatorial manner, providing a plethora of related, but structurally complex toxins...... to be exploited in biological studies. Here, we have used solid-phase synthetic methodology for the efficient synthesis of Joro spider toxin-4 (JSTX-4) (1) from Nephila clavata, providing sufficient amounts of the toxin for biological evaluation at iGlu receptor subtypes using electrophysiology. Biological...

Synthesis and magnetic properties of Zn Spinel ceramics

Czech Academy of Sciences Publication Activity Database

Huber, Š.; Sofer, Z.; Nádherný, L.; Jankovský, O.; Šimek, P.; Sedmidubský, D.; Maryško, Miroslav

2013-01-01

Roč. 57, č. 2 (2013), s. 162-166 ISSN 0862-5468 R&D Projects: GA ČR GA13-17538S; GA MŠk(CZ) 7AMB12FR019 Institutional support: RVO:68378271 Keywords : Zn spinel * synthesis * magnetic properties * antiferromagnet * bulk ZnO Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.434, year: 2013

The Use of Supported Acidic Ionic Liquids in Organic Synthesis

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Rita Skoda-Földes

2014-06-01

Full Text Available Catalysts obtained by the immobilisation of acidic ionic liquids (ILs on solid supports offer several advantages compared to the use of catalytically active ILs themselves. Immobilisation may result in an increase in the number of accessible active sites of the catalyst and a reduction of the amount of the IL required. The ionic liquid films on the carrier surfaces provide a homogeneous environment for catalytic reactions but the catalyst appears macroscopically as a dry solid, so it can simply be separated from the reaction mixture. As another advantage, it can easily be applied in a continuous fixed bed reactor. In the present review the main synthetic strategies towards the preparation of supported Lewis acidic and Brønsted acidic ILs are summarised. The most important characterisation methods and structural features of the supported ionic liquids are presented. Their efficiency in catalytic reactions is discussed with special emphasis on their recyclability.

Development of a poly(dimethylacrylamide) based matrix material for solid phase high density peptide array synthesis employing a laser based material transfer

International Nuclear Information System (INIS)

Ridder, Barbara; Foertsch, Tobias C.; Welle, Alexander; Mattes, Daniela S.; Bojnicic-Kninski, Clemens M. von; Loeffler, Felix F.; Nesterov-Mueller, Alexander; Meier, Michael A.R.; Breitling, Frank

2016-01-01

Highlights: • New matrix material for peptide array synthesis from a ‘solid solvent’. • Resolution was increased with possible spot densities of up to 20.000 spots per cm"2. • The coupling depth and the effectiveness of washing steps analyzed by ToF-SIMS. • Adaptations and custom changes of the matrix material are possible. - Abstract: Poly(dimethylacrylamide) (PDMA) based matrix materials were developed for laser-based in situ solid phase peptide synthesis to produce high density arrays. In this specific array synthesis approach, amino acid derivatives are embedded into a matrix material, serving as a “solid” solvent material at room temperature. Then, a laser pulse transfers this mixture to the target position on a synthesis slide, where the peptide array is synthesized. Upon heating above the glass transition temperature of the matrix material, it softens, allowing diffusion of the amino acid derivatives to the synthesis surface and serving as a solvent for peptide bond formation. Here, we synthesized PDMA six-arm star polymers, offering the desired matrix material properties, using atom transfer radical polymerization. With the synthesized polymers as matrix material, we structured and synthesized arrays with combinatorial laser transfer. With densities of up to 20,000 peptide spots per cm"2, the resolution could be increased compared to the commercially available standard matrix material. Time-of-Flight Secondary Ion Mass Spectrometry experiments revealed the penetration behavior of an amino acid derivative into the prepared acceptor synthesis surface and the effectiveness of the washing protocols.

Development of a poly(dimethylacrylamide) based matrix material for solid phase high density peptide array synthesis employing a laser based material transfer

Energy Technology Data Exchange (ETDEWEB)

Ridder, Barbara [Institute of Microstructure Technology (IMT), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Institute of Organic Chemistry (IOC), Karlsruhe Institute of Technology (KIT), Fritz-Haber-Weg 6, 76131 Karlsruhe (Germany); Foertsch, Tobias C. [Institute of Microstructure Technology (IMT), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Welle, Alexander [Karlsruhe Nano Micro Facility (KNMF), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Mattes, Daniela S. [Institute of Microstructure Technology (IMT), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Institute of Organic Chemistry (IOC), Karlsruhe Institute of Technology (KIT), Fritz-Haber-Weg 6, 76131 Karlsruhe (Germany); Bojnicic-Kninski, Clemens M. von; Loeffler, Felix F.; Nesterov-Mueller, Alexander [Institute of Microstructure Technology (IMT), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Meier, Michael A.R., E-mail: m.a.r.meier@kit.edu [Institute of Organic Chemistry (IOC), Karlsruhe Institute of Technology (KIT), Fritz-Haber-Weg 6, 76131 Karlsruhe (Germany); Breitling, Frank, E-mail: frank.breitling@kit.edu [Institute of Microstructure Technology (IMT), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany)

2016-12-15

Highlights: • New matrix material for peptide array synthesis from a ‘solid solvent’. • Resolution was increased with possible spot densities of up to 20.000 spots per cm{sup 2}. • The coupling depth and the effectiveness of washing steps analyzed by ToF-SIMS. • Adaptations and custom changes of the matrix material are possible. - Abstract: Poly(dimethylacrylamide) (PDMA) based matrix materials were developed for laser-based in situ solid phase peptide synthesis to produce high density arrays. In this specific array synthesis approach, amino acid derivatives are embedded into a matrix material, serving as a “solid” solvent material at room temperature. Then, a laser pulse transfers this mixture to the target position on a synthesis slide, where the peptide array is synthesized. Upon heating above the glass transition temperature of the matrix material, it softens, allowing diffusion of the amino acid derivatives to the synthesis surface and serving as a solvent for peptide bond formation. Here, we synthesized PDMA six-arm star polymers, offering the desired matrix material properties, using atom transfer radical polymerization. With the synthesized polymers as matrix material, we structured and synthesized arrays with combinatorial laser transfer. With densities of up to 20,000 peptide spots per cm{sup 2}, the resolution could be increased compared to the commercially available standard matrix material. Time-of-Flight Secondary Ion Mass Spectrometry experiments revealed the penetration behavior of an amino acid derivative into the prepared acceptor synthesis surface and the effectiveness of the washing protocols.

Solid-Phase Synthesis of Molecularly Imprinted Polymer Nanoparticles with a Reusable Template – “Plastic Antibodies”

Science.gov (United States)

Poma, Alessandro; Guerreiro, Antonio; Whitcombe, Michael J.; Piletska, Elena V.; Turner, Anthony P.F.; Piletsky, Sergey A.

2016-01-01

Molecularly Imprinted Polymers (MIPs) are generic alternatives to antibodies in sensors, diagnostics and separations. To displace biomolecules without radical changes in infrastructure in device manufacture, MIPs should share their characteristics (solubility, size, specificity and affinity, localized binding domain) whilst maintaining the advantages of MIPs (low-cost, short development time and high stability) hence the interest in MIP nanoparticles. Herein we report a reusable solid-phase template approach (fully compatible with automation) for the synthesis of MIP nanoparticles and their precise manufacture using a prototype automated UV photochemical reactor. Batches of nanoparticles (30-400 nm) with narrow size distributions imprinted with: melamine (d = 60 nm, Kd = 6.3 × 10−8 m), vancomycin (d = 250 nm, Kd = 3.4 × 10−9 m), a peptide (d = 350 nm, Kd = 4.8 × 10−8 m) and proteins have been produced. Our instrument uses a column packed with glass beads, bearing the template. Process parameters are under computer control, requiring minimal manual intervention. For the first time we demonstrate the reliable re-use of molecular templates in the synthesis of MIPs (≥ 30 batches of nanoMIPs without loss of performance). NanoMIPs are produced template-free and the solid-phase acts both as template and affinity separation medium. PMID:26869870

Synthesis of POSS-based ionic conductors with low glass transition temperatures for efficient solid-state dye-sensitized solar cells.

Science.gov (United States)

Zhang, Wei; Wang, Zhong-Sheng

2014-07-09

Replacing liquid-state electrolytes with solid-state electrolytes has been proven to be an effective way to improve the durability of dye-sensitized solar cells (DSSCs). We report herein the synthesis of amorphous ionic conductors based on polyhedral oligomeric silsesquioxane (POSS) with low glass transition temperatures for solid-state DSSCs. As the ionic conductor is amorphous and in the elastomeric state at the operating temperature of DSSCs, good pore filling in the TiO2 film and good interfacial contact between the solid-state electrolyte and the TiO2 film can be guaranteed. When the POSS-based ionic conductor containing an allyl group is doped with only iodine as the solid-state electrolyte without any other additives, power conversion efficiency of 6.29% has been achieved with good long-term stability under one-sun soaking for 1000 h.

Selective synthesis of thioethers in the presence of a transition-metal-free solid Lewis acid

Directory of Open Access Journals (Sweden)

Federica Santoro

2016-12-01

Full Text Available The synthesis of thioethers starting from alcohols and thiols in the presence of amorphous solid acid catalysts is reported. A silica alumina catalyst with a very low content in alumina gave excellent results in terms of both activity and selectivity also under solvent-free conditions. The reaction rate follows the electron density of the carbinol atom in the substrate alcohol and yields up to 99% and can be obtained for a wide range of substrates under mild reaction conditions.

Solid-Phase Synthesis of Modified Peptides as Putative Inhibitors of Histone Modifying Enzymes

DEFF Research Database (Denmark)

Cohrt, Anders Emil O'Hanlon

to be compatible with all 20 naturally occurring amino acids, and were furthermore feasible on several commonly used polymeric supports. By using dilute SnCl4 for N -Boc deprotection, and NaOH for the release of material from the solid support, N -modified peptides were cleanly obtained in excellent yields...

Supported molybdenum carbide for higher alcohol synthesis from syngas

DEFF Research Database (Denmark)

Wu, Qiongxiao; Christensen, Jakob Munkholt; Chiarello, Gian Luca

2013-01-01

Molybdenum carbide supported on active carbon, carbon nanotubes, and titanium dioxide, and promoted by K2CO3, has been prepared and tested for methanol and higher alcohol synthesis from syngas. At optimal conditions, the activity and selectivity to alcohols (methanol and higher alcohols) over...... carbide, while the selectivity to methanol follows the opposite trend. The effect of Mo2C loading on the alcohol selectivity at a fixed K/Mo molar ratio of 0.14 could be related to the amount of K2CO3 actually on the active Mo2C phase and the size, structure and composition of the supported carbide...... alcohols is obtained at a K/Mo molar ratio of 0.21 over the active carbon supported Mo2C (20wt%)....

Green synthesis of 3,4-dihydropyrimidinones using nano Fe3O4@meglumine sulfonic acid as a new efficient solid acid catalyst under microwave irradiation

Directory of Open Access Journals (Sweden)

Leila Moradi

2018-01-01

Full Text Available Design, synthesis and characterization of nano Fe3O4@meglumine sulfonic acid as a new solid acid catalyst for the simple and green one pot multicomponent synthesis of 3,4-dihydropyrimidin-2(1H-ones/thiones was studied. New solid acid catalyst was prepared through a clean and simple protocol and characterized using FTIR, VSM, TGA, SEM, elemental analysis (CHN and XRD techniques. Heterogenization of homogeneous catalyst as a green approach is a useful method for enhancing the efficiency of catalyst. Presented study was a new method for attachment of homogeneous highly soluble catalyst (meglumine sulfate to the magnetite nanoparticle surfaces for preparing a heterogeneous and effective catalyst. Obtained heterogeneous and reusable solid acid catalyst has high performance in the synthesis of Biginelli compounds. The reaction was performed under microwave irradiation as a rapid and green condition. Easy work up as well as excellent yield (90–98% of products in short reaction times (40–200 s and reusable catalyst are the main advantages of presented procedure. Reaction products were characterized in details using physical and chemical techniques such as melting point, 1H NMR, 13C NMR and FTIR.

One-pot synthesis of graphene supported platinum–cobalt nanoparticles as electrocatalysts for methanol oxidation

International Nuclear Information System (INIS)

Kepenienė, V.; Tamašauskaitė-Tamašiūnaitė, L.; Jablonskienė, J.; Semaško, M.; Vaičiūnienė, J.; Vaitkus, R.; Norkus, E.

2016-01-01

In the present study the graphene supported platinum–cobalt nanoparticles were prepared via microwave synthesis. The composition of prepared catalysts was examined by Inductively Coupled Plasma Optical Emission Spectroscopy. The shape and size of catalyst particles were determined by Transmission Electron Microscopy. The electrocatalytic activity of the graphene supported platinum–cobalt nanoparticles was investigated towards the electro-oxidation of methanol in an alkaline medium. It has been found that the graphene supported platinum–cobalt nanoparticles having the Pt:Co molar ratio 1:7 show the highest activity towards the electro-oxidation of methanol among the catalysts with the Pt:Co molar ratios equal to 1:1 and 1:44, graphene supported bare Co and Pt/C catalysts. - Highlights: • Preparation of graphene supported Pt-Co nanoparticles by microwave synthesis. • Electrocatalysts for oxidation of methanol. • Higher activity of PtCo/graphene towards methanol oxidation.

One-pot synthesis of graphene supported platinum–cobalt nanoparticles as electrocatalysts for methanol oxidation

Energy Technology Data Exchange (ETDEWEB)

Kepenienė, V., E-mail: virginalisk@gmail.com [Department of Catalysis, Center for Physical Sciences and Technology, Vilnius LT 01108 (Lithuania); Tamašauskaitė-Tamašiūnaitė, L.; Jablonskienė, J.; Semaško, M.; Vaičiūnienė, J. [Department of Catalysis, Center for Physical Sciences and Technology, Vilnius LT 01108 (Lithuania); Vaitkus, R. [Faculty of Chemistry, Vilnius University, Vilnius LT 03225 (Lithuania); Norkus, E. [Department of Catalysis, Center for Physical Sciences and Technology, Vilnius LT 01108 (Lithuania)

2016-03-01

In the present study the graphene supported platinum–cobalt nanoparticles were prepared via microwave synthesis. The composition of prepared catalysts was examined by Inductively Coupled Plasma Optical Emission Spectroscopy. The shape and size of catalyst particles were determined by Transmission Electron Microscopy. The electrocatalytic activity of the graphene supported platinum–cobalt nanoparticles was investigated towards the electro-oxidation of methanol in an alkaline medium. It has been found that the graphene supported platinum–cobalt nanoparticles having the Pt:Co molar ratio 1:7 show the highest activity towards the electro-oxidation of methanol among the catalysts with the Pt:Co molar ratios equal to 1:1 and 1:44, graphene supported bare Co and Pt/C catalysts. - Highlights: • Preparation of graphene supported Pt-Co nanoparticles by microwave synthesis. • Electrocatalysts for oxidation of methanol. • Higher activity of PtCo/graphene towards methanol oxidation.

Numerical evaluation of micro-structural parameters of porous supports in metal-supported solid oxide fuel cells

DEFF Research Database (Denmark)

Reiss, Georg; Frandsen, Henrik Lund; Brandstätter, Wilhelm

2014-01-01

Metallic supported Solid Oxide Fuel Cells (SOFCs) are considered as a durable and cost effective alternative to the state-of-the-art ceramic supported cell designs. In order to understand the mass and charge transport in the metal-support of this new type of cell a novel technique involving X......-ray tomography and micro-structural modelling is presented in this work. The simulation technique comprises a novel treatment of the boundary conditions, which leads to more accurate effective transport parameters compared to those, which can be achieved with the conventional homogenisation procedures....... Furthermore, the porosity distribution in the metal-support was determined, which provided information about the inhomogeneous nature of the material. In addition to that, transport parameters for two identified, different dense layers of the metal-support are evaluated separately. The results...

Solid-phase-assisted synthesis of targeting peptide-PEG-oligo(ethane amino)amides for receptor-mediated gene delivery.

Science.gov (United States)

Martin, Irene; Dohmen, Christian; Mas-Moruno, Carlos; Troiber, Christina; Kos, Petra; Schaffert, David; Lächelt, Ulrich; Teixidó, Meritxell; Günther, Michael; Kessler, Horst; Giralt, Ernest; Wagner, Ernst

2012-04-28

In the forthcoming era of cancer gene therapy, efforts will be devoted to the development of new efficient and non-toxic gene delivery vectors. In this regard, the use of Fmoc/Boc-protected oligo(ethane amino)acids as building blocks for solid-phase-supported assembly represents a novel promising approach towards fully controlled syntheses of effective gene vectors. Here we report on the synthesis of defined polymers containing the following: (i) a plasmid DNA (pDNA) binding domain of eight succinoyl-tetraethylenpentamine (Stp) units and two terminal cysteine residues; (ii) a central polyethylene glycol (PEG) chain (with twenty-four oxyethylene units) for shielding; and (iii) specific peptides for targeting towards cancer cells. Peptides B6 and c(RGDfK), which bind transferrin receptor and α(v)β(3) integrin, respectively, were chosen because of the high expression of these receptors in many tumoral cells. This study shows the feasibility of designing these kinds of fully controlled vectors and their success for targeted pDNA-based gene transfer. This journal is © The Royal Society of Chemistry 2012

Synthesis and characterization of MCM-41-supported nano zirconia catalysts

Directory of Open Access Journals (Sweden)

Mohamed S. Abdel Salam

2015-03-01

Full Text Available Series of MCM-41 supported sulfated Zirconia (SZ catalysts with different loadings (2.5–7.5% wt. were prepared using direct impregnation method. The acquired solid catalysts were characterized structurally and chemically using X-RD, HRTEM, BET, FT-IR, Raman spectroscopy and TPD analysis. The acidity of the solid catalysts was investigated through cumene cracking and isopropanol dehydration at different temperatures. As the SZ loading increases, the surface acidity of the mesoporous catalysts was enhanced, this was reflected by the higher catalytic activity toward cumene cracking and isopropanol dehydration.

Effects of inherent/enhanced solid acidity and morphology of diatomite templates on the synthesis and porosity of hierarchically porous carbon.

Science.gov (United States)

Liu, Dong; Yuan, Peng; Tan, Daoyong; Liu, Hongmei; Fan, Mingde; Yuan, Aihua; Zhu, Jianxi; He, Hongping

2010-12-21

The inherent or enhanced solid acidity of raw or activated diatomite is found to have significant effects on the synthesis of hierarchically porous diatomite-templated carbon with high surface area and special porous structure. The solid acidity makes raw/activated diatomite a catalyst for the generation of porous carbon, and the porous parameters of the carbon products are strongly dependent on the solid acidity of diatomite templates. The morphology of diatomite also dramatically affects the textural structure of porous carbon. Two types of macroporous structures in the carbon product, the partially solid pillars and the ordered hollow tubes, derive from the replication of the central and the edge pores of diatom shell, respectively. The hierarchically porous carbon shows good capability for the adsorption of solvent naphtha and H(2), enabling potential applications in adsorption and gas storage.

Nafion®-catalyzed microwave-assisted Ritter reaction: An atom-economic solvent-free synthesis of amides

Science.gov (United States)

An atom-economic solvent-free synthesis of amides by the Ritter reaction of alcohols and nitriles under microwave irradiation is reported. This green protocol is catalyzed by solid supported Nafion®NR50 with improved efficiency and reduced waste production.

Process for the liquefaction of solid carbonaceous materials wherein nitrogen is separated from hydrogen via ammonia synthesis

Science.gov (United States)

Stetka, Steven S.; Nazario, Francisco N.

1982-01-01

In a process for the liquefaction of solid carbonaceous materials wherein bottoms residues are upgraded with a process wherein air is employed, the improvement wherein nitrogen buildup in the system is avoided by ammonia synthesis. In a preferred embodiment hydrogen from other portions of the liquefaction process will be combined with hydrogen produced as a result of the bottoms upgrading to increase the H.sub.2 :N.sub.2 ratio in the ammonia reactor.

Microwave heating in solid-phase peptide synthesis

DEFF Research Database (Denmark)

Pedersen, Søren Ljungberg; Shelton, Anne Pernille Tofteng; Malik, Leila

2012-01-01

synthesis, precise microwave irradiation to heat the reaction mixture during coupling and N(a)-deprotection has become increasingly popular. It has often provided dramatic reductions in synthesis times, accompanied by an increase in the crude peptide purity. Microwave heating has been proven especially...... relevant for sequences which might form ß-sheet type structures and for sterically difficult couplings. The beneficial effect of microwave heating appears so far to be due to the precise nature of this type of heating, rather than a peptide-specific microwave effect. However, microwave heating...... in microwave heating for peptide synthesis, with a focus on systematic studies and general protocols, as well as important applications. The assembly of ß-peptides, peptoids and pseudopeptides are also evaluated in this critical review (254 references)....

Automated Solid-Phase Radiofluorination Using Polymer-Supported Phosphazenes

DEFF Research Database (Denmark)

Mathiessen, Bente; Zhuravlev, Fedor

2013-01-01

of [18F]FDG. The combination of compact form factor, simplicity of [18F]F− recovery and processing, and column reusability can make solid phase radiofluorination an attractive radiochemistry platform for the emerging dose-on-demand instruments for bedside production of PET radiotracers.......The polymer supported phosphazene bases PS-P2tBu and the novel PS-P2PEG allowed for efficient extraction of [18F]F− from proton irradiated [18O]H2O and subsequent radiofluorination of a broad range of substrates directly on the resin. The highest radiochemical yields were obtained with aliphatic...

Typical Mexican agroindustrial residues as supports for solid-state fermentation

DEFF Research Database (Denmark)

Flores-Maltos, Dulce A.; Mussatto, Solange Ines; Contreras Esquivel, Juan Carlos

2014-01-01

. These biological wastes can be used as support-substrates in Solid-State Fermentation (SSF) to produce industrially relevant metabolites with great economical advantage. In addition, it is an environment friendly method of waste management. In this study were analyzed six different Mexican agro industrial residues...... process. The results provided important knowledge about the characteristics of these materials revealing their potential for use in fermentation processes....

Synthesis of 1,2-Disubstituted Benzimidazoles in the Presence of SBA-Pr-SO3H as a Nano Solid Acid Catalyst

Directory of Open Access Journals (Sweden)

G. Mohammadi Ziarani

2012-06-01

Full Text Available In this article, simple, convenient synthesis of 2-aryl-1- arylmethyl-1H-1,3-benzimidazole (1,2-disubstituted benzimidazoles via condensation of 1,2-phenylenediamine and aromatic aldehydes using SBA-Pr-SO3H as a nanoporous solid acid catalyst in green protocol was reported.

daf-16/FoxO promotes gluconeogenesis and trehalose synthesis during starvation to support survival.

Science.gov (United States)

Hibshman, Jonathan D; Doan, Alexander E; Moore, Brad T; Kaplan, Rebecca Ew; Hung, Anthony; Webster, Amy K; Bhatt, Dhaval P; Chitrakar, Rojin; Hirschey, Matthew D; Baugh, L Ryan

2017-10-24

daf-16 /FoxO is required to survive starvation in Caenorhabditis elegans , but how daf-16I FoxO promotes starvation resistance is unclear. We show that daf-16 /FoxO restructures carbohydrate metabolism by driving carbon flux through the glyoxylate shunt and gluconeogenesis and into synthesis of trehalose, a disaccharide of glucose. Trehalose is a well-known stress protectant, capable of preserving membrane organization and protein structure during abiotic stress. Metabolomic, genetic, and pharmacological analyses confirm increased trehalose synthesis and further show that trehalose not only supports survival as a stress protectant but also serves as a glycolytic input. Furthermore, we provide evidence that metabolic cycling between trehalose and glucose is necessary for this dual function of trehalose. This work demonstrates that daf-16 /FoxO promotes starvation resistance by shifting carbon metabolism to drive trehalose synthesis, which in turn supports survival by providing an energy source and acting as a stress protectant.

daf-16/FoxO promotes gluconeogenesis and trehalose synthesis during starvation to support survival

Science.gov (United States)

Hibshman, Jonathan D; Doan, Alexander E; Moore, Brad T; Kaplan, Rebecca EW; Hung, Anthony; Webster, Amy K; Bhatt, Dhaval P; Chitrakar, Rojin; Hirschey, Matthew D

2017-01-01

daf-16/FoxO is required to survive starvation in Caenorhabditis elegans, but how daf-16IFoxO promotes starvation resistance is unclear. We show that daf-16/FoxO restructures carbohydrate metabolism by driving carbon flux through the glyoxylate shunt and gluconeogenesis and into synthesis of trehalose, a disaccharide of glucose. Trehalose is a well-known stress protectant, capable of preserving membrane organization and protein structure during abiotic stress. Metabolomic, genetic, and pharmacological analyses confirm increased trehalose synthesis and further show that trehalose not only supports survival as a stress protectant but also serves as a glycolytic input. Furthermore, we provide evidence that metabolic cycling between trehalose and glucose is necessary for this dual function of trehalose. This work demonstrates that daf-16/FoxO promotes starvation resistance by shifting carbon metabolism to drive trehalose synthesis, which in turn supports survival by providing an energy source and acting as a stress protectant. PMID:29063832

Photo and radiation induced synthesis of (Ni, Zn)O or mixed NiO–ZnO oxides

Czech Academy of Sciences Publication Activity Database

Pavelková, T.; Procházková, L.; Čuba, V.; Múčka, V.; Pospíšil, M.; Jakubec, Ivo

2015-01-01

Roč. 304, č. 1 (2015), s. 245-250 ISSN 0236-5731 Institutional support: RVO:61388980 Keywords : Nickel oxide * Solid solution * Zinc oxide * Ionizing radiation * UV radiation * Chemical synthesis Subject RIV: CA - Inorganic Chemistry Impact factor: 0.983, year: 2015

Eco-friendly synthesis for MCM-41 nanoporous materials using the non-reacted reagents in mother liquor.

Science.gov (United States)

Ng, Eng-Poh; Goh, Jia-Yi; Ling, Tau Chuan; Mukti, Rino R

2013-03-04

Nanoporous materials such as Mobil composite material number 41 (MCM-41) are attractive for applications such as catalysis, adsorption, supports, and carriers. Green synthesis of MCM-41 is particularly appealing because the chemical reagents are useful and valuable. We report on the eco-friendly synthesis of MCM-41 nanoporous materials via multi-cycle approach by re-using the non-reacted reagents in supernatant as mother liquor after separating the solid product. This approach was achieved via minimal requirement of chemical compensation where additional fresh reactants were added into the mother liquor followed by pH adjustment after each cycle of synthesis. The solid product of each successive batch was collected and characterized while the non-reacted reagents in supernatant can be recovered and re-used to produce subsequent cycle of MCM-41. The multi-cycle synthesis is demonstrated up to three times in this research. This approach suggests a low cost and eco-friendly synthesis of nanoporous material since less waste is discarded after the product has been collected, and in addition, product yield can be maintained at the high level.

Synthesis of high-purity Li{sub 8}ZrO{sub 6} powder by solid state reaction under hydrogen atmosphere

Energy Technology Data Exchange (ETDEWEB)

Shin-mura, Kiyoto; Otani, Yu; Ogawa, Seiya [Course of Mechanical Engineering, Graduate School of Engineering, Tokai University, 4-1-1 Kitakaname, Hiratsuka, Kanagawa 259-1292 (Japan); Niwa, Eiki; Hashimoto, Takuya [Department of Physics, College of Humanities and Sciences, Nihon University, 3-8-1 Sakurajousui, Setagaya-ku, Tokyo 156-8550 (Japan); Hoshino, Tsuyoshi [Breeding Functional Materials Development Group, Department of Blanket Systems Research, Rokkasho Fusion Institute, Sector of Fusion Research and Development, Japan Atomic Energy Agency, 2-166 Obuchi, Omotedate, Rokkasho-mura, Kamikita-gun, Aomori 039-3212 (Japan); Sasaki, Kazuya, E-mail: k_sasaki@tokai-u.ac.jp [Course of Mechanical Engineering, Graduate School of Engineering, Tokai University, 4-1-1 Kitakaname, Hiratsuka, Kanagawa 259-1292 (Japan); Department of Prime Mover Engineering, School of Engineering, Tokai University, 4-1-1 Kitakaname, Hiratsuka, Kanagawa 259-1292 (Japan)

2016-11-01

Highlights: • A fine pure Li{sub 8}ZrO{sub 6} powder was synthesized by using Li{sub 2}CO{sub 3} and ZrO{sub 2} via a solid state reaction. • Influences on the purity of product powder, lattice defect, and crystal orientation were revealed. • The suitable synthesis conditions of the fine and high purity Li{sub 8}ZrO{sub 6} powder were found. • The reaction process of the synthesis of Li{sub 8}ZrO{sub 6} was estimated. - Abstract: Li{sub 8}ZrO{sub 6} contains a large amount of Li and has a significant potential as a tritium breeder. However, few syntheses of fine-grain, high-purity Li{sub 8}ZrO{sub 6} powder have been reported. In this study, a high-purity powder of Li{sub 8}ZrO{sub 6} was synthesized by solid state reaction under hydrogen atmosphere combined with an effective lithium source and a suitable initial Li:Zr molar ratio. Mixed powders of Li{sub 2}CO{sub 3} and ZrO{sub 2} were fired at around 630 °C in H{sub 2} for several hours and several firing cycles. The low firing temperature inhibited the vaporization of Li during the heating, so that excessive amounts of Li were not needed for the synthesis, and the Li:Zr ratio in the starting material was 10:1 (mol:mol). In this synthesis, Li{sub 2}O was generated via the decomposition of Li{sub 2}CO{sub 3} during firing in H{sub 2}, and reacted with ZrO{sub 2} to form Li{sub 6}Zr{sub 2}O{sub 7}, which reacted with itself to form Li{sub 8}ZrO{sub 6}.

Solid-soluted content of cerium in solid solution of sphene

International Nuclear Information System (INIS)

Zhao Wei; Teng Yuancheng; Li Yuxiang; Ren Xuetan; Huang Junjun

2010-01-01

The sphene solid solution was synthesized by solid-state method,with calcium carbonate, silica, titanium dioxide, cerium oxalate and alumina as raw materials. The solid-soluted content of cerium in sphene was researched by means of X-ray diffraction (XRD), backscattering scanning electron microscopy (BSE), energy dispersive spectroscopy (EDS) and so on. The influence of A l3+ ion introduction to sphene on the solid-soluted content of cerium in sphene solid solution was studied. The results indicate that when introducing Al 3+ to sphene as electrovalence compensation, Ce 4+ could be well solidified to Ca 1-x Ce x Ti 1-2x A l2x SiO 5 , and the solid-soluted content is approximately 12.61%. With no electrovalence compensation, Ce 4+ could be solidified to Ca 1-2x Ce x TiSiO 5 , and the solid-soluted content is approximately 10.98%. The appropriate synthesis temperature of sphene solid solution is 1 260 degree C.(authors)

NaCl as a solid solvent to assist the mechanochemical synthesis and post-synthesis of hierarchical porous MOFs with high I2 vapour uptake.

Science.gov (United States)

Yang, Junyi; Feng, Xiao; Lu, Guangnong; Li, Yulin; Mao, Chaochao; Wen, Zhongliang; Yuan, Wenbing

2018-04-03

The use of salts as grinding media to assist the mechanosynthesis, and the following one-pot mechanochemical post-synthesis, of hierarchically porous MOFs was carried out efficiently by ball milling. NaCl or KCl were used as a solid solvent to initially pre-grind with 1,3,5-benzenetricarboxylic acid (H3BTC) and copper acetate monhydrate, respectively, for 1 minute, then both mixtures were combined together for a further 20 minutes of grinding, and the resultant mixture was finally washed with ethanol and water to obtain the hierarchically micro-, meso- and macroporous HKUST-1 with a high yield. Moreover, the post-synthesis of these as-obtained hierarchically porous HKUST-1 was easily performed via grinding triethylenediamine (TED) with the above unwashed crude-products for 20 minutes. By adjusting the amount of NaCl and TED added, we simply fabricated the pore- and function-adjustable hierarchically porous HKUST-1. Furthermore, these as-obtained HKUST-1 products showed high performance in the capture of volatile iodine.

Synthesis, characterization, and photocatalytic properties of core/shell mesoporous silica nanospheres supporting nanocrystalline titania

International Nuclear Information System (INIS)

Cendrowski, K.; Chen, X.; Zielinska, B.; Kalenczuk, R. J.; Rümmeli, M. H.; Büchner, B.; Klingeler, R.; Borowiak-Palen, E.

2011-01-01

The facile bulk synthesis of silica nanospheres makes them an attractive support for the transport of chemical compounds such as nanocrystalline titanium dioxide. In this contribution we present a promising route for the synthesis of mesoporous silica nanospheres (m-SiO 2 ) with diameter in range 200 nm, which are ideal supports for nanocrystalline titanium dioxide (TiO 2 ). The detailed microscopic and spectroscopic characterizations of core/shell structure (m-SiO 2 /TiO 2 ) were conducted. Moreover, the photocatalytic potential of the nanostructures was investigated via phenol decomposition and hydrogen generation. A clear enhancement of photoactivity in both reactions as compared to commercial TiO 2 -Degussa P25 catalyst is detected.

Synthesis, characterization, and photocatalytic properties of core/shell mesoporous silica nanospheres supporting nanocrystalline titania

Science.gov (United States)

Cendrowski, K.; Chen, X.; Zielinska, B.; Kalenczuk, R. J.; Rümmeli, M. H.; Büchner, B.; Klingeler, R.; Borowiak-Palen, E.

2011-11-01

The facile bulk synthesis of silica nanospheres makes them an attractive support for the transport of chemical compounds such as nanocrystalline titanium dioxide. In this contribution we present a promising route for the synthesis of mesoporous silica nanospheres (m-SiO2) with diameter in range 200 nm, which are ideal supports for nanocrystalline titanium dioxide (TiO2). The detailed microscopic and spectroscopic characterizations of core/shell structure (m-SiO2/TiO2) were conducted. Moreover, the photocatalytic potential of the nanostructures was investigated via phenol decomposition and hydrogen generation. A clear enhancement of photoactivity in both reactions as compared to commercial TiO2-Degussa P25 catalyst is detected.

Synthesis of lucifensin by native chemical ligation and characteristics of its isomer having different disulfide bridge pattern

Czech Academy of Sciences Publication Activity Database

Stanchev, Stancho; Zawada, Zbigniew; Monincová, Lenka; Bednárová, Lucie; Slaninová, Jiřina; Fučík, Vladimír; Čeřovský, Václav

2014-01-01

Roč. 20, č. 9 (2014), s. 725-735 ISSN 1075-2617 Institutional support: RVO:61388963 Keywords : lucifensin * native chemical ligation * solid-phase peptide synthesis * antimicrobial activity * CD spectroscopy * DTT reduction Subject RIV: CE - Biochemistry Impact factor: 1.546, year: 2014

Development of seismic support snubber using solid lubricant

International Nuclear Information System (INIS)

Sunakoda, Katsuaki; Akimoto, Kohichi; Uchi, Toshiyasu

1990-01-01

Solid lubricant MoS 2 films deposited by radio-frequency sputtering and a new physical process were applied to bearings and ball screws used in seismic support mechanical snubbers. The lubricity of MoS 2 films was maintained throughout 720 hours of exposure at a temperature of 200 degC. The endurance life of MoS 2 films using both radio-frequency sputtering and a new physical process was investigated by subjecting the mechanical snubber to a drag force test. Cumulative drag length reached 100 meters and 400 meters, respectively, for the two methods. The dynamic characteristics and durability of mechanical snubbers in an abnormal environment were also investigated. (author)

{alpha}-Al{sub 2}O{sub 3} catalyst supports for synthesis gas production: influence of different alumina bonding agents on support and catalyst properties

Energy Technology Data Exchange (ETDEWEB)

Marturano, M. [Centro de Investigacion y Desarrollo en Procesos Cataliticos, La Plata (Argentina); Aglietti, E.F. [Centro de Tecnologia de Recursos Minerales y Ceramica (CETMIC), Gonnet (Argentina); Ferretti, O. [Centro de Investigacion y Desarrollo en Procesos Cataliticos, La Plata (Argentina)]|[Univ. Nacional de La Plata, Dept. de Ingenieria Quimica de la Facultad de Ingenieria, La Plata (Argentina)

1997-02-01

Aluminas are widely used as catalytic supports in chemical reactions. Reforming reactions to obtain synthesis gas requires good mechanical strength and low sintering behaviour. In this work, the influence of bentonite, aluminium phosphate and alumina gel as binder agents of a calcined {alpha}-Al{sub 2}O{sub 3} are analyzed with respect to support and catalytic properties. The {alpha}-Al{sub 2}O{sub 3} supports, calcined at 1300 C, are then impregnated with solutions of Ni and Al inorganic salts to obtain the catalysts and are finally tested in the reforming reaction of methane to synthesis gas at 500-900 C. Supports and catalysts are characterized by XRD, SEM, N{sub 2} adsorption, mechanical strength test and other techniques. Mechanical strength depends on the type and quantity of binder material used during support preparation. The influence of the support on the performance of the resulting catalyst is evidenced by means of catalytic tests. (orig.) 8 refs.

Cobalt supported on carbon nanofibers as catalysts for the Fischer-Tropsch synthesis

NARCIS (Netherlands)

Bezemer, G.L.

2006-01-01

The Fischer-Tropsch (FT) process converts synthesis gas (H2/CO) over a heterogeneous catalyst into hydrocarbons. Generally, cobalt catalysts supported on oxidic carriers are used for the FT process, however it appears to be difficult to obtain and maintain fully reduced cobalt particles. To overcome

N-Branched acyclic nucleoside phosphonates as monomers for the synthesis of modified oligonucleotides

Czech Academy of Sciences Publication Activity Database

Hocková, Dana; Rosenbergová, Šárka; Ménová, Petra; Páv, Ondřej; Pohl, Radek; Novák, Pavel; Rosenberg, Ivan

2015-01-01

Roč. 13, č. 15 (2015), s. 4449-4458 ISSN 1477-0520 R&D Projects: GA ČR GAP207/11/0108; GA ČR GA13-26526S Institutional support: RVO:61388963 Keywords : acyclic nucleoside phosphonates * oligonucleotides * solid phase synthesis Subject RIV: CC - Organic Chemistry Impact factor: 3.559, year: 2015

Synthesis of Thin Film Composite Metal-Organic Frameworks Membranes on Polymer Supports

KAUST Repository

Barankova, Eva

2017-06-01

Since the discovery of size-selective metal-organic frameworks (MOF) researchers have tried to manufacture them into gas separation membranes. ZIF-8 became the most studied MOF for membrane applications mainly because of its simple synthesis, good chemical and thermal stability, recent commercial availability and attractive pore size. The aim of this work is to develop convenient methods for growing ZIF thin layers on polymer supports to obtain defect-free ZIF membranes with good gas separation properties. We present new approaches for ZIF membranes preparation on polymers. We introduce zinc oxide nanoparticles in the support as a secondary metal source for ZIF-8 growth. Initially the ZnO particles were incorporated into the polymer matrix and later on the surface of the polymer by magnetron sputtering. In both cases, the ZnO facilitated to create more nucleation opportunities and improved the ZIF-8 growth compared to the synthesis without using ZnO. By employing the secondary seeded growth method, we were able to obtain thin (900 nm) ZIF-8 layer with good gas separation performance. Next, we propose a metal-chelating polymer as a suitable support for growing ZIF layers. Defect-free ZIF-8 films with a thickness of 600 nm could be obtained by a contra-diffusion method. ZIF-8 membranes were tested for permeation of hydrogen and hydrocarbons, and one of the highest selectivities reported so far for hydrogen/propane, and propylene/propane was obtained. Another promising method to facilitate the growth of MOFs on polymeric supports is the chemical functionalization of the support surface with functional groups, which can complex metal ions and which can covalently bond the MOF crystals. We functionalized the surface of a common porous polymeric membrane with amine groups, which took part in the reaction to form ZIF-8 nanocrystals. We observed an enhancement in adhesion between the ZIF layer and the support. The effect of parameters of the contra-diffusion experiment

Synthesis of Poly(3,4-Ethylenedioxy thiophene)-Poly(Styrene-4-Sulfonate) Composites for Support Fuel Cell Catalyst Layer

International Nuclear Information System (INIS)

Eko Sulistiyono; Murni Handayani

2009-01-01

Synthesis of poly(3,4-ethylenedioxy thiophene)-poly(styrene-4-sulfonate) composites for support fuel cell catalyst layer are synthesis composites which become fuel cell catalyst support so that catalyst has optimal performance. Main function of composites is support platinum particle for application in fuel cell. This article explains the result of composites production process from ( 3,4 Ethylenedioxy thiophene) and Sodium poly( styrene - 4-sulfonate) using two methods Jingning Shan method (method 1) and Zhigang Qi and Peter G.Pickup method (method 2). Analysis of the synthesis results used Scanning Electron Microscopic –Electron Dispersive X – Ray Spectrophotometer (SEM-EDS ). The analysis result show that both methods produce polymer agglomerate into a sponge-like morphology. Composite from method 1 has morphology, pores and proton transport better than composite produced by method 2. (author)

The combined effect of interferon synthesis inductors, radiosensitizing and antitumoral agents on solid tumors

International Nuclear Information System (INIS)

Leonidze, D.L.

1987-01-01

In experiments with mice bearing solid sarcoma 37 a study was conducted on the combined effect of radiation and inductors of endogenous inerferon synthesis (IEIS), together with hyperthermia or together with an alkylating and carbomoilating agent, dimethinur. The effect was estimated by the tumor growth coefficient and by the number of animals with the regressed tumors. Poly I; polyC was not shiown to influence the efficiency of hyperthermia combined with radiation with radiation; dextransulphate and tiloron increased the radiosensitizing effect of hyperthermia. Dimethinur aggravated the effect of radiation, but with IEIS used together with dimethynur and radiation, the response of the tumor increased insignificantly as compared to the effect of IEIS together with radiation

Solid State Division Progress Report for period ending March 31, 1986

International Nuclear Information System (INIS)

Green, P.H.; Watson, D.M.

1986-08-01

This report is divided into: theoretical solid-state physics, surface and near-surface properties of solids, defects in solids, transport properties of solids, neutron scattering, and synthesis and properties of novel materials

Two-dimensional parallel array technology as a new approach to automated combinatorial solid-phase organic synthesis

Science.gov (United States)

Brennan; Biddison; Frauendorf; Schwarcz; Keen; Ecker; Davis; Tinder; Swayze

1998-01-01

An automated, 96-well parallel array synthesizer for solid-phase organic synthesis has been designed and constructed. The instrument employs a unique reagent array delivery format, in which each reagent utilized has a dedicated plumbing system. An inert atmosphere is maintained during all phases of a synthesis, and temperature can be controlled via a thermal transfer plate which holds the injection molded reaction block. The reaction plate assembly slides in the X-axis direction, while eight nozzle blocks holding the reagent lines slide in the Y-axis direction, allowing for the extremely rapid delivery of any of 64 reagents to 96 wells. In addition, there are six banks of fixed nozzle blocks, which deliver the same reagent or solvent to eight wells at once, for a total of 72 possible reagents. The instrument is controlled by software which allows the straightforward programming of the synthesis of a larger number of compounds. This is accomplished by supplying a general synthetic procedure in the form of a command file, which calls upon certain reagents to be added to specific wells via lookup in a sequence file. The bottle position, flow rate, and concentration of each reagent is stored in a separate reagent table file. To demonstrate the utility of the parallel array synthesizer, a small combinatorial library of hydroxamic acids was prepared in high throughput mode for biological screening. Approximately 1300 compounds were prepared on a 10 μmole scale (3-5 mg) in a few weeks. The resulting crude compounds were generally >80% pure, and were utilized directly for high throughput screening in antibacterial assays. Several active wells were found, and the activity was verified by solution-phase synthesis of analytically pure material, indicating that the system described herein is an efficient means for the parallel synthesis of compounds for lead discovery. Copyright 1998 John Wiley & Sons, Inc.

In situ synthesis of molecularly imprinted nanoparticles in porous support membranes using high-viscosity polymerization solvents.

Science.gov (United States)

Renkecz, Tibor; László, Krisztina; Horváth, Viola

2012-06-01

There is a growing need in membrane separations for novel membrane materials providing selective retention. Molecularly imprinted polymers (MIPs) are promising candidates for membrane functionalization. In this work, a novel approach is described to prepare composite membrane adsorbers incorporating molecularly imprinted microparticles or nanoparticles into commercially available macroporous filtration membranes. The polymerization is carried out in highly viscous polymerization solvents, and the particles are formed in situ in the pores of the support membrane. MIP particle composite membranes selective for terbutylazine were prepared and characterized by scanning electron microscopy and N₂ porosimetry. By varying the polymerization solvent microparticles or nanoparticles with diameters ranging from several hundred nanometers to 1 µm could be embedded into the support. The permeability of the membranes was in the range of 1000 to 20,000 Lm⁻²  hr⁻¹  bar⁻¹. The imprinted composite membranes showed high MIP/NIP (nonimprinted polymer) selectivity for the template in organic media both in equilibrium-rebinding measurements and in filtration experiments. The solid phase extraction of a mixture of the template, its analogs, and a nonrelated compound demonstrated MIP/NIP selectivity and substance selectivity of the new molecularly imprinted membrane. The synthesis technique offers a potential for the cost-effective production of selective membrane adsorbers with high capacity and high throughput. Copyright © 2012 John Wiley & Sons, Ltd.

Synthesis of PD particles by alcohols-assisted photoreduction for use in supported catalysts

Science.gov (United States)

Burton, Patrick David; Boyle, Timothy J; Datye, Abhaya

2015-02-24

The present disclosure provides a novel synthesis method for palladium nanoparticles and palladium nanoparticles made using the method. The nanoparticles resulting from the method are highly reactive and, when deposited on a support, are highly suitable for use as catalytic material.

On the role of the activation procedure of supported hydrotalcites for base catalyzed reactions: Glycerol to glycerol carbonate and self-condensation of acetone

NARCIS (Netherlands)

Alvarez, M.G.; Frey, A.M.; Bitter, J.H.; Segarra, A.M.; Jong, de K.P.; Medina, F.

2013-01-01

Bulk and carbon nanofiber supported MgAl hydrotalcites have been investigated as solid base catalysts for the synthesis of glycerol carbonate and dicarbonate and for the self-condensation of acetone. The supported materials exhibited a 300 times higher activity compared to bulk activated

Synthesis of methyl esters from waste cooking oil using construction waste material as solid base catalyst.

Science.gov (United States)

Balakrishnan, K; Olutoye, M A; Hameed, B H

2013-01-01

The current research investigates synthesis of methyl esters by transesterification of waste cooking oil in a heterogeneous system, using barium meliorated construction site waste marble as solid base catalyst. The pretreated catalyst was calcined at 830 °C for 4h prior to its activity test to obtained solid oxide characterized by scanning electron microscopy/energy dispersive spectroscopy, BET surface area and pore size measurement. It was found that the as prepared catalyst has large pores which contributed to its high activity in transesterification reaction. The methyl ester yield of 88% was obtained when the methanol/oil molar ratio was 9:1, reaction temperature at 65 °C, reaction time 3h and catalyst/oil mass ratio of 3.0 wt.%. The catalyst can be reused over three cycles, offer low operating conditions, reduce energy consumption and waste generation in the production of biodiesel. Copyright © 2012 Elsevier Ltd. All rights reserved.

Solid State Division Progress Report for period ending March 31, 1986

Energy Technology Data Exchange (ETDEWEB)

Green, P.H.; Watson, D.M. (eds.)

1986-08-01

This report is divided into: theoretical solid-state physics, surface and near-surface properties of solids, defects in solids, transport properties of solids, neutron scattering, and synthesis and properties of novel materials. (DLC)

Solid-Phase Iminium Cyclization Reactions for the Synthesis of Natural Product-Like Diketopiperazines

DEFF Research Database (Denmark)

Petersen, Rico

The development of methodology for the solid-phase synthesis of fused 2,5-diketopiperazines with an emphasis on structural and stereochemical control, has been accomplished through two different approaches. The first approach was based on a highly trans-stereoselective (82% d.e.) intramolecular N...... inhibitors based on the 2,5-diketopiperazino[6,1-a]tetrahydroisoquinoline scaffold was prepared and subsequently evaluated for biologically activity. The compounds showed inhibitory activity against a nuclear extract of HeLa cells, on average 200-fold lower than the activity of SAHA. When screened towards...... HDAC 1 the compounds showed a lower inhibitor activity, compared to the nuclear extract, except for one of the compounds which showed increased activity. The compound represents a clear case of stereodifferentiation. Finally, and most importantly, when screening the compounds towards HDAC 8 an activity...

Solid state chemistry and its applications

CERN Document Server

West, Anthony R

2013-01-01

Solid State Chemistry and its Applications, 2nd Edition: Student Edition is an extensive update and sequel to the bestselling textbook Basic Solid State Chemistry, the classic text for undergraduate teaching in solid state chemistry worldwide. Solid state chemistry lies at the heart of many significant scientific advances from recent decades, including the discovery of high-temperature superconductors, new forms of carbon and countless other developments in the synthesis, characterisation and applications of inorganic materials. Looking forward, solid state chemistry will be crucial for the

A green synthesis of a layered titanate, potassium lithium titanate; lower temperature solid-state reaction and improved materials performance

International Nuclear Information System (INIS)

Ogawa, Makoto; Morita, Masashi; Igarashi, Shota; Sato, Soh

2013-01-01

A layered titanate, potassium lithium titanate, with the size range from 0.1 to 30 µm was prepared to show the effects of the particle size on the materials performance. The potassium lithium titanate was prepared by solid-state reaction as reported previously, where the reaction temperature was varied. The reported temperature for the titanate preparation was higher than 800 °C, though 600 °C is good enough to obtain single-phase potassium lithium titanate. The lower temperature synthesis is cost effective and the product exhibit better performance as photocatalysts due to surface reactivity. - Graphical abstract: Finite particle of a layered titanate, potassium lithium titanate, was prepared by solid-state reaction at lower temperature to show modified materials performance. Display Omitted - Highlights: • Potassium lithium titanate was prepared by solid-state reaction. • Lower temperature reaction resulted in smaller sized particles of titanate. • 600 °C was good enough to obtain single phased potassium lithium titanate. • The product exhibited better performance as photocatalyst

Synthesis and characterization of cobaltite nanotubes for solid-oxide fuel cell cathodes

Energy Technology Data Exchange (ETDEWEB)

Napolitano, F; Baque, L; Troiani, H; Granada, M; Serquis, A, E-mail: aserquis@cab.cnea.gov.a [Instituto Balseiro-Centro Atomico Bariloche and CONICET, San Carlos de Bariloche (Argentina)

2009-05-01

La{sub 1-x}Sr{sub x}Co{sub 1-y}FeyO{sub 3-d}elta oxides are good candidates for solid oxide fuel cell (SOFC) cathodes because these materials present high ionic and electronic conductivity, and compatibility with Cerium Gadolinium Oxide (CGO) electrolytes allowing a lower operation temperature. In this work, we report the synthesis of La{sub 0.4}Sr{sub 0.6}Co{sub 0.8}Fe{sub 0.2}O{sub 3-d}elta (LSCF) nanotubes prepared by a porous polycarbonate membrane approach, obtaining different microstructures depending on sintering conditions. The structure and morphology of the nanotubes and deposited films were characterized by X-ray diffraction, transmission and scanning microscopy. Finally, we obtained nanostructured films of vertically aligned LSCF tubes deposited over the whole surface of CGO pellets with diameter up to 2.5cm in a direct and single step process.

Solid Base Catalysis

CERN Document Server

Ono, Yoshio

2011-01-01

The importance of solid base catalysts has come to be recognized for their environmentally benign qualities, and much significant progress has been made over the past two decades in catalytic materials and solid base-catalyzed reactions. The book is focused on the solid base. Because of the advantages over liquid bases, the use of solid base catalysts in organic synthesis is expanding. Solid bases are easier to dispose than liquid bases, separation and recovery of products, catalysts and solvents are less difficult, and they are non-corrosive. Furthermore, base-catalyzed reactions can be performed without using solvents and even in the gas phase, opening up more possibilities for discovering novel reaction systems. Using numerous examples, the present volume describes the remarkable role solid base catalysis can play, given the ever increasing worldwide importance of "green" chemistry. The reader will obtain an overall view of solid base catalysis and gain insight into the versatility of the reactions to whic...

Stoichiometric control in Bi₄Ti₃O₁₂ synthesis by novel hybrid solid state reaction

DEFF Research Database (Denmark)

Gadea, C.; Phatharapeetranun, N.; Ksapabutr, B.

2018-01-01

The synthesis of bismuth titanate Bi4Ti3O12 (BiT) is performed via a novel solid state reaction. The reaction is designed to control the stoichiometric content of the highly volatile element, i.e. Bi. The chemical route consists in trapping bismuth oxide colloids in a stabilized titanium based sol...

Synthesis, morphological control, and antibacterial properties of hollow/solid Ag2S/Ag heterodimers

KAUST Repository

Pang, Maolin

2010-08-11

Ag2S and Ag are important functional materials that have received considerable research interest in recent years. In this work, we develop a solution-based synthetic method to combine these two materials into hollow/solid Ag2S/Ag heterodimers at room temperature. Starting from monodisperse Cu2O solid spheres, CuS hollow spheres can be converted from Cu2O through a modified Kirkendall process, and the obtained CuS can then be used as a solid precursor for preparation of the Ag2S/Ag heterodimers through ion exchange and photo-assisted reduction. We have found that formation of the Ag2S/Ag heterodimers is instantaneous, and the size of Ag nanocrystals on the hollow spheres of Ag2S can be controlled by changing the concentration and power of reducing agents in the synthesis. The growth of Ag nanoparticles on hollow spheres of Ag2S in the dimers is along the [111] direction of the silver crystal; the light absorption properties have also been investigated. Furthermore, coupling or tripling of Ag2S/Ag heterodimers into dumbbell-like trimers ((Ag 2S)2/Ag, linear) and triangular tetramers ((Ag 2S)3/Ag, coplanar) can also be attained at 60°C by adding the bidentate ligand ethylenediamine as a cross-linking agent. To test the applicability of this highly asymmetric dipolar composite, photocatalytic inactivation of Escherichia coli K-12 in the presence of the as-prepared Ag 2S/Ag heterodimers has been carried out under UV irradiation. The added Ag2S/Ag heterodimers show good chemical stability under prolonged UV irradiation, and no appreciable solid dissolution is found. Possible mechanisms regarding the enhanced antibacterial activity have also been addressed. © 2010 American Chemical Society.

Process for preparation of a solid-phase radioimmunoassay support and use thereof

International Nuclear Information System (INIS)

Meriadec, B.; Roubertie, P.

1979-01-01

A process is described for the preparation of a support useful in radioimmunoassay chromatographic columns. The process involves the preparation of a chromatographic gel capable of selectively retaining one or more components contained in an antigen-antibody-containing solution. The gel is bound to the appropriate antiserum, then freeze-dried, pulverized and compressed into a tablet. The tablet support swells upon contact with an antigen-antibody-containing solution to conform to the shape of the columns. An example of the application of this support in the radioimmunoassay of thyroid-stimulating hormone is described. This type of support is also particularly useful in second antibody solid phase radioimmunoassays since there is no limit to the size of the antigen to which this technology may be applied. (U.K.)

Defined media and inert supports : their potential as solid-state fermentation production systems

NARCIS (Netherlands)

Ooijkaas, L.P.; Weber, F.J.; Buitelaar, R.M.; Tramper, J.; Rinzema, A.

2000-01-01

Solid-state fermentation (SSF) using inert supports impregnated with chemically defined liquid media has several potential applications in both scientific studies and in the industrial production of high-value products, such as metabolites, biological control agents and enzymes. As a result of its

Protein production by Arthrospira (Spirulina platensis in solid state cultivation using sugarcane bagasse as support

Directory of Open Access Journals (Sweden)

Lúcia Helena Pelizer

2015-03-01

Full Text Available The genus Arthrospira comprises a group of filamentous multicellular cyanobacteria and can be used for animal feed and human food. Solid state fermentation or cultivation (SSF involves the use of a culture medium composed of solid material with given moisture content. No studies have been published about the cultivation of microalgae or cyanobacteria on solid medium. Furthermore, although sugar-cane bagasse is used as source of energy in alcohol distilleries in Brazil, the excess could be a support to photosynthetic microorganism growth. The experimental design methodology was used to evaluate the protein production by Arthrospira platensis under SSF using sugarcane bagasse as support, taking into account the moisture content of the medium, light intensity and inoculum concentration. Moisture was found to have a strong influence on the performance of the process. The best conditions were: moisture of 98.8%; inoculum concentration of 0.15 g biomass·kg wet culture medium−1 and light intensity of 6.0 klx.

Synthesis, characterization and thermal stability of solid solutions Zr (Y, Fe, MoO2

Directory of Open Access Journals (Sweden)

Felipe Legorreta-García

2015-05-01

Full Text Available The synthesis of Fe3+, Mo4+ and Y3+ fully stabilized zirconia by the nitrate/urea combustion route and thermal stability in air was investigated. The solid solution obtained was characterized by X ray diffraction (XRD, scanning electron microscopy (SEM and used the BET method for determining specific surface. The ceramic powders obtained were calcined at 1473 K in air atmosphere in order to determine their thermal stability. The scanning electron microscopy (SEM results showed a homogeneous grain surface, measuring several tens of micrometers across. The crystallographic study revealed that by this method it was successfully achieved zirconia doped with Fe3+, Mo4+ and Y3+ ions in the zirconia tetragonal monophase, even after calcinations.

Perspective: Toward "synthesis by design": Exploring atomic correlations during inorganic materials synthesis

Science.gov (United States)

Soderholm, L.; Mitchell, J. F.

2016-05-01

Synthesis of inorganic extended solids is a critical starting point from which real-world functional materials and their consequent technologies originate. However, unlike the rich mechanistic foundation of organic synthesis, with its underlying rules of assembly (e.g., functional groups and their reactivities), the synthesis of inorganic materials lacks an underpinning of such robust organizing principles. In the latter case, any such rules must account for the diversity of chemical species and bonding motifs inherent to inorganic materials and the potential impact of mass transport on kinetics, among other considerations. Without such assembly rules, there is less understanding, less predictive power, and ultimately less control of properties. Despite such hurdles, developing a mechanistic understanding for synthesis of inorganic extended solids would dramatically impact the range of new material discoveries and resulting new functionalities, warranting a broad call to explore what is possible. Here we discuss our recent approaches toward a mechanistic framework for the synthesis of bulk inorganic extended solids, in which either embryonic atomic correlations or fully developed phases in solutions or melts can be identified and tracked during product selection and crystallization. The approach hinges on the application of high-energy x-rays, with their penetrating power and large Q-range, to explore reaction pathways in situ. We illustrate this process using two examples: directed assembly of Zr clusters in aqueous solution and total phase awareness during crystallization from K-Cu-S melts. These examples provide a glimpse of what we see as a larger vision, in which large scale simulations, data-driven science, and in situ studies of atomic correlations combine to accelerate materials discovery and synthesis, based on the assembly of well-defined, prenucleated atomic correlations.

Protocol for the Solid-phase Synthesis of Oligomers of RNA Containing a 2'-O-thiophenylmethyl Modification and Characterization via Circular Dichroism.

Science.gov (United States)

Francis, Andrew J; Resendiz, Marino J E

2017-07-28

Solid-phase synthesis has been used to obtain canonical and modified polymers of nucleic acids, specifically of DNA or RNA, which has made it a popular methodology for applications in various fields and for different research purposes. The procedure described herein focuses on the synthesis, purification, and characterization of dodecamers of RNA 5'-[CUA CGG AAU CAU]-3' containing zero, one, or two modifications located at the C2'-O-position. The probes are based on 2-thiophenylmethyl groups, incorporated into RNA nucleotides via standard organic synthesis and introduced into the corresponding oligonucleotides via their respective phosphoramidites. This report makes use of phosphoramidite chemistry via the four canonical nucleobases (Uridine (U), Cytosine (C), Guanosine (G), Adenosine (A)), as well as 2-thiophenylmethyl functionalized nucleotides modified at the 2'-O-position; however, the methodology is amenable for a large variety of modifications that have been developed over the years. The oligonucleotides were synthesized on a controlled-pore glass (CPG) support followed by cleavage from the resin and deprotection under standard conditions, i.e., a mixture of ammonia and methylamine (AMA) followed by hydrogen fluoride/triethylamine/N-methylpyrrolidinone. The corresponding oligonucleotides were purified via polyacrylamide electrophoresis (20% denaturing) followed by elution, desalting, and isolation via reversed-phase chromatography (Sep-pak, C18-column). Quantification and structural parameters were assessed via ultraviolet-visible (UV-vis) and circular dichroism (CD) photometric analysis, respectively. This report aims to serve as a resource and guide for beginner and expert researchers interested in embarking in this field. It is expected to serve as a work-in-progress as new technologies and methodologies are developed. The description of the methodologies and techniques within this document correspond to a DNA/RNA synthesizer (refurbished and purchased in

FSILP: fuzzy-stochastic-interval linear programming for supporting municipal solid waste management.

Science.gov (United States)

Li, Pu; Chen, Bing

2011-04-01

Although many studies on municipal solid waste management (MSW management) were conducted under uncertain conditions of fuzzy, stochastic, and interval coexistence, the solution to the conventional linear programming problems of integrating fuzzy method with the other two was inefficient. In this study, a fuzzy-stochastic-interval linear programming (FSILP) method is developed by integrating Nguyen's method with conventional linear programming for supporting municipal solid waste management. The Nguyen's method was used to convert the fuzzy and fuzzy-stochastic linear programming problems into the conventional linear programs, by measuring the attainment values of fuzzy numbers and/or fuzzy random variables, as well as superiority and inferiority between triangular fuzzy numbers/triangular fuzzy-stochastic variables. The developed method can effectively tackle uncertainties described in terms of probability density functions, fuzzy membership functions, and discrete intervals. Moreover, the method can also improve upon the conventional interval fuzzy programming and two-stage stochastic programming approaches, with advantageous capabilities that are easily achieved with fewer constraints and significantly reduces consumption time. The developed model was applied to a case study of municipal solid waste management system in a city. The results indicated that reasonable solutions had been generated. The solution can help quantify the relationship between the change of system cost and the uncertainties, which could support further analysis of tradeoffs between the waste management cost and the system failure risk. Copyright © 2010 Elsevier Ltd. All rights reserved.

Fully automated synthesis of ¹¹C-acetate as tumor PET tracer by simple modified solid-phase extraction purification.

Science.gov (United States)

Tang, Xiaolan; Tang, Ganghua; Nie, Dahong

2013-12-01

Automated synthesis of (11)C-acetate ((11)C-AC) as the most commonly used radioactive fatty acid tracer is performed by a simple, rapid, and modified solid-phase extraction (SPE) purification. Automated synthesis of (11)C-AC was implemented by carboxylation reaction of MeMgBr on a polyethylene Teflon loop ring with (11)C-CO2, followed by acidic hydrolysis with acid and SCX cartridge, and purification on SCX, AG11A8 and C18 SPE cartridges using a commercially available (11)C-tracer synthesizer. Quality control test and animals positron emission tomography (PET) imaging were also carried out. A high and reproducible decay-uncorrected radiochemical yield of (41.0 ± 4.6)% (n=10) was obtained from (11)C-CO2 within the whole synthesis time about 8 min. The radiochemical purity of (11)C-AC was over 95% by high-performance liquid chromatography (HPLC) analysis. Quality control test and PET imaging showed that (11)C-AC injection produced by the simple SPE procedure was safe and efficient, and was in agreement with the current Chinese radiopharmaceutical quality control guidelines. The novel, simple, and rapid method is readily adapted to the fully automated synthesis of (11)C-AC on several existing commercial synthesis module. The method can be used routinely to produce (11)C-AC for preclinical and clinical studies with PET imaging. Copyright © 2013 Elsevier Ltd. All rights reserved.

Nanoparticles Formed Onto/Into Halloysite Clay Tubules: Architectural Synthesis and Applications.

Science.gov (United States)

Vinokurov, Vladimir A; Stavitskaya, Anna V; Glotov, Aleksandr P; Novikov, Andrei A; Zolotukhina, Anna V; Kotelev, Mikhail S; Gushchin, Pawel A; Ivanov, Evgenii V; Darrat, Yusuf; Lvov, Yuri M

2018-01-04

Nanoparticles, being objects with high surface area are prone to agglomeration. Immobilization onto solid supports is a promising method to increase their stability and it allows for scalable industrial applications, such as metal nanoparticles adsorbed to mesoporous ceramic carriers. Tubular nanoclay - halloysite - can be an efficient solid support, enabling the fast and practical architectural (inside / outside) synthesis of stable metal nanoparticles. The obtained halloysite-nanoparticle composites can be employed as advanced catalysts, ion-conducting membrane modifiers, inorganic pigments, and optical markers for biomedical studies. Here, we discuss the possibilities to synthesize halloysite decorated with metal, metal chalcogenide, and carbon nanoparticles, and to use these materials in various fields, especially in catalysis and petroleum refinery. © 2018 The Chemical Society of Japan & Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solid state synthesis and sintering of monazite-type ceramics: application to minor actinides conditioning

International Nuclear Information System (INIS)

Bregiroux, D.

2005-11-01

In the framework of the French law of 1991 concerning the nuclear waste management, several studies are undertaken to develop specific crystalline conditioning matrices. Monazite, a rare earth (TR 3+ ) orthophosphate with a general formula TR 3+ PO 4 , is a natural mineral containing significant amount of thorium and uranium. Monazite has been proposed as a host matrix for the minor actinides (Np, Am and Cm) specific conditioning, thanks to its high resistance to self irradiation and its low solubility. Its is now of prime importance to check the conservation of these properties on synthesized materials, which implies to master all the stages of the elaboration process, from the powder synthesis to the sintering of controlled microstructure pellets. This work can be divided into two main parts: The first part deals with the synthesis by high temperature solid state route of TR 3+ PO 4 powders (with TR 3+ = La 3+ to Gd 3+ , Pu 3+ and Am 3+ ). The chemical reactions occurring during the firing of starting reagents are described in the case of monazite with only one or several cations. From these results, a protocol of synthesis is described. The incorporation of tetravalent cations (Ce 4+ , U 4+ , Pu 4+ ) in the monazite structure was also studied. The second part of the present work deals with the elaboration of controlled density and microstructure monazite pellets and their related mechanical and thermal properties. The study of crushing and sintering is presented. For the first time, experimental results are confronted with theoretical models in order to deduce the densification and grain growth mechanisms. By the comprehension of the various physicochemical phenomena occurring during the various stages of the monazite pellets elaboration process (powder synthesis, crushing, sintering...), this work allowed the development of a protocol of elaboration of controlled microstructure monazite TR 3+ PO 4 pellets. The determination of some mechanical and thermal

Advanced technologies available for future solid propellant grains

Energy Technology Data Exchange (ETDEWEB)

Thepenier, J. [SNPE Propulsion, St Medard en Jalles (France); Fonblanc, G. [SNPE Propulsion, Vert le Petit (France). Centre de Recherche de Bouchet

2001-06-01

Significant advances have been made during the last decade in several fields of solid propulsion: the advances have enabled new savings in the motor development phase and in recurring costs, because they help limit the number of prototypes and tests. The purpose of the paper is to describe the improvements achieved by SNPE in solid grain technologies, making these technologies available for new developments in more efficient and reliable future SRMs: new energetic molecules, new solid propellants, new processes for grain manufacturing, quick response grain design tools associated with advanced models for grain performance predictions. Using its expertise in chemical synthesis, SNPE develops new molecules to fit new energetic material requirements. Tests based on new propellant formulations have produced good results in the propellant performance/safety behavior ratio. New processes have been developed simultaneously to reduce the manufacturing costs of the new propellants. In addition, the grain design has been optimized by using the latest generation of predictive theoretical tools supported by a large data bank of experimental parameters resulting from over 30 years' experience in solid propulsion: computer-aided method for the preliminary grain design; advanced models for SRM operating and performance predictions. All these technologies are available for industrial applications in future developments of solid propellant grains. (author)

Synthesis and characterization of platinum supported on alumina doped with cerium catalyst

International Nuclear Information System (INIS)

Yusof Abdullah; Abd Fatah Awang Mat; Mohd Ali Sufi; Sarimah Mahat; Razali Kassim; Nurhaslinda Abdullah.

1996-03-01

The synthesis and characterization of gamma-alumina doped with cerium as platinum support for the automobile exhaust catalyst are described. Platinum/alumina/ceria catalyst were prepared by impregnation of hexachloroplatinic acid and sintered at 500 degree Celsius to obtain metal dispersions of 1.0 wt%. Catalyst distribution inside the powder and the effects of the addition of cerium to alumina were analyzed by the scanning electron microscopy (SEM) and x-ray fluorescence spectroscopy (XRF). The results showed that the alumina - supported catalysts contained well dispersion of the noble metal

Requirements Development Issues for Advanced Life Support Systems: Solid Waste Management

Science.gov (United States)

Levri, Julie A.; Fisher, John W.; Alazraki, Michael P.; Hogan, John A.

2002-01-01

Long duration missions pose substantial new challenges for solid waste management in Advanced Life Support (ALS) systems. These possibly include storing large volumes of waste material in a safe manner, rendering wastes stable or sterilized for extended periods of time, and/or processing wastes for recovery of vital resources. This is further complicated because future missions remain ill-defined with respect to waste stream quantity, composition and generation schedule. Without definitive knowledge of this information, development of requirements is hampered. Additionally, even if waste streams were well characterized, other operational and processing needs require clarification (e.g. resource recovery requirements, planetary protection constraints). Therefore, the development of solid waste management (SWM) subsystem requirements for long duration space missions is an inherently uncertain, complex and iterative process. The intent of this paper is to address some of the difficulties in writing requirements for missions that are not completely defined. This paper discusses an approach and motivation for ALS SWM requirements development, the characteristics of effective requirements, and the presence of those characteristics in requirements that are developed for uncertain missions. Associated drivers for life support system technological capability are also presented. A general means of requirements forecasting is discussed, including successive modification of requirements and the need to consider requirements integration among subsystems.

Synthesis, electronic structure, elastic properties, and interfacial behavior of icosahedral boron-rich solids

Energy Technology Data Exchange (ETDEWEB)

Hunold, Oliver

2017-08-01

Boron-rich solids are commonly characterized by icosahedral clusters, where 12 B atoms form an icosahedron, giving rise to outstanding mechanical and transport properties. However, broader applications are limited due to the high synthesis temperature required to obtain the icosahedra-based crystalline structure. Utilizing high power pulsed magnetron sputtering (HPPMS), the deposition temperature may be lowered as compared to direct current magnetron sputtering by enhanced surface diffusion. Therefore, HPPMS was utilized to investigate the influence of the substrate temperature on the structural evolution of B-rich Al-Y-B thin films. The formation of the intended AlYB{sub 14} phase together with the (Y,Al)B{sub 6} impurity phase, containing 1.8 at.% less B than AlYB{sub 14}, was observed at a growth temperature of 800 C and hence 600 C below the bulk synthesis temperature. Based on density functional theory (DFT) calculations it is inferred that minute compositional variations may lead to formation of competing phases, such as (Y,Al)B{sub 6}. Furthermore, 800 C still limits the usage significantly. Therefore, quantum mechanical material design was applied to identify phases with even higher phase stabilities compared to AlYB{sub 14}. Phase stability of T{sub 0.75}Y{sub 0.75}B{sub 14} (T= Sc, Ti, V, Y, Zr, Nb, Si) critically depends on the exact magnitude of charge transferred by T and Y to the B icosahedra. The highest phase stabilities have been identified for Sc{sub 0.75}Y{sub 0.75}B{sub 14}, Ti{sub 0.75}Y{sub 0.75}B{sub 14}, and Zr{sub 0.75}Y{sub 0.75}B{sub 14}. ln combination with Young's modulus values up to 517 GPa these phases are very interesting from a wear-resistance point of view. Still high synthesis temperatures limit the use of such systems onto technologically relevant substrate materials. However, amorphous B-rich solids, which can be synthesized without additional heating, exhibit attractive mechanical and electrical properties. Within these

Assaying the proton transport and regulation of UCP1 using solid supported membranes.

Science.gov (United States)

Blesneac, Iulia; Ravaud, Stéphanie; Machillot, Paul; Zoonens, Manuela; Masscheylen, Sandrine; Miroux, Bruno; Vivaudou, Michel; Pebay-Peyroula, Eva

2012-08-01

The uncoupling protein 1 (UCP1) is a mitochondrial protein that carries protons across the inner mitochondrial membrane. It has an important role in non-shivering thermogenesis, and recent evidence suggests its role in human adult metabolism. Using rapid solution exchange on solid supported membranes, we succeeded in measuring electrical currents generated by the transport activity of UCP1. The protein was purified from mouse brown adipose tissue, reconstituted in liposomes and absorbed on solid supported membranes. A fast pH jump activated the ion transport, and electrical signals could be recorded. The currents were characterized by a fast rise and a slow decay, were stable over time, inhibited by purine nucleotides and activated by fatty acids. This new assay permits direct observation of UCP1 activity in controlled cell-free conditions, and opens up new possibilities for UCP1 functional characterization and drug screening because of its robustness and its potential for automation.

Synthesis of crystalline ceramics for actinide immobilisation

International Nuclear Information System (INIS)

Burakov, B.; Gribova, V.; Kitsay, A.; Ojovan, M.; Hyatt, N.C.; Stennett, M.C.

2007-01-01

Methods for the synthesis of ceramic wasteforms for the immobilization of actinides are common to those for non-radioactive ceramics: hot uniaxial pressing (HUP); hot isostatic pressing (HIP); cold pressing followed by sintering; melting (for some specific ceramics, such as garnet/perovskite composites). Synthesis of ceramics doped with radionuclides is characterized with some important considerations: all the radionuclides should be incorporated into crystalline structure of durable host-phases in the form of solid solutions and no separate phases of radionuclides should be present in the matrix of final ceramic wasteform; all procedures of starting precursor preparation and ceramic synthesis should follow safety requirements of nuclear industry. Synthesis methods that avoid the use of very high temperatures and pressures and are easily accomplished within the environment of a glove-box or hot cell are preferable. Knowledge transfer between the V. G. Khlopin Radium Institute (KRI, Russia) and Immobilisation Science Laboratory (ISL, UK) was facilitated in the framework of a joint project supported by UK Royal Society. In order to introduce methods of precursor preparation and ceramic synthesis we selected well-known procedures readily deployable in radiochemical processing plants. We accounted that training should include main types of ceramic wasteforms which are currently discussed for industrial applications. (authors)

Antisolvent Precipitation for the Synthesis of Monodisperse Mesoporous Niobium Oxide Spheres as Highly Effective Solid Acid Catalysts

KAUST Repository

Li, Cheng Chao; Dou, Jian; Chen, Luwei; Lin, Jianyi; Zeng, Hua Chun

2012-01-01

We have developed a low-cost reaction protocol to synthesize mesoporous Nb 2O 5-based solid acid catalysts with external shape control. In the synthesis, monodisperse glycolated niobium oxide spheres (GNOS) were prepared by means of a simple antisolvent precipitation approach and subsequently converted to mesoporous niobium oxide spheres (MNOS) with a large surface area of 312m 2g -1 by means of the hydrothermal treatment. The antisolvent acetone used to obtain GNOS was recovered through distillation at high purity. The obtained mesoporous MNOS were functionalized further with sulfate anions at different temperatures or incorporated with tungstophosphoric acid to obtain recyclable solid acid catalysts. These MNOS-based catalysts showed excellent performance in a wide range of acid-catalyzed reactions, such as Friedel-Crafts alkylation, esterification, and hydrolysis of acetates. As they are monodisperse spheres with diameters in the submicrometer range, the catalysts can be easily separated and reused. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Antisolvent Precipitation for the Synthesis of Monodisperse Mesoporous Niobium Oxide Spheres as Highly Effective Solid Acid Catalysts

KAUST Repository

Li, Cheng Chao

2012-03-20

We have developed a low-cost reaction protocol to synthesize mesoporous Nb 2O 5-based solid acid catalysts with external shape control. In the synthesis, monodisperse glycolated niobium oxide spheres (GNOS) were prepared by means of a simple antisolvent precipitation approach and subsequently converted to mesoporous niobium oxide spheres (MNOS) with a large surface area of 312m 2g -1 by means of the hydrothermal treatment. The antisolvent acetone used to obtain GNOS was recovered through distillation at high purity. The obtained mesoporous MNOS were functionalized further with sulfate anions at different temperatures or incorporated with tungstophosphoric acid to obtain recyclable solid acid catalysts. These MNOS-based catalysts showed excellent performance in a wide range of acid-catalyzed reactions, such as Friedel-Crafts alkylation, esterification, and hydrolysis of acetates. As they are monodisperse spheres with diameters in the submicrometer range, the catalysts can be easily separated and reused. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solid-State Synthesis and Effect of Temperature on Optical Properties of CuO Nanoparticles

Institute of Scientific and Technical Information of China (English)

C.C.Vidyasagar; Y.Arthoba Naik; T.G.Venkatesha; R.Viswanatha

2012-01-01

Modulation of band energies through size control offers new ways to control photoresponse and photoconversion efficiency of the solar cell. The P-type semiconductor of copper oxide is an important functional material used for photovoltaic cells. Cu O is attractive as a selective solar absorber since it has high solar absorbance and a low thermal emittance. The present work describes the synthesis and characterization of semiconducting Cu O nanoparticles via one-step, solid-state reaction in the presence of Polyethylene glycol400 as size controlling agent for the preparation of Cu O nanoparticles at different temperatures. Solid-state mechanochemical processing, which is not only a physical size reduction process in conventional milling but also a chemical reaction, is mechanically activated at the nanoscale during grinding. The present method is a simple and efficient method of preparing nanoparticles with high yield at low cost. The structural and chemical composition of the nanoparticles were analyzed by X-ray diffraction, field emission scanning electron microscopy and energy-dispersive spectrometer, respectively. Optical properties and band gap of Cu O nanoparticles were studied by UV-Vis spectroscopy. These results showed that the band gap energy decreased with increase of annealing temperature, which can be attributed to the improvement in grain size of the samples.

Ignition and wave processes in combustion of solids

CERN Document Server

Rubtsov, Nickolai M; Alymov, Michail I

2017-01-01

This book focuses on the application of classical combustion theory to ignition and flame propagation in solid-solid and gas-solid systems. It presents experimental investigations in the areas of local ignition, filtration combustion, self-propagating high temperature synthesis and nanopowders protection. The authors highlight analytical formulas used in different areas of combustion in solids and propose an approach based on classical combustion theory. The book attempts to analyze the basic approaches to understanding of solid-solid and solid - gas combustion presented in contemporary literature in a unified approach based on classical combustion theory. .

Development of a Novel Ceramic Support Layer for Planar Solid Oxide Cells

DEFF Research Database (Denmark)

Klemensø, Trine; Boccaccini, Dino; Brodersen, Karen

2014-01-01

The conventional solid oxide cell is based on a Ni–YSZ support layer, placed on the fuel side of the cell, also known as the anode supported SOFC. An alternative design, based on a support of porous 3YSZ (3 mol.% Y2O3–doped ZrO2), placed on the oxygen electrode side of the cell, is proposed...... of the support can be done simultaneously with forming the oxygen electrode, since some of the best performing oxygen electrodes are based on infiltrated LSC. The potential of the proposed structure was investigated by testing the mechanical and electrical properties of the support layer. Comparable strength...... properties to the conventional Ni/YSZ support were seen, and sufficient and fairly stable conductivity of LSC infiltrated 3YSZ was observed. The conductivity of 8–15 S cm–1 at 850 °C seen for over 600 h, corresponds to a serial resistance of less than 3.5 m Ω cm2 of a 300 μm thick support layer....

A New Nano Silica Gel Supported by Thionyl Chloride as a Solid Acid for the Efficient Diazotization of Aniline Derivatives: Application and Synthesis of Azo Dyes

Directory of Open Access Journals (Sweden)

Mohammad Mirjalili

2012-01-01

Full Text Available A new nano silicagel supported by thionyl chloride as a solid acid was synthesized and used as a increasing the production yield of dye to affect the efficient diazotization of arylamines. The diazonium salts thus obtained were coupled, using standard experimental procedures, to anilines and naphthols to afford the requisite azo dyes in good yield. The diazotization and subsequent azo-coupling generated the related azo dyes at low temperature in short reaction times with a simple experimental procedure.

Synthesis of modified calcium aluminate with lanthanum manganite (LSM) for possible use in solid oxide fuel cell (SOFC)

International Nuclear Information System (INIS)

Veiga, F.C.T.; Jurado, J.; Sousa, V.C. de

2016-01-01

The fuel cells solid oxide (SOFC) is made up of three basic elements: two electrodes, the anode and cathode and a conductive electrolyte ions. The objective of this work consists of calcium aluminate synthesis modified LSM in a 1: 1 by combustion synthesis method with a view to its use as a cathode in SOFC. The characterization of the post was carried out by the methods of XRD, TEM and EIS. After heat treatment at 1200°C/4 hours it was possible to obtain Ca0.5Sr1.5MnO4 and CaMnO2.56 phases. The material showed a semiconductor characteristics because with increasing temperature the electrical resistance value tends to decrease obtaining electrical conductivity greater than 10-6S / cm featuring an extrinsic semiconductor with an activation energy of 0.12. Therefore, with an activation energy value within the range of materials used for a SOFC cathodes. (author)

Towards High Power Density Metal Supported Solid Oxide Fuel Cell for Mobile Applications

DEFF Research Database (Denmark)

Nielsen, Jimmi; Persson, Åsa H.; Muhl, Thuy Thanh

2018-01-01

For use of metal supported solid oxide fuel cell (MS-SOFC) in mobile applications it is important to reduce the thermal mass to enable fast startup, increase stack power density in terms of weight and volume and reduce costs. In the present study, we report on the effect of reducing the Technical...

Effects of accelerated degradation on metal supported thin film-based solid oxide fuel cell

DEFF Research Database (Denmark)

Reolon, R. P.; Sanna, S.; Xu, Yu

2018-01-01

A thin film-based solid oxide fuel cell is deposited on a Ni-based metal porous support by pulsed laser deposition with a multi-scale-graded microstructure design. The fuel cell, around 1 μm in thickness, is composed of a stabilized-zirconia/doped-ceria bi-layered dense electrolyte and nanostruct......A thin film-based solid oxide fuel cell is deposited on a Ni-based metal porous support by pulsed laser deposition with a multi-scale-graded microstructure design. The fuel cell, around 1 μm in thickness, is composed of a stabilized-zirconia/doped-ceria bi-layered dense electrolyte......, electrochemical performances are steady, indicating the stability of the cell. Under electrical load, a progressive degradation is activated. Post-test analysis reveals both mechanical and chemical degradation of the cell. Cracks and delamination of the thin films promote a significant nickel diffusion and new...

Synthesis, characterization and thermal stability of solid solutions Zr (Y, Fe, Mo)O {sub 2}

Energy Technology Data Exchange (ETDEWEB)

Legorreta-Garcia, F.; Esperanza Hernandez-Cruz, L.; Villanueva-Ibanez, M.; Flores-Gonzalez, M. A.

2015-10-01

The synthesis of Fe{sup 3}+, Mo{sup 4+} and Y{sup 3+} fully stabilized zirconia by the nitrate/urea combustion route and thermal stability in air was investigated. The solid solution obtained was characterized by X ray diffraction (XRD), scanning electron microscopy (SEM) and used the BET method for determining specific surface. The ceramic powders obtained were calcined at 1473 K in air atmosphere in order to determine their thermal stability. The scanning electron microscopy (SEM) results showed a homogeneous grain surface, measuring several tens of micrometers across. The crystallographic study revealed that by this method it was successfully achieved zirconia doped with Fe{sup 3+}, Mo{sup 4+} and Y{sup 3+} ions in the zirconia tetragonal monophase, even after calcinations. (Author)

Investigation of Novel Electrocatalysts for Metal Supported Solid Oxide Fuel Cells - Ru:GDC

DEFF Research Database (Denmark)

Sudireddy, Bhaskar Reddy; Nielsen, Jimmy; Thydén, Karl Tor Sune

2015-01-01

The electrochemical performance and stability of the planar metal supported solid oxide fuel cells (MS-SOFC) with two different electrocatalytically active materials, namely, Ni:GDC and Ru:GDC were investigated. Ru:GDC with an ASR of 0.322 Ωcm2 performed better than Ni:GDC with an ASR of 0.453 Ωc...

Effects of size reduction on the structure and magnetic properties of core-shell Ni3Si/silica nanoparticles prepared by electrochemical synthesis

Czech Academy of Sciences Publication Activity Database

Pigozzi, G.; Mukherji, D.; Elerman, Y.; Strunz, Pavel; Gilles, R.; Hoelzel, M.; Barbier, B.; Schmutz, P.

2014-01-01

Roč. 584, JAN (2014), s. 119-127 ISSN 0925-8388 Institutional support: RVO:61389005 Keywords : intermetallics * nanostructured materials * transition metal alloys and compounds * electrochemical synthesis * crystal structure * magnetic measurements Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.999, year: 2014

Break‐down of Losses in High Performing Metal‐Supported Solid Oxide Fuel Cells

DEFF Research Database (Denmark)

Kromp, A.; Nielsen, Jimmi; Blennow Tullmar, Peter

2013-01-01

in the metal support, the electrochemical fuel oxidation at the anode and the oxygen reduction in the mixed ionic electronic conducting cathode. An additional process with a rather high relaxation frequency was attributed to the formation of insulating interlayers at the cathode/electrolyte‐interface. Based...... on these results, selective measures to improve performance and stability, such as (i) PVD‐deposited CGO buffer layer preventing solid state reaction between cathode and the zirconia‐based electrolyte, (ii) LSC‐CGO based in‐situ sintered cathodes and (iii) reduced corrosion of the metal support, were adopted...

Study of ion separation through solid-supported liquid membrane

International Nuclear Information System (INIS)

Kang, Young Ho; Kim, Jung Do; Kim, Kyoung Ho

1990-01-01

The membranes used in this study consist of a microporous polymeric support with the solvent contraining alamine 336, Tri-N-Octyl phosphine oxide, Tri-N-butyl phosphate, Di-(2-ethylhexyl) phosphoric acid as a carrier within the pores by the capillary forces. When this liquid membrane is interposed between aqueous feed and product solutions, the carrier serving as a complexing agent, can pick up the uranium ions on the feed side of the membrane and carry them across the membrane by diffusion. In this study, the uranium flux through the solid-supported liquid membrane was analyzed as a function of carrier concentration and acidity of the feed solution for the carrier species. Also, the Gel-liquid extraction of uranium ions from aqueous solution was performed. The adsorbents were prepared by casting the polymer solution composed of polyvinyl chloride, TOPO, and additions. The extraction of uranyl nitrate ions has been investigated as a function of TOPO/PVC ratio, evaporation time, and the stability. The results show that is maybe possible to develop an alternative uranium purification process. (author)

Flow synthesis of phenylserine using threonine aldolase immobilized on Eupergit support

Science.gov (United States)

Tibhe, Jagdish D; Fu, Hui; Noël, Timothy; Wang, Qi; Meuldijk, Jan

2013-01-01

Summary Threonine aldolase (TA) from Thermotoga maritima was immobilized on an Eupergit support by both a direct and an indirect method. The incubation time for the direct immobilization method was optimized for the highest amount of enzyme on the support. By introducing the immobilized TA in a packed-bed microreactor, a flow synthesis of phenylserine was developed, and the effects of temperature and residence time were studied in particular. Calculations of the Damköhler number revealed that no mass transfer limitations are given in the micro-interstices of the packed bed. The yield does not exceed 40% and can be rationalized by the natural equilibrium as well as product inhibition which was experimentally proven. The flow synthesis with the immobilized enzyme was compared with the corresponding transformation conducted with the free enzyme. The product yield was further improved by operating under slug flow conditions which is related to the very short residence time distribution. In all cases 20% diastereomeric excess (de) and 99% enantiomeric excess (ee) were observed. A continuous run of the reactant solution was carried out for 10 hours in order to check enzyme stability at higher temperature. Stable operation was achieved at 20 minute residence time. Finally, the productivity of the reactor was calculated, extrapolated to parallel run units, and compared with data collected previously. PMID:24204429

Flow synthesis of phenylserine using threonine aldolase immobilized on Eupergit support

Directory of Open Access Journals (Sweden)

Jagdish D. Tibhe

2013-10-01

Full Text Available Threonine aldolase (TA from Thermotoga maritima was immobilized on an Eupergit support by both a direct and an indirect method. The incubation time for the direct immobilization method was optimized for the highest amount of enzyme on the support. By introducing the immobilized TA in a packed-bed microreactor, a flow synthesis of phenylserine was developed, and the effects of temperature and residence time were studied in particular. Calculations of the Damköhler number revealed that no mass transfer limitations are given in the micro-interstices of the packed bed. The yield does not exceed 40% and can be rationalized by the natural equilibrium as well as product inhibition which was experimentally proven. The flow synthesis with the immobilized enzyme was compared with the corresponding transformation conducted with the free enzyme. The product yield was further improved by operating under slug flow conditions which is related to the very short residence time distribution. In all cases 20% diastereomeric excess (de and 99% enantiomeric excess (ee were observed. A continuous run of the reactant solution was carried out for 10 hours in order to check enzyme stability at higher temperature. Stable operation was achieved at 20 minute residence time. Finally, the productivity of the reactor was calculated, extrapolated to parallel run units, and compared with data collected previously.

A green protocol for the synthesis of quinoxaline derivatives catalyzed by polymer supported sulphanilic acid

Directory of Open Access Journals (Sweden)

Umesh P. Tarpada

2017-05-01

Full Text Available Polymer supported sulphanilic acid was found to be an effective heterogeneous catalyst for one pot synthesis of various quinoxaline derivatives from the condensation reaction between 1,2-diamines and 1,2-dicarbonyl compounds in ethanol. Synthesis was attempted under reflux as well as at room temperature using ethanol as the solvent to afford excellent yields. Heterogeneity of the catalyst allowed its recycling for five times with almost retention in catalytic activity. Prepared quinoxaline derivatives were also tested for their antioxidant activity by the FRAP assay method.

Binding of monoclonal antibody to protein antigen in fluid phase or bound to solid supports

Energy Technology Data Exchange (ETDEWEB)

Kennel, S J

1982-01-01

Rat monoclonal antibody (MoAb) to fragment D (FgD) of human fibrinogen was used to characterize the direct binding of antibody to protein in solution or bound to solid supports. Purified IgG, F(ab')/sub 2/ and Fab' were prepared from ascites fluid of hybridoma 104-14B which is a fusion product of spleen cells from a rat immunized with FgD and the mouse myeloma cell line, P3-X63-Ag8. Two-dimensional electrophoresis of radioiodinated antibody preparations demonstrated the presence of hybrid immunoglobulin molecules, but only structures having rat heavy and rat light chains had active antibody combinig sites. The affinity constant for IgG as well as F(ab')/sub 2/ and Fab', 6x10/sup 9/ M/sup -1/, was identical when tested using fluid phase antigen (/sup 125/I-labeled FgD). Affinity constants determined for direct binding of iodinated IgG using FgD immobilized on solid supports showed a slight dependence on the antigen concentration used in the measurement. These values ranged from 0.5x10/sup 9/ M/sup -1/ at high antigen concentrations (1.3x10/sup -7/ M) to 9x10/sup 9/ M/sup -1/ at low antigen concentration (1.3x10/sup -10/ M). Binding constants for F(ab')/sub 2/ and Fab' gave similar results indicating that binding was homogeneous and univalent. The capacity of solid state antigen to bind antibody varied with the method used to bind FgD to the solid support. FgD bound directly to polystyrene plates was least efficient at binding labeled antibody; FgD bound to plates through intermediate carriers poly(L-lysine) was only slightly more efficient, while antigen bound to Sepharose beads by cyanogen bromide activation was the most active.

Nanostructured carbon-supported Pd electrocatalysts for ethanol oxidation: synthesis and characterization

Science.gov (United States)

Gacutan, E. M.; Climaco, M. I.; Telan, G. J.; Malijan, F.; Hsu, H. Y.; Garcia, J.; Fulo, H.; Tongol, B. J.

2012-12-01

The need to lower the construction cost of fuel cells calls for the development of non-Pt based electrocatalysts. Among others, Pd has emerged as a promising alternative to Pt for fuel cell catalysis. This research aims to investigate the synthesis and characterization of nanostructured Pd-based catalysts dispersed on carbon support as anode materials in direct ethanol fuel cells. For the preparation of the first Pd-based electrocatalyst, palladium nanoparticles (NPs) were synthesized via oleylamine (OAm)-mediated synthesis and precursor method with a mean particle size of 3.63 ± 0.59 nm as revealed by transmission electron microscopy (TEM). Carbon black was used as a supporting matrix for the OAm-capped Pd NPs. Thermal annealing and acetic acid washing were used to remove the OAm capping agent. To evaluate the electrocatalytic activity of the prepared electrocatalyst towards ethanol oxidation, cyclic voltammetry (CV) studies were performed using 1.0 M ethanol in basic medium. The CV data revealed the highest peak current density of 11.05 mA cm-2 for the acetic acid-washed Pd/C electrocatalyst. Meanwhile, the fabrication of the second Pd-based electrocatalyst was done by functionalization of the carbon black support using 3:1 (v/v) H2SO4:HNO3. The metal oxide, NiO, was deposited using precipitation method while polyol method was used for the deposition of Pd NPs. X-ray diffraction (XRD) analysis revealed that the estimated particle size of the synthesized catalysts was at around 9.0-15.0 nm. CV results demonstrated a 36.7% increase in the catalytic activity of Pd-NiO/C (functionalized) catalyst towards ethanol oxidation compared to the non-functionalized catalyst.

Introduction to solid supported membrane based electrophysiology.

Science.gov (United States)

Bazzone, Andre; Costa, Wagner Steuer; Braner, Markus; Călinescu, Octavian; Hatahet, Lina; Fendler, Klaus

2013-05-11

The electrophysiological method we present is based on a solid supported membrane (SSM) composed of an octadecanethiol layer chemisorbed on a gold coated sensor chip and a phosphatidylcholine monolayer on top. This assembly is mounted into a cuvette system containing the reference electrode, a chlorinated silver wire. After adsorption of membrane fragments or proteoliposomes containing the membrane protein of interest, a fast solution exchange is used to induce the transport activity of the membrane protein. In the single solution exchange protocol two solutions, one non-activating and one activating solution, are needed. The flow is controlled by pressurized air and a valve and tubing system within a faraday cage. The kinetics of the electrogenic transport activity is obtained via capacitive coupling between the SSM and the proteoliposomes or membrane fragments. The method, therefore, yields only transient currents. The peak current represents the stationary transport activity. The time dependent transporter currents can be reconstructed by circuit analysis. This method is especially suited for prokaryotic transporters or eukaryotic transporters from intracellular membranes, which cannot be investigated by patch clamp or voltage clamp methods.

Ductility improvement of Mg alloys by solid solution: Ab initio modeling, synthesis and mechanical properties

Czech Academy of Sciences Publication Activity Database

Sandlöbes, S.; Pei, Z.; Friák, Martin; Zhu, L.-F.; Wang, F.; Zaefferer, S.; Raabe, D.; Neugebauer, J.

2014-01-01

Roč. 70, MAY (2014), s. 92-104 ISSN 1359-6454 Grant - others:GA MŠk(CZ) LM2010005 Institutional support: RVO:68081723 Keywords : Magnesium * Rare-earth elements * Ductility * Modeling * Ab initio Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 4.465, year: 2014

Honeycomb supports with high thermal conductivity for the Tischer-Tropsch synthesis

Energy Technology Data Exchange (ETDEWEB)

Visconti, C.G.; Rronconi, E.; Groppi, G.; Lietti, L. [Politecnico di Milano (Italy). Dipt. di Energia; Iovane, M.; Rossini, S.; Zennaro, R. [Eni S.p.A., San Donato Milanese (Italy). Div. Exploration and Production

2011-07-01

The potential of multitubular reactors loaded with washcoated structured catalysts having highly conductive honeycomb supports is investigated herein in the low temperature Fischer- Tropsch synthesis by means of a theoretical investigation. Simulation results indicate that extruded aluminum honeycomb monoliths, washcoated with a Co-based catalyst, are promising for the application at the industrial scale, in particular when adopting supports with high cell densities and catalysts with high activity. Limited temperature gradients within the reactor are in fact possible even at extreme process conditions, thus leading to interesting volumetric reactor yields with negligible pressure drop. This result is achieved without the need of cofeeding to the reactor large amounts of liquid hydrocarbons to remove the reaction heat, as opposite to existing industrial Fischer-Tropsch packed-bed reactors. (orig.)

Long-Term Condition Self-Management Support in Online Communities: A Meta-Synthesis of Qualitative Papers

Science.gov (United States)

Vassilev, Ivaylo; Kennedy, Anne; Rogers, Anne

2016-01-01

Background Recent years have seen an exponential increase in people with long-term conditions using the Internet for information and support. Prior research has examined support for long-term condition self-management through the provision of illness, everyday, and emotional work in the context of traditional offline communities. However, less is known about how communities hosted in digital spaces contribute through the creation of social ties and the mobilization of an online illness “workforce.” Objective The aim was to understand the negotiation of long-term condition illness work in patient online communities and how such work may assist the self-management of long-term conditions in daily life. Methods A systematic search of qualitative papers was undertaken using various online databases for articles published since 2004. A total of 21 papers met the inclusion criteria of using qualitative methods and examined the use of peer-led online communities for those with a long-term condition. A qualitative meta-synthesis was undertaken and the review followed a line of argument synthesis. Results The main themes identified in relation to the negotiation of self-management support were (1) redressing offline experiential information and knowledge deficits, (2) the influence of modeling and learning behaviors from others on self-management, (3) engagement that validates illness and negates offline frustrations, (4) tie formation and community building, (5) narrative expression and cathartic release, and (6) dissociative anonymity and invisibility. These translated into a line of argument synthesis in which four network mechanisms for self-management support in patient online communities were identified. These were (1) collective knowledge and identification through lived experience; (2) support, information, and engagement through readily accessible gifting relationships; (3) sociability that extends beyond illness; and (4) online disinhibition as a facilitator

Synthesis, structural and semiconducting properties of Ba(Cu1/3 Sb2/3)O3-PbTiO3 solid solutions

Science.gov (United States)

Singh, Chandra Bhal; Kumar, Dinesh; Prashant, Verma, Narendra Kumar; Singh, Akhilesh Kumar

2018-05-01

We report the synthesis and properties of a new solid solution 0.05Ba(Cu1/3Sb2/3)O3-0.95PbTiO3 (BCS-PT) which shows the semiconducting properties. In this study, we have designed new perovskite-type (ABO3) solid solution of BCS-PT that have tunable optical band gap. BCS-PT compounds were prepared by conventional solid-state reaction method and their structural, micro-structural and optical properties were analyzed. The calcination temperature for BCS-PT solid solutions has been optimized to obtain a phase pure system. The Reitveld analysis of X-ray data show that all samples crystallize in tetragonal crystal structure with space group P4mm. X-ray investigation revealed that increase in calcination temperature led to increase of lattice parameter `a' while `c' parameter value lowered. The band gap of PbTiO3 is reduced from 3.2 eV to 2.8 eV with BCS doping and with increasing calcination temperature it further reduces to 2.56 eV. The reduced band gap indicated that the compounds are semiconducting and can be used for photovoltaic device applications.

Solid state green synthesis and catalytic activity of CuO nanorods in thermal decomposition of potassium periodate

Science.gov (United States)

Patel, Vinay Kumar; Bhattacharya, Shantanu

2017-09-01

The present study reports a facile solid state green synthesis process using the leaf extracts of Hibiscus rosa-sinensis to synthesize CuO nanorods with average diameters of 15-20 nm and lengths up to 100 nm. The as-synthesized CuO nanorods were characterized by x-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy and selected area electron diffraction. The formation mechanism of CuO nanorods has been explained by involving the individual role of amide I (amino groups) and carboxylate groups under excess hydroxyl ions released from NaOH. The catalytic activity of CuO nanorods in thermal decomposition of potassium periodate microparticles (µ-KIO4) microparticles was studied by thermo gravimetric analysis measurement. The original size (~100 µm) of commercially procured potassium periodate was reduced to microscale length scale to about one-tenth by PEG200 assisted emulsion process. The CuO nanorods prepared by solid state green route were found to catalyze the thermal decomposition of µ-KIO4 with a reduction of 18 °C in the final thermal decomposition temperature of potassium periodate.

Synthesis of monoclinic Celsian from Coal Fly Ash by using a one-step solid-state reaction process

Energy Technology Data Exchange (ETDEWEB)

Long-Gonzalez, D.; Lopez-Cuevas, J.; Gutierrez-Chavarria, C.A.; Pena, P.; Baudin, C.; Turrillas, X. [CINVESTAV, Coahuila (Mexico)

2010-03-15

Monoclinic (Celsian) and hexagonal (Hexacelsian) Ba1-xSrxAl{sub 2}Si2O8 solid solutions, where x=0, 0.25, 0.375, 0.5, 0.75 or 1, were synthesized by using Coal Fly Ash (CFA) as main raw material, employing a simple one-step solid-state reaction process involving thermal treatment for 5 h at 850-1300{sup o}C. Fully monoclinic Celsian was obtained at 1200{sup o} C/5 h, for SrO contents of 0.25 {<=} x {<=} 0.75. However, an optimum SrO level of 0.25 {<=} x {<=} 0.375 was recommended for the stabilization of Celsian. These synthesis conditions represent a significant improvement over the higher temperatures, longer times and/or multi-step processes needed to obtain fully monoclinic Celsian, when other raw materials are used for this purpose, according to previous literature. These results were attributed to the role of the chemical and phase constitution of CFA as well as to a likely mineralizing effect of CaO and TiO{sub 2} present in it, which enhanced the Hexacelsian to Celsian conversion.

Synthesis of carbon nanotubes by CVD method using iron and molybdenum-based catalysts supported on ceramic matrices

International Nuclear Information System (INIS)

Teixeira, Ana Paula de Carvalho

2010-01-01

Molybdenum is known for its synergistic effect in the synthesis of carbon nanotubes (CNs) by chemical vapor deposition (CVD method). When added to typical catalysts like iron, nickel, and cobalt, even in small quantities, it is increases the yield of these nanostructures. The presence of Mo also has an influence on the type and number of CN walls formed. Although this effect is widely documented in the literature, there is not yet a consensus about the mechanism of action of molybdenum in catalytic systems. The objective of the present work is to study the influence of molybdenum on the catalytic activity of iron nanoparticle-based catalysts supported on magnesium oxide (Fe/MgO system) in the synthesis of carbon nanotubes by the CVD method. The Mo concentration was systematically varied from null to molar ratio values four times greater than the quantity of Fe, and the obtained material (catalysts and carbon nanotubes) were broadly characterized by different techniques. In order to also study the influence of the preparation method on the final composition of the catalytic system phases, the catalytic systems (Fe/MgO e FeMo x /MgO) were synthesized by two different methods: co-precipitation and impregnation. The greatest CN yields were observed for the catalysts prepared by coprecipitation. The difference was attributed to better dispersion of the Fe and Mo phases in the catalyst ceramic matrix. In the precipitation stage, it was observed the formation of layered double hydroxides whose concentration increased with the Mo content up to the ratio of Mo/Fe equal to 0.2. This phase is related to a better distribution of Fe and Mo in this concentration range. Another important characteristic observed is that the ceramic matrix is not inert. It can react both with Fe and Mo and form the iron solid solution in the magnesium oxide and the phases magnesium-ferrite (MgFe 2 0 4 ) and magnesium molybdate (MgMo0 4 ). The MgFe 2 0 4 phase is observed in all catalytic systems

Flow-Solution-Liquid-Solid Growth of Semiconductor Nanowires: A Novel Approach for Controlled Synthesis

Energy Technology Data Exchange (ETDEWEB)

Hollingsworth, Jennifer A. [Los Alamos National Laboratory; Palaniappan, Kumaranand [Los Alamos National Laboratory; Laocharoensuk, Rawiwan [National Science and Technology Center, Thailand; Smith, Nickolaus A. [Los Alamos National Laboratory; Dickerson, Robert M. [Los Alamos National Laboratory; Casson, Joanna L. [Los Alamos National Laboratory; Baldwin, Jon K. [Los Alamos National Laboratory

2012-06-07

Semiconductor nanowires (SC-NWs) have potential applications in diverse technologies from nanoelectronics and photonics to energy harvesting and storage due to their quantum-confined opto-electronic properties coupled with their highly anisotropic shape. Here, we explore new approaches to an important solution-based growth method known as solution-liquid-solid (SLS) growth. In SLS, molecular precursors are reacted in the presence of low-melting metal nanoparticles that serve as molten fluxes to catalyze the growth of the SC-NWs. The mechanism of growth is assumed to be similar to that of vapor-liquid-solid (VLS) growth, with the clear distinctions of being conducted in solution in the presence of coordinating ligands and at relatively lower temperatures (<300 C). The resultant SC-NWs are soluble in common organic solvents and solution processable, offering advantages such as simplified processing, scale-up, ultra-small diameters for quantum-confinement effects, and flexible choice of materials from group III-V to groups II-VI, IV-VI, as well as truly ternary I-III-VI semiconductors as we recently demonstrates. Despite these advantages of SLS growth, VLS offers several clear opportunities not allowed by conventional SLS. Namely, VLS allows sequential addition of precursors for facile synthesis of complex axial heterostructures. In addition, growth proceeds relatively slowly compared to SLS, allowing clear assessments of growth kinetics. In order to retain the materials and processing flexibility afforded by SLS, but add the elements of controlled growth afforded by VLS, we transformed SLS into a flow based method by adapting it to synthesis in a microfluidic system. By this new method - so-called 'flow-SLS' (FSLS) - we have now demonstrated unprecedented fabrication of multi-segmented SC-NWs, e.g., 8-segmented CdSe/ZnSe defined by either compositionally abrupt or alloyed interfaces as a function of growth conditions. In addition, we have studied growth

Microwave-assisted solid-phase peptide synthesis of the 60-110 domain of human pleiotrophin on 2-chlorotrityl resin.

Science.gov (United States)

Friligou, Irene; Papadimitriou, Evangelia; Gatos, Dimitrios; Matsoukas, John; Tselios, Theodore

2011-05-01

A fast and efficient microwave-assisted solid phase peptide synthesis (MW-SPPS) of a 51mer peptide, the main heparin-binding site (60-110) of human pleiotrophin (hPTN), using 2-chlorotrityl chloride resin (CLTR-Cl) following the 9-fluorenylmethyloxycarbonyl/tert-butyl (Fmoc/tBu) methodology and with the standard N,N'-diisopropylcarbodiimide/1-hydroxybenzotriazole (DIC/HOBt) coupling reagents, is described. An MW-SPPS protocol was for the first time successfully applied to the acid labile CLTR-Cl for the faster synthesis of long peptides (51mer peptide) and with an enhanced purity in comparison to conventional SPPS protocols. The synthesis of such long peptides is not trivial and it is generally achieved by recombinant techniques. The desired linear peptide was obtained in only 30 h of total processing time and in 51% crude yield, in which 60% was the purified product obtained with 99.4% purity. The synthesized peptide was purified by reversed phase high performance liquid chromatography (RP-HPLC) and identified by electrospray ionization mass spectrometry (ESI-MS). Then, the regioselective formation of the two disulfide bridges of hPTN 60-110 was successfully achieved by a two-step procedure, involving an oxidative folding step in dimethylsulfoxide (DMSO) to form the Cys(77)-Cys(109) bond, followed by iodine oxidation to form the Cys(67)-Cys(99) bond.

Solid-Phase Synthesis of a New Diphosphate 5-Aminoimidazole-4-carboxamide Riboside (AICAR Derivative and Studies toward Cyclic AICAR Diphosphate Ribose

Directory of Open Access Journals (Sweden)

Gennaro Piccialli

2011-09-01

Full Text Available The solid-phase synthesis of the first example of a new diphosphate AICAR derivative is reported. The new substance is characterized by the presence of a 5'-phosphate group while a second phosphate moiety is installed on a 5-hydroxypentyl chain attached to the 4-N-position of AICAR. Cyclization of the diphosphate derivative by pyrophosphate bond formation allowed for the formation of a novel AICAR-based cyclic ADP-ribose (cADPR mimic.

Complex plasmochemical processing of solid fuel

Directory of Open Access Journals (Sweden)

Vladimir Messerle

2012-12-01

Full Text Available Technology of complex plasmaochemical processing of solid fuel by Ecibastuz bituminous and Turgay brown coals is presented. Thermodynamic and experimental study of the technology was fulfilled. Use of this technology allows producing of synthesis gas from organic mass of coal and valuable components (technical silicon, ferrosilicon, aluminum and silicon carbide and microelements of rare metals: uranium, molybdenum, vanadium etc. from mineral mass of coal. Produced a high-calorific synthesis gas can be used for methanol synthesis, as high-grade reducing gas instead of coke, as well as energy gas in thermal power plants.

Nanostructured carbon-supported Pd electrocatalysts for ethanol oxidation: synthesis and characterization

International Nuclear Information System (INIS)

Gacutan, E M; Tongol, B J; Climaco, M I; Telan, G J; Malijan, F; Hsu, H Y; Garcia, J; Fulo, H

2012-01-01

The need to lower the construction cost of fuel cells calls for the development of non-Pt based electrocatalysts. Among others, Pd has emerged as a promising alternative to Pt for fuel cell catalysis. This research aims to investigate the synthesis and characterization of nanostructured Pd-based catalysts dispersed on carbon support as anode materials in direct ethanol fuel cells. For the preparation of the first Pd-based electrocatalyst, palladium nanoparticles (NPs) were synthesized via oleylamine (OAm)-mediated synthesis and precursor method with a mean particle size of 3.63 ± 0.59 nm as revealed by transmission electron microscopy (TEM). Carbon black was used as a supporting matrix for the OAm-capped Pd NPs. Thermal annealing and acetic acid washing were used to remove the OAm capping agent. To evaluate the electrocatalytic activity of the prepared electrocatalyst towards ethanol oxidation, cyclic voltammetry (CV) studies were performed using 1.0 M ethanol in basic medium. The CV data revealed the highest peak current density of 11.05 mA cm −2 for the acetic acid-washed Pd/C electrocatalyst. Meanwhile, the fabrication of the second Pd-based electrocatalyst was done by functionalization of the carbon black support using 3:1 (v/v) H 2 SO 4 :HNO 3 . The metal oxide, NiO, was deposited using precipitation method while polyol method was used for the deposition of Pd NPs. X-ray diffraction (XRD) analysis revealed that the estimated particle size of the synthesized catalysts was at around 9.0–15.0 nm. CV results demonstrated a 36.7% increase in the catalytic activity of Pd–NiO/C (functionalized) catalyst towards ethanol oxidation compared to the non-functionalized catalyst. (paper)

Magnetron sputtered gadolinia-doped ceria diffusion barriers for metal-supported solid oxide fuel cells

DEFF Research Database (Denmark)

Sønderby, Steffen; Klemensø, Trine; Christensen, Bjarke H.

2014-01-01

Gadolinia-doped ceria (GDC) thin films are deposited by reactive magnetron sputtering in an industrial-scale setup and implemented as barrier layers between the cathode and electrolyte in metal-based solid oxide fuel cells consisting of a metal support, an electrolyte of ZrO2 co-doped with Sc2O3...

Magnetic nanoparticle supported phosphotungstic acid: An efficient catalyst for the synthesis of xanthene derivatives

Science.gov (United States)

Patel, Nipun; Katheriya, Deepak; Dadhania, Harsh; Dadhania, Abhishek

2018-05-01

Magnetic nanoparticle supported phosphotungstic acid (Fe3O4@SiO2-HPW) was applied as a highly efficient catalyst for the synthesis of 14H-dibenzoxanthene derivatives via condensation reaction of 2-naphthol and aryl aldehydes. The catalyst was found highly efficient for the synthesis of xanthene derivatives under solvent free condition. The catalyst showed high activity and stability during the reaction and provided excellent yield of the corresponding products in short reaction time. All the synthesized compounds were characterized through FT-IR, 1H-NMR and 13C-NMR spectroscopic techniques. Furthermore, the catalyst is magnetically recoverable and can be reused several times without significant loss of its catalytic activity.

Synthesis of a nano-crystalline solid acid catalyst from fly ash and its catalytic performance

Energy Technology Data Exchange (ETDEWEB)

Chitralekha Khatri; Ashu Rani [Government P.G. College, Kota (India). Environmental Chemistry Laboratory

2008-10-15

The synthesis of nano-crystalline activated fly ash catalyst (AFAC) with crystallite size of 12 nm was carried out by chemical and thermal treatment of fly ash, a waste material generated from coal-burning power plants. Fly ash was chemically activated using sulfuric acid followed by thermal activation at 600{sup o}C. The variation of surface and physico-chemical properties of the fly ash by activation methods resulted in improved acidity and therefore, catalytic activity for acid catalyzed reactions. The AFAC was characterized by X-ray diffraction, FT-IR spectroscopy, N{sub 2}-adsorption-desorption isotherm, scanning electron microscopy, flame atomic absorption spectrophotometry and sulfur content by CHNS/O elemental analysis. It showed amorphous nature due to high silica content (81%) and possessed high BET surface area (120 m{sup 2}/g). The catalyst was found to be highly active solid acid catalyst for liquid phase esterification of salicylic acid with acetic anhydride and methanol giving acetylsalicylic acid and methyl salicylate respectively. A maximum yield of 97% with high purity of acetylsalicylic acid (aspirin) and a very high conversion 87% of salicylic acid to methyl salicylate (oil of wintergreen) was obtained with AFAC. The surface acidity and therefore, catalytic activity in AFAC was originated by increased silica content, hydroxyl content and higher surface area as compared to fly ash. The study shows that coal generated fly ash can be converted into potential solid acid catalyst for acid catalyzed reactions. Furthermore, this catalyst may replace conventional environmentally hazardous homogeneous liquid acids making an ecofriendly; solvent free, atom efficient, solid acid based catalytic process. 27 refs., 5 figs., 2 tabs.

Solid State Division: Progress report for period ending September 30, 1987

Energy Technology Data Exchange (ETDEWEB)

Green, P.H.; Watson, D.M. (eds.)

1988-03-01

This paper contains a collection of articles on research done at the Solid State Division of ORNL. General topics covered are: theoretical solid state physics; neutron scattering; physical properties of superconductors and ceramics; synthesis and characterization of solids; ion beam and laser processing; and surface and defect studies. (LSP)

Solid State Division: Progress report for period ending September 30, 1987

International Nuclear Information System (INIS)

Green, P.H.; Watson, D.M.

1988-03-01

This paper contains a collection of articles on research done at the Solid State Division of ORNL. General topics covered are: theoretical solid state physics; neutron scattering; physical properties of superconductors and ceramics; synthesis and characterization of solids; ion beam and laser processing; and surface and defect studies

Directing chondrogenic differentiation of mesenchymal stem cells with a solid-supported chitosan thermogel for cartilage tissue engineering

International Nuclear Information System (INIS)

Huang, Hongjie; Zhang, Xin; Hu, Xiaoqing; Dai, Linghui; Zhu, Jingxian; Man, Zhentao; Ao, Yingfang; Chen, Haifeng; Zhou, Chunyan

2014-01-01

Hydrogels are attractive for cartilage tissue engineering because of their high plasticity and similarity with the native cartilage matrix. However, one critical drawback of hydrogels for osteochondral repair is their inadequate mechanical strength. To address this limitation, we constructed a solid-supported thermogel comprising a chitosan hydrogel system and demineralized bone matrix. Scanning electron microscopy, the equilibrium scanning ratio, the biodegradation rate, biomechanical tests, biochemical assays, metabolic activity tests, immunostaining and cartilage-specific gene expression analysis were used to evaluate the solid-supported thermogel. Compared with pure hydrogel or demineralized matrix, the hybrid biomaterial showed superior porosity, equilibrium swelling and degradation rate. The hybrid scaffolds exhibited an increased mechanical strength: 75% and 30% higher compared with pure hydrogels and demineralized matrix, respectively. After three days culture, bone-derived mesenchymal stem cells (BMSCs) maintained viability above 90% in all three materials; however, the cell retention of the hybrid scaffolds was more efficient and uniform than the other materials. Matrix production and chondrogenic differentiation of BMSCs in the hybrid scaffolds were superior to its precursors, based on glycosaminoglycan quantification and hyaline cartilage marker expression after three weeks in culture. Its easy preparation, favourable biophysical properties and chondrogenic capacity indicated that this solid-supported thermogel could be an attractive biomaterial framework for cartilage tissue engineering. (paper)

Synthesis and characterization of nanocrystalline nuclear ceramics

International Nuclear Information System (INIS)

Ananthasivan, K.; Anthonysamy, S.; Chandramouli, V.; Vasudeva Rao, P.R.

2006-01-01

This paper highlights the utility of the gel-combustion synthesis in making solid solutions containing the oxides of U, Th, and Ce. The synthesis of a series of solid solutions of ceria with thoria and urania using the gel-combustion technique with citric acid as the fuel is presented as a typical case. The x-ray crystallite size, specific surface area, and residual carbon of the precursors and final products are discussed. The sinterability of these powders is analysed using their sintered densities. Solid solutions of thoria-ceria with a density higher than 85% TD (theoretical density) and those of urania ceria with a density as high as 96% TD were obtained. The microstructure of the thoria-ceria powders were analysed using high resolution electron microscopy. (author)

Microwave promoted simple, efficient and regioselective synthesis of trisubstituted imidazo[1,2-a]benzimidazoles on soluble support.

Science.gov (United States)

Chen, Li-Hsun; Hsiao, Ya-Shan; Yellol, Gorakh S; Sun, Chung-Ming

2011-03-14

An efficient microwave-assisted and soluble polymer-supported synthesis of medicinally important imidazole-fused benzimidazoles has been developed. The protocol involves the rapid condensation of polymer-bound amino benzimidazoles with various α-bromoketones and subsequent in situ intramolecular cyclization under microwave irradiation resulting in a one pot synthesis of imidazole interlacing benzimidazole polymer conjugates. The condensed product was obtained with excellent regioselectivity. The biologically interesting imidazo[1,2-a]benzimidazoles was released from polymer support at ambient temperature. Diversity in the triheterocyclic nucleus was achieved by the different substitutions at its 2, 3, and 9 positions. The new protocol has the advantages of short reaction time, easy workup process, excellent yields, reduced environmental impact, wide substrate scope and convenient procedure.

A simple method for the small scale synthesis and solid-phase extraction purification of steroid sulfates.

Science.gov (United States)

Waller, Christopher C; McLeod, Malcolm D

2014-12-01

Steroid sulfates are a major class of steroid metabolite that are of growing importance in fields such as anti-doping analysis, the detection of residues in agricultural produce or medicine. Despite this, many steroid sulfate reference materials may have limited or no availability hampering the development of analytical methods. We report simple protocols for the rapid synthesis and purification of steroid sulfates that are suitable for adoption by analytical laboratories. Central to this approach is the use of solid-phase extraction (SPE) for purification, a technique routinely used for sample preparation in analytical laboratories around the world. The sulfate conjugates of sixteen steroid compounds encompassing a wide range of steroid substitution patterns and configurations are prepared, including the previously unreported sulfate conjugates of the designer steroids furazadrol (17β-hydroxyandrostan[2,3-d]isoxazole), isofurazadrol (17β-hydroxyandrostan[3,2-c]isoxazole) and trenazone (17β-hydroxyestra-4,9-dien-3-one). Structural characterization data, together with NMR and mass spectra are reported for all steroid sulfates, often for the first time. The scope of this approach for small scale synthesis is highlighted by the sulfation of 1μg of testosterone (17β-hydroxyandrost-4-en-3-one) as monitored by liquid chromatography-mass spectrometry (LCMS). Copyright © 2014 Elsevier Inc. All rights reserved.

Technologies and decision support systems to aid solid-waste management: a systematic review.

Science.gov (United States)

Vitorino de Souza Melaré, Angelina; Montenegro González, Sahudy; Faceli, Katti; Casadei, Vitor

2017-01-01

Population growth associated with population migration to urban areas and industrial development have led to a consumption relation that results in environmental, social, and economic problems. With respect to the environment, a critical concern is the lack of control and the inadequate management of the solid waste generated in urban centers. Among the challenges are proper waste-collection management, treatment, and disposal, with an emphasis on sustainable management. This paper presents a systematic review on scientific publications concerning decision support systems applied to Solid Waste Management (SWM) using ICTs and OR in the period of 2010-2013. A statistical analysis of the eighty-seven most relevant publications is presented, encompassing the ICTs and OR methods adopted in SWM, the processes of solid-waste management where they were adopted, and which countries are investigating solutions for the management of solid waste. A detailed discussion on how the ICTs and OR methods have been combined in the solutions was also presented. The analysis and discussion provided aims to help researchers and managers to gather insights on technologies/methods suitable the SWM challenges they have at hand, and on gaps that can be explored regarding technologies/methods that could be useful as well as the processes in SWM that currently do not benefit from using ICTs and OR methods. Copyright © 2016 Elsevier Ltd. All rights reserved.

Solid state synthesis of water-dispersible silicon nanoparticles from silica nanoparticles

International Nuclear Information System (INIS)

Kravitz, Keren; Kamyshny, Alexander; Gedanken, Aharon; Magdassi, Shlomo

2010-01-01

A solid state synthesis for obtaining nanocrystalline silicon was performed by high temperature reduction of commercial amorphous nanosilica with magnesium powder. The obtained silicon powder contains crystalline silicon phase with lattice spacings characteristic of diamond cubic structure (according to high resolution TEM), and an amorphous phase. In 29 Si CP MAS NMR a broad multicomponent peak corresponding to silicon is located at -61.28 to -69.45 ppm, i.e. between the peaks characteristic of amorphous and crystalline Si. The powder has displayed red luminescence while excited under UV illumination, due to quantum confinement within the nanocrystals. The silicon nanopowder was successfully dispersed in water containing poly(vinyl alcohol) as a stabilizing agent. The obtained dispersion was also characterized by red photoluminescence with a band maximum at 710 nm, thus enabling future functional coating applications. - Graphical abstract: High temperature reduction of amorphous nanosilica with magnesium powder results in the formation of powder containing crystalline silicon phase The powder displays red luminescence while excited under UV illumination, due to quantum confinement within the Si nanocrystals, and can be successfully dispersed in water containing poly(vinyl alcohol) as a stabilizing agent. The obtained dispersion was also characterized by red photoluminescence, thus enabling future functional coating applications.

Preparation, characterization and first application of aerosil silica supported acidic ionic liquid as a reusable heterogeneous catalyst for the synthesis of 2,3-dihydroquinazoline-4(1H)-ones

Energy Technology Data Exchange (ETDEWEB)

Yassaghi, Ghazaleh; Davodnia, Abolghasem; Allameh, Sadegh; Zarebidaki, Atefeh; Tavakolihoseini, Niloofar [Islamic Azad Univ., Mashhad (Iran, Islamic Republic of)

2012-04-15

A new heterogeneous acidic catalyst was successfully prepared by impregnation of silica (Aerosil 300) by an acidic ionic liquid, named 1-(4-sulfonic acid)butyl pyridinium hydrogen sulfate [PYC{sub 4}SO{sub 3}H][HSO{sub 4}], and characterized using FT-IR spectroscopy, the N{sub 2} adsorption/desorption analysis (BET), thermal analysis (TG/DTG), and X-ray diffraction (XRD) techniques. The amount of loaded acidic ionic liquid on Aerosil 300 support was determined by acid-base titration. This new solid acidic supported heterogeneous catalyst exhibits excellent activity in the synthesis of 2-aryl-2,3-dihydroquinazoline-4(1H)-ones by cyclo condensation reaction of 2-aminobenzamide with aromatic aldehydes under solvent-free conditions and the desired products were obtained in very short reaction times with high yields. This catalyst has the advantages of an easy catalyst separation from the reaction medium and lower problems of corrosion. Recycling of the catalyst and avoidance of using harmful organic solvent are other advantages of this simple procedure.

Soluble Polymer-supported Synthesis of Indoles via Palladium-mediat -ed Heteroannulation of Terminal Alkynes with o-Iodoanilines

Institute of Scientific and Technical Information of China (English)

无

2002-01-01

A soluble polymer-supported synthesis of indoles via palladium-mediated hetero- annulation of terminal alkynes with o-iodoanilines has been described. The protocol provides a useful tool for constructing combinatorial indole libraries.

Low-temperature solid-state synthesis and optical properties of ZnO/CdS nanocomposites

International Nuclear Information System (INIS)

Liu, Jinsong; Zhu, Kongjun; Sheng, Beibei; Li, Ziquan; Tai, Guoan; Qiu, Jinhao; Wang, Jing; Chen, Jiankang; You, Yuncheng; Gu, Qilin; Liu, Pengcheng

2015-01-01

Highlights: • Using a low-temperature solid-state method, ZnO/CdS nanocomposites were obtained • Grain growth kinetics of cubic CdS and hexagonal ZnO phase was described. • Sufficient grinding and heating treatment was a key for formation of composites. • Optical properties could be easily manipulated by reaction temperature and time. - Abstract: A simple low-temperature solid-state reaction in the presence of the surfactant PEG400 was developed to obtain ZnO/CdS nanocomposites. The effects of synthesis temperature and reaction time on crystal structure and optical properties of the nanocomposites were investigated by several technologies. X-ray diffraction (XRD) and high resolution transmission electron microscope (HRTEM) characterizations showed that the products consisted of the nanoparticles, and the grain growth kinetics of the cubic CdS and the hexagonal ZnO phase in the nanocomposites was described. The mechanism analysis suggested that sufficient grinding and heating treatment was a key to form the ZnO/CdS nanocomposites, and the surfactant PEG400 was proved not to involve the reaction and prevent the nanoparticles from aggregating to larger in whole grinding and heat-treatment process. Ultraviolet–visible (UV–vis) spectra revealed that the band gaps of the nanocomposites could be tuned by the reaction temperature and reaction time. Photoluminescence (PL) spectra showed that the changing position and the intensity of the emission peaks resulted from the rate of electron transfer and recombination probability under the different conditions

New two-step synthesis of N-(2-ethylhexyl)-2,7-diiodocarbazole as a monomer for conjugated polymers

Czech Academy of Sciences Publication Activity Database

Výprachtický, Drahomír; Kmínek, Ivan; Pokorná, Veronika; Kaňková, Dana; Cimrová, Věra

2013-01-01

Roč. 16, č. 1 (2013), s. 31-37 ISSN 1385-772X R&D Projects: GA MŠk(CZ) 1M06031; GA ČR GAP106/12/0827 Institutional research plan: CEZ:AV0Z40500505 Institutional support: RVO:61389013 Keywords : monomer synthesis * carbazole * ring closure Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.210, year: 2013

Lipases Immobilization for Effective Synthesis of Biodiesel Starting from Coffee Waste Oils

Directory of Open Access Journals (Sweden)

Lucia Gardossi

2013-08-01

Full Text Available Immobilized lipases were applied to the enzymatic conversion of oils from spent coffee ground into biodiesel. Two lipases were selected for the study because of their conformational behavior analysed by Molecular Dynamics (MD simulations taking into account that immobilization conditions affect conformational behavior of the lipases and ultimately, their efficiency upon immobilization. The enzymatic synthesis of biodiesel was initially carried out on a model substrate (triolein in order to select the most promising immobilized biocatalysts. The results indicate that oils can be converted quantitatively within hours. The role of the nature of the immobilization support emerged as a key factor affecting reaction rate, most probably because of partition and mass transfer barriers occurring with hydrophilic solid supports. Finally, oil from spent coffee ground was transformed into biodiesel with yields ranging from 55% to 72%. The synthesis is of particular interest in the perspective of developing sustainable processes for the production of bio-fuels from food wastes and renewable materials. The enzymatic synthesis of biodiesel is carried out under mild conditions, with stoichiometric amounts of substrates (oil and methanol and the removal of free fatty acids is not required.

Synthesis and characterization of inverse spinels, intercalation materials for Li-ion batteries

NARCIS (Netherlands)

Van Landschoot, N.

2006-01-01

Chapter 2 describes the solid-state synthesis of LiNiVO4 and LiCoVO4. The materials are prepared at 800C and are phase pure, as shown by X-ray diffraction and have the inverse spinel structure. Due to the solid-state synthesis the particle size is quite large and the particle size distribution is

Synthesis of Carbon Nano tubes Using Anadara Granosa Shells as Catalyst Support

International Nuclear Information System (INIS)

Mohd Zobir Hussein; Mohd Zobir Hussein; Salwani Asyikin Zakarya; Siti Halimah Sarijo

2011-01-01

The synthesis of carbon nano tubes (CNTs) by chemical vapor deposition (CVD) method using natural calcite prepared from Anadara granosa shells (CS), as metal catalyst support was studied. Hexane and iron were used as carbon precursor and catalyst, respectively. The as synthesised CNTs was characterized using XRD, TEM and FESEM. From the XRD patterns the CNTs peak can be seen more incisive after purification process and from the FESEM micrographs the CNTs can be seen as a bunch of rope-like structures. (author)

Accelerated creep in solid oxide fuel cell anode supports during reduction

DEFF Research Database (Denmark)

Frandsen, Henrik Lund; Makowska, Malgorzata Grazyna; Greco, Fabio

2016-01-01

To evaluate the reliability of solid oxide fuel cell (SOFC) stacks during operation, the stress field in the stack must be known. During operation the stress field will depend on time as creep processes relax stresses. The creep of reduced Ni-YSZ anode support at operating conditions has been...... studied previously. In this work a newly discovered creep phenomenon taking place during the reduction is reported. This relaxes stresses at a much higher rate (∼ x104) than creep during operation. The phenomenon was studied both in three-point bending and uniaxial tension. Differences between the two...... the NiO and the YSZ phases occurs during reduction. The accelerated creep should practically eliminate any residual stress in the anode support in an SOFC stack, as has previously been indirectly observed. This phenomenon has to be taken into account both in the production of stacks and in the simulation...

Solid-State Synthesis and Effect of Temp erature on Optical Prop erties of CuO Nanoparticles

Institute of Scientific and Technical Information of China (English)

C. C. Vidyasagar; Y. Arthoba Naik∗; T. G. Venkatesha; R. Viswanatha

2012-01-01

Modulation of band energies through size control offers new ways to control photoresponse and photoconversion efficiency of the solar cell. The P-type semiconductor of copper oxide is an important functional material used for photovoltaic cells. CuO is attractive as a selective solar absorber since it has high solar absorbance and a low thermal emittance. The present work describes the synthesis and characterization of semiconducting CuO nanoparticles via one-step, solid-state reaction in the presence of Polyethylene glycol 400 as size controlling agent for the preparation of CuO nanoparticles at different temperatures. Solid-state mechanochemical processing, which is not only a physical size reduction process in conventional milling but also a chemical reaction, is mechanically activated at the nanoscale during grinding. The present method is a simple and efficient method of preparing nanoparticles with high yield at low cost. The structural and chemical composition of the nanoparticles were analyzed by X-ray diffraction, field emission scanning electron microscopy and energy-dispersive spectrometer, respectively. Optical properties and band gap of CuO nanoparticles were studied by UV-Vis spectroscopy. These results showed that the band gap energy decreased with increase of annealing temperature, which can be attributed to the improvement in grain size of the samples.

Novel Fluorinated Indanone, Tetralone and Naphthone Derivatives: Synthesis and Unique Structural Features

Directory of Open Access Journals (Sweden)

Joseph C. Sloop

2012-02-01

Full Text Available Several fluorinated and trifluoromethylated indanone, tetralone and naphthone derivatives have been prepared via Claisen condensations and selective fluorinations in yields ranging from 22–60%. In addition, we report the synthesis of new, selectively fluorinated bindones in yields ranging from 72–92%. Of particular interest is the fluorination and trifluoroacetylation regiochemistry observed in these fluorinated products. We also note unusual transformations including a novel one pot, dual trifluoroacetylation, trifluoroacetylnaphthone synthesis via a deacetylation as well as an acetyl-trifluoroacetyl group exchange. Solid-state structural features exhibited by these compounds were investigated using crystallographic methods. Crystallographic results, supported by spectroscopic data, show that trifluoroacetylated ketones prefer a chelated cis-enol form whereas fluorinated bindone products exist primarily as the cross-conjugated triketo form.

Synthesis and regulation of α-LiZnPO4.H2O via a solid-state reaction at low-heating temperatures

International Nuclear Information System (INIS)

Liao Sen; Chen Zhipeng; Tian Xiaozhen; Wu Wenwei

2009-01-01

A simple and novel route for the synthesis of a lithium zinc phosphate hydrate, α-LiZnPO 4 .H 2 O, was studied, and the target product was obtained with LiH 2 PO 4 .H 2 O and ZnCO 3 as raw materials and polyethylene glycol-400 (PEG-400) as a surfactant via a one step solid-state reaction at room temperature (25 deg. C). The product was characterized with X-ray powder diffraction (XRD), thermogravimetric analysis and the 1st derivativative of thermogravimetric analysis (TG/DTG) and Fourier transform infrared spectroscopy (FTIR). The comparison experimental results suggested that aging temperature controlled the products of the synthesis, that is, the α-LiZnPO 4 .H 2 O was formed when the reaction mixture was aged at room temperature, and the α-LiZnPO 4 was obtained when the reaction mixture was aged at 80 deg. C.

Valine but not leucine or isoleucine supports neurotransmitter glutamate synthesis during synaptic activity in cultured cerebellar neurons

DEFF Research Database (Denmark)

Bak, Lasse Kristoffer; Johansen, Maja L.; Schousboe, Arne

2012-01-01

Synthesis of neuronal glutamate from a-ketoglutarate for neurotransmission necessitates an amino group nitrogen donor; however, it is not clear which amino acid(s) serves this role. Thus, the ability of the three branched-chain amino acids (BCAAs), leucine, isoleucine, and valine, to act as amino...... group nitrogen donors for synthesis of vesicular neurotransmitter glutamate was investigated in cultured mouse cerebellar (primarily glutamatergic) neurons. The cultures were superfused in the presence of (15) N-labeled BCAAs, and synaptic activity was induced by pulses of N-methyl-D-aspartate (300 µ......]valine was able to maintain the amount of vesicular glutamate during synaptic activity. This indicates that, among the BCAAs, only valine supports the increased need for synthesis of vesicular glutamate. © 2012 Wiley Periodicals, Inc....

Cermet materials prepared by combustion synthesis and metal infiltration

Science.gov (United States)

Holt, Joseph B.; Dunmead, Stephen D.; Halverson, Danny C.; Landingham, Richard L.

1991-01-01

Ceramic-metal composites (cermets) are made by a combination of self-propagating high temperature combustion synthesis and molten metal infiltration. Solid-gas, solid-solid and solid-liquid reactions of a powder compact produce a porous ceramic body which is infiltrated by molten metal to produce a composite body of higher density. AlN-Al and many other materials can be produced.

Regenerable mixed copper-iron-inert support oxygen carriers for solid fuel chemical looping combustion process

Energy Technology Data Exchange (ETDEWEB)

Siriwardane, Ranjani V.; Tian, Hanjing

2016-12-20

The disclosure provides an oxygen carrier for a chemical looping cycle, such as the chemical looping combustion of solid carbonaceous fuels, such as coal, coke, coal and biomass char, and the like. The oxygen carrier is comprised of at least 24 weight % (wt %) CuO, at least 10 wt % Fe2O3, and an inert support, and is typically a calcine. The oxygen carrier exhibits a CuO crystalline structure and an absence of iron oxide crystalline structures under XRD crystallography, and provides an improved and sustained combustion reactivity in the temperature range of 600.degree. C.-1000.degree. C. particularly for solid fuels such as carbon and coal.

Supported Catalysts Useful in Ring-Closing Metathesis, Cross Metathesis, and Ring-Opening Metathesis Polymerization

Directory of Open Access Journals (Sweden)

Jakkrit Suriboot

2016-04-01

Full Text Available Ruthenium and molybdenum catalysts are widely used in synthesis of both small molecules and macromolecules. While major developments have led to new increasingly active catalysts that have high functional group compatibility and stereoselectivity, catalyst/product separation, catalyst recycling, and/or catalyst residue/product separation remain an issue in some applications of these catalysts. This review highlights some of the history of efforts to address these problems, first discussing the problem in the context of reactions like ring-closing metathesis and cross metathesis catalysis used in the synthesis of low molecular weight compounds. It then discusses in more detail progress in dealing with these issues in ring opening metathesis polymerization chemistry. Such approaches depend on a biphasic solid/liquid or liquid separation and can use either always biphasic or sometimes biphasic systems and approaches to this problem using insoluble inorganic supports, insoluble crosslinked polymeric organic supports, soluble polymeric supports, ionic liquids and fluorous phases are discussed.

Optimization of synthesis technique and luminescent properties in Eu{sup 3+}-activated NaCaPO{sub 4} phosphor for solid state lighting applications

Energy Technology Data Exchange (ETDEWEB)

Ratnam, B.V. [Department of Physics, Changwon National University, Changwon 51140 (Korea, Republic of); Sahu, Mukesh K.; Vishwakarma, Amit K.; Jha, Kaushal [Luminescent Materials Research Lab (LMRL), Department of Applied Physics, Delhi Technological University, Delhi 110042 (India); Woo, Hyun-Joo [Department of Physics, Changwon National University, Changwon 51140 (Korea, Republic of); Jang, Kiwan, E-mail: kwjang@changwon.ac.kr [Department of Physics, Changwon National University, Changwon 51140 (Korea, Republic of); Jayasimhadri, M., E-mail: jayaphysics@yahoo.com [Luminescent Materials Research Lab (LMRL), Department of Applied Physics, Delhi Technological University, Delhi 110042 (India)

2017-05-15

Europium activated NaCaPO{sub 4} phosphor has been synthesized by various synthesis techniques such as solid-state reaction (SSR), molten salt synthesis (MSS) and sol-gel combustion (SGC) method to optimize the synthesis procedure. The comparative investigations of structural and luminescent properties have been studied to know the best synthesis method. The XRD patterns and Rietveld refinement analysis of the synthesized phosphors confirmed the single phase orthorhombic structure of NaCaPO{sub 4}. Excitation spectra indicate the strong absorption in near ultraviolet (n-UV) region and the emission spectra exhibit strong emission band at 595 nm corresponds to {sup 5}D{sub 0}→{sup 7}F{sub 1} transition under n-UV (λ{sub ex}=392 nm) excitation. The SGC route synthesized phosphor exhibit intense emission than that of the SSR and MSS method. Therefore, the effect of dopant (Eu{sup 3+}) concentration on the emission intensity and concentration quenching mechanism has been discussed in detail for the Eu{sup 3+} doped NaCaPO{sub 4} phosphor synthesized by SGC method. The CIE chromaticity coordinates have been calculated for the phosphors synthesized by SSR, MSS and SGC methods to reveal the emitting color and also to know the utility of this phosphor for white LEDs.

Synthesis of refractory organic matter in the ionized gas phase of the solar nebula.

Science.gov (United States)

Kuga, Maïa; Marty, Bernard; Marrocchi, Yves; Tissandier, Laurent

2015-06-09

In the nascent solar system, primitive organic matter was a major contributor of volatile elements to planetary bodies, and could have played a key role in the development of the biosphere. However, the origin of primitive organics is poorly understood. Most scenarios advocate cold synthesis in the interstellar medium or in the outer solar system. Here, we report the synthesis of solid organics under ionizing conditions in a plasma setup from gas mixtures (H2(O)-CO-N2-noble gases) reminiscent of the protosolar nebula composition. Ionization of the gas phase was achieved at temperatures up to 1,000 K. Synthesized solid compounds share chemical and structural features with chondritic organics, and noble gases trapped during the experiments reproduce the elemental and isotopic fractionations observed in primitive organics. These results strongly suggest that both the formation of chondritic refractory organics and the trapping of noble gases took place simultaneously in the ionized areas of the protoplanetary disk, via photon- and/or electron-driven reactions and processing. Thus, synthesis of primitive organics might not have required a cold environment and could have occurred anywhere the disk is ionized, including in its warm regions. This scenario also supports N2 photodissociation as the cause of the large nitrogen isotopic range in the solar system.

One-pot synthesis of amides by aerobic oxidative coupling of alcohols or aldehydes with amines using supported gold and base as catalysts

DEFF Research Database (Denmark)

Kegnæs, Søren; Mielby, Jerrik Jørgen; Mentzel, Uffe Vie

2012-01-01

Synthesis of amides by aerobic oxidative coupling of alcohols or aldehydes with amines via intermediate formation of methyl esters is highly efficient and selective when using a catalytic system comprised of supported gold nanoparticles and added base in methanol.......Synthesis of amides by aerobic oxidative coupling of alcohols or aldehydes with amines via intermediate formation of methyl esters is highly efficient and selective when using a catalytic system comprised of supported gold nanoparticles and added base in methanol....

Ion conduction in crystalline superionic solids and its applications

Science.gov (United States)

Chandra, Angesh

2014-06-01

Superionic solids an area of multidisciplinary research activity, incorporates to study the physical, chemical and technological aspects of rapid ion movements within the bulk of the special class of ionic materials. It is an emerging area of materials science, as these solids show tremendous technological scopes to develop wide variety of solid state electrochemical devices such as batteries, fuel cells, supercapacitors, sensors, electrochromic displays (ECDs), memories, etc. These devices have wide range of applicabilities viz. power sources for IC microchips to transport vehicles, novel sensors for controlling atmospheric pollution, new kind of memories for computers, smart windows/display panels, etc. The field grew with a rapid pace since then, especially with regards to designing new materials as well as to explore their device potentialities. Amongst the known superionic solids, fast Ag+ ion conducting crystalline solid electrolytes are attracted special attention due to their relatively higher room temperature conductivity as well as ease of materials handling/synthesis. Ion conduction in these electrolytes is very much interesting part of today. In the present review article, the ion conducting phenomenon and some device applications of crystalline/polycrystalline superionic solid electrolytes have been reviewed in brief. Synthesis and characterization tools have also been discussed in the present review article.

Synthesis of nucleosides and dNTPs bearing oligopyridine ligands linked through an octadiyne tether, their incorporation into DNA and complexation with transition metal cations

Czech Academy of Sciences Publication Activity Database

Kalachová, Lubica; Pohl, Radek; Bednárová, Lucie; Fanfrlík, Jindřich; Hocek, Michal

2013-01-01

Roč. 11, č. 1 (2013), s. 78-89 ISSN 1477-0520 R&D Projects: GA ČR GA203/09/0317 Institutional support: RVO:61388963 Keywords : cross - coupling reactions * base-pair * solid-phase synthesis * polymerase incorporation Subject RIV: CC - Organic Chemistry Impact factor: 3.487, year: 2013

Synthesis of supported silver nano-spheres on zinc oxide nanorods for visible light photocatalytic applications

Energy Technology Data Exchange (ETDEWEB)

Saoud, Khaled [Virginia Commonwealth University-Qatar, Doha (Qatar); Alsoubaihi, Rola [Virginia Commonwealth University, Richmond, VA (United States); Bensalah, Nasr [Qatar University, Doha (Qatar); Bora, Tanujjal [Chair in Nanotechnology, Water Research Center, Sultan Qaboos University, P.O. Box 33, Al-Khoudh-123 (Oman); Bertino, Massimo [Virginia Commonwealth University, Richmond, VA (United States); Dutta, Joydeep, E-mail: dutta@squ.edu.om [Chair in Nanotechnology, Water Research Center, Sultan Qaboos University, P.O. Box 33, Al-Khoudh-123 (Oman)

2015-03-15

Highlights: • Synthesis of supported Ag NPs on ZnO nanorods using open vessel microwave reactor. • Use of the Ag/ZnO NPs as an efficient visible light photocatalyst. • Complete degradation of methylene blue in 1 h with 0.5 g/L Ag/ZnO NPs. - Abstract: We report the synthesis of silver (Ag) nano-spheres (NS) supported on zinc oxide (ZnO) nanorods through two step mechanism, using open vessel microwave reactor. Direct reduction of ZnO from zinc nitrates was followed by deposition precipitation of the silver on the ZnO nanorods. The supported Ag/ZnO nanoparticles were then characterized by electron microscopy, X-ray diffraction, FTIR, photoluminescence and UV–vis spectroscopy. The visible light photocatalytic activity of Ag/ZnO system was investigated using a test contaminant, methylene blue (MB). Almost complete removal of MB in about 60 min for doses higher than 0.5 g/L of the Ag/ZnO photocatalyst was achieved. This significant improvement in the photocatalytic efficiency of Ag/ZnO photocatalyst under visible light irradiation can be attributed to the presence of Ag nanoparticles on the ZnO nanoparticles which greatly enhances absorption in the visible range of solar spectrum enabled by surface plasmon resonance effect from Ag nanoparticles.

Comparative solution and solid-phase glycosylations toward a disaccharide library

DEFF Research Database (Denmark)

Agoston, K.; Kröger, Lars; Agoston, Agnes

2009-01-01

A comparative study on solution-phase and solid-phase oligosaccharide synthesis was performed. A 16-member library containing all regioisomers of Glc-Glc, Glc-Gal, Gal-Glc, and Gal-Gal disaccharides was synthesized both in solution and on solid phase. The various reaction conditions for different...

Fluorescent magnetic nanoparticles for cell labeling: flux synthesis of manganite particles and novel functionalization of silica shell

Czech Academy of Sciences Publication Activity Database

Kačenka, Michal; Kaman, Ondřej; Kikerlová, S.; Pavlů, B.; Jirák, Zdeněk; Jirák, D.; Herynek, Vít; Černý, J.; Chaput, F.; Laurent, S.; Lukeš, I.

2015-01-01

Roč. 47, Jun (2015), s. 97-106 ISSN 0021-9797 R&D Projects: GA ČR(CZ) GAP108/11/0807; GA MŠk(CZ) ED1.1.00/02.0109 Institutional support: RVO:68378271 ; RVO:68378041 Keywords : manganites * magnetic nanoparticles * molten salt synthesis * silica coating * dual probes * MRI * cell labeling Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 3.782, year: 2015

Solid-state synthesis of Li{sub 4}Ti{sub 5}O{sub 12} for high power lithium ion battery applications

Energy Technology Data Exchange (ETDEWEB)

Han, Seung-Woo [School of Materials Science and Engineering, Yeungnam University, Gyeongsan 712-749 (Korea, Republic of); Ryu, Ji Heon [Graduate School of Knowledge-Based Technology and Energy, Korea Polytechnic University, Siheung 429-793 (Korea, Republic of); Jeong, Joayoung [Cell Precedence Development Group, Samsung SDI, Yongin 446-577 (Korea, Republic of); Yoon, Dang-Hyok, E-mail: dhyoon@ynu.ac.kr [School of Materials Science and Engineering, Yeungnam University, Gyeongsan 712-749 (Korea, Republic of)

2013-09-05

Highlights: •High energy milling using 0.30 and 0.45 mm beads for Li{sub 4}Ti{sub 5}O{sub 12} synthesis. •Synthesis of 162 nm-sized pure Li{sub 4}Ti{sub 5}O{sub 12} by solid-state reaction. •Spray drying using fine starting materials to confer paste tackiness. •High capacity of 174 mAh/g and adequate rate properties for high power LIBs applications. -- Abstract: Li{sub 4}Ti{sub 5}O{sub 12} was synthesized by a solid-state reaction between Li{sub 2}CO{sub 3} and anatase TiO{sub 2} for applications to high power lithium ion batteries. The starting materials underwent 6 h of high energy milling using ZrO{sub 2} beads with two different sizes, 0.30 and 0.45 mm. The smaller ZrO{sub 2} beads resulted in finer starting materials. Spray drying was also performed on the 0.30 mm beads-treated particles to enhance the screen printability of a paste containing this powder. The finer starting materials showed a pure 162 nm-sized Li{sub 4}Ti{sub 5}O{sub 12} due to the decreased diffusion length for a solid-state reaction, whereas the 0.45 mm beads-treated starting materials resulted in a 242 nm-sized Li{sub 4}Ti{sub 5}O{sub 12} phase containing 2 wt.% of rutile TiO{sub 2} that had transformed from the anatase phase during heat treatment at 800 °C for 3 h. The finer Li{sub 4}Ti{sub 5}O{sub 12} showed higher charge capacity and better charge/discharge rates than the coarser particles, which highlights the importance of the primary particle size on the electrochemical properties of Li{sub 4}Ti{sub 5}O{sub 12} for high power applications. The fine Li{sub 4}Ti{sub 5}O{sub 12} particles had a discharge capacity of 174 mAh/g at 0.1 C and capacity retention of 80% at 10.0 C.

Synthesis and characterization of scandia ceria stabilized zirconia powders prepared by polymeric precursor method for integration into anode-supported solid oxide fuel cells

Science.gov (United States)

Tu, Hengyong; Liu, Xin; Yu, Qingchun

2011-03-01

Scandia ceria stabilized zirconia (10Sc1CeSZ) powders are synthesized by polymeric precursor method for use as the electrolyte of anode-supported solid oxide fuel cell (SOFC). The synthesized powders are characterized in terms of crystalline structure, particle shape and size distribution by X-ray diffraction (XRD), transmission electron microscopy (TEM) and photon correlation spectroscopy (PCS). 10Sc1CeSZ electrolyte films are deposited on green anode substrate by screen-printing method. Effects of 10Sc1CeSZ powder characteristics on sintered films are investigated regarding the integration process for application as the electrolytes in anode-supported SOFCs. It is found that the 10Sc1CeSZ films made from nano-sized powders with average size of 655 nm are very porous with many open pores. In comparison, the 10Sc1CeSZ films made from micron-sized powders with average size of 2.5 μm, which are obtained by calcination of nano-sized powders at higher temperatures, are much denser with a few closed pinholes. The cell performances are 911 mW cm-2 at the current density of 1.25 A cm-2 and 800 °C by application of Ce0.8Gd0.2O2 (CGO) barrier layer and La0.6Sr0.4CoO3 (LSC) cathode.

Solid-phase route to Fmoc-protected cationic amino acid building blocks

DEFF Research Database (Denmark)

Clausen, Jacob Dahlqvist; Linderoth, Lars; Nielsen, Hanne Mørck

2012-01-01

Diamino acids are commonly found in bioactive compounds, yet only few are commercially available as building blocks for solid-phase peptide synthesis. In the present work a convenient, inexpensive route to multiple-charged amino acid building blocks with varying degree of hydrophobicity...... was developed. A versatile solid-phase protocol leading to selectively protected amino alcohol intermediates was followed by oxidation to yield the desired di- or polycationic amino acid building blocks in gram-scale amounts. The synthetic sequence comprises loading of (S)-1-(p-nosyl)aziridine-2-methanol onto...... of simple neutral amino acids as well as analogs displaying high bulkiness or polycationic side chains was prepared. Two building blocks were incorporated into peptide sequences using microwave-assisted solid-phase peptide synthesis confirming their general utility....

Synthesis, characterization, and thermochemistry of the solid state coordination compound Zn(Nic){sub 2} . H{sub 2}O(s) (Nic = nicotinic acid)

Energy Technology Data Exchange (ETDEWEB)

Di Youying [College of Chemistry and Chemical Engineering, Liaocheng University, Liaocheng 252059, Shandong (China)], E-mail: yydi@lcu.edu.cn; Hong Yuanping; Kong Yuxia; Yang Weiwei [College of Chemistry and Chemical Engineering, Liaocheng University, Liaocheng 252059, Shandong (China); Tan Zhicheng [Thermochemistry Laboratory, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023 (China)

2009-01-15

A novel compound, viz. zinc nicotinate monohydrate, was synthesized by the method of room temperature solid phase synthesis. The techniques of FT-IR chemical and elemental analyses and X-ray powder diffraction were applied to characterise the structure and composition of the complex. In accordance with Hess' law, a thermochemical cycle was designed and the enthalpy change of the solid phase reaction of nicotinic acid with hydrated zinc acetate was determined to be {delta}{sub r}H{sub m}{sup 0}=(46.71{+-}0.21)kJ.mol{sup -1} by use of an isoperibol solution-reaction calorimeter. The standard molar enthalpy of formation of the title complex Zn(Nic){sub 2} . H{sub 2}O(s) was calculated as -(1062.3 {+-} 2.0) kJ . mol{sup -1} by use of the enthalpies of dissolution and other auxiliary thermodynamic data.

Human life support during interplanetary travel and domicile. V - Mars expedition technology trade study for solid waste management

Science.gov (United States)

Ferrall, Joe; Rohatgi, Naresh K.; Seshan, P. K.

1992-01-01

A model has been developed for NASA to quantitatively compare and select life support systems and technology options. The model consists of a modular, top-down hierarchical breakdown of the life support system into subsystems, and further breakdown of subsystems into functional elements representing individual processing technologies. This paper includes the technology trades for a Mars mission, using solid waste treatment technologies to recover water from selected liquid and solid waste streams. Technologies include freeze drying, thermal drying, wet oxidation, combustion, and supercritical-water oxidation. The use of these technologies does not have any significant advantages with respect to weight; however, significant power penalties are incurred. A benefit is the ability to convert hazardous waste into a useful resource, namely water.

Selective Aerobic Oxidation of 5-Hydroxymethylfurfural in Water Over Solid Ruthenium Hydroxide Catalysts with Magnesium-Based Supports

DEFF Research Database (Denmark)

Gorbanev, Yury; Kegnæs, Søren; Riisager, Anders

2011-01-01

Solid catalyst systems comprised of ruthenium hydroxide supported on magnesium-based carrier materials (spinel, magnesium oxide and hydrotalcite) were investigated for the selective, aqueous aerobic oxidation of the biomass-derived chemical 5-hydroxymethylfurfural into 2,5-furandicarboxylic acid...

N-Confused Porphyrin Immobilized on Solid Supports: Synthesis and Metal Ions Sensing Efficacy

Directory of Open Access Journals (Sweden)

Sara R. D. Gamelas

2018-04-01

Full Text Available In this work, the N-confused porphyrin 5,10,15,20-tetraphenyl-2-aza-21-carbaporphyrin (NCTPP was immobilized on neutral or cationic supports based on silica and on Merrifield resin. The new materials were characterized by appropriate techniques (UV-Vis spectroscopy, SEM, and zeta potential analysis. Piezoelectric quartz crystal gold electrodes were coated with the different hybrids and their ability to interact with heavy metals was evaluated. The preliminary results obtained showed that the new materials can be explored for metal cations detection and the modification of the material surface is a key factor in tuning the metal selectivity.

Bioinspired magnetite synthesis via solid precursor phases

NARCIS (Netherlands)

Lenders, J.J.M.; Mirabello, G.; Sommerdijk, N.A.J.M.

2016-01-01

Living organisms often exploit solid but poorly ordered mineral phases as precursors in the biomineralization of their inorganic body parts. Generally speaking, such precursor-based approaches allow the organisms-without the need of high supersaturation levels-to accumulate significant quantities of

High-flexibility combinatorial peptide synthesis with laser-based transfer of monomers in solid matrix material.

Science.gov (United States)

Loeffler, Felix F; Foertsch, Tobias C; Popov, Roman; Mattes, Daniela S; Schlageter, Martin; Sedlmayr, Martyna; Ridder, Barbara; Dang, Florian-Xuan; von Bojničić-Kninski, Clemens; Weber, Laura K; Fischer, Andrea; Greifenstein, Juliane; Bykovskaya, Valentina; Buliev, Ivan; Bischoff, F Ralf; Hahn, Lothar; Meier, Michael A R; Bräse, Stefan; Powell, Annie K; Balaban, Teodor Silviu; Breitling, Frank; Nesterov-Mueller, Alexander

2016-06-14

Laser writing is used to structure surfaces in many different ways in materials and life sciences. However, combinatorial patterning applications are still limited. Here we present a method for cost-efficient combinatorial synthesis of very-high-density peptide arrays with natural and synthetic monomers. A laser automatically transfers nanometre-thin solid material spots from different donor slides to an acceptor. Each donor bears a thin polymer film, embedding one type of monomer. Coupling occurs in a separate heating step, where the matrix becomes viscous and building blocks diffuse and couple to the acceptor surface. Furthermore, we can consecutively deposit two material layers of activation reagents and amino acids. Subsequent heat-induced mixing facilitates an in situ activation and coupling of the monomers. This allows us to incorporate building blocks with click chemistry compatibility or a large variety of commercially available non-activated, for example, posttranslationally modified building blocks into the array's peptides with >17,000 spots per cm(2).

Solid Matter

CERN Document Server

Angelo, Joseph A

2011-01-01

Supported by a generous quantity of full-color illustrations and interesting sidebars, Solid Matter introduces the basic characteristics and properties of solid matter. It briefly describes the cosmic connection of the elements, leading readers through several key events in human pre-history that resulted in more advanced uses of matter in the solid state. Chapters include:. -Solid Matter: An Initial Perspective. -Physical Behavior of Matter. -The Gravity of Matter. -Fundamentals of Materials Science. -Rocks and Minerals. -Metals. -Building Materials. -Carbon Earth's Most Versatile Element. -S

Failure analysis of electrolyte-supported solid oxide fuel cells

Science.gov (United States)

Fleischhauer, Felix; Tiefenauer, Andreas; Graule, Thomas; Danzer, Robert; Mai, Andreas; Kuebler, Jakob

2014-07-01

For solid oxide fuel cells (SOFCs) one key aspect is the structural integrity of the cell and hence its thermo mechanical long term behaviour. The present study investigates the failure mechanisms and the actual causes for fracture of electrolyte supported SOFCs which were run using the current μ-CHP system of Hexis AG, Winterthur - Switzerland under lab conditions or at customer sites for up to 40,000 h. In a first step several operated stacks were demounted for post-mortem inspection, followed by a fractographic evaluation of the failed cells. The respective findings are then set into a larger picture including an analysis of the present stresses acting on the cell like thermal and residual stresses and the measurements regarding the temperature dependent electrolyte strength. For all investigated stacks, the mechanical failure of individual cells can be attributed to locally acting bending loads, which rise due to an inhomogeneous and uneven contact between the metallic interconnect and the cell.

Comparison of bacterial cells and amine-functionalized abiotic surfaces as support for Pd nanoparticle synthesis

DEFF Research Database (Denmark)

De Corte, Simon; Bechstein, Stefanie; Lokanathan, Arcot R.

2013-01-01

An increasing demand for catalytic Pd nanoparticles has motivated the search for sustainable production methods. An innovative approach uses bacterial cells as support material for synthesizing Pd nanoparticles by reduction of Pd(II) with e.g. hydrogen or formate. Nevertheless, drawbacks...... nanoparticles, and that abiotic surfaces could support the Pd particle synthesis as efficiently as bacteria. In this study, we explore the possibility of replacing bacteria with amine-functionalized materials, and we compare different functionalization strategies. Pd nanoparticles formed on the support...... on these surfaces was higher than for Pd particles formed on Shewanella oneidensis cells. Smaller Pd nanoparticles generally have better catalytic properties, and previous studies have shown that the particle size can be lowered by increasing the amount of support material used during Pd particle formation. However...

Synthesis of 3'-, or 5'-, or internal methacrylamido-modified oligonucleotides

Science.gov (United States)

Golova, Julia B.; Chernov, Boris K.

2010-04-27

New modifiers were synthesized for incorporation of a methacrylic function in 3'-, 5'- and internal positions of oligonucleotides during solid phase synthesis. A modifier was used for synthesis of 5'-methacrylated oligonucleotides for preparation of microarrays by a co-polymerization method.

Prospects of Fe/MCM-41 as a Catalyst for Hydrocarbon Synthesis

International Nuclear Information System (INIS)

Cagnoli, Maria V.; Gallegos, Norma G.; Bengoa, Jose F.; Alvarez, Ana M.; Marchetti, Sergio G.; Moreno, Sergio M. J.; Roig, Anna; Mercader, Roberto C.

2005-01-01

We report the synthesis of cylindrical nanoparticles of metallic Fe entirely included in MCM-41 pores. Their dimensions are approx.3 nm diameter and approx. 3.8 nm length. We show that a coherent analysis of the results yielded by the various techniques is essential to obtain a catalyst supported on an MCM-41 matrix of ≅ 3 nm average pore diameter, which is active and selective toward olefins. The solids were characterized by low-angle x-ray diffraction, high-resolution transmission electron microscopy, high-resolution scanning transmission electron microscopy equipped with a high-angle annular dark-field, CO chemisorption, volumetric oxidation, and Moessbauer spectroscopy (in controlled atmosphere for the reduced catalysts). Catalytic results in the Fischer-Tropsch synthesis, as well as some unexpected results --like the inhomogeneous pore filling and discontinuous Fe particles-- are also discussed

Synthesis, Characterization, and Optimization of Novel Solid Oxide Fuel Cell Anodes

Science.gov (United States)

Miller, Elizabeth C.

(SLT) anode supports, thin La1--xSr x Ga0.8Mg0.2O3 (x = 0.1, 0.2) dense electrolytes, and porous LSGM anode functional layers. The SLT support and the LSGM functional layer are infiltrated with nanoscale Ni, creating extensive electrochemically active triple phase boundary area. The scope of the work presented here encompasses every step of cell development including powder synthesis, optimization of firing conditions, and long-term stability testing. Using an optimized fabrication process, cells with power density > 1.2 W cm-2 were fabricated. Dry pressing and colloidal de-position were used to make the first generation of these cells, and once suitable times and temperatures were determined, the process was shifted to tape casting to make larger batches of uniform cells. After obtaining initial results of low anode polarization resistance and high power density, the long-term stability of the Ni-infiltrated anodes was examined. A coarsening model was developed using the data from accelerated degradation tests to predict cell performance over a typical device lifetime. This thesis encompasses a broad range of novel SOFC anode materials, each of which has its own strengths and weaknesses. Presenting several possible avenues for SOFC development provides a complete picture of the ?eld and its current focuses. The wide scope of this work offers multiple solutions for the SOFC community and demonstrates that SOFCs are a strong candidate for meeting the United States' need for energy conversion and storage.

Cerium Modified Pillared Montmorillonite Supported Cobalt Catalysts for Fischer Tropsch Synthesis

International Nuclear Information System (INIS)

Ahmad, N.; Ali, Z.; Abbas, S. M.; Hussain, F.

2015-01-01

Fischer-Tropsch (FT) synthesis was accomplished over Al-pillared Montmorillonite supported 20 wt% Co modified with different weight% of cerium catalysts. These catalysts were prepared by impregnation method while structural characterizations of the prepared samples were performed by XRD, TPR, NH/sub 3/TPD, TGA, BET, XRF and SEM techniques. The Fischer Tropsch reaction was studied in fixed bed micro catalytic reactor at temperature range of 220, 260 and 275 degree C and at different pressure (1, 5 and 10 bars). From the activity results, it was found that by pillaring NaMMT with Al higher catalytic activity and lower methane selectivity of NaMMT was achieved. Furthermore, the results of FT synthesis reaction revealed that cerium incorporation increased the dispersion of Co/sub 3/O/sub 4/ on the surface and consequently resulted in enhanced catalytic activity. Additionally, the C/sub 5/-C/sub 12/ hydrocarbons and methane selectivity increased while C/sub 22+/ hydrocarbons selectivity was decreased over cerium modified catalysts. Higher reaction temperature (>220 degree C) resulted in significant enhancement in CO conversion and methane selectivity. Though, increase in pressure from 1 to 10 bars eventually resulted in increase in C/sub 5+/ hydrocarbons and decrease in methane and C/sub 2/-C/sub 5/ hydrocarbons selectivity. (author)

Steric effects in release of amides from linkers in solid-phase synthesis. Molecular mechanics modeling of key step in peptide and combinatorial chemistry

DEFF Research Database (Denmark)

Norrby, Per-Ola; Jensen, Knud Jørgen

2006-01-01

Acidolytic release of an amide from a solid support by C-N bond cleavage is all ubiquitous and crucial step in many solid-phase syntheses. We have used molecular modeling of a pseudo-equilibrium to explore substituent and steric effects in the release of peptides. The high acid-lability of the ba......Acidolytic release of an amide from a solid support by C-N bond cleavage is all ubiquitous and crucial step in many solid-phase syntheses. We have used molecular modeling of a pseudo-equilibrium to explore substituent and steric effects in the release of peptides. The high acid......-lability of the backbone amide linkage (BAL), which releases sec. amides, compared to C-terminal amide anchoring, which releases primary amides, was rationalized by steric relief upon cleavage. Thus, the relative stability of the carbenium ion formed from the linker in the acidolytic release is an insufficient measure...

Synthesis and characterization of nano-crystalline Ce_1-xGd _xO_2-x/2 (x = 0-0.30) solid solutions

DEFF Research Database (Denmark)

Jadhav, L. D.; Chourashiya, M. G.; Jamale, A. P.

2010-01-01

glycine-nitrate process (GNP) has been presented. Evolution of structural and morphological properties of nano-powders as a function of heat treatment has also been studied. The prepared samples were characterized using TG-DTA, FT-IR, Raman spectroscopy, XRD, SEM, etc. In addition, the effect of Gd......In recent years, doped ceria is an established and promising candidate as solid electrolyte for intermediate temperature solid oxide fuel cell (IT-SOFC). In this investigation, synthesis and characterizations of nano-crystalline Gd doped ceria, (Ce1-xGdxO2-x/2, where x = 0-0.3), prepared using...... of sintered samples was observed to hinder with an increase in Gd content....

Synthesis and ceramic processing of zirconia alumina composites for application as solid oxide fuel cell electrolytes

International Nuclear Information System (INIS)

Garcia, Rafael Henrique Lazzari

2007-01-01

The global warmness and the necessity to obtain clean energy from alternative methods than petroleum raises the importance of developing cleaner and more efficient systems of energy generation, among then, the solid oxide fuel cell (SOFC). Cubic stabilized zirconia (CSZ) has been the most studied material as electrolyte in SOFC, due to its ionic conductivity and great stability at operation conditions. However, its low fracture toughness difficulties its application as a thin layer, what could lead to an improvement of cell efficiency. In this sense, the alumina addition in CSZ forms a composite, which can shift its mechanical properties, without compromising its electrical properties. In this work, coprecipitation synthesis route and ceramic processing of zirconia-alumina composites were studied, in order to establish optimum conditions to attain high density, homogeneous microstructure, and better mechanical properties than CSZ, without compromising ionic conductivity. For this purpose, composites containing up to 40 wt % of alumina, in a 9 mol % yttria-stabilized zirconia (9Y-CSZ) matrix were evaluated. In order to optimize the synthesis of the composites, a preliminary study of powder obtaining and processing were carried out, at compositions containing 20 wt % of alumina, in 9Y-CSZ. The ceramic powders were characterized by helium picnometry, X-ray diffraction, scanning electronic microscopy, transmission electronic microscopy, thermogravimetry, differential scanning calorimetry, granulometry by laser diffraction and gas adsorption (BET). The characterization of sinterized compacts were performed by X-ray diffraction, scanning electron microscopy, optical microscopy, density measurements, Vickers indentation and impedance spectroscopy. The obtained results show that the alumina addition, in the 9Y-CSZ matrix powders, raises the specific surface area, promotes deagglomeration of powders and elevates the oxides crystallization temperature, requiring higher

“Flash” Solvent-free Synthesis of Triazoles Using a Supported Catalyst

Directory of Open Access Journals (Sweden)

Ibtissem Jlalia

2009-01-01

Full Text Available A solvent-free synthesis of 1,4-disubstituted-1,2,3-triazoles using neat azides and alkynes and a copper(I polymer supported catalyst (Amberlyst® A21•CuI is presented herein. As it provides the products in high yields and purities within minutes, this method thus being characterized as a "flash" synthesis, and was exemplified through the synthesis of a 24-compound library on a small scale.

Synthesis and characterization of 12-phosphotungstic acid supported on BEA zeolite

Energy Technology Data Exchange (ETDEWEB)

Jović, A.; Bajuk-Bogdanović, D.; Nedić Vasiljević, B. [Faculty of Physical Chemistry, University of Belgrade, Studentski trg 12-16, 11000 Belgrade (Serbia); Milojević-Rakić, M., E-mail: maja@ffh.bg.ac.rs [Faculty of Physical Chemistry, University of Belgrade, Studentski trg 12-16, 11000 Belgrade (Serbia); Krajišnik, D. [Department of Pharmaceutical Technology and Cosmetology, University of Belgrade-Faculty of Pharmacy, Vojvode Stepe 450, 11000 Belgrade (Serbia); Dondur, V. [Faculty of Physical Chemistry, University of Belgrade, Studentski trg 12-16, 11000 Belgrade (Serbia); Popa, A. [Institute of Chemistry Timisoara, Bl. Mihai Viteazul 24, 300223 Timisoara (Romania); Uskoković-Marković, S. [Department of Analytical Chemistry, University of Belgrade-Faculty of Pharmacy, Vojvode Stepe 450, 11000 Belgrade (Serbia); Holclajtner-Antunović, I. [Faculty of Physical Chemistry, University of Belgrade, Studentski trg 12-16, 11000 Belgrade (Serbia)

2017-01-15

An optimized synthetic route for obtaining heteropoly acid (HPA) species supported on BEA zeolite was applied, and different samples, comprising 20 to 50 wt% of 12-phosphotungstic acid (HPW) were prepared. The as-synthesized supported HPW were subjected to different post-synthesis routes, which involved calcination and ultrasound treatment. Characterization of these materials was performed by means of Scanning Electron Microscopy, zeta potential measurements, Infrared Spectroscopy and X-ray Powder Diffraction analysis. Results suggest strong interaction of HPW with the support and revealed that ultrasound treatment resulted in better dispersion of active phase and thus homogeneous morphology of the samples. The zeta potential was found to be dependent on the preparation procedure and HPW content in these materials, while higher HPW loadings induced its agglomeration. Catalytic activity of the synthesized materials was investigated in an ethanol dehydration reaction, where lower HPW loadings induced higher ethanol conversion. Acid sites distribution and accessibility for ethanol molecules were found to be more essential for catalytic activity than HPW loadings, i.e., amount of active sites present in these hybrid materials. - Highlights: • An optimized route for supporting heteropoly acid on beta zeolite is applied. • Ultrasound treatment of the composites gives dispersed morphology. • Lower heteropoly acid amount induces higher conversion in ethanol dehydration. • Acid sites distribution and accessibility for ethanol are essential for catalytic activity.

Synthesis and characterization of 12-phosphotungstic acid supported on BEA zeolite

International Nuclear Information System (INIS)

Jović, A.; Bajuk-Bogdanović, D.; Nedić Vasiljević, B.; Milojević-Rakić, M.; Krajišnik, D.; Dondur, V.; Popa, A.; Uskoković-Marković, S.; Holclajtner-Antunović, I.

2017-01-01

An optimized synthetic route for obtaining heteropoly acid (HPA) species supported on BEA zeolite was applied, and different samples, comprising 20 to 50 wt% of 12-phosphotungstic acid (HPW) were prepared. The as-synthesized supported HPW were subjected to different post-synthesis routes, which involved calcination and ultrasound treatment. Characterization of these materials was performed by means of Scanning Electron Microscopy, zeta potential measurements, Infrared Spectroscopy and X-ray Powder Diffraction analysis. Results suggest strong interaction of HPW with the support and revealed that ultrasound treatment resulted in better dispersion of active phase and thus homogeneous morphology of the samples. The zeta potential was found to be dependent on the preparation procedure and HPW content in these materials, while higher HPW loadings induced its agglomeration. Catalytic activity of the synthesized materials was investigated in an ethanol dehydration reaction, where lower HPW loadings induced higher ethanol conversion. Acid sites distribution and accessibility for ethanol molecules were found to be more essential for catalytic activity than HPW loadings, i.e., amount of active sites present in these hybrid materials. - Highlights: • An optimized route for supporting heteropoly acid on beta zeolite is applied. • Ultrasound treatment of the composites gives dispersed morphology. • Lower heteropoly acid amount induces higher conversion in ethanol dehydration. • Acid sites distribution and accessibility for ethanol are essential for catalytic activity.

The Progress of SBIR Supported R and D of Solid State Pulse Modulators

International Nuclear Information System (INIS)

Koontz, R

2004-01-01

The Small Business Innovative Research (SBIR) grant program funded by the US Department of Energy makes a number of awards each year for R and D in the field of accelerator technology including high power pulse modulators and their components. This paper outlines program requirements, and reviews some of the awards made in the last three years in support of high power modulator systems and solid state switching. A number of award recipients are presenting the results of their SBIR R and D at this workshop

Solid State Division progress report for period ending March 31, 1992

International Nuclear Information System (INIS)

Green, P.H.; Hinton, L.W.

1992-09-01

During this period, the division conducted a broad, interdisciplinary materials research program with emphasis on theoretical solid state physics, superconductivity, neutron scattering, synthesis and characterization of materials, ion beam and laser processing, and the structure of solids and surfaces. The High Flux Isotope Reactor was returned to full operation

Solid State Division progress report for period ending March 31, 1992

Energy Technology Data Exchange (ETDEWEB)

Green, P.H.; Hinton, L.W. (eds.)

1992-09-01

During this period, the division conducted a broad, interdisciplinary materials research program with emphasis on theoretical solid state physics, superconductivity, neutron scattering, synthesis and characterization of materials, ion beam and laser processing, and the structure of solids and surfaces. The High Flux Isotope Reactor was returned to full operation.

Synthesis of (U,Zr)C solid solutions under exothermic conditions

International Nuclear Information System (INIS)

Wang, L.L.; Moore, H.G.; Gladson, J.W.

1993-01-01

The reactions of forming (U,Zr)C solid solutions from their elemental components or similarly less stable reactants such as UC 2 are strongly exothermic due to the high stability of these solid solutions. A simple approach of utilizing this heat of formation energy to assist the solid solution reaction process is to intimately mix the less stable reactant powders and then pressed them into a compact. The compact is then heated to the ignition temperature of the reaction. The feasibility of this reaction method to synthesize (U,Zr)C solid solutions has been demonstrated in this study. The preliminary results also show that both the initial composition and the heating rate have a significant effect on the nature of the reaction process. As expected the degree of powder mixing was also found to affect the completeness of the reaction

Synthesis and Characterization of Novel Quaternary Thioaluminogermanates

KAUST Repository

Al-Bloushi, Mohammed

2013-05-01

Metal chalcogenides form an important class of inorganic materials, which include several technologically important applications. The design of metal chlcogenides is of technological interest and has encouraged recent research into moderate temperature solid-state synthetic methods for the single crystal growth of new materials. The aim of this project is the investigation and development of synthetic methodology for the synthesis of novel metal chlcogenides. The new inorganic compounds of the type “M(AlS2)(GeS2)” (M = Na and K) are new metal-chalcogenides, synthesized by the classical solid state approach. The characterization of these compounds was carried out by Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS), Single crystal and powder X-ray diffraction, solid state Nuclear Magnetic Resonance (NMR), Ultraviolet-visible (UV-VIS), Infrared (IR) and Raman spectroscopy. These theses study the synthesis of metal chalcogenides through the use of standard chemical techniques. The systematic studies demonstrate the effect of the reactants ratio and reaction temperature on the synthesis and growth of the single crystals. Metal chalcogenides have several potential applications in gas separation, ion exchange, environmental remediation, and energy storage. Especially, the ion exchange materials have found\\tpossible applications in waste-water treatment, water softening, metal separation, and production of high purity water.

Synthesis of Single-Walled Carbon Nanotubes: Effects of Active Metals, Catalyst Supports, and Metal Loading Percentage

Directory of Open Access Journals (Sweden)

Wei-Wen Liu

2013-01-01

Full Text Available The effects of active metals, catalyst supports, and metal loading percentage on the formation of single-walled carbon nanotubes (SWNTs were studied. In particular, iron, cobalt, and nickel were investigated for SWNTs synthesis. Iron was found to grow better-quality SWNTs compared to cobalt and nickel. To study the effect of catalyst supports, magnesium oxide, silicon oxide, and aluminium oxide were chosen for iron. Among the studied supports, MgO was identified to be a suitable support for iron as it produced SWNTs with better graphitisation determined by Raman analysis. Increasing the iron loading decreased the quality of SWNTs due to extensive agglomeration of the iron particles. Thus, lower metal loading percentage is preferred to grow better-quality SWNTs with uniform diameters.

CTAB assisted microwave synthesis of ordered mesoporous carbon supported Pt nanoparticles for hydrogen electro-oxidation

International Nuclear Information System (INIS)

Zhou, Jian-Hua; He, Jian-Ping; Ji, Ya-Jun; Dang, Wang-Juan; Liu, Xiao-Lei; Zhao, Gui-Wang; Zhang, Chuan-Xiang; Zhao, Ji-Shuang; Fu, Qing-Bin; Hu, Huo-Ping

2007-01-01

Mesoporous carbon with ordered hexagonal structure derived from the co-assembly of triblock copolymer F127 and resol was employed as the carbon support of Pt catalysts for hydrogen electro-oxidation. Structural characterizations revealed that the mesoporous carbon exhibited large surface area and uniform mesopores. The Pt nanoparticles supported on the novel mesoporous carbon were fabricated by a facile CTAB assisted microwave synthesis process, wherein CTAB was expected to improve the wettability of carbon support as well as the dispersion of Pt nanoparticles. X-ray diffraction and transmission electron microscopy were applied to characterize the Pt catalysts. It was found that the Pt nanoparticles were uniform in size and highly dispersed on the mesoporous carbon supports. The cyclic voltammograms in sulfuric acid demonstrated that the electrochemical active surface area of Pt catalysts prepared with CTAB was two times than that without CTAB

Anionic solid lipid nanoparticles supported on protamine/DNA complexes

International Nuclear Information System (INIS)

Ye Jiesheng; Liu Chunxi; Chen Zhijin; Zhang Na; Wang Aihua

2008-01-01

The objective of this study was to design novel anionic ternary nanoparticles for gene delivery. These ternary nanoparticles were equipped with protamine/DNA binary complexes (150-200 nm) as the support, and the anionic formation was achieved by absorption of anionic solid lipid nanoparticles (≤20 nm) onto the surface of the binary complexes. The small solid lipid nanoparticles (SLNs) were prepared by a modified film dispersion-ultrasonication method, and adsorption of the anionic SLNs onto the binary complexes was typically carried out in water via electrostatic interaction. The formulated ternary nanoparticles were found to be relatively uniform in size (257.7 ± 10.6 nm) with a 'bumpy' surface, and the surface charge inversion from 19.28 ± 1.14 mV to -17.16 ± 1.92 mV could be considered as evidence of the formation of the ternary nanoparticles. The fluorescence intensity measurements from three batches of the ternary nanoparticles gave a mean adsorption efficiency of 96.75 ± 1.13%. Circular dichroism spectra analysis showed that the protamine/DNA complexes had been coated by small SLNs, and that the anionic ternary nanoparticles formed did not disturb the construction of the binary complexes. SYBR Green I analysis suggested that the ternary nanoparticles could protect the DNA from nuclease degradation, and cell viability assay results showed that they exhibit lower cytotoxicity to A549 cells compared with the binary complexes and lipofectamine. The transfection efficiency of the ternary nanoparticles was better than that of naked DNA and the binary complexes, and almost equal to that of lipofectamine/DNA complexes, as revealed by inversion fluorescence microscope observation. These results indicated that the anionic ternary nanoparticles could facilitate gene transfer in cultured cells, and might alleviate the drawbacks of the conventional cationic vector/DNA complexes for gene delivery in vivo

Characterization of 12-molybdophosphoric acid supported on mesoporous silica MCM-41 and its catalytic performance in the synthesis of hydroquinone diacetate

International Nuclear Information System (INIS)

Ahmed, Awad I.; Samra, S.E.; El-Hakam, S.A.; Khder, A.S.; El-Shenawy, H.Z.; El-Yazeed, W.S. Abo

2013-01-01

12-molybdophosphoric acid (PMA) was supported on mesoporous molecular sieves MCM-41 by impregnation of 12-molybdophosphoric acid followed by calcination. The nanochannels of MCM-41 provide a large surface area for the solid state dispersion of 12-molybdophosphoric acid. The samples have been characterized by N 2 adsorption–desorption at −196 °C, transmission electron microscopy (TEM), powder X-ray diffraction (PXRD), and FT-IR measurements. The acidity and catalytic activity have been, respectively, examined by nonaqueous titration of n-butylamine in acetonitrile and synthesis of hydroquinone diacetate. The results showed that ordered hexagonal pore structure was observed in the synthesized MCM-41. Also the results indicate that PMA are highly dispersed on mesoporous silica MCM-41 spherical nanoparticles while PMA retains its Keggin structure. On the other hand, with increasing the introduced PMA amount, the specific surface area decreases, and the mesoporous ordering of the samples become poor. Both the surface acidity and the catalytic activity sharply increase with the modification of MCM-41 by PMA but decrease by increasing the calcination temperature. The sample with 55 wt% PMA/MCM-41 calcined at 350 °C shows the highest acidity and catalytic activity.

Fabrication and Characterization of Graded Anodes for Anode-Supported Solid Oxide Fuel Cells by Tape Casting and Lamination

DEFF Research Database (Denmark)

Beltran-Lopez, J.F.; Laguna-Bercero, M.A.; Gurauskis, Jonas

2014-01-01

Graded anodes for anode-supported solid oxide fuel cells (SOFCs) are fabricated by tape casting and subsequent cold lamination of plates using different compositions. Rheological parameters are adjusted to obtain stable suspensions for tape casting. The conditions for the tape casting and laminat......Graded anodes for anode-supported solid oxide fuel cells (SOFCs) are fabricated by tape casting and subsequent cold lamination of plates using different compositions. Rheological parameters are adjusted to obtain stable suspensions for tape casting. The conditions for the tape casting...... and lamination will be described. Flexural strength of the reduced cermets measured using three-point bending configuration is 468±37MPa. The graded anode supports are characterized by scanning electron microscope observations, mercury porosimetry intrusion, and resistivity measurements, showing an adequate...... of tapes at room temperature without using plasticizers. This is made by the combination of two different binders with varying Tg (glass transition temperature) which resulted in plastic deformation at room temperature. Those results indicate that the proposed process is a cost-effective method...

Shifting mindsets: a realist synthesis of evidence from self-management support training.

Science.gov (United States)

Davies, Freya; Wood, Fiona; Bullock, Alison; Wallace, Carolyn; Edwards, Adrian

2018-03-01

Accompanying the growing expectation of patient self-management is the need to ensure health care professionals (HCPs) have the required attitudes and skills to provide effective self-management support (SMS). Results from existing training interventions for HCPs in SMS have been mixed and the evidence base is weaker for certain settings, including supporting people with progressive neurological conditions (PNCs). We set out to understand how training operates, and to identify barriers and facilitators to training designed to support shifts in attitudes amongst HCPs. We undertook a realist literature synthesis focused on: (i) the influence of how HCPs, teams and organisations view and adopt self-management; and (ii) how SMS needs to be tailored for people with PNCs. A traditional database search strategy was used alongside citation tracking, grey literature searching and stakeholder recommendations. We supplemented PNC-specific literature with data from other long-term conditions. Key informant interviews and stakeholder advisory group meetings informed the synthesis process. Realist context-mechanism-outcome configurations were generated and mapped onto the stages described in Mezirow's Transformative Learning Theory. Forty-four original articles were included (19 relating to PNCs), from which seven refined theories were developed. The theories identified important training elements (evidence provision, building skills and confidence, facilitating reflection and generating empathy). The significant influence of workplace factors as possible barriers or facilitators was highlighted. Embracing SMS often required challenging traditional professional role boundaries. The integration of SMS into routine care is not an automatic outcome from training. A transformative learning process is often required to trigger the necessary mindset shift. Training should focus on how individual HCPs define and value SMS and how their work context (patient group and organisational

Municipal solid waste management system: decision support through systems analysis

OpenAIRE

Pires, Ana Lúcia Lourenço

2010-01-01

Thesis submitted to the Universidade Nova de Lisboa, Faculdade de Ciências e Tecnologia for the degree of Doctor of Philosophy in Environmental Engineering The present study intends to show the development of systems analysis model applied to solid waste management system, applied into AMARSUL, a solid waste management system responsible for the management of municipal solid waste produced in Setúbal peninsula, Portugal. The model developed intended to promote sustainable decision making, ...

Solid waste containing method and solid waste container

International Nuclear Information System (INIS)

Sawai, Takeshi.

1997-01-01

Solid wastes are filled in a sealed vessel, and support spacers are inserted to the gap between the inner wall of a vessel main body and the solid wastes. The solid wastes comprise shorn pieces (crushed pieces) of spent fuel rod cladding tubes, radioactively contaminated metal pieces and miscellaneous solids pressed into a disk-like shape. The sealed vessel comprises, for example, a stainless steel. The solid wastes are filled while being stacked in a plurality of stages. A solidifying filler is filled into the gap between the inner wall and the solid wastes in the vessel main body by way of an upper opening, and the upper opening is closed by a closing lid to provide an entirely sealed state. Alumina particles having high heat conductivity and excellent heat durability are used for the solid filler. It is preferable to fill an inert gas such as a dried nitrogen gas in the sealed vessel. (I.N.)

Fabrication of Cu{sub 2}ZnSn(S,Se){sub 4} (CZTSSe) absorber films based on solid-phase synthesis and blade coating processes

Energy Technology Data Exchange (ETDEWEB)

Ma, Ruixin, E-mail: mrx_601@126.com [School of Metallurgy and Ecological Engineering, University of Science and Technology Beijing, Beijing 100083 (China); Beijing Key Laboratory of Special Melting and Preparation of High-end Metal Materials, Beijing 100083 (China); Yang, Fan; Li, Shina; Zhang, Xiaoyong; Li, Xiang; Cheng, Shiyao; Liu, Zilin [School of Metallurgy and Ecological Engineering, University of Science and Technology Beijing, Beijing 100083 (China)

2016-04-15

Graphical abstract: - Highlights: • Pure CZTS nano-crystalline have been prepared based on solid-phase synthesis. • A simple and modified doctor blade process followed by a selenization technique was utilized to fabricate CZTSSe absorber films. • Comparative studies on the properties of CZTS and CZTSSe absorber films have been investigated. • The band gap of CZTSSe absorber films was determined to be 1.26 eV. - Abstract: CZTSSe is an important earth abundant collection of materials for the development of low cost and high efficiency thin film solar cells. This work developed a simple non-vacuum-based route to fabricate CZTSSe absorber films. This was demonstrated by first synthesizing Cu{sub 2}ZnSnS{sub 4} (CZTS) nano-crystalline based on solid-phase synthesis. Then a stable colloidal ink composed of CZTS nano-crystalline was blade coated on Mo-coated substrates followed by an annealing process under Ar atmosphere. After CZTS films formation, the films were sintered into CZTSSe absorber films by exposing them under Selenium vapor. The formation of a kesterite type CZTS was confirmed using X-ray diffraction and Raman scattering measurements. The band gap of CZTSSe absorber films was determined to be 1.26 eV, which was appropriate for use as an absorber layer in thin film solar cells. The CZTSSe absorber films showed a good photovoltatic performance, demonstrating this simple approach had great potential for CZTSSe solar cell production.

Construction of an Immobilized Thermophilic Esterase on Epoxy Support for Poly(ε-caprolactone) Synthesis.

Science.gov (United States)

Ren, Hui; Xing, Zhen; Yang, Jiebing; Jiang, Wei; Zhang, Gang; Tang, Jun; Li, Quanshun

2016-06-18

Developing an efficient immobilized enzyme is of great significance for improving the operational stability of enzymes in poly(ε-caprolactone) synthesis. In this paper, a thermophilic esterase AFEST from the archaeon Archaeoglobus fulgidus was successfully immobilized on the epoxy support Sepabeads EC-EP via covalent attachment, and the immobilized enzyme was then employed as a biocatalyst for poly(ε-caprolactone) synthesis. The enzyme loading and recovered activity of immobilized enzyme was measured to be 72 mg/g and 10.4 U/mg using p-nitrophenyl caprylate as the substrate at 80 °C, respectively. Through the optimization of reaction conditions (enzyme concentration, temperature, reaction time and medium), poly(ε-caprolactone) was obtained with 100% monomer conversion and low number-average molecular weight (Mn enzyme exhibited excellent reusability, with monomer conversion values exceeding 75% during 15 batch reactions. Finally, poly(ε-caprolactone) was enzymatically synthesized with an isolated yield of 75% and Mn value of 3005 g/mol in a gram-scale reaction.

Microwave-induced solid-state synthesis of TiO2(B) nanobelts with enhanced lithium-storage properties

International Nuclear Information System (INIS)

Qiao Yun; Hu Xianluo; Huang Yunhui

2012-01-01

A fast and economical route based on an efficient microwave-induced solid-state process has been developed to synthesize metastable TiO 2 (B) nanobelts with widths of 30–100 nm and lengths up to a few micrometers on a large scale. This new method reduces the synthesis time for the preparation of TiO 2 (B) nanobelts to less than half an hour, allowing the screening of a wide range of reaction conditions for optimizing and scaling up the production and facilitating the formation of metastable phase TiO 2 (B). The as-formed TiO 2 (B) nanobelts exhibit enhanced lithium-storage performances, compared with the TiO 2 (B) product obtained by the conventional heating. This study provides a new way for large-scale industrial production of high-quality metastable TiO 2 (B) nanostructures. The products were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and Raman spectroscopy.

Low-temperature solid-state synthesis and optical properties of CdS-ZnS and ZnS-CdS alloy nanoparticles

International Nuclear Information System (INIS)

Liu Jinsong; Zhao Chuanbao; Li Ziquan; Chen Jiankang; Zhou Hengzhi; Gu Shanqun; Zeng Youhong; Li Yongchan; Huang Yongbing

2011-01-01

Highlights: → Using a simple low-temperature solid-state synthetic method, ZnS-CdS and CdS-ZnS alloy nanoparticles were obtained, respectively. → The size of the nanoparticles increased with increasing reaction temperature, and reaction sequence had no effect on the size of the nanoparticles under the same temperature. → The particle diameters of the CdS-ZnS products decreased gradually with increasing Cd 2+ /Zn 2+ molar ratio, whereas those of the ZnS-CdS products increased gradually with increasing Zn 2+ /Cd 2+ molar ratio. → The study shows that sufficient grinding and crystalline water may be a key in forming the alloy nanoparticles. → Optical properties of the products depend on reaction temperature, reactant addition sequence, and reactant molar ratio. - Abstract: A simple low-temperature solid-state synthetic method was employed to obtain ZnS-CdS and CdS-ZnS alloy nanoparticles. The effects of reaction sequence, reactant molar ratios, and synthesis temperature on the products were investigated. The crystal structure and morphology of the products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and fourier transform infrared (FT-IR) spectroscopy. The results show that the products are alloy nanoparticles with a cubic phase structure. The formation mechanism of the alloy nanoparticles is briefly discussed. Sufficient grinding and crystalline water may be essential to form alloy nanoparticles. Ultraviolet-visible (UV-vis) spectra show that the edge absorptions of the CdS-ZnS and ZnS-CdS nanoparticles were located between those of ZnS and CdS bulks, and the absorbance at the peak maximum was practically dependent on reaction temperature, reaction sequence, and molar ratio. Extrinsic deep-level emission resulted in strong peaks in the photoluminescence (PL) spectra. The position and intensity of the emission peaks varied with the conditions during synthesis.

Synthesis of Chalcone and Flavanone Compound Using Raw Material of Acetophenone and Benzaldehyde Derivative

Directory of Open Access Journals (Sweden)

Ismiyarto Ismiyarto

2010-06-01

Full Text Available Synthesis of flavanoid compounds of chalcone and flavanone groups have been conducted. Flavanoid Is one of the group natural products which is mostly found in plants and have been proved to have physiological activity as drug. In this research, chalcone proup compounds that being synthesized are: chalcone, 3,4-dimethoxychalcone, 2'-hidroxy-3,4-dimethoxychalcone where as compound of flavanone group that being synthesized is 3',4'-dimethoxyflavanone. The synthesis of chalcone group are carried out based on Claisen-Schmidt reaction by using raw material of aromatic aldehydes and aromatic ketones. The synthesis in carried out by stirring at the room temperature using alkali solution as catalyst and ethanol as solvent. The synthesis of 3',4'-dimethoxyflanone is made based on the nucleophilic 1,4 addition of the unsaturated α,β ketone. The synthesis is made by refluxing 2'-hydroxy-3,4-dimethoxychalcone in alkali condition for 12 hours. The identification of flavanoid compound is carried out by using spectroscopic IR, GC-MS and 1H-NMR methods. The result of each synthesis chalcone group are follows: chalcone as yellowish solid with m.p= 50 °C and the yield is 83.39%; 3,4-dimethoxychalcone as yellow solid with m.p= 57°C and the yield is 76.00% ; 2'-hydroxy-3,4-dimethoxychalcone as orange solid with m.p= 90 °C and the yield is 74.29%, for 3',4'-dimethoxyflavanone as pale yellow solid with m.p= 80 °C and the yield is 72.00%.

Activity and selectivity regulation of synthesis gas reaction over supported ruthenium catalysts

Energy Technology Data Exchange (ETDEWEB)

Fujimoto, K; Nobusawa, T; Fukushima, T; Tominaga, H

1985-01-01

The catalytic activities of supported ruthenium for synthesis-gas conversion to hydrocarbons was found to be in the following order: TiOS > Nb2O3 > ZrO2 > SiO2 > Ta2O5 > Al2O3 > V2O5 > MoO3 > WO3 > MnO2 > ZnO. Turnover frequencies of the supported ruthenium increased with decrease in dispersion of the metal particles for every carrier material. Even the activities per unit weight of metals were higher for low-dispersion ruthenium of Al2O3, TiO2, and ZrO2. The chain-growth probability of a hydrocarbon product, which is characterized by the Schulz-Flory distribution, increased markedly with decrease in the metal dispersion irrespective of the carrier material. The catalytic activity of ruthenium particles with a dispersed ruthenium increased almost linearly with an increase in reaction pressure (up to at least 2.0 MPa). 23 references, 10 figures, 3 tables.

Lithium-ion transport in inorganic solid state electrolyte

International Nuclear Information System (INIS)

Gao Jian; Li Hong; Zhao Yu-Sheng; Shi Si-Qi

2016-01-01

An overview of ion transport in lithium-ion inorganic solid state electrolytes is presented, aimed at exploring and designing better electrolyte materials. Ionic conductivity is one of the most important indices of the performance of inorganic solid state electrolytes. The general definition of solid state electrolytes is presented in terms of their role in a working cell (to convey ions while isolate electrons), and the history of solid electrolyte development is briefly summarized. Ways of using the available theoretical models and experimental methods to characterize lithium-ion transport in solid state electrolytes are systematically introduced. Then the various factors that affect ionic conductivity are itemized, including mainly structural disorder, composite materials and interface effects between a solid electrolyte and an electrode. Finally, strategies for future material systems, for synthesis and characterization methods, and for theory and calculation are proposed, aiming to help accelerate the design and development of new solid electrolytes. (topical review)

Hydrothermal synthesis of layered iron-chalcogenide superconductors and related compounds

International Nuclear Information System (INIS)

Pachmayr, Ursula Elisabeth

2017-01-01

This thesis provides a new preparative approach to iron-chalcogenide based superconductors. The hydrothermal synthesis of anti-PbO type FeSe, which can be seen as basis structure of the compounds of interest was successfully developed. Along with this, some insights regarding the influence of synthesis parameters were gained featuring a basis for further hydrothermal syntheses of new iron-chalcogenide compounds. The potential of this method, primarily the extension of the so far limited accessibility of iron-chalcogenide based superconductors by solid-state sythesis, was revealed within the present work. The solid-solution FeSe_1_-_xS_x was prepared for the whole substitution range, whereas solid-state synthesis exhibits a solubility limit at x = 0.3. Furthermore, the new compounds [(Li_0_._8Fe_0_._2)OH]FeX (X = Se, S) were synthesized which are exclusively accessible via hydrothermal method. The compounds, where layers of (Li_0_._8Fe_0_._2)OH alternate with FeX layers, feature exceptional physical properties, notably a coexistence of superconductivity and ferromagnetism. They were intensively studied within this work. By combination of solid-state and hydrothermal ion-exchange synthesis even large crystals necessary for subsequent physical measurements are accessible. Apart from these layered iron-chalcogenide superconductors, further compounds which likewise exhibit building blocks of edge-sharing FeSe_4 tetrahedra were found via this synthesis method. The iron selenides A_2Fe_4Se_6 (A = K, Rb, Cs) consist of double chains of [Fe_2Se_3]"1"-, whereas a new compound Na_6(H_2O)_1_8Fe_4Se_8 exhibits [Fe_4Se_8]"6"- 'stella quadrangula' clusters. This structural diversity as well as the associated physical properties of the compounds demonstrates the numerous capabilities of hydrothermal synthesis in the field of iron-chalcogenide compounds. In particular with regard to iron-chalcogenide based superconductors this synthesis strategy is encouraging. It seems probable

Hydrothermal synthesis of layered iron-chalcogenide superconductors and related compounds

Energy Technology Data Exchange (ETDEWEB)

Pachmayr, Ursula Elisabeth

2017-04-06

This thesis provides a new preparative approach to iron-chalcogenide based superconductors. The hydrothermal synthesis of anti-PbO type FeSe, which can be seen as basis structure of the compounds of interest was successfully developed. Along with this, some insights regarding the influence of synthesis parameters were gained featuring a basis for further hydrothermal syntheses of new iron-chalcogenide compounds. The potential of this method, primarily the extension of the so far limited accessibility of iron-chalcogenide based superconductors by solid-state sythesis, was revealed within the present work. The solid-solution FeSe{sub 1-x}S{sub x} was prepared for the whole substitution range, whereas solid-state synthesis exhibits a solubility limit at x = 0.3. Furthermore, the new compounds [(Li{sub 0.8}Fe{sub 0.2})OH]FeX (X = Se, S) were synthesized which are exclusively accessible via hydrothermal method. The compounds, where layers of (Li{sub 0.8}Fe{sub 0.2})OH alternate with FeX layers, feature exceptional physical properties, notably a coexistence of superconductivity and ferromagnetism. They were intensively studied within this work. By combination of solid-state and hydrothermal ion-exchange synthesis even large crystals necessary for subsequent physical measurements are accessible. Apart from these layered iron-chalcogenide superconductors, further compounds which likewise exhibit building blocks of edge-sharing FeSe{sub 4} tetrahedra were found via this synthesis method. The iron selenides A{sub 2}Fe{sub 4}Se{sub 6} (A = K, Rb, Cs) consist of double chains of [Fe{sub 2}Se{sub 3}]{sup 1-}, whereas a new compound Na{sub 6}(H{sub 2}O){sub 18}Fe{sub 4}Se{sub 8} exhibits [Fe{sub 4}Se{sub 8}]{sup 6-} 'stella quadrangula' clusters. This structural diversity as well as the associated physical properties of the compounds demonstrates the numerous capabilities of hydrothermal synthesis in the field of iron-chalcogenide compounds. In particular with regard

NAA-modified DNA oligonucleotides with zwitterionic backbones: stereoselective synthesis of A-T phosphoramidite building blocks.

Science.gov (United States)

Schmidtgall, Boris; Höbartner, Claudia; Ducho, Christian

2015-01-01

Modifications of the nucleic acid backbone are essential for the development of oligonucleotide-derived bioactive agents. The NAA-modification represents a novel artificial internucleotide linkage which enables the site-specific introduction of positive charges into the otherwise polyanionic backbone of DNA oligonucleotides. Following initial studies with the introduction of the NAA-linkage at T-T sites, it is now envisioned to prepare NAA-modified oligonucleotides bearing the modification at X-T motifs (X = A, C, G). We have therefore developed the efficient and stereoselective synthesis of NAA-linked 'dimeric' A-T phosphoramidite building blocks for automated DNA synthesis. Both the (S)- and the (R)-configured NAA-motifs were constructed with high diastereoselectivities to furnish two different phosphoramidite reagents, which were employed for the solid phase-supported automated synthesis of two NAA-modified DNA oligonucleotides. This represents a significant step to further establish the NAA-linkage as a useful addition to the existing 'toolbox' of backbone modifications for the design of bioactive oligonucleotide analogues.

Preliminary Electrochemical Characterization of Anode Supported Solid Oxide Cell (AS-SOC) Produced in the Institute of Power Engineering Operated in Electrolysis Mode (SOEC)

Science.gov (United States)

Kupecki, Jakub; Motyliński, Konrad; Skrzypkiewicz, Marek; Wierzbicki, Michał; Naumovich, Yevgeniy

2017-12-01

The article discusses the operation of solid oxide electrochemical cells (SOC) developed in the Institute of Power Engineering as prospective key components of power-to-gas systems. The fundamentals of the solid oxide cells operated as fuel cells (SOFC - solid oxide fuel cells) and electrolysers (SOEC - solid oxide fuel cells) are given. The experimental technique used for electrochemical characterization of cells is presented. The results obtained for planar cell with anodic support are given and discussed. Based on the results, the applicability of the cells in power-to-gas systems (P2G) is evaluated.

Optimisation of the synthesis of vancomycin-selective molecularly imprinted polymer nanoparticles using automatic photoreactor

OpenAIRE

Muzyka, Kateryna; Karim, Khalku; Guerreiro, Antonio; Poma, Alessandro; Piletsky, Sergey

2014-01-01

A novel optimized protocol for solid-state synthesis of molecularly imprinted polymer nanoparticles (nanoMIPs) with specificity for antibiotic vancomycin is described. The experimental objective was optimization of the synthesis parameters (factors) affecting the yield of obtained nanoparticles which have been synthesized using the first prototype of an automated solid-phase synthesizer. Applications of experimental design (or design of experiments) in optimization of nanoMIP yield were carri...

Solid state synthesis and structural refinement of polycrystalline ...

Indian Academy of Sciences (India)

Unknown

This makes them a potential material for nuclear waste management in synthetic ... solid solution of lanthanum substituted calcium titanate. The SEM and EDAX .... symmetry operations to complete the coverage (figure 3). The plots are square ...

Peptide Macrocycles Featuring a Backbone Secondary Amine: A Convenient Strategy for the Synthesis of Lipidated Cyclic and Bicyclic Peptides on Solid Support

DEFF Research Database (Denmark)

Oddo, Alberto; Münzker, Lena; Hansen, Paul Robert

2015-01-01

A convenient strategy for the on-resin synthesis of macrocyclic peptides (3- to 13-mers) via intramolecular halide substitution by a diamino acid is described. The method is compatible with standard Fmoc/tBu SPPS and affords a tail-to-side-chain macrocyclic peptide featuring an endocyclic secondary...

Synthesis and Characterization of Zeolite Na−Y and Its Conversion to the Solid Acid Zeolite H−Y

DEFF Research Database (Denmark)

Warner, Terence Edwin; Galsgaard Klokker, Mads; Nielsen, Ulla Gro

2017-01-01

Zeolite Y has an iconic crystal structure, but more importantly, the hydrogen modification zeolite H−Y is the classic example of a solid acid which is used extensively as a catalyst in the oil industry. This metastable compound cannot be synthesized directly, which creates an opportunity to discuss...... various preparative strategies with the students, such as the three-stage procedure described here. Stage I concerns the hydrothermal synthesis of zeolite Na−Y, followed by ion-exchange with an ammonium acetate solution to form zeolite NH4−Y, and the latter is subsequently converted to zeolite H......−Y by thermolysis. Stages II and III may instead be performed using commercially available zeolites, Na−Y and NH4−Y, respectively, which shifts the learning objectives to structural characterization of zeolites. The characterization of the product and intermediate materials gives the students a practical insight...

Photocatalytic Properties of Nb/MCM-41 Molecular Sieves: Effect of the Synthesis Conditions

Directory of Open Access Journals (Sweden)

Caterine Daza Gomez

2015-08-01

Full Text Available The effect of synthesis conditions and niobium incorporation levels on the photocatalytic properties of Nb/MCM-41 molecular sieves was assessed. Niobium pentoxide supported on MCM-41 mesoporous silica was obtained using two methods: sol-gel and incipient impregnation, in each case also varying the percentage of niobium incorporation. The synthesized Nb-MCM-41 ceramic powders were characterized using the spectroscopic techniques of infrared spectroscopy (IR, Raman spectroscopy, X-ray diffraction (XRD, and transmission electron microscopy (TEM. The photodegradation capacity of the powders was studied using the organic molecule, methylene blue. The effect of both the method of synthesis and the percentage of niobium present in the sample on the photodegradation action of the solids was determined. The mesoporous Nb-MCM-41 that produced the greatest photodegradation response was obtained using the sol-gel method and 20% niobium incorporation.

On-bead chemical synthesis and display of phosphopeptides for affinity pull-down proteomics

DEFF Research Database (Denmark)

Malene, Brandt; Madsen, Jens C.; Bunkenborg, Jakob

2006-01-01

We describe a new method for phosphopeptide proteomics based on the solid-phase synthesis of phosphopeptides on beads suitable for affinity pull-down experiments. Peptide sequences containing the Bad Ser112 and Ser136 phosphorylation motifs were used as bait in affinity pull-down experiments...... (aldehyde) at the C terminus for potential activity-based proteomics. The synthetic support-bound Bad phosphopeptides were able to pull down 14-3-3zeta. Furthermore, Bad phosphopeptides bound endogenous 14-3-3 proteins, and all seven members of the 14-3-3 family were identified by mass spectrometry....... In control experiments, none of the unphosphorylated Bad peptides bound transfected 14-3-3zeta or endogenous 14-3-3. We conclude that the combined synthesis and display of phosphopeptides on-bead is a fast and efficient method for affinity pull-down proteomics....

Evidence for H2/D2 isotope effects on Fischer-Tropsch synthesis over supported ruthenium catalysts

International Nuclear Information System (INIS)

Kellner, C.S.; Bell, A.T.

1981-01-01

The effects of using D 2 rather than H 2 during Fischer-Tropsch synthesis were investigated using alumina- and silica-supported Ru catalysts. For the alumina-supported catalysts, the rate of CD 4 formation was 1.4 to 1.6 times faster than the formation of CH 4 . A noticeable isotope effect was also observed for higher molecular weight products. The magnitude of the isotope effects observed using the silica-supported catalyst was much smaller than that found using the alumina-supported catalysts. The formation of olefins relative to paraffins was found to be higher when H 2 rather than D 2 was used, independent of the catalyst support. The observed isotope effects are explained in terms of a mechanism for CO hydrogenation and are shown to arise from a complex combination of the kinetic and equilibrium isotope effects associated with elementary processes occurring on the catalyst surface

Synthesis and bioactive evaluations of novel benzotriazole ...

Indian Academy of Sciences (India)

Synthesis and bioactive evaluations of novel benzotriazole compounds as ... School of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715, .... −3 mol/L) was prepared by dissolving its solid in doubly distilled water.

Synthesis and characterization of type solid solution in the binary ...

Indian Academy of Sciences (India)

We have investigated Bi2O3–Eu2O3 binary system by doping with Eu2O3 in the composition range from 1 to 10 mole% via solid state reactions and succeeded to stabilize -Bi2O3 ... Our experimental observations strongly suggested that oxygen deficiency type non-stoichiometry is present in doped type solid solutions.

Core-Shell Diamond as a Support for Solid-Phase Extraction and High-Performance Liquid Chromatography

Energy Technology Data Exchange (ETDEWEB)

Saini, Gaurav; Jensen, David S.; Wiest, Landon A.; Vail, Michael A.; Dadson, Andrew; Lee, Milton L.; Shutthanandan, V.; Linford, Matthew R.

2010-06-01

We report the formation of core-shell diamond particles for solid phase extraction (SPE) and high performance liquid chromatography (HPLC) made by layer-by-layer (LbL) deposition. Their synthesis begins with the amine functionalization of microdiamond by its immersion in an aqueous solution of a primary amine-containing polymer (polyallylamine (PAAm)). The amine-terminated microdiamond is then immersed in an aqueous suspension of nanodiamond, which leads to adsorption of the nanodiamond. Alternating (self-limiting) immersions in the solutions of the amine-containing polymer and the suspension of nanodiamond are continued until the desired number of nanodiamond layers is formed around the microdiamond. Finally, the core-shell particles are cross-linked with 1,2,5,6-diepoxycyclooctane or reacted with 1,2-epoxyoctadecane. Layer-by-layer deposition of PAAm and nanodiamond is also studied on planar Si/SiO2 surfaces, which were characterized by SEM, Rutherford backscattering spectrometry (RBS) and nuclear reaction analysis (NRA). Core-shell particles are characterized by diffuse reflectance infrared Fourier transform spectroscopy (DRIFT), environmental scanning electron microscopy (ESEM), and Brunauer Emmett Teller (BET) surface area and pore size measurements. Larger (ca. 50 μm) core-shell diamond particles have much higher surface areas, and analyte loading capacities in SPE than nonporous solid diamond particles. Smaller (ca. 3 μm), normal and reversed phase, core-shell diamond particles have been used for HPLC, with 36,300 plates per meter for mesitylene in a separation of benzene and alkyl benzenes on a C18 adsorbent, and 54,800 plates per meter for diazinon in a similar separation of two pesticides.

Core-shell diamond as a support for solid-phase extraction and high-performance liquid chromatography.

Science.gov (United States)

Saini, Gaurav; Jensen, David S; Wiest, Landon A; Vail, Michael A; Dadson, Andrew; Lee, Milton L; Shutthanandan, V; Linford, Matthew R

2010-06-01

We report the formation of core-shell diamond particles for solid-phase extraction (SPE) and high-performance liquid chromatography (HPLC) made by layer-by-layer (LbL) deposition. Their synthesis begins with the amine functionalization of microdiamond by its immersion in an aqueous solution of a primary amine-containing polymer (polyallylamine (PAAm)). The amine-terminated microdiamond is then immersed in an aqueous suspension of nanodiamond, which leads to adsorption of the nanodiamond. Alternating (self-limiting) immersions in the solutions of the amine-containing polymer and the suspension of nanodiamond are continued until the desired number of nanodiamond layers is formed around the microdiamond. Finally, the core-shell particles are cross-linked with 1,2,5,6-diepoxycyclooctane or reacted with 1,2-epoxyoctadecane. Layer-by-layer deposition of PAAm and nanodiamond is also studied on planar Si/SiO(2) surfaces, which were characterized by scanning electron microscopy (SEM), Rutherford backscattering spectrometry (RBS), and nuclear reaction analysis (NRA). Core-shell particles are characterized by diffuse reflectance infrared Fourier transform spectroscopy (DRIFT), environmental scanning electron microscopy (ESEM), and Brunauer-Emmett-Teller (BET) surface area and pore size measurements. Larger (ca. 50 microm) core-shell diamond particles have much higher surface areas and analyte loading capacities in SPE than nonporous solid diamond particles. Smaller (ca. 3 microm), normal and reversed-phase, core-shell diamond particles have been used for HPLC, with 36,300 plates/m for mesitylene in a separation of benzene and alkyl benzenes and 54,800 plates/m for diazinon in a similar separation of two pesticides on a C(18) adsorbent.

Core-Shell Diamond as a Support for Solid-Phase Extraction and High-Performance Liquid Chromatography

International Nuclear Information System (INIS)

Saini, Gaurav; Jensen, David S.; Wiest, Landon A.; Vail, Michael A.; Dadson, Andrew; Lee, Milton L.; Shutthanandan, V.; Linford, Matthew R.

2010-01-01

We report the formation of core-shell diamond particles for solid phase extraction (SPE) and high performance liquid chromatography (HPLC) made by layer-by-layer (LbL) deposition. Their synthesis begins with the amine functionalization of microdiamond by its immersion in an aqueous solution of a primary amine-containing polymer (polyallylamine (PAAm)). The amine-terminated microdiamond is then immersed in an aqueous suspension of nanodiamond, which leads to adsorption of the nanodiamond. Alternating (self-limiting) immersions in the solutions of the amine-containing polymer and the suspension of nanodiamond are continued until the desired number of nanodiamond layers is formed around the microdiamond. Finally, the core-shell particles are cross-linked with 1,2,5,6-diepoxycyclooctane or reacted with 1,2-epoxyoctadecane. Layer-by-layer deposition of PAAm and nanodiamond is also studied on planar Si/SiO2 surfaces, which were characterized by SEM, Rutherford backscattering spectrometry (RBS) and nuclear reaction analysis (NRA). Core-shell particles are characterized by diffuse reflectance infrared Fourier transform spectroscopy (DRIFT), environmental scanning electron microscopy (ESEM), and Brunauer Emmett Teller (BET) surface area and pore size measurements. Larger (ca. 50 ?m) core-shell diamond particles have much higher surface areas, and analyte loading capacities in SPE than nonporous solid diamond particles. Smaller (ca. 3 ?m), normal and reversed phase, core-shell diamond particles have been used for HPLC, with 36,300 plates per meter for mesitylene in a separation of benzene and alkyl benzenes on a C18 adsorbent, and 54,800 plates per meter for diazinon in a similar separation of two pesticides.

The Synthesis of cis- and trans-Fused Bicyclic Sugar Amino Acids

NARCIS (Netherlands)

Risseeuw, Martijn D.P.; Grotenbreg, Gijsbert M.; Witte, Martin D.; Tuin, Adriaan W.; Leeuwenburgh, Michiel A.; Marel, Gijsbert A. van der; Overkleeft, Herman S.; Overhand, Mark

2006-01-01

Four isomeric bicyclic sugar amino acids (SAAs) were prepared from an α-acetylenic-C-glucoside by employing a Petasis olefination and a ring-closing metathesis (RCM) as key steps. The applicability of the resulting SAAs in solid-phase peptide synthesis was demonstrated by the synthesis of a

1H MAS NMR (magic-angle spinning nuclear magnetic resonance) techniques for the quantitative determination of hydrogen types in solid catalysts and supports.

Science.gov (United States)

Kennedy, Gordon J; Afeworki, Mobae; Calabro, David C; Chase, Clarence E; Smiley, Randolph J

2004-06-01

Distinct hydrogen species are present in important inorganic solids such as zeolites, silicoaluminophosphates (SAPOs), mesoporous materials, amorphous silicas, and aluminas. These H species include hydrogens associated with acidic sites such as Al(OH)Si, non-framework aluminum sites, silanols, and surface functionalities. Direct and quantitative methodology to identify, measure, and monitor these hydrogen species are key to monitoring catalyst activity, optimizing synthesis conditions, tracking post-synthesis structural modifications, and in the preparation of novel catalytic materials. Many workers have developed several techniques to address these issues, including 1H MAS NMR (magic-angle spinning nuclear magnetic resonance). 1H MAS NMR offers many potential advantages over other techniques, but care is needed in recognizing experimental limitations and developing sample handling and NMR methodology to obtain quantitatively reliable data. A simplified approach is described that permits vacuum dehydration of multiple samples simultaneously and directly in the MAS rotor without the need for epoxy, flame sealing, or extensive glovebox use. We have found that careful optimization of important NMR conditions, such as magnetic field homogeneity and magic angle setting are necessary to acquire quantitative, high-resolution spectra that accurately measure the concentrations of the different hydrogen species present. Details of this 1H MAS NMR methodology with representative applications to zeolites, SAPOs, M41S, and silicas as a function of synthesis conditions and post-synthesis treatments (i.e., steaming, thermal dehydroxylation, and functionalization) are presented.

Highly durable anode supported solid oxide fuel cell with an infiltrated cathode

DEFF Research Database (Denmark)

Samson, Alfred Junio; Hjalmarsson, Per; Søgaard, Martin

2012-01-01

An anode supported solid oxide fuel cell with an La0.6Sr0.4Co1.05O3_δ (LSC) infiltrated-Ce0.9Gd0.1O1.95 (CGO) cathode that shows a stable performance has been developed. The cathode was prepared by screen printing a porous CGO backbone on top of a laminated and co-fired anode supported half cell...... was tested at 700 deg. C under a current density of 0.5 A cm-2 for 1500 h using air as oxidant and humidified hydrogen as fuel. The electrochemical performance of the cell was analyzed by impedance spectroscopy and current evoltage relationships. No measurable degradation in the cell voltage or increase...... in the resistance from the recorded impedance was observed during long term testing. The power density reached 0.79Wcm-2 at a cell voltage of 0.6 V at 750 deg. C. Post test analysis of the LSC infiltrated-CGO cathode by scanning electron microscopy revealed no significant micro-structural difference...

Influence of the Synthesis Method for Pt Catalysts Supported on Highly Mesoporous Carbon Xerogel and Vulcan Carbon Black on the Electro-Oxidation of Methanol

Directory of Open Access Journals (Sweden)

Cinthia Alegre

2015-03-01

Full Text Available Platinum catalysts supported on carbon xerogel and carbon black (Vulcan were synthesized with the aim of investigating the influence of the characteristics of the support on the electrochemical performance of the catalysts. Three synthesis methods were compared: an impregnation method with two different reducing agents, sodium borohydride and formic acid, and a microemulsion method, in order to study the effect of the synthesis method on the physico-chemical properties of the catalysts. X-ray diffraction and transmission electron microscopy were applied. Cyclic voltammetry and chronoamperometry were used for studying carbon monoxide and methanol oxidation. Catalysts supported on carbon xerogel presented higher catalytic activities towards CO and CH3OH oxidation than catalysts supported on Vulcan. The higher mesoporosity of carbon xerogel was responsible for the favored diffusion of reagents towards catalytic centers.

Preparation and characterization of bismuth ruthenate pyrochlore via solid state reaction and sol-gel methods

Directory of Open Access Journals (Sweden)

Mayuree Sansernnivet

2010-01-01

Full Text Available Bismuth ruthenate pyrochlores, potential cathode materials for intermediate temperature solid oxide fuel cells(ITSOFCs, were prepared via solid-state and sol-gel method. Effects of the preparation routes and conditions on the phase and microstructures of the materials were investigated in this study using XRD and SEM. The study showed that the preparation method and the adding sequence of the starting meterials have a significant effect on the crystal phase and the particle size obtained. Sol-gel synthesis could yield a material with only pyrochlore structure, i.e. Bi2Ru2O7, while the solid state method yielded powder with a small amount of the secondary RuO2 phase. The sol-gel synthesis resulted in materialswith a finer particle size (~0.3-1.0 μm compared to powder synthesized via the solid state reaction method.

Mixed and Doped Solid Sorbents for CO₂ Capture Applications

Energy Technology Data Exchange (ETDEWEB)

Duan, Yuhua [National Energy Technology Lab. (NETL), Albany, OR (United States)

2016-06-14

The objectives of this presentation are to capture CO2 we need materials with optimal performance and low costs; establish a theoretical procedure to identify most potential candidates of CO₂ solid sorbents from a large solid material databank; computational synthesis new materials to fit industrial needs; and explore the optimal working conditions for the promised CO₂ solid sorbents, especially from room to warm T ranges with optimal energy usage.

Study on the effect of the metal–support (Fe-MgO and Pt-MgO) interaction in alcohol-CVD synthesis of carbon nanotubes

International Nuclear Information System (INIS)

Steplewska, Anna; Borowiak-Palen, Ewa

2011-01-01

This study presents the effect of the metal–support interaction in two systems: (1) iron particle, and (2) platinum particles, being supported on magnesium oxide (MgO) nanopowder in alcohol-CVD process for carbon nanotubes (CNTs) growth. The employment of the different metals but the same substrate (with equal molar ratio) resulted in the synthesis of single-walled CNTs (SWCNTs) or double-walled CNTs (DWCNTs), using iron and platinum, respectively. Furthermore, along with the prolongation of the process time, the decrease of the mean nanotubes diameter in case of iron-catalyzed materials was detected. Interestingly, the extention of the growth time in the synthesis using Pt/MgO resulted in the synthesis of the thicker mean nanotubes diameter. However, for both applied catalytic systems the reduction of the diameter distribution of the tubes and the increase of relative purity of the samples upon the growth time increase were detected.

Study on the effect of the metal-support (Fe-MgO and Pt-MgO) interaction in alcohol-CVD synthesis of carbon nanotubes

Energy Technology Data Exchange (ETDEWEB)

Steplewska, Anna, E-mail: asteplewska@zut.edu.pl; Borowiak-Palen, Ewa [West Pomeranian University of Technology, Centre of Knowledge Based Nanomaterials and Technologies, Institute of Chemical and Environment Engineering (Poland)

2011-05-15

This study presents the effect of the metal-support interaction in two systems: (1) iron particle, and (2) platinum particles, being supported on magnesium oxide (MgO) nanopowder in alcohol-CVD process for carbon nanotubes (CNTs) growth. The employment of the different metals but the same substrate (with equal molar ratio) resulted in the synthesis of single-walled CNTs (SWCNTs) or double-walled CNTs (DWCNTs), using iron and platinum, respectively. Furthermore, along with the prolongation of the process time, the decrease of the mean nanotubes diameter in case of iron-catalyzed materials was detected. Interestingly, the extention of the growth time in the synthesis using Pt/MgO resulted in the synthesis of the thicker mean nanotubes diameter. However, for both applied catalytic systems the reduction of the diameter distribution of the tubes and the increase of relative purity of the samples upon the growth time increase were detected.

Synthesis of f metal coordination polymers: properties and conversion into inorganic solids

International Nuclear Information System (INIS)

Demars, Thomas

2012-01-01

Coordination polymers (CP) are of great academic and industrial interest due to flexible structure and composition and offer prospects for original chemical (catalysis, soft-hard materials conversion..) and physical properties (magnetism, optics..). The major interest of these studies is to check the transfer of the structure, meso-structure and composition from the CP to the ceramic via a thermal treatment. In this context, this thesis describes studies on conversion of coordination polymers obtained by self-assembly of 4f and 5f metal ions with 2,5-dihydroxy-1,4-benzoquinone (DHBQ). Aqueous and anhydrous synthetic ways were developed, which yielded different kinds of CPs (4f, 4f-4f, 4f-5f); solid solutions were obtained with the mixed compounds. The products were characterized and their behaviour under thermal treatment was studied. The main results show that the DHBQ-based precursors obtained by aqueous way have a micrometric meso-structure, formed by the assembly of micro-crystalline subunits which all posses the same crystallographic structure. The study of the assembly of the meso-structure allowed controlling the morphology of the elementary grain (cylinder, cube, disk...) with very good size distribution. The implementation of anhydrous systems in a controlled atmosphere allowed yielded a wider range of micro-structural parameters (surface area, porosity...). For all CP-type compounds, the thermal conversion to ceramic has barely altered the morphology of the materials. The microstructural aspects could be controlled via the method of synthesis. (author) [fr

Solid phase assays

International Nuclear Information System (INIS)

Reese, M.G.; Johnson, L.R.; Ransom, D.K.

1980-01-01

In a solid phase assay for quantitative determination of biological and other analytes, a sample such as serum is contacted with a receptor for the analyte being assayed, the receptor being supported on a solid support. No tracer for the analyte is added to the sample before contacting with the receptor; instead the tracer is contacted with the receptor after unbound analyte has been removed from the receptor. The assay can be otherwise performed in a conventional manner but can give greater sensitivity. (author)

Type synthesis and preliminary design of devices supporting lower limb's rehabilitation.

Science.gov (United States)

Olinski, Michał; Lewandowski, Bogusz; Gronowicz, Antoni

2015-01-01

Based on the analysis of existing solutions, biomechanics of human lower limbs and anticipated applications, results of con- siderations concerning the necessary number of degrees of freedom for the designed device supporting rehabilitation of lower extremities are presented. An analysis was carried out in order to determine the innovative kinematic structure of the device, ensuring sufficient mobility and functionality while minimizing the number of degrees of freedom. With the aid of appropriate formalised meth- ods, for instance, type synthesis, a complete variety of solutions for leg joints were obtained in the form of basic and kinematic schemes, having the potential to find application in devices supporting lower limb rehabilitation. A 3D model of ankle joint module was built in Autodesk Inventor System, then imported to Adams and assembled into a moving numerical model of a mechanism. Several conducted simulations resulted in finding the required maximum stroke of the cylinders. A comparison of the angular ranges of ankle joint and similar devices with the ones achieved by the designed device indicated a sufficient reserve allowing not only movements typical of gait, but approximately achieving the passive range of motion for the ankle joint.

Synthesis of nanoparticles and nanomaterials biological approaches

CERN Document Server

Abdullaeva, Zhypargul

2017-01-01

This book covers biological synthesis approaches for nanomaterials and nanoparticles, including introductory material on their structure, phase compositions and morphology, nanomaterials chemical, physical, and biological properties. The chapters of this book describe in sequence the synthesis of various nanoparticles by microorganisms, bacteria, yeast, algae, and actynomycetes; plant and plant extract-based synthesis; and green synthesis methods. Each chapter provides basic knowledge on the synthesis of nanomaterials, defines fundamental terms, and aims to build a solid foundation of knowledge, followed by explanations, examples, visual photographs, schemes, tables and illustrations. Each chapter also contains control questions, problem drills, as well as case studies that clarify theory and the explanations given in the text. This book is ideal for researchers and advanced graduate students in materials engineering, biotechnology, and nanotechnology fields. As a reference book this work is also appropriate ...

On the Synthesis of Carbon Nanotubes from Waste Solid Hydrocarbons

Science.gov (United States)

Zhuo, Chuanwei

Carbon nanotubes (CNTs) are allotropes of carbon with a cylindrical nanostructure. They consist of coaxial tubular graphene sheets, with diameters in the order of nanometers (1 x 10-9 m) and lengths in the order of micrometers (1 x 10-6 m). The latter can now be extended into the order of meters. Carbon nanotubes (CNTs) have been studied for more than 20 years. CNTs possess superior electrical, mechanical, thermal, chemical, and structural properties, which make their potential applications nowadays overwhelmingly widespread. Now entering into the growth phase of product life cycle, increasing usage of CNTs in commercial products is part of the beginning of the nano-technological revolution. Expanding markets for CNTs' large volume applications place ever-increasing demands on lowering their production costs to the level acceptable by the end-user applications. It is estimated that the mass application of CNTs will be facilitated only when the price of CNTs approaches that of conductive carbon black. The synthesis of CNTs involves three elements: the carbonaceous feedstocks (raw materials), the catalysts, and the necessary process power consumption. Therefore, they jointly contribute to the major operation expenditures in CNT synthesis/production. Current technologies for large-scale production of CNTs (either chemical vapor deposition, CVD, or combustion synthesis) require intensive consumption of premium feedstocks and catalysts, and the CVD process requires high energy consumption. Therefore, there is a pressing need for resource-benign and energy-benign, cost-effective nano-manufacturing processes. In the search for sustainable alternatives, it would be prudent to explore renewable and/or replenishable low-cost feedstocks, such as those found in municipal, industrial, and agricultural recycling streams. In the search for low cost catalysts, stainless steels have been proposed as cost-effective dual purpose substrates and catalysts, as they contain transition

Accelerated creep in solid oxide fuel cell anode supports during reduction

DEFF Research Database (Denmark)

Frandsen, Henrik Lund; Makowska, Malgorzata Grazyna; Greco, Fabio

2016-01-01

To evaluate the reliability of solid oxide fuel cell (SOFC) stacks during operation, the stress field in the stack must be known. During operation the stress field will depend on time as creep processes relax stresses. The creep of reduced Ni-YSZ anode support at operating conditions has been...... studied previously. In this work a newly discovered creep phenomenon taking place during the reduction is reported. This relaxes stresses at a much higher rate (∼ x104) than creep during operation. The phenomenon was studied both in three-point bending and uniaxial tension. Differences between the two...... measurements could be explained by newly observed stress promoted reduction. Finally, samples exposed to a small tensile stress (∼ 0.004 MPa) were observed to expand during reduction, which is in contradiction to previous literature. These observations suggest that release of internal residual stresses between...

Creep behaviour of porous metal supports for solid oxide fuel cells

DEFF Research Database (Denmark)

Boccaccini, Dino; Frandsen, Henrik Lund; Sudireddy, Bhaskar Reddy

2014-01-01

The creep behaviour of porous ironechromium alloy used as solid oxide fuel cell support was investigated, and the creep parameters are compared with those of dense strips of similar composition under different testing conditions. The creep parameters were determined using a thermo......-mechanical analyser with applied stresses in the range from 1 to 15 MPa and temperatures between 650 and 800 _C. The GibsoneAshby and Mueller models developed for uniaxial creep of open-cell foams were used to analyse the results. The influence of scale formation on creep behaviour was assessed by comparing the creep...... data for the samples tested in reducing and oxidising atmospheres. The influence of preoxidation on creep behaviour was also investigated. In-situ oxidation during creep experiments increases the strain rate while pre-oxidation of samples reduces it. Debonding of scales at high stress regime plays...

Synthesis of 6-Methyl-9-n-propyldibenzothiophene-4-ol

Energy Technology Data Exchange (ETDEWEB)

Eisenbraun, E.J.

1991-04-27

The material covered here can be divided into 3 parts: large-scale synthesis of 200+ grams of distilled 1,4-diethyl-2-[(2'- methoxyphenyl)thio]benzene, synthesis of sulfones both as starting materials for chemical cyclization reactions and as solid derivatives for identification purposes, and continued investigation of the cyclization to dibenzothiophenes both by chemical and photochemical means. 5 refs, figs.

SUPPORTING INFORMATION Transition metal-promoted synthesis ...

Indian Academy of Sciences (India)

takahashi

v) MR: BUCHI Corporation M-565 instrument for identify melting range of solid compounds. vi) Hazardous: All products are smelly compounds. General experimental procedure: Compounds a to r were prepared by following a general synthetic procedure in which the solution of. 1,4-dihydroquinazoline-2-thiol (100 mg, ...

Structural and Biochemical Characterization of Chlamydia trachomatis Hypothetical Protein CT263 Supports That Menaquinone Synthesis Occurs through the Futalosine Pathway*

Science.gov (United States)

Barta, Michael L.; Thomas, Keisha; Yuan, Hongling; Lovell, Scott; Battaile, Kevin P.; Schramm, Vern L.; Hefty, P. Scott

2014-01-01

The obligate intracellular human pathogen Chlamydia trachomatis is the etiological agent of blinding trachoma and sexually transmitted disease. Genomic sequencing of Chlamydia indicated this medically important bacterium was not exclusively dependent on the host cell for energy. In order for the electron transport chain to function, electron shuttling between membrane-embedded complexes requires lipid-soluble quinones (e.g. menaquionone or ubiquinone). The sources or biosynthetic pathways required to obtain these electron carriers within C. trachomatis are poorly understood. The 1.58Å crystal structure of C. trachomatis hypothetical protein CT263 presented here supports a role in quinone biosynthesis. Although CT263 lacks sequence-based functional annotation, the crystal structure of CT263 displays striking structural similarity to 5′-methylthioadenosine nucleosidase (MTAN) enzymes. Although CT263 lacks the active site-associated dimer interface found in prototypical MTANs, co-crystal structures with product (adenine) or substrate (5′-methylthioadenosine) indicate that the canonical active site residues are conserved. Enzymatic characterization of CT263 indicates that the futalosine pathway intermediate 6-amino-6-deoxyfutalosine (kcat/Km = 1.8 × 103 m−1 s−1), but not the prototypical MTAN substrates (e.g. S-adenosylhomocysteine and 5′-methylthioadenosine), is hydrolyzed. Bioinformatic analyses of the chlamydial proteome also support the futalosine pathway toward the synthesis of menaquinone in Chlamydiaceae. This report provides the first experimental support for quinone synthesis in Chlamydia. Menaquinone synthesis provides another target for agents to combat C. trachomatis infection. PMID:25253688

Thermal expansion studies on uranium-neodymium mixed oxide solid solutions

International Nuclear Information System (INIS)

Panneerselvam, G.; Venkata Krishnan, R.; Antony, M.P.; Nagarajan, K.

2012-01-01

Uranium-Neodymium mixed oxides solid solutions (U 1-y Nd y ) O 2 (y=0.2-0.95) were prepared by combustion synthesis using citric acid as fuel. Structural characterization and computation of lattice parameter was carried out from room temperature X-ray diffraction measurements. Single-phase fluorite structure was observed up to y=0.80. For solid solutions with y>0.80 additional Nd 2 O 3 lines were visible

Saponification of esters of chiral alpha-amino acids anchored through their amine function on solid support.

Science.gov (United States)

Cantel, Sonia; Desgranges, Stéphane; Martinez, Jean; Fehrentz, Jean-Alain

2004-06-01

Anchoring an alpha-amino acid residue by its amine function onto a solid support is an alternative to develop chemistry on its carboxylic function. This strategy can involve the use of amino-acid esters as precursors of the carboxylic function. A complete study on the Wang-resin was performed to determine the non racemizing saponification conditions of anchored alpha-amino esters. The use of LiOH, NaOH, NaOSi(Me)3, various solvents and temperatures were tested for this reaction. After saponification and cleavage from the support, samples were examined through their Marfey's derivatives by reversed phase HPLC to evaluate the percentage of racemization.

Construction of an Immobilized Thermophilic Esterase on Epoxy Support for Poly(ε-caprolactone Synthesis

Directory of Open Access Journals (Sweden)

Hui Ren

2016-06-01

Full Text Available Developing an efficient immobilized enzyme is of great significance for improving the operational stability of enzymes in poly(ε-caprolactone synthesis. In this paper, a thermophilic esterase AFEST from the archaeon Archaeoglobus fulgidus was successfully immobilized on the epoxy support Sepabeads EC-EP via covalent attachment, and the immobilized enzyme was then employed as a biocatalyst for poly(ε-caprolactone synthesis. The enzyme loading and recovered activity of immobilized enzyme was measured to be 72 mg/g and 10.4 U/mg using p-nitrophenyl caprylate as the substrate at 80 °C, respectively. Through the optimization of reaction conditions (enzyme concentration, temperature, reaction time and medium, poly(ε-caprolactone was obtained with 100% monomer conversion and low number-average molecular weight (Mn < 1300 g/mol. Further, the immobilized enzyme exhibited excellent reusability, with monomer conversion values exceeding 75% during 15 batch reactions. Finally, poly(ε-caprolactone was enzymatically synthesized with an isolated yield of 75% and Mn value of 3005 g/mol in a gram-scale reaction.

Recent Developments in the Site-Specific Immobilization of Proteins onto Solid Supports

Energy Technology Data Exchange (ETDEWEB)

Camarero, J A

2007-02-21

Immobilization of proteins onto surfaces is of great importance in numerous applications, including protein analysis, drug screening, and medical diagnostics, among others. The success of all these technologies relies on the immobilization technique employed to attach a protein to the corresponding surface. Non-specific physical adsorption or chemical cross-linking with appropriate surfaces results in the immobilization of the protein in random orientations. Site-specific covalent attachment, on the other hand, leads to molecules being arranged in a definite, orderly fashion and allows the use of spacers and linkers to help minimize steric hindrances between the protein and the surface. The present work reviews the latest chemical and biochemical developments for the site-specific covalent attachment of proteins onto solid supports.

Optimization of spin-coated electrodes for electrolyte-supported solid oxide fuel cells

International Nuclear Information System (INIS)

Nobrega, Shayenne Diniz da; Monteiro, Natalia Kondo; Tabuti, Francisco; Fonseca, Fabio Coral; Florio, Daniel Zanetti de

2017-01-01

Electrodes for electrolyte-supported solid oxide fuel cells (SOFC’s) were fabricated by spin coating. Strontium-doped lanthanum manganite (LSM) cathode and nickel yttria-stabilized zirconia cermet anodes were synthesized and processed for enhanced deposition conditions. The influence of electrode microstructural parameters was investigated by a systematic experimental procedure aiming at optimized electrochemical performance of single cells. Polarization curves showed a strong dependence on both electrode thickness and sintering temperature. By a systematic control of such parameters, the performance of single cells was significantly enhanced due to decreasing of polarization resistance from 26 Ω cm² to 0.6 Ω cm² at 800°C. The results showed that spin-coated electrodes can be optimized for fast and cost effective fabrication of SOFCs. (author)

Optimization of spin-coated electrodes for electrolyte-supported solid oxide fuel cells

Energy Technology Data Exchange (ETDEWEB)

Nobrega, Shayenne Diniz da; Monteiro, Natalia Kondo; Tabuti, Francisco; Fonseca, Fabio Coral, E-mail: shaynnedn@hotmail.com, E-mail: nataliakm@usp.br, E-mail: fntabuti@ipen.br, E-mail: fabiocf@usp.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN-CNEN/SP), Sao Paulo, SP (Brazil); Florio, Daniel Zanetti de, E-mail: daniel.florio@ufabc.edu.br [Universidade Federal do ABC (UFABC), Santo Andre, SP (Brazil)

2017-01-15

Electrodes for electrolyte-supported solid oxide fuel cells (SOFC’s) were fabricated by spin coating. Strontium-doped lanthanum manganite (LSM) cathode and nickel yttria-stabilized zirconia cermet anodes were synthesized and processed for enhanced deposition conditions. The influence of electrode microstructural parameters was investigated by a systematic experimental procedure aiming at optimized electrochemical performance of single cells. Polarization curves showed a strong dependence on both electrode thickness and sintering temperature. By a systematic control of such parameters, the performance of single cells was significantly enhanced due to decreasing of polarization resistance from 26 Ω cm² to 0.6 Ω cm² at 800°C. The results showed that spin-coated electrodes can be optimized for fast and cost effective fabrication of SOFCs. (author)

Microwave Assisted Solvent Free Synthesis of Azomethines from Aryl Aldehydes on Melamin Formaldehyde as Solid Support

Directory of Open Access Journals (Sweden)

Ramin Rezaei

2011-01-01

Full Text Available Various aryl aldehydes underwent prompt one pot conversion into the corresponding azomethines in high yields by reacting with hydroxylamine hydrochloride supported on melamine formaldehyde under microwave irradiation.

Bioinspired Synthesis of Monolithic and Layered Aerogels.

Science.gov (United States)

Han, Xiao; Hassan, Khalil T; Harvey, Alan; Kulijer, Dejan; Oila, Adrian; Hunt, Michael R C; Šiller, Lidija

2018-04-25

Aerogels are the least dense and most porous materials known to man, with potential applications from lightweight superinsulators to smart energy materials. To date their use has been seriously hampered by their synthesis methods, which are laborious and expensive. Taking inspiration from the life cycle of the damselfly, a novel ambient pressure-drying approach is demonstrated in which instead of employing low-surface-tension organic solvents to prevent pore collapse during drying, sodium bicarbonate solution is used to generate pore-supporting carbon dioxide in situ, significantly reducing energy, time, and cost in aerogel production. The generic applicability of this readily scalable new approach is demonstrated through the production of granules, monoliths, and layered solids with a number of precursor materials. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Phase transitions of sodium niobate powder and ceramics, prepared by solid state synthesis

Science.gov (United States)

Koruza, J.; Tellier, J.; Malič, B.; Bobnar, V.; Kosec, M.

2010-12-01

Phase transitions of sodium niobate, prepared by the solid state synthesis method, were examined using dielectric measurements, differential scanning calorimetry, and high temperature x-ray diffraction, in order to contribute to the clarification of its structural behavior below 400 °C. Four phase transitions were detected in the ceramic sample using dielectric measurements and differential scanning calorimetry and the obtained temperatures were in a good agreement with previous reports for the transitions of the P polymorph. The anomaly observed by dielectric measurements in the vicinity of 150 °C was frequency dependent and could be related to the dynamics of the ferroelectric nanoregions. The phase transitions of the as-synthesized NaNbO3 powder were investigated using differential scanning calorimetry and high temperature x-ray diffraction. The results show the existence of the Q polymorph at room temperature, not previously reported for the powder, which undergoes a transition to the R polymorph upon heating through a temperature region between 265 and 326.5 °C. This transition is mainly related to the displacement of Na into a more symmetric position and a minor change in the tilting system. The structures at room temperature, 250, 300, and 420 °C were refined by the Rietveld method and the evolution of the tilting system of the octahedral network and cationic displacement are reported.

Phase transitions of sodium niobate powder and ceramics, prepared by solid state synthesis

International Nuclear Information System (INIS)

Koruza, J.; Tellier, J.; Malic, B.; Bobnar, V.; Kosec, M.

2010-01-01

Phase transitions of sodium niobate, prepared by the solid state synthesis method, were examined using dielectric measurements, differential scanning calorimetry, and high temperature x-ray diffraction, in order to contribute to the clarification of its structural behavior below 400 deg. C. Four phase transitions were detected in the ceramic sample using dielectric measurements and differential scanning calorimetry and the obtained temperatures were in a good agreement with previous reports for the transitions of the P polymorph. The anomaly observed by dielectric measurements in the vicinity of 150 deg. C was frequency dependent and could be related to the dynamics of the ferroelectric nanoregions. The phase transitions of the as-synthesized NaNbO 3 powder were investigated using differential scanning calorimetry and high temperature x-ray diffraction. The results show the existence of the Q polymorph at room temperature, not previously reported for the powder, which undergoes a transition to the R polymorph upon heating through a temperature region between 265 and 326.5 deg. C. This transition is mainly related to the displacement of Na into a more symmetric position and a minor change in the tilting system. The structures at room temperature, 250, 300, and 420 deg. C were refined by the Rietveld method and the evolution of the tilting system of the octahedral network and cationic displacement are reported.

Performance of a novel type of electrolyte-supported solid oxide fuel cell with honeycomb structure

Energy Technology Data Exchange (ETDEWEB)

Ruiz-Morales, Juan Carlos; Savvin, Stanislav N.; Nunez, Pedro [Departmento de Quimica Inorganica, Universidad de La Laguna, 38200 Tenerife (Spain); Marrero-Lopez, David [Departamento de Fisica Aplicada I, Universidad de Malaga, 29071 Malaga (Spain); Pena-Martinez, Juan; Canales-Vazquez, Jesus [Instituto de Energias Renovables-Universidad de Castilla la Mancha, 02006 Albacete (Spain); Roa, Joan Josep; Segarra, Merce [DIOPMA, Departamento de Ciencia de los Materiales e Ing. Metalurgica, 08028 Barcelona (Spain)

2010-01-15

A novel design, alternative to the conventional electrolyte-supported solid oxide fuel cell (SOFC) is presented. In this new design, a honeycomb-electrolyte is fabricated from hexagonal cells, providing high mechanical strength to the whole structure and supporting the thin layer used as electrolyte of a SOFC. This new design allows a reduction of {proportional_to}70% of the electrolyte material and it renders modest performances over 320 mW cm{sup -2} but high volumetric power densities, i.e. 1.22 W cm{sup -3} under pure CH{sub 4} at 900 C, with a high OCV of 1.13 V, using the standard Ni-YSZ cermet as anode, Pt as cathode material and air as the oxidant gas. (author)

Synthesis, characterization and catalytic application of silica supported tin oxide nanoparticles for synthesis of 2,4,5-tri and 1,2,4,5-tetrasubstituted imidazoles under solvent-free conditions

Directory of Open Access Journals (Sweden)

Ashok V. Borhade

2017-02-01

Full Text Available Highly efficient and eco-friendly, one pot synthesis of 1,2,4,5-tetra substituted imidazoles and 2,4,5-trisubstituted imidazoles was reported under solvent free conditions using nanocrystalline silica supported tin oxide (SiO2:SnO2 as a catalyst with excellent yield. The present methodology offers several advantages such as mild reaction conditions, short reaction time, good yield, high purity of product, recyclable catalyst without a noticeable decrease in catalytic activity and can be used for large scale synthesis. The synthesized SiO2:SnO2 nanocrystalline catalyst was characterized by XRD, BET surface area and TEM techniques.

Flexible solid-state supercapacitors based on carbon nanoparticles/MnO2 nanorods hybrid structure.

Science.gov (United States)

Yuan, Longyan; Lu, Xi-Hong; Xiao, Xu; Zhai, Teng; Dai, Junjie; Zhang, Fengchao; Hu, Bin; Wang, Xue; Gong, Li; Chen, Jian; Hu, Chenguo; Tong, Yexiang; Zhou, Jun; Wang, Zhong Lin

2012-01-24

A highly flexible solid-state supercapacitor was fabricated through a simple flame synthesis method and electrochemical deposition process based on a carbon nanoparticles/MnO(2) nanorods hybrid structure using polyvinyl alcohol/H(3)PO(4) electrolyte. Carbon fabric is used as a current collector and electrode (mechanical support), leading to a simplified, highly flexible, and lightweight architecture. The device exhibited good electrochemical performance with an energy density of 4.8 Wh/kg at a power density of 14 kW/kg, and a demonstration of a practical device is also presented, highlighting the path for its enormous potential in energy management. © 2011 American Chemical Society

Immobilization methods for the rapid total chemical synthesis of proteins on microtiter plates.

Science.gov (United States)

Zitterbart, Robert; Krumrey, Michael; Seitz, Oliver

2017-07-01

The chemical synthesis of proteins typically involves the solid-phase peptide synthesis of unprotected peptide fragments that are stitched together in solution by native chemical ligation (NCL). The process is slow, and throughput is limited because of the need for repeated high performance liquid chromatography purification steps after both solid-phase peptide synthesis and NCL. With an aim to provide faster access to functional proteins and to accelerate the functional analysis of synthetic proteins by parallelization, we developed a method for the high performance liquid chromatography-free synthesis of proteins on the surface of microtiter plates. The method relies on solid-phase synthesis of unprotected peptide fragments, immobilization of the C-terminal fragment and on-surface NCL with an unprotected peptide thioester in crude form. Herein, we describe the development of a suitable immobilization chemistry. We compared (i) formation of nickel(II)-oligohistidine complexes, (ii) Cu-based [2 + 3] alkine-azide cycloaddition and (iii) hydrazone ligation. The comparative study identified the hydrazone ligation as most suitable. The sequence of immobilization via hydrazone ligation, on-surface NCL and radical desulfurization furnished the targeted SH3 domains in near quantitative yield. The synthetic proteins were functional as demonstrated by an on-surface fluorescence-based saturation binding analysis. Copyright © 2017 European Peptide Society and John Wiley & Sons, Ltd. Copyright © 2017 European Peptide Society and John Wiley & Sons, Ltd.

5' modification of duplex DNA with a ruthenium electron donor-acceptor pair using solid-phase DNA synthesis

Science.gov (United States)

Frank, Natia L.; Meade, Thomas J.

2003-01-01

Incorporation of metalated nucleosides into DNA through covalent modification is crucial to measurement of thermal electron-transfer rates and the dependence of these rates with structure, distance, and position. Here, we report the first synthesis of an electron donor-acceptor pair of 5' metallonucleosides and their subsequent incorporation into oligonucleotides using solid-phase DNA synthesis techniques. Large-scale syntheses of metal-containing oligonucleotides are achieved using 5' modified phosporamidites containing [Ru(acac)(2)(IMPy)](2+) (acac is acetylacetonato; IMPy is 2'-iminomethylpyridyl-2'-deoxyuridine) (3) and [Ru(bpy)(2)(IMPy)](2+) (bpy is 2,2'-bipyridine; IMPy is 2'-iminomethylpyridyl-2'-deoxyuridine) (4). Duplexes formed with the metal-containing oligonucleotides exhibit thermal stability comparable to the corresponding unmetalated duplexes (T(m) of modified duplex = 49 degrees C vs T(m) of unmodified duplex = 47 degrees C). Electrochemical (3, E(1/2) = -0.04 V vs NHE; 4, E(1/2) = 1.12 V vs NHE), absorption (3, lambda(max) = 568, 369 nm; 4, lambda(max) = 480 nm), and emission (4, lambda(max) = 720 nm, tau = 55 ns, Phi = 1.2 x 10(-)(4)) data for the ruthenium-modified nucleosides and oligonucleotides indicate that incorporation into an oligonucleotide does not perturb the electronic properties of the ruthenium complex or the DNA significantly. In addition, the absence of any change in the emission properties upon metalated duplex formation suggests that the [Ru(bpy)(2)(IMPy)](2+)[Ru(acac)(2)(IMPy)](2+) pair will provide a valuable probe for DNA-mediated electron-transfer studies.

A Laboratory Preparation of Aspartame Analogs Using Simultaneous Multiple Parallel Synthesis Methodology

Science.gov (United States)

Qvit, Nir; Barda, Yaniv; Gilon, Chaim; Shalev, Deborah E.

2007-01-01

This laboratory experiment provides a unique opportunity for students to synthesize three analogues of aspartame, a commonly used artificial sweetener. The students are introduced to the powerful and useful method of parallel synthesis while synthesizing three dipeptides in parallel using solid-phase peptide synthesis (SPPS) and simultaneous…

Supported liquid membrane based removal of lead(II) and cadmium(II) from mixed feed: Conversion to solid waste by precipitation

Energy Technology Data Exchange (ETDEWEB)

Bhatluri, Kamal Kumar; Manna, Mriganka Sekhar; Ghoshal, Aloke Kumar; Saha, Prabirkumar, E-mail: p.saha@iitg.ac.in

2015-12-15

Highlights: • Simultaneous removal of two heavy metals lead and cadmium. • Conversion of liquid waste to solid precipitation. • Precipitation facilitates the metals transportation through LM. • Solidification of liquid waste minimizes the final removal of waste. - Abstract: Simultaneous removal of two heavy metals, lead(II) and cadmium(II), from mixed feed using supported liquid membrane (SLM) based technique is investigated in this work. The carrier-solvent combination of “sodium salt of Di-2-ethylhexylphosphoric acid (D2EHPA) (4% w/w) in environmentally benign coconut oil” was immobilized into the pores of solid polymeric polyvinylidene fluoride (PVDF) support. Sodium carbonate (Na{sub 2}CO{sub 3}) was used as the stripping agent. Carbonate salts of lead(II) and cadmium(II) were formed in the stripping side interface and they were insoluble in water leading to precipitation inside the stripping solution. The transportation of solute is positively affected due to the precipitation. Lead(II) removal was found to be preferential due to its favorable electronic configuration. The conversion of the liquid waste to the solid one was added advantage for the final removal of hazardous heavy metals.

Municipal Solid Waste Gasification with Solid Oxide Fuel Cells and Stirling Engine

DEFF Research Database (Denmark)

Rokni, Masoud

2014-01-01

Municipal Solid Waste (MSW) can be considered a valid biomass to be used in a power plant. The major advantage is the reduction of pollutants and greenhouse gases emissions not only within large cities but also globally. Another advantage is that by th eir use it is possible to reduce the waste...... studied to optimize the plant efficiency in terms of operating conditions. Compared with modern waste incinerators with heat recovery, the gasification process integrated with SOFC and Stirling engine permits an increase in electricity output up of 50%, which means that the solid waste gasification......, waste is subject to chemical treatments through air or/and steam utilization; the result is a synthesis gas, called “Syngas” which is principally composed of hydrogen and carbon monoxide. Traces of hydrogen sulfide could also be present which can easily be separated in a desulfurization reactor...

Solid, double-metal cyanide catalysts for synthesis of ...

Indian Academy of Sciences (India)

Sci. Vol. 126, No. 2, March 2014, pp. 499–509. c Indian Academy of Sciences. Solid, double-metal cyanide catalysts for ... drimers, HPs have a highly branched structural design ... geneous catalysts and corrosion of the reactor lin- ... Carbon dioxide is a greenhouse gas. .... polymer product was reprecipitated from the liquid.

An Efficient Protocol for the Synthesis of Quinoxaline Derivatives at Room Temperature Using Recyclable Alumina-Supported Heteropolyoxometalates

Directory of Open Access Journals (Sweden)

Diego M. Ruiz

2012-01-01

Full Text Available We report a suitable quinoxaline synthesis using molybdophosphovanadates supported on commercial alumina cylinders as catalysts. These catalysts were prepared by incipient wetness impregnation. The catalytic test was performed under different reaction conditions in order to know the performance of the synthesized catalysts. The method shows high yields of quinoxaline derivatives under heterogeneous conditions. Quinoxaline formation was obtained using benzyl, o-phenylenediamine, and toluene as reaction solvent at room temperature. The CuH2PMo11VO40 supported on alumina showed higher activity in the tested reaction. Finally, various quinoxalines were prepared under mild conditions and with excellent yields.

Preparation and application of zirconium sulfate supported on SAPO-34 molecular sieve as solid acid catalyst for esterification

Energy Technology Data Exchange (ETDEWEB)

Xu, Dongyan, E-mail: xdy0156@sina.com; Ma, Hong; Cheng, Fei

2014-05-01

Graphical abstract: - Highlights: • SAPO-34 supported zirconium sulfate solid acid catalyst was prepared. • Esterification of acetic acid with ethanol can be catalyzed by ZS/SAPO-34. • The hydration of ZS is vital to the acidic property and catalytic performance. • The ZS/SAPO-34 catalyst treated at 200 °C shows good reusability. - Abstract: Zirconium sulfate (ZS) was supported on SAPO-34 molecular sieve by using an incipient wetness impregnation method with zirconium sulfate as the precursor. The as-prepared catalysts were used as solid acid catalyst for esterification reaction of acetic acid with ethanol. The influence of calcination temperature on the acidic property, catalytic activity, and reusability of ZS/SAPO-34 catalysts were mainly investigated. FT-IR, SEM, EDS and TG analysis have been carried out to demonstrate the characteristics of ZS/SAPO-34 catalysts. It was found that the 30 wt%ZS/SAPO-34 catalysts display the property of superacid irrespective of calcination temperature. The ZS/SAPO-34 catalyst treated at 200 °C can enhance the interaction between the supported ZS and SAPO-34 and keep the catalyst remaining substantially active after several reaction cycles. However, further increasing calcination temperature will cause the transfer of ZS from hydrate to anhydrous phase, and thus the decrease of activity.

Preparation and application of zirconium sulfate supported on SAPO-34 molecular sieve as solid acid catalyst for esterification

International Nuclear Information System (INIS)

Xu, Dongyan; Ma, Hong; Cheng, Fei

2014-01-01

Graphical abstract: - Highlights: • SAPO-34 supported zirconium sulfate solid acid catalyst was prepared. • Esterification of acetic acid with ethanol can be catalyzed by ZS/SAPO-34. • The hydration of ZS is vital to the acidic property and catalytic performance. • The ZS/SAPO-34 catalyst treated at 200 °C shows good reusability. - Abstract: Zirconium sulfate (ZS) was supported on SAPO-34 molecular sieve by using an incipient wetness impregnation method with zirconium sulfate as the precursor. The as-prepared catalysts were used as solid acid catalyst for esterification reaction of acetic acid with ethanol. The influence of calcination temperature on the acidic property, catalytic activity, and reusability of ZS/SAPO-34 catalysts were mainly investigated. FT-IR, SEM, EDS and TG analysis have been carried out to demonstrate the characteristics of ZS/SAPO-34 catalysts. It was found that the 30 wt%ZS/SAPO-34 catalysts display the property of superacid irrespective of calcination temperature. The ZS/SAPO-34 catalyst treated at 200 °C can enhance the interaction between the supported ZS and SAPO-34 and keep the catalyst remaining substantially active after several reaction cycles. However, further increasing calcination temperature will cause the transfer of ZS from hydrate to anhydrous phase, and thus the decrease of activity

Solid-Phase Synthesis for the Construction of Biologically Interesting Molecules and the Total Synthesis of Trioxacarcin DC-45-A2

DEFF Research Database (Denmark)

Mikkelsen, Remi Jacob Thomsen

. Furthermore a route to another key building block was developed featuring a Stille cross-coupling.Synthesis of Poly-fused Heterocycles. In the search for new biologically active compounds a methodology for the synthesis of polyfused heterocycles was investigated. This led to the development and optimization...

Total synthesis of sannanine and analogues thereof

Indian Academy of Sciences (India)

BADHER NAVEEN

2018-03-02

Mar 2, 2018 ... further characterized HRMS and IR spectral analysis. For all the newly synthesized by solid ..... Burst in a Model of Gouty Arthritis J. Nat. Prod. 70. 936. 3. ... Synthesis, Spectroscopic Characterisation, X-ray Struc- ture and DFT ...

Synthesis of pure Portland cement phases

DEFF Research Database (Denmark)

Wesselsky, Andreas; Jensen, Ole Mejlhede

2009-01-01

Pure phases commonly found in Portland cement clinkers are often used to test cement hydration behaviour in simplified experimental conditions. The synthesis of these phases is covered in this paper, starting with a description of phase relations and possible polymorphs of the four main phases...... in Portland cement, i.e. tricalcium silicate, dicalcium silicate, tricalcium aluminate and tetracalcium alumino ferrite. Details of the The process of solid state synthesis are is described in general including practical advice on equipment and techniques. Finally In addition, some exemplary mix compositions...

Supporting Information Synthesis of fatty monoester lubricant base ...

Indian Academy of Sciences (India)

Synthesis of fatty monoester lubricant base oil catalyzed by Fe-Zn ... Physical properties of fatty acid monoesters viz., kinematic viscosity, viscosity index, density ... The analysis method involves titration of the diluted sample with ethanolic alkali ...

Evaluation of alternative environmentally friendly matrix solid phase dispersion solid supports for the simultaneous extraction of 15 pesticides of different chemical classes from drinking water treatment sludge.

Science.gov (United States)

Soares, Karina Lotz; Cerqueira, Maristela Barnes Rodrigues; Caldas, Sergiane Souza; Primel, Ednei Gilberto

2017-09-01

This study describes the development, optimization and validation of a method for the extraction of 15 pesticides of different chemical classes in drinking water treatment sludge (DWTS) by vortex-assisted Matrix Solid Phase Dispersion (MSPD) with determination by gas chromatography coupled to mass spectrometry. It focused on the application of alternative and different solid supports to the extraction step of the MSPD. The main parameters that influenced the extraction were studied in order to obtain better recovery responses. Recoveries ranged from 70 to 120% with RSD below 20% for all analytes. Limits of quantification (LOQ) of the method ranged from 5 to 500 μg kg -1 whereas the analytical curves showed correlation coefficients above 0.997. The method under investigation used low volume of solvent (5 mL), low sample mass (1.5 g) and low mass of chitin (0.5 g), an environmentally friendly support. It has advantages, such as speed, simplicity and low cost material, over other methods. When the method was applied, 4 out of 15 pesticides were detected in the DWTS samples in concentrations below the LOQ. Copyright © 2017 Elsevier Ltd. All rights reserved.

Microwave-assisted solid phase conversion study of Meldrum's acid to ethylenetetracarboxylic dianhydride (C 6O 6)

Science.gov (United States)

Taherpour, Avat (Arman)

2010-01-01

Utilization of microwave irradiation provides an effective method for fast synthesizing of some important compounds. Microwave-assisted solid phase is an especial class in chemical synthesis. By the use of MW-irradiation on chemicals, sometimes interesting results can be seen. The synthesis of the interesting molecule ethylenetetracarboxylic dianhydride (C 6O 6) was attempted with a few different methods. In this study, the microwave-assisted solid phase conversion of Meldrum's acid to ethylenetetracarboxylic dianhydride was reported. This conversion was characterized by FT-IR, GC/MS and NMR spectroscopy results.

B-site substituted solid solutions on the base of sodium-bismuth titanate

Directory of Open Access Journals (Sweden)

V. M. Ishchuk

2016-12-01

Full Text Available The paper presents results of studies of the formation of phases during the solid-state synthesis in the [(Na0.5Bi0.50.80Ba0.20](Ti1–yByO3 system of solid solutions with B-site substitutions. The substitutions by zirconium, tin and ion complexes (In0.5Nb0.5 and (Fe0.5Nb0.5 have been studied. It has been found that the synthesis is a multi-step process associated with the formation of a number of intermediate phases (depending on the compositions and calcination temperatures. Single-phase solid solutions have been produced at the calcination temperatures in the interval 1000–1100∘C. An increase in the substituting ions concentration leads to a linear increase of the crystal cell size. At the same time, the tolerance factor gets reduced boosting the stability of the antiferroelectric phase as compared to that of the ferroelectric phase.

Synthesis and characterization of saturated polyester and ...

Indian Academy of Sciences (India)

but which can actually be used for processes, which pro- duce interesting ... ing the synthesis of saturated polyester (from GPET waste). This has been done for the .... The solid product obtained from the glycolysis of PET was bis(hydroxy ethyl ...

Synthesis and characterization of tungsten carbide doped cobalt via gas-solid reaction in rotary bed reactor; Sintese e caracterizacao de carbeto de tungstenio dopado com cobalto via reacao gas-solido em reator de leito rotativo

Energy Technology Data Exchange (ETDEWEB)

Tertuliano, R.S.C.; Araujo, C.P.B. de; Frota, A.V.V.M.; Moriyama, A.L.L.; Souza, C.P. de, E-mail: ruasavio@hotmail.com [Universidade Federal do Rio Grande do Norte (UFRN), Natal, RN (Brazil). Departamento de Engenharia Quimica

2016-07-01

The search for materials with high added value, high applicability and sustainability, motivates innovations in all areas of engineering. In this context, so-called doped carbides, ceramic and metal compounds are included. This work proposes the synthesis and characterization of tungsten carbide doped cobalt (WC-Co) through the gas-solid reaction in a rotating bed reactor. The production stages of the material are: precursor synthesis by wetting, drying at 80 deg C, characterization of the precursor by MEV, DRX and FRX, gas-solid reaction at 750 deg C in a reducing atmosphere of CH{sub 4} / H{sub 2} in a rotary reactor at 34 rpm and characterization of the reaction product by the techniques already mentioned. The results showed that tungsten carbide powders were produced with cobalt inserted into the structure, with high surface area, nanometric grains and with potential for applications in the areas of catalysis, reactors and fuel cells, showing the relevance of this type of research.

Synthesis and characterization of NaCo(1-x)MnxO2 solid electrolyte using sol-gel method: the effect of milling speed variations

Science.gov (United States)

Suyati, L.; Widyayanti, O. A.; Qushoyyi, M.; Darmawan, A.; Nuryanto, R.

2018-04-01

Battery is a device that converts chemical energy into electrical energy through electrochemical process. Further research on the synthesis of cathode of Na-ion battery that has good conductivity to maximize the battery performance needs to be conducted. One of the production steps of the NaCo(1-x)NaCo cathode synthesis in the Na-Ion battery was a ball-milling process, in which by the ball-milling process, the crystal size of NaCo(1-x)MnxO2 cathode can be minimized. The purpose of this study was to determine the effect of variation of ball-milling speed to the characteristics of resulting product including the oxide types composing NaCo(1-x)MnxO2 cathode, surface morphology, and conductivity. The main ingredients used were sodium acetate, manganese acetate, cobalt acetate with molar ratio of 0.7: 0.66: 0.22, respectively and citric acid as chelating agent with the M/CA ratio of 1: 1. The variations of milling speed were 0, 300, 400, 500, 600 and 700 rpm. Characterization of the product was conducted using XRD, SEM-EDS, and conductivity meter (LCR-meter). The result showed that a solid electrolyte of NaCo(1-x)MnxO2 consisting of NaMnO2, NaO2, CoO, Co2O3, MnO2 components was successfully synthesized. The observation on the milling speed at 400 rpm showed that the solid electrolyte produced had the highest conductivity i.e. 4.08 x 10-6 Scm-1 with a homogeneous surface morphology and had a spinel formula NaCo0,65Mn0,35O2.

Topotactic synthesis of vanadium nitride solid foams

International Nuclear Information System (INIS)

Oyama, S.T.; Kapoor, R.; Oyama, H.T.; Hofmann, D.J.; Matijevic, E.

1993-01-01

Vanadium nitride has been synthesized with a surface area of 120 m 2 g -1 by temperature programmed nitridation of a foam-like vanadium oxide (35 m 2 g -1 ), precipitated from vanadate solutions. The nitridation reaction was established to be topotactic and pseudomorphous by x-ray powder diffraction and scanning electron microscopy. The crystallographic relationship between the nitride and oxide was {200}//{001}. The effect of precursor geometry on the product size and shape was investigated by employing vanadium oxide solids of different morphologies

In situ synthesis and catalytic application of reduced graphene oxide supported cobalt nanowires

Science.gov (United States)

Xu, Zhiqiang; Long, Qin; Deng, Yi; Liao, Li

2018-05-01

Controlled synthesis of magnetic nanocomposite with outstanding catalytic performances is a promising strategy in catalyst industry. We proposed a novel concept for fabrication of reduced graphene oxide-supported cobalt nanowires (RGO/Co-NWs) nanocomposite as high-efficient magnetic catalyst. Unlike the majority of experiments necessitating harsh synthesis conditions such as high-pressure, high-temperature and expensive template, here the RGO/Co-NWs were successfully prepared in aqueous solution under mild conditions with the assistance of external magnetic field. The synthetic process was facile and external magnetic force was adopted to induce the unidirectional self-assembly of cobalt crystals on graphene oxide to form RGO/Co-NWs. The possible formation mechanism laid on the fact that the dipole magnetic moments of the nanoparticles were aligned along the magnetic induction lines with the external magnetic field direction resulting in the formation of nanowires elongating in the direction of the magnetization axis. Simultaneously, a series of controlled reactions were conducted to illuminate the effect of graphene oxide, external magnetic field and PVP on the morphology and size of RGO/Co-NWs in the present approach. More importantly, the nanocomposite exhibited a high catalytic performance towards ammonia borane. Hence the novel nanocomposite holds a great potential for technological applications such as catalyst industry.

Alternative Processes for Water Reclamation and Solid Waste Processing in a Physical/chemical Bioregenerative Life Support System

Science.gov (United States)

Rogers, Tom D.

1990-01-01

Viewgraphs on alternative processes for water reclamation and solid waste processing in a physical/chemical-bioregenerative life support system are presented. The main objective is to focus attention on emerging influences of secondary factors (i.e., waste composition, type and level of chemical contaminants, and effects of microorganisms, primarily bacteria) and to constructively address these issues by discussing approaches which attack them in a direct manner.

OMS-2-Supported Cu Hydroxide-Catalyzed Benzoxazoles Synthesis from Catechols and Amines via Domino Oxidation Process at Room Temperature.

Science.gov (United States)

Meng, Xu; Wang, Yanmin; Wang, Yuanguang; Chen, Baohua; Jing, Zhenqiang; Chen, Gexin; Zhao, Peiqing

2017-07-07

In the presence of manganese oxide octahedral molecular sieve (OMS-2) supported copper hydroxide Cu(OH) x /OMS-2, aerobic synthesis of benzoxazoles from catechols and amines via domino oxidation/cyclization at room temperature is achieved. This heterogeneous benzoxazoles synthesis initiated by the efficient oxidation of catechols over Cu(OH) x /OMS-2 tolerates a variety of substrates, especially amines containing sensitive groups (hydroxyl, cyano, amino, vinyl, ethynyl, ester, and even acetyl groups) and heterocycles, which affords functionalized benzoxazoles in good to excellent yields by employing low catalyst loading (2 mol % Cu). The characterization and plausible catalytic mechanism of Cu(OH) x /OMS-2 are described. The notable features of our catalytic protocol such as the use of air as the benign oxidant and EtOH as the solvent, mild conditions, ease of product separation, being scalable up to the gram level, and superior reusability of catalyst (up to 10 cycles) make it more practical and environmentally friendly for organic synthesis.

Identifying a compound modifying a cellular response, comprises attaching cells having a reporter system onto solid supports, releasing a library member, screening and identifying target cells

DEFF Research Database (Denmark)

2011-01-01

The present invention relates to methods for identifying compounds capable of modulating a cellular response. The methods involve attaching living cells to solid supports comprising a library of test compounds. Test compounds modulating a cellular response, for example via a cell surface molecule...... may be identified by selecting solid supports comprising cells, wherein the cellular response of interest has been modulated. The cellular response may for example be changes in signal transduction pathways modulated by a cell surface molecule....

Polyvinylpolypyrrolidone-Supported Boron Trifluoride; Highly Efficient Catalyst for the Synthesis of N-tert-Butyl Amides

Directory of Open Access Journals (Sweden)

Masoud Mokhtary

2012-01-01

Full Text Available Highly efficient method for the preparation of N-tert-butyl amides by reaction of nitriles with tert-butyl acetate is described using polyvinylpolypyrrolidone-supported boron trifluoride (PVPP-BF3 at 70°C in good to excellent yields. Selective amidation of benzonitrile in the presence of acetonitrile was also achieved. polyvinylpolypyrrolidone-boron trifluoride complex shows non-corrosive and stable solid catalyst elevated Lewis acid property.

hydrothermal synthesis and characterisation of amine-templated

African Journals Online (AJOL)

PROF EKWUEME

showed that the complexes were insoluble in water, ethanol, DMF and DMSO. KEYWORDS: Hydrothermal synthesis, metal phosphates, p-aminobenzoic acid, ethylacetoacetate, ethylammonium-. 4-aminobenzoate. INTRODUCTION. One of the major areas of materials science is the development of solid state materials with ...

Green Synthesis of a Fluorescent Natural Product

Science.gov (United States)

Young, Douglas M.; Welker, Jacob J. C.; Doxsee, Kenneth M.

2011-01-01

Synthesis of 4-methylumbelliferone via the acid-catalyzed Pechmann condensation introduces students to several types of organic reactions: transesterification, electrophilic aromatic substitution, and alcohol dehydration. Performed with a recyclable, solid catalyst and under solvent-free conditions, the experiment illustrates many of the…

Synthesis and electrochemical analysis of AlVMoO7 oxide prepared ...

Indian Academy of Sciences (India)

2018-05-16

May 16, 2018 ... solid solution and two-phase regimes. In the voltage ... LiMn2O4) [1]. Among these compounds, olivine LiFePO4, ... polyanions provide numerous metal oxidation states, struc- tural stability ... 2.1a Sol–gel synthesis (SG): In SG synthesis method, ... AlVMoO7 and confirms that only a single phase is formed.

Production of α-amylase by solid state fermentation by Rhizopus ...

African Journals Online (AJOL)

2015-02-18

Feb 18, 2015 ... However, only a few strains of fungi and bacteria meet the criteria for production of ... amylase production, but solid-state fermentation (SSF) is emerging as a ..... synthesis of lactic acid in R. oryzae and Rhizopus arrhizus using ...

Solid Waste Management Requirements Definition for Advanced Life Support Missions: Results

Science.gov (United States)

Alazraki, Michael P.; Hogan, John; Levri, Julie; Fisher, John; Drysdale, Alan

2002-01-01

Prior to determining what Solid Waste Management (SWM) technologies should be researched and developed by the Advanced Life Support (ALS) Project for future missions, there is a need to define SWM requirements. Because future waste streams will be highly mission-dependent, missions need to be defined prior to developing SWM requirements. The SWM Working Group has used the mission architecture outlined in the System Integration, Modeling and Analysis (SIMA) Element Reference Missions Document (RMD) as a starting point in the requirement development process. The missions examined include the International Space Station (ISS), a Mars Dual Lander mission, and a Mars Base. The SWM Element has also identified common SWM functionalities needed for future missions. These functionalities include: acceptance, transport, processing, storage, monitoring and control, and disposal. Requirements in each of these six areas are currently being developed for the selected missions. This paper reviews the results of this ongoing effort and identifies mission-dependent resource recovery requirements.

Mechanistic modelling of a cathode-supported solid oxide fuel cell. Paper no. IGEC-1-103

International Nuclear Information System (INIS)

Suwanwarangkul, R.; Croiset, E.; Pritzker, M.D.; Fowler, M.W.; Douglas, P.L.; Entchev, E.

2005-01-01

A model for a cathode-supported tubular solid oxide fuel cell operating with humidified H 2 has been developed. Momentum-, mass-, energy- and charge-transport equations coupled with electrochemical reactions (H 2 oxidation and O 2 reduction) are considered in the model. The model also takes into account the radiative heat transfer between the cell and air-preheating tube. The model is validated against published experimental data ands shows a good agreement. The distributions of temperature, current density, reversible cell voltage, overpotential and species mole fractions within the cell are discussed in detail. (author)

Supporting international medical graduates' transition to their host-country: realist synthesis.

Science.gov (United States)

Kehoe, Amelia; McLachlan, John; Metcalf, Jane; Forrest, Simon; Carter, Madeline; Illing, Jan

2016-10-01

Many health services and systems rely on the contribution of international medical graduates (IMGs) to the workforce. However, concern has grown around their regulation and professional practice. There is a need, in the absence of strong evidence and a robust theoretical base, for a deeper understanding of the efficacy of interventions used to support IMGs' transition to their host countries. This study seeks to explore and synthesise evidence relating to interventions developed for IMGs. It aims to provide educators and policy makers with an understanding of how interventions should be developed to support IMGs in their transition to the workplace, particularly looking to identify how and why they are effective. The realist synthesis involved an initial systematic search of the literature for the period January 1990 to April 2015. Secondary searches were conducted throughout the review in order to inform and test the developing programme theory. The context, mechanism and outcome data were extracted from all sources meeting the inclusion criteria. Fourteen case studies were included to further aid theory refinement. Sixty-two articles were identified, describing diverse interventions of varying intensity. A further 26 articles were identified through a secondary search. The findings illustrate that, alongside a developed programme, ongoing support and cultural awareness at organisational and training levels are crucial. Individual differences must also be taken into consideration. This will ensure that IMGs engage in transformative learning, increase their levels of self-efficacy and cultural health capital, and reduce feelings of stress and anxiety. These factors will have an impact on work, interactions and cultural adjustment. Organisational, training and individual contexts all play a role in IMGs' adjustment during the transition process. Establishing ongoing support is critical. A list of recommendations for implementation is given. © 2016 The Authors

One pot synthesis of magnetic graphene/carbon nanotube composites as magnetic dispersive solid-phase extraction adsorbent for rapid determination of oxytetracycline in sewage water.

Science.gov (United States)

Sun, Yunyun; Tian, Jing; Wang, Lu; Yan, Hongyuan; Qiao, Fengxia; Qiao, Xiaoqiang

2015-11-27

A simple and time-saving one pot synthesis of magnetic graphene/carbon nanotube composites (M-G/CNTs) was developed that could avoid the tedious drying process of graphite oxide, and G/CNTs were modified by Fe3O4 nanoparticles in the reduction procedure. It contributed to a shorten duration of the synthesis process of M-G/CNTs. The obtained M-G/CNTs were characterized and the results indicated that CNTs and Fe3O4 nanoparticles were served as spacer distributing to the layers of graphene, which was beneficial for enlarging surface area and improving extraction efficiency. Moreover, M-G/CNTs showed good magnetic property and outstanding thermal stability. Then M-G/CNTs were applied as adsorbent of magnetic dispersive solid-phase extraction for rapid extraction and determination of oxytetracycline in sewage water. Under the optimum conditions, good linearity was obtained in the range of 20-800ngmL(-1) and the recoveries were ranged from 95.5% to 112.5% with relative standard deviations less than 5.8%. Copyright © 2015 Elsevier B.V. All rights reserved.

Catalytic Production of Ethanol from Biomass-Derived Synthesis Gas

Energy Technology Data Exchange (ETDEWEB)

Trewyn, Brian G. [Colorado School of Mines, Golden, CO (United States); Smith, Ryan G. [Iowa State Univ., Ames, IA (United States)

2016-06-01

Heterogeneous catalysts have been developed for the conversion of biomass-derived synthetic gas (syngas) to ethanol. The objectives of this project were to develop a clean synthesis gas from biomass and develop robust catalysts with high selectivity and lifetime for C₂ oxygenate production from biomass-derived syngas and surrogate syngas. During the timeframe for this project, we have made research progress on the four tasks: (1) Produce clean bio-oil generated from biomass, such as corn stover or switchgrass, by using fast pyrolysis system, (2) Produce clean, high pressure synthetic gas (syngas: carbon monoxide, CO, and hydrogen, H₂) from bio-oil generated from biomass by gasification, (3) Develop and characterize mesoporous mixed oxide-supported metal catalysts for the selective production of ethanol and other alcohols, such as butanol, from synthesis gas, and (4) Design and build a laboratory scale synthesis gas to ethanol reactor system evaluation of the process. In this final report, detailed explanations of the research challenges associated with this project are given. Progress of the syngas production from various biomass feedstocks and catalyst synthesis for upgrading the syngas to C₂-oxygenates is included. Reaction properties of the catalyst systems under different reaction conditions and different reactor set-ups are also presented and discussed. Specifically, the development and application of mesoporous silica and mesoporous carbon supports with rhodium nanoparticle catalysts and rhodium nanoparticle with manganese catalysts are described along with the significant material characterizations we completed. In addition to the synthesis and characterization, we described the activity and selectivity of catalysts in our micro-tubular reactor (small scale) and fixed bed reactor (larger scale). After years of hard work, we are proud of the work done on this project, and do believe that this work will provide a solid

An overview of Engineering Aspects of Solid State Fermentation

Directory of Open Access Journals (Sweden)

Prabhakar, A.

2005-01-01

Full Text Available Solid substrate cultivation (SSC or solid state fermentation (SSF is envisioned as a prominent bio conversion technique to transform natural raw materials into a wide variety of chemical as well as bio-chemical products. This process involves the fermentation of solid substrate medium with microorganism in the absence of free flowing water. Recent developments and concerted focus on SSF enabled it to evolve as a potential bio- technology as an alternative to thetraditional chemical synthesis. SSF is being successfully exploited for food production, fuels, enzymes, antibiotics, animal feeds and also for dye degradation. This paper discusses the various micro and macro level engineering problems associated with SSF and some possible solutions for its full commercial realization.

Synthesis and properties of hydroxy acrylic resin with high solid content

Science.gov (United States)

Yu, Zhen; Hu, Mingguang; Cui, Han; Xiao, Jijun

2017-10-01

Manufacturers of automotive repair finishes are tending to reduce more and more the level of volatile organic compounds in their paints in order to comply with increasingly strict environmental legislation. A high solid hydroxy acrylic resin was synthesised using CARDURA E10 and a type of hydroxyacrylic acid resin, its' acid value, hydroxylvalue, viscosity, structure, morphology was measured and film-forming properties after curing were characterised. The results show that the addition of CARDURA E10 in the copolymer composition significantly reduced the viscosity of the polymer system, improved the solid content of the resin and the physical properties of the coating. The hydroxyl acrylate resin with solid content of 90% and excellent comprehensive performance were successfully prepared by controlling the initiator dosage, polymerization temperature and monomer ratio.

Synthesis of 10-Ethyl Flavin: A Multistep Synthesis Organic Chemistry Laboratory Experiment for Upper-Division Undergraduate Students

Science.gov (United States)

Sichula, Vincent A.

2015-01-01

A multistep synthesis of 10-ethyl flavin was developed as an organic chemistry laboratory experiment for upper-division undergraduate students. Students synthesize 10-ethyl flavin as a bright yellow solid via a five-step sequence. The experiment introduces students to various hands-on experimental organic synthetic techniques, such as column…

Cooperative catalysis designing efficient catalysts for synthesis

CERN Document Server

Peters, René

2015-01-01

Written by experts in the field, this is a much-needed overview of the rapidly emerging field of cooperative catalysis. The authors focus on the design and development of novel high-performance catalysts for applications in organic synthesis (particularly asymmetric synthesis), covering a broad range of topics, from the latest progress in Lewis acid / Br?nsted base catalysis to e.g. metal-assisted organocatalysis, cooperative metal/enzyme catalysis, and cooperative catalysis in polymerization reactions and on solid surfaces. The chapters are classified according to the type of cooperating acti

Solid State Division progress report for period ending September 30, 1993

Energy Technology Data Exchange (ETDEWEB)

Green, P.H.; Hinton, L.W. [eds.

1994-08-01

This report covers research progress in the Solid State Division from April 1, 1992, to September 30, 1993. During this period, the division conducted a broad, interdisciplinary materials research program with emphasis on theoretical solid state physics, neutron scattering, synthesis and characterization of materials, ion beam and laser processing, and the structure of solids and surfaces. This research effort was enhanced by new capabilities in atomic-scale materials characterization, new emphasis on the synthesis and processing of materials, and increased partnering with industry and universities. The theoretical effort included a broad range of analytical studies, as well as a new emphasis on numerical simulation stimulated by advances in high-performance computing and by strong interest in related division experimental programs. Superconductivity research continued to advance on a broad front from fundamental mechanisms of high-temperature superconductivity to the development of new materials and processing techniques. The Neutron Scattering Program was characterized by a strong scientific user program and growing diversity represented by new initiatives in complex fluids and residual stress. The national emphasis on materials synthesis and processing was mirrored in division research programs in thin-film processing, surface modification, and crystal growth. Research on advanced processing techniques such as laser ablation, ion implantation, and plasma processing was complemented by strong programs in the characterization of materials and surfaces including ultrahigh resolution scanning transmission electron microscopy, atomic-resolution chemical analysis, synchrotron x-ray research, and scanning tunneling microscopy.

Solid State Division progress report for period ending September 30, 1993

International Nuclear Information System (INIS)

Green, P.H.; Hinton, L.W.

1994-08-01

This report covers research progress in the Solid State Division from April 1, 1992, to September 30, 1993. During this period, the division conducted a broad, interdisciplinary materials research program with emphasis on theoretical solid state physics, neutron scattering, synthesis and characterization of materials, ion beam and laser processing, and the structure of solids and surfaces. This research effort was enhanced by new capabilities in atomic-scale materials characterization, new emphasis on the synthesis and processing of materials, and increased partnering with industry and universities. The theoretical effort included a broad range of analytical studies, as well as a new emphasis on numerical simulation stimulated by advances in high-performance computing and by strong interest in related division experimental programs. Superconductivity research continued to advance on a broad front from fundamental mechanisms of high-temperature superconductivity to the development of new materials and processing techniques. The Neutron Scattering Program was characterized by a strong scientific user program and growing diversity represented by new initiatives in complex fluids and residual stress. The national emphasis on materials synthesis and processing was mirrored in division research programs in thin-film processing, surface modification, and crystal growth. Research on advanced processing techniques such as laser ablation, ion implantation, and plasma processing was complemented by strong programs in the characterization of materials and surfaces including ultrahigh resolution scanning transmission electron microscopy, atomic-resolution chemical analysis, synchrotron x-ray research, and scanning tunneling microscopy

Solid state synthesis and sintering of monazite-type ceramics: application to minor actinides conditioning; Synthese par voie solide et frittage de ceramiques a structure monazite. Application au conditionnement des actinides mineurs

Energy Technology Data Exchange (ETDEWEB)

Bregiroux, D

2005-11-15

In the framework of the French law of 1991 concerning the nuclear waste management, several studies are undertaken to develop specific crystalline conditioning matrices. Monazite, a rare earth (TR{sup 3+}) orthophosphate with a general formula TR{sup 3+}PO{sub 4}, is a natural mineral containing significant amount of thorium and uranium. Monazite has been proposed as a host matrix for the minor actinides (Np, Am and Cm) specific conditioning, thanks to its high resistance to self irradiation and its low solubility. Its is now of prime importance to check the conservation of these properties on synthesized materials, which implies to master all the stages of the elaboration process, from the powder synthesis to the sintering of controlled microstructure pellets. This work can be divided into two main parts: The first part deals with the synthesis by high temperature solid state route of TR{sup 3+}PO{sub 4} powders (with TR{sup 3+} = La{sup 3+} to Gd{sup 3+}, Pu{sup 3+} and Am{sup 3+}). The chemical reactions occurring during the firing of starting reagents are described in the case of monazite with only one or several cations. From these results, a protocol of synthesis is described. The incorporation of tetravalent cations (Ce{sup 4+}, U{sup 4+}, Pu{sup 4+}) in the monazite structure was also studied. The second part of the present work deals with the elaboration of controlled density and microstructure monazite pellets and their related mechanical and thermal properties. The study of crushing and sintering is presented. For the first time, experimental results are confronted with theoretical models in order to deduce the densification and grain growth mechanisms. By the comprehension of the various physicochemical phenomena occurring during the various stages of the monazite pellets elaboration process (powder synthesis, crushing, sintering...), this work allowed the development of a protocol of elaboration of controlled microstructure monazite TR{sup 3+}PO{sub 4

The synthesis of nanostructured, phase pure catalysts by hydrodynamic cavitation

Energy Technology Data Exchange (ETDEWEB)

Moser, W.R.; Sunstrom, J.E.; Marshik-Geurts, B.J. [Worcester Polytechnic Institute, Worcester, MA (United States)

1995-12-01

A new process for the synthesis of advanced catalytic materials based on performing the synthesis under hydrodynamic cavitation conditions has been discovered. This continuous process for catalyst synthesis resulted in the formation of both supported and unsupported catalysts. The advantage of the process over classical methods of synthesis is that it permits the formation of a wide variety of nanostructured catalysts in exceptionally high phase purities. The synthesis of platinum and palladium catalysts supported on alumina and other supports resulted in high dispersions of the noble metals. The synthesis of alpha, beta- and gamma-bismuth molybdates resulted in catalysts having superior phase purities as compared to several other classical methods of synthesis. The beta-bismuth molybdate was synthesized directly onto Cabosil. These studies showed that the particle size of the active component could be varied from a few manometers to much larger grains. The process enabled the synthesis of other complex metal oxides like perovskites as pure phases. The process uses a commercially available Microfluidizer.

Supervision, support and mentoring interventions for health practitioners in rural and remote contexts: an integrative review and thematic synthesis of the literature to identify mechanisms for successful outcomes.

Science.gov (United States)

Moran, Anna M; Coyle, Julia; Pope, Rod; Boxall, Dianne; Nancarrow, Susan A; Young, Jennifer

2014-02-13

To identify mechanisms for the successful implementation of support strategies for health-care practitioners in rural and remote contexts. This is an integrative review and thematic synthesis of the empirical literature that examines support interventions for health-care practitioners in rural and remote contexts. This review includes 43 papers that evaluated support strategies for the rural and remote health workforce. Interventions were predominantly training and education programmes with limited evaluations of supervision and mentoring interventions. The mechanisms associated with successful outcomes included: access to appropriate and adequate training, skills and knowledge for the support intervention; accessible and adequate resources; active involvement of stakeholders in programme design, implementation and evaluation; a needs analysis prior to the intervention; external support, organisation, facilitation and/or coordination of the programme; marketing of the programme; organisational commitment; appropriate mode of delivery; leadership; and regular feedback and evaluation of the programme. Through a synthesis of the literature, this research has identified a number of mechanisms that are associated with successful support interventions for health-care practitioners in rural and remote contexts. This research utilised a methodology developed for studying complex interventions in response to the perceived limitations of traditional systematic reviews. This synthesis of the evidence will provide decision-makers at all levels with a collection of mechanisms that can assist the development and implementation of support strategies for staff in rural and remote contexts.

Myocardial Oxidative Metabolism and Protein Synthesis during Mechanical Circulatory Support by Extracorporeal Membrane Oxygenation

Energy Technology Data Exchange (ETDEWEB)

Priddy, MD, Colleen M.; Kajimoto, Masaki; Ledee, Dolena; Bouchard, Bertrand; Isern, Nancy G.; Olson, Aaron; Des Rosiers, Christine; Portman, Michael A.

2013-02-01

Extracorporeal membrane oxygenation (ECMO) provides mechanical circulatory support essential for survival in infants and children with acute cardiac decompensation. However, ECMO also causes metabolic disturbances, which contribute to total body wasting and protein loss. Cardiac stunning can also occur which prevents ECMO weaning, and contributes to high mortality. The heart may specifically undergo metabolic impairments, which influence functional recovery. We tested the hypothesis that ECMO alters oxidative. We focused on the amino acid leucine, and integration with myocardial protein synthesis. We used a translational immature swine model in which we assessed in heart (i) the fractional contribution of leucine (FcLeucine) and pyruvate (FCpyruvate) to mitochondrial acetyl-CoA formation by nuclear magnetic resonance and (ii) global protein fractional synthesis (FSR) by gas chromatography-mass spectrometry. Immature mixed breed Yorkshire male piglets (n = 22) were divided into four groups based on loading status (8 hours of normal circulation or ECMO) and intracoronary infusion [13C6,15N]-L-leucine (3.7 mM) alone or with [2-13C]-pyruvate (7.4 mM). ECMO decreased pulse pressure and correspondingly lowered myocardial oxygen consumption (~ 40%, n = 5), indicating decreased overall mitochondrial oxidative metabolism. However, FcLeucine was maintained and myocardial protein FSR was marginally increased. Pyruvate addition decreased tissue leucine enrichment, FcLeucine, and Fc for endogenous substrates as well as protein FSR. Conclusion: The heart under ECMO shows reduced oxidative metabolism of substrates, including amino acids, while maintaining (i) metabolic flexibility indicated by ability to respond to pyruvate, and (ii) a normal or increased capacity for global protein synthesis, suggesting an improved protein balance.

Long-term Steam Electrolysis with Electrolyte-Supported Solid Oxide Cells

International Nuclear Information System (INIS)

Schefold, Josef; Brisse, Annabelle; Poepke, Hendrik

2015-01-01

Steam electrolysis over 11000 h with an electrolyte-supported solid oxide cell is discussed. The cell of 45 cm"2 area consists of a scandia/ceria doped zirconia electrolyte (6Sc1CeSZ), CGO diffusion-barrier/adhesion layers, a lanthanum strontium cobaltite ferrite (LSCF) oxygen electrode, and a nickel steam/hydrogen electrode. After initial 2500 h operation with lower current-density magnitude, the current density was set to j = -0.9 A cm"−"2 and the steam conversion rate to 51%. This led to a cell voltage of 1.185 V at 847 °C cell temperature. Average voltage degradation was 7.3 mV/1000 h ( 100% throughout the test (with an external heat source for evaporation). Impedance spectroscopic measurements revealed a degradation almost entirely due to increasing ohmic resistance. The rate of resistance increase was initially faster (up to 40 mΩ cm"2/1000 h) and stabilised after several 1000 h operation. After 9000 h a small (non-ohmic) electrode degradation became detectable (<2 mV/1000 h), superimposed to ohmic degradation. The small electrode degradation is understood as indication for largely reversible (electrolysis cell/fuel cell) behaviour.

Supported liquid membrane based removal of lead(II) and cadmium(II) from mixed feed: Conversion to solid waste by precipitation.

Science.gov (United States)

Bhatluri, Kamal Kumar; Manna, Mriganka Sekhar; Ghoshal, Aloke Kumar; Saha, Prabirkumar

2015-12-15

Simultaneous removal of two heavy metals, lead(II) and cadmium(II), from mixed feed using supported liquid membrane (SLM) based technique is investigated in this work. The carrier-solvent combination of "sodium salt of Di-2-ethylhexylphosphoric acid (D2EHPA) (4% w/w) in environmentally benign coconut oil" was immobilized into the pores of solid polymeric polyvinylidene fluoride (PVDF) support. Sodium carbonate (Na2CO3) was used as the stripping agent. Carbonate salts of lead(II) and cadmium(II) were formed in the stripping side interface and they were insoluble in water leading to precipitation inside the stripping solution. The transportation of solute is positively affected due to the precipitation. Lead(II) removal was found to be preferential due to its favorable electronic configuration. The conversion of the liquid waste to the solid one was added advantage for the final removal of hazardous heavy metals. Copyright © 2015 Elsevier B.V. All rights reserved.

Microwave Assisted Convenient One-Pot Synthesis of Coumarin Derivatives via Pechmann Condensation Catalyzed by FeF3 under Solvent-Free Conditions and Antimicrobial Activities of the Products

Directory of Open Access Journals (Sweden)

Vahid Vahabi

2014-08-01

Full Text Available A rapid and efficient solvent-free one-pot synthesis of coumarin derivatives by Pechmann condensation reactions of phenols with ethyl acetoacetate using FeF3 as a catalyst under microwave irradiation is described. This one-pot synthesis on a solid inorganic support provides the products in good yields. The newly synthesized compounds were systematically characterized by IR, 1H-NMR, 13C-NMR, MS and elemental CHN analyses. The proposed solvent-free microwave irradiation method using the environmentally friendly catalyst FeF3 offers the unique advantages of high yields, shorter reaction times, easy and quick isolation of the products, excellent chemoselectivity, and a one-pot, green synthesis. The products were screened for antimicrobial activity, and the results showed that the compounds reacted against all the tested bacteria.

Mechanical Properties of Supports and Half‐Cells for Solid Oxide Electrolysis Influenced by Alumina‐Zirconia Composites

DEFF Research Database (Denmark)

Charlas, Benoit; Ni, De Wei; Frandsen, Henrik Lund

2017-01-01

In order to improve the durability and robustness of solid oxide electrolysis cells (SOEC) and stacks, it is necessary to improve the strength of its components. In cathode supported SOEC, the main structural component is the Ni(O)- YSZ support. But the strength of the half-cell or cell is also...... determined by the strength of other weaker components and by the residual stress state induced by the thermal expansion mismatch. In this study, the mechanical properties of Ni(O)-3YSZ supports with a reference composition and with substitution of 3YSZ by 20A3YSZ (3YSZ with 20 wt.% Al2O3) have been tested...... and compared. The initial interest of this substitution are a decrease of the coefficient of thermal expansion (CTE) mismatch within the half-cell and the fact that 20A3YSZ is stronger than 3YSZ. The influence of the process on the composition, strength, elastic properties and electrical conductivity...

Performance characterization of solid oxide cells under high pressure

DEFF Research Database (Denmark)

Sun, Xiufu; Bonaccorso, Alfredo Damiano; Graves, Christopher R.

2014-01-01

in both fuel cell mode and electrolysis mode. In electrolysis mode at low current density, the performance improvement was counteracted by the increase in open circuit voltage, but it has to be born in mind that the pressurised gas contains higher molar free energy. Operating at high current density...... hydrocarbon fuels, which is normally performed at high pressure to achieve a high yield. Operation of SOECs at elevated pressure will therefore facilitate integration with the downstream fuel synthesis and is furthermore advantageous as it increases the cell performance. In this work, recent pressurised test...... results of a planar Ni-YSZ (YSZ: Yttria stabilized Zirconia) supported solid oxide cell are presented. The test was performed at 800 °C at pressures up to 15 bar. A comparison of the electrochemical performance of the cell at 1 and 3 bar shows a significant and equal performance gain at higher pressure...

CuO-Nanoparticles Catalyzed Synthesis of 1,4-Disubstituted-1,2,3 ...

Indian Academy of Sciences (India)

John Paul Raj

2018-04-13

Apr 13, 2018 ... has been developed for the synthesis of 1,2,3-triazoles. A library of 1 ... Kuang et al., described Cu-catalyzed synthesis of 1H-. 1,2,3-triazoles from 1 ..... Tornøe C W, Christensen C and Meldal M 2002 Peptido- triazoles on solid ... 2015 Copper-catalyzed [3+2] cycloaddition/oxidation reactions between ...

Synthesis of supported metallic nano-particles and their use in air depollution

International Nuclear Information System (INIS)

Barrault, J.; Valange, S.; Tatibouet, J.M.; Thollon, St.; Herlin-Boime, N.; Giraud, S.; Ruiz, J.Ch.; Bergaya, B.; Joulin, J.P.; Delbianco, N.; Gabelica, Z.; Daturi, M.

2009-01-01

The main objectives of the 'NACACOMO' Consortium ('Nano-materials: Catalysts for the Conversion of organic Molecules. Uses in fine chemicals and environment protection ') consisted in generating novel catalysts composed of nanoparticles of metals (Pt, Pd, Ag...) and/or oxides (TiO 2 ...) stabilized and well distributed over the surface of a support (foams, ceramics), by monitoring both the particle size and the 'coating' process itself, using new technologies: CVD, plasma-spray, laser pyrolysis, supercritical preparation, which were compared to conventional soft chemistry recipes. The most accurate characterization of particle morphology, local structure, texture, spatial arrangement but also of their reactivity, were achieved by privileging the utilization of various in situ methods. Details on formation mechanisms of a solid nano-particle at the atomic level (nucleation, growth and particle (re)distribution over the support...) could be obtained in selected cases, with opportunities for scaling up and shaping. The (chemical) nature of the so-obtained nano-materials was monitored for selected catalytic applications involving the development of environmental friendly processes, such as oxidation of VOC, with a priority for aromatics and chlorinated compounds. (authors)

Development and optimisation of synthesis, characterisation and physical properties of solid materials for strip conductors; purpose oriented synthesis of novel systems. Final report

International Nuclear Information System (INIS)

Guenther, W.; Schoellhorn, R.

1995-06-01

The project reported is part of studies into the performance of HTSC, and was responsible for the following essential tasks: synthesis, characterisation, and optimisation of oxocuprates of the type (RE)Ba 2 Cu 3 O 7 , examination of the relevant corrosion processes and reactivity of the phases, and synthesis of novel systems guided by special model concepts, applying kinetics-controlled low-temperature synthesis. (orig./MM) [de

Uranothorite solid solutions: From synthesis to dissolution

International Nuclear Information System (INIS)

Costin, Dan-Tiberiu

2012-01-01

USiO 4 coffinite appears as one of the potential phases formed in the back-end of the alteration of spent fuel, in reducing storage conditions. A study aiming to assess the thermodynamic data associated with coffinite through an approach based on the preparation of Th 1-x U x SiO 4 uranothorite solid solutions was then developed during this work. First, the preparation of uranothorite samples was successfully undertaken in hydrothermal conditions. However, the poly-phased samples systematically formed for x ≥ 0,2 underlined the kinetic hindering linked with the preparation of uranium-enriched samples, including coffinite end-member. Nevertheless, the characterization of the various samples led to confirm the formation of an ideal solid solution and allowed the constitution of a spectroscopic database. The purification of the samples was then performed by the means of different protocols based on physical (dispersion-centrifugation) or chemical (selective dissolution of secondary phases) methods. This latter led to a complete of the impurities (Th 1-y U y O 2 mixed oxide and amorphous silica) through successive washing steps in acid then basic media. Finally, dissolution experiments were undertaken on uranothorite samples (0 ≤ xexp. ≤ 0,5) and allowed pointing out the influence of composition, pH and temperature on the normalized dissolution rate of the compounds. Also, the associated thermodynamic data, such as activation energy, indicate that the reaction is controlled by surface reactions. Once the equilibrium is reached, the analogous solubility constants were determined for each composition studied, then allowing the extrapolation to coffinite value. It was then finally possible to conclude on the inversion of coffinitisation reaction with temperature. (author) [fr

Municipal solid waste composition determination supporting the integrated solid waste management system in the island of Crete

International Nuclear Information System (INIS)

Gidarakos, E.; Havas, G.; Ntzamilis, P.

2006-01-01

A one-year survey was conducted in the greater region of Crete (located at the lower region of the Aegean Sea) for the purpose of identifying waste composition (including chemical and physical characterization), as well as any seasonal variation. The investigation was carried out repeatedly at seven landfills and one transfer station in Crete, in four phases. Each sampling phase corresponded to a season (autumn, winter, spring, summer). ASTM D5231-92(2003) standard method and RCRA Waste Sampling Draft Technical Guidance were used. Hand sorting was used for classifying the collected wastes into the following categories: plastics, paper, metals, aluminium, leather-wood-textiles-rubbers, organic wastes, non-combustibles and miscellaneous. Further analysis included proximate and ultimate analysis of combustible materials. Metals such as lead, cadmium and mercury were also investigated. The results show that there has been a significant decrease of organic wastes during the last decade due to the increase of packaging materials, as a result of a change in consumption patterns. Three main waste categories were determined: organic wastes, paper and plastics, which combined represent 76% of the total waste in Crete. Furthermore, a high fraction of glass and a seasonal variation of aluminium indicate a strong correlation of waste composition with certain human activities, such as tourism. There is also a variation between the municipal solid waste (MSW) composition in the region of Crete (2003-2004) and MSW composition suggested in the National Solid Waste Planning (2000) [National Solid Waste Planning, 2000. Completion and particularization of Common Ministerial Act 113944//1944/1997: National Solid Waste Planning, June 2000]. The results of this survey are to be utilized by the regional solid waste authorities in order to establish an integrated waste treatment site, capable of fulfilling the regional waste management demands

Municipal solid waste composition determination supporting the integrated solid waste management system in the island of Crete.

Science.gov (United States)

Gidarakos, E; Havas, G; Ntzamilis, P

2006-01-01

A one-year survey was conducted in the greater region of Crete (located at the lower region of the Aegean Sea) for the purpose of identifying waste composition (including chemical and physical characterization), as well as any seasonal variation. The investigation was carried out repeatedly at seven landfills and one transfer station in Crete, in four phases. Each sampling phase corresponded to a season (autumn, winter, spring, summer). ASTM D5231-92(2003) standard method and RCRA Waste Sampling Draft Technical Guidance were used. Hand sorting was used for classifying the collected wastes into the following categories: plastics, paper, metals, aluminium, leather-wood-textiles-rubbers, organic wastes, non-combustibles and miscellaneous. Further analysis included proximate and ultimate analysis of combustible materials. Metals such as lead, cadmium and mercury were also investigated. The results show that there has been a significant decrease of organic wastes during the last decade due to the increase of packaging materials, as a result of a change in consumption patterns. Three main waste categories were determined: organic wastes, paper and plastics, which combined represent 76% of the total waste in Crete. Furthermore, a high fraction of glass and a seasonal variation of aluminium indicate a strong correlation of waste composition with certain human activities, such as tourism. There is also a variation between the municipal solid waste (MSW) composition in the region of Crete (2003-2004) and MSW composition suggested in the National Solid Waste Planning (2000) [National Solid Waste Planning, 2000. Completion and particularization of Common Ministerial Act 113944//1944/1997: National Solid Waste Planning, June 2000]. The results of this survey are to be utilized by the regional solid waste authorities in order to establish an integrated waste treatment site, capable of fulfilling the regional waste management demands.

Synthesis of homo- and heteromultivalent carbohydrate-functionalized oligo(amidoamines using novel glyco-building blocks

Directory of Open Access Journals (Sweden)

Felix Wojcik

2013-11-01

Full Text Available We present the solid phase synthesis of carbohydrate-functionalized oligo(amidoamines with different functionalization patterns utilizing a novel alphabet of six differently glycosylated building blocks. Highly efficient in flow conjugation of thioglycosides to a double-bond presenting diethylentriamine precursor is the key step to prepare these building blocks suitable for fully automated solid-phase synthesis. Introduction of the sugar ligands via functionalized building blocks rather than postfunctionalization of the oligomeric backbone allows for the straightforward synthesis of multivalent glycoligands with full control over monomer sequence and functionalization pattern. We demonstrate the potential of this building-block approach by synthesizing oligomers with different numbers and spacing of carbohydrates and also show the feasibility of heteromultivalent glycosylation patterns by combining building blocks presenting different mono- and disaccharides.

A hydronitrogen solid: high pressure ab initio evolutionary structure searches

International Nuclear Information System (INIS)

Hu Anguang; Zhang Fan

2011-01-01

High pressure ab initio evolutionary structure searches resulted in a hydronitrogen solid with a composition of (NH) 4 . The structure searches also provided two molecular isomers, ammonium azide (AA) and trans-tetrazene (TTZ) which were previously discovered experimentally and can be taken as molecular precursors for high pressure synthesis of the hydronitrogen solid. The computed pressure versus enthalpy diagram showed that the transformation pressure to the hydronitrogen solid is 36 GPa from AA and 75 GPa from TTZ. Its metastability was analyzed by the phonon dispersion spectrum and room-temperature vibrational density of state together with the transformation energy barrier back to molecular phases at 298 K. The predicted energy barrier of 0.21 eV/atom means that the proposed hydronitrogen solid should be very stable at ambient conditions. (fast track communication)

Self-propagating high-temperature synthesis of La(Sr)Ga(Mg)O3-δ for electrolyte of solid oxide fuel cells

International Nuclear Information System (INIS)

Ishikawa, Hiroyuki; Enoki, Makiko; Ishihara, Tatsumi; Akiyama, Tomohiro

2007-01-01

This paper describes self-propagating high-temperature synthesis (SHS) of an electrolyte for solid oxide fuel (SOFC), in comparison to a conventional solid-state reaction method (SRM). Doped-lanthanum gallate: La 0.9 Sr 0.1 Ga 0.8 Mg 0.2 O 3-δ (LSGM9182) and LSGM9173 as the SOFC electrolyte, was prepared by the SHS and sintered at different temperatures, for measuring the electrical conductivity of the sintered LSGM and the power generating performance at 1073 K, in comparison to the SRM. In the SHS, the LSGM powders with smaller size were obtained and easily sintered at the 100 K-lower temperature, 1673 K, than in the SRM. Most significantly, the electrical conductivity of the sintered LSGM9182 was as high as 0.11 S cm -1 and its maximum power density was a value of 245 mW cm -2 in the cell configuration of Ni/LSGM9182 (0.501 mm in thickness)/Sm 0.5 Sr 0.5 CoO 3 . The conclusion was that the proposed SHS-sintering method with many benefits of minimizing the energy requirement and the processing time in the production, easing temperature restriction for the sintering, and improving the electrolyte performance up to a conventional level is practicable for producing the LSGM-electrolyte of SOFC at an intermediate-temperature application

Electrode Design for Low Temperature Direct-Hydrocarbon Solid Oxide Fuel Cells

Science.gov (United States)

Chen, Fanglin (Inventor); Zhao, Fei (Inventor); Liu, Qiang (Inventor)

2015-01-01

In certain embodiments of the present disclosure, a solid oxide fuel cell is described. The solid oxide fuel cell includes a hierarchically porous cathode support having an impregnated cobaltite cathode deposited thereon, an electrolyte, and an anode support. The anode support includes hydrocarbon oxidation catalyst deposited thereon, wherein the cathode support, electrolyte, and anode support are joined together and wherein the solid oxide fuel cell operates a temperature of 600.degree. C. or less.

Electrode design for low temperature direct-hydrocarbon solid oxide fuel cells

Science.gov (United States)

Chen, Fanglin; Zhao, Fei; Liu, Qiang

2015-10-06

In certain embodiments of the present disclosure, a solid oxide fuel cell is described. The solid oxide fuel cell includes a hierarchically porous cathode support having an impregnated cobaltite cathode deposited thereon, an electrolyte, and an anode support. The anode support includes hydrocarbon oxidation catalyst deposited thereon, wherein the cathode support, electrolyte, and anode support are joined together and wherein the solid oxide fuel cell operates a temperature of 600.degree. C. or less.

Fluorous Parallel Synthesis of A Hydantoin/Thiohydantoin Library

Science.gov (United States)

Lu, Yimin; Zhang, Wei

2007-01-01

Fluorous tagging strategy is applied to solution-phase parallel synthesis of a library containing hydantoin and thiohydantoin analogs. Two perfluoroalkyl (Rf)-tagged α-amino esters each react with 6 aromatic aldehydes under reductive amination conditions. Twelve amino esters then each react with 10 isocyanates and isothiocyanates in parallel. The resulting 120 ureas and thioureas undergo spontaneous cyclization to form the corresponding hydantoins and thiohydantoins. The intermediate and final product purifications are performed with solid-phase extraction (SPE) over FluoroFlash™ cartridges, no chromatography is required. Using standard instruments and straightforward SPE technique, one chemist accomplished the 120-member library synthesis in less than 5 working days, including starting material synthesis and product analysis. PMID:15789556

One-Pot Synthesis of Hierarchical Flower-Like Pd-Cu Alloy Support on Graphene Towards Ethanol Oxidation

Science.gov (United States)

Zhang, Jingyi; Feng, Anni; Bai, Jie; Tan, Zhibing; Shao, Wenyao; Yang, Yang; Hong, Wenjing; Xiao, Zongyuan

2017-09-01

The synergetic effect of alloy and morphology of nanocatalysts play critical roles towards ethanol electrooxidation. In this work, we developed a novel electrocatalyst fabricated by one-pot synthesis of hierarchical flower-like palladium (Pd)-copper (Cu) alloy nanocatalysts supported on reduced graphene oxide (Pd-Cu(F)/RGO) for direct ethanol fuel cells. The structures of the catalysts were characterized by using scanning electron microscopy (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectrometer (XPS). The as-synthesized Pd-Cu(F)/RGO nanocatalyst was found to exhibit higher electrocatalytic performances towards ethanol electrooxidation reaction in alkaline medium in contrast with RGO-supported Pd nanocatalyst and commercial Pd black catalyst in alkaline electrolyte, which could be attributed to the formation of alloy and the morphology of nanoparticles. The high performance of nanocatalyst reveals the great potential of the structure design of the supporting materials for the future fabrication of nanocatalysts.

Synthesis of nitrogen-doped graphene via solid microwave method

Energy Technology Data Exchange (ETDEWEB)

Zhang, Li, E-mail: zhangli379@sohu.com [School of Electrical Engineering, Dalian University of Technology, Dalian, Liaoning 116024 (China); Ji, Bingcheng, E-mail: debbo.jee@outlook.com [School of Electrical Engineering, Dalian University of Technology, Dalian, Liaoning 116024 (China); Wang, Kai [School of Electrical Engineering, Dalian University of Technology, Dalian, Liaoning 116024 (China); Song, Jinyan [School of Information Engineering, Dalian Ocean University, Dalian, Liaoning 116024 (China)

2014-07-01

Graphical abstract: - Highlights: • A direct solid microwave method is developed to prepare nitrogen-doped graphene. • The method consists of two steps, namely the functionalization and microwave irradiation. • Melamine can serve as not only functionalizing agent but also nitrogen source. - Abstract: In this paper, we propose a solid microwave-mediated method for scalable production of nitrogen-doped graphene sheets (NGS) using low-cost industrial material melamine as functionalizing agent and nitrogen source. The strong interaction of microwaves with graphene oxide has been fully utilized to generate in situ heating that induces the decompose melamine and nitrogen doping of graphene. The morphology, structure, and components of the as-produced nitrogen-doped graphene are characterized by scanning electron microscopy (SEM), transmission electron microscope (TEM), Brunauer–Emmett–Teller (BET), pore-size distribution (PSD), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectra (XPS), X-ray diffraction (XRD), and Raman spectroscopy. The results show NGS can be successfully synthesized via this strategy.

Synthesis of nitrogen-doped graphene via solid microwave method

International Nuclear Information System (INIS)

Zhang, Li; Ji, Bingcheng; Wang, Kai; Song, Jinyan

2014-01-01

Graphical abstract: - Highlights: • A direct solid microwave method is developed to prepare nitrogen-doped graphene. • The method consists of two steps, namely the functionalization and microwave irradiation. • Melamine can serve as not only functionalizing agent but also nitrogen source. - Abstract: In this paper, we propose a solid microwave-mediated method for scalable production of nitrogen-doped graphene sheets (NGS) using low-cost industrial material melamine as functionalizing agent and nitrogen source. The strong interaction of microwaves with graphene oxide has been fully utilized to generate in situ heating that induces the decompose melamine and nitrogen doping of graphene. The morphology, structure, and components of the as-produced nitrogen-doped graphene are characterized by scanning electron microscopy (SEM), transmission electron microscope (TEM), Brunauer–Emmett–Teller (BET), pore-size distribution (PSD), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectra (XPS), X-ray diffraction (XRD), and Raman spectroscopy. The results show NGS can be successfully synthesized via this strategy

Fabrication and characterization of a cathode-supported tubular solid oxide fuel cell

Energy Technology Data Exchange (ETDEWEB)

Zhao, Chunhua; Liu, Renzhu; Wang, Shaorong; Wang, Zhenrong; Qian, Jiqin; Wen, Tinglian [CAS Key Laboratory of Materials for Energy Conversion, Shanghai Institute of Ceramics, Chinese Academy of Sciences (SICCAS), 1295 Dingxi Road, Shanghai 200050 (China)

2009-07-15

A cathode-supported tubular solid oxide fuel cell (CTSOFC) with the length of 6.0 cm and outside diameter of 1.0 cm has been successfully fabricated via dip-coating and co-sintering techniques. A crack-free electrolyte film with a thickness of {proportional_to}14 {mu}m was obtained by co-firing of cathode/cathode active layer/electrolyte/anode at 1250 C. The relative low densifying temperature for electrolyte was attributed to the large shrinkage of the green tubular which assisted the densification of electrolyte. The assembled cell was electrochemically characterized with humidified H{sub 2} as fuel and O{sub 2} as oxidant. The open circuit voltages (OCV) were 1.1, 1.08 and 1.06 V at 750, 800 and 850 C, respectively, with the maximum power densities of 157, 272 and 358 mW cm{sup -2} at corresponding temperatures. (author)

Iron based superconductors and related compounds synthesized by solid state metathesis and high temperature reactions

International Nuclear Information System (INIS)

Frankovsky, Rainer

2013-01-01

The results of this thesis can be divided into three major topics, which can also be seen as different approaches of solid state chemistry to reveal interesting features of known and unknown compounds and to develop alternative synthesis routes. Firstly, known compounds with related structural motifs to the superconducting iron-arsenides were investigated regarding their structural and physical properties. In case of La 3 Pd 4 Ge 4 the influence of Fe doping on the properties was studied, whereas in the series ZrMAs (M=Ti,V) the physical properties have not yet been reported at all and were investigated for the first time. Secondly, an alternative synthesis route has been developed for the synthesis of superconducting LaFeAsO 1-x F x . This solid state metathesis reaction distinctly increased the quality of the samples compared to conventionally prepared products. Furthermore, the reaction pathway was investigated and clarified, which helps to understand the processes during high temperature solid state metathesis reactions in general. Thirdly, this alternative synthesis route was expanded to other systems and new compounds like co-substituted LaFe 1-x Mn x AsO 1-y F y were prepared and thoroughly investigated. This led to a complex study of the interplay of magnetism, electronic and structural conditions and the occurrence of superconducting properties. The investigation and understanding of such complex coherences will probably be decisive for the further understanding of the superconducting mechanism in iron based superconductors.

2-Methyltetrahydrofuran and cyclopentyl methyl ether for green solid-phase peptide synthesis.

Science.gov (United States)

Jad, Yahya E; Acosta, Gerardo A; Khattab, Sherine N; de la Torre, Beatriz G; Govender, Thavendran; Kruger, Hendrik G; El-Faham, Ayman; Albericio, Fernando

2016-02-01

2-MeTHF and CPME were evaluated as greener alternatives for the most employed solvents in peptide synthesis. The ability of these solvents to dissolve amino acid derivatives and a range of coupling reagents were evaluated as well as the swelling of polystyrene and polyethylene glycol resins. In addition, racemization and coupling efficiencies were also determined. We concluded that the use of 2-MeTHF with combination of DIC/OxymaPure gave the lowest racemization level during stepwise synthesis of Z-Phg-Pro-NH2 and the highest purity during SPPS of Aib-enkephalin pentapeptide (H-Tyr-Aib-Aib-Phe-Leu-NH2).

Efficient assessment of modified nucleoside stability under conditions of automated oligonucleotide synthesis: characterization of the oxidation and oxidative desulfurization of 2-thiouridine.

Science.gov (United States)

Sochacka, E

2001-01-01

In order to efficiently assess the chemical stability of modified nucleosides to the reagents and conditions of automated oligonucleotide synthesis, we designed, developed and tested a scheme in which the modified nucleoside, directly attached to a solid support, is exposed to the cyclic chemistry of the instrument. Stability of 2-thiouridine against different oxidizers was investigated. Tertbutyl hydroperoxide (1 M) in anhydrous acetonitrile was a more effective oxidizer for the incorporation of 2-thiouridine into oligonucleotide chains than the same oxidizer in methylene chloride. Carbon tetrachloride/water in the presence of a basic catalyst was superior in maintaining the thiocarbonyl function, but its utility for RNA synthesis has yet to be fully tested, whereas 2-phenylsulfonyloxaziridine was a very efficient reagent for oxidative desulfurization of 2-thiouridine.

Investigation of methane steam reforming in planar porous support of solid oxide fuel cell

International Nuclear Information System (INIS)

Yang Yongping; Du Xiaoze; Yang Lijun; Huang Yuan; Xian Haizhen

2009-01-01

Adopting the porous support in integrated-planar solid oxide fuel cell (IP-SOFC) can reduce the operating temperature by reducing thickness of electrolyte layer, and also, provide internal reforming environment for hydrogen-rich fuel gas. The distributions of reactant and product components, and temperature of methane steam reforming for IP-SOFC were investigated by the developed physical and mathematical model with thermodynamic analysis, in which eleven possible reaction mechanisms were considered by the source terms and Arrhenius relationship. Numerical simulation of the model revealed that the progress of reforming reaction and the distribution of the product, H 2 , were influenced by the operating conditions, included that of temperature, ratio of H 2 O and CH 4 , as well as by the porosity of the supporting material. The simulating results indicate that the methane conversion rate can reach its maximum value under the operating temperature of 800 deg. C and porosity of ε = 0.4, which rather approximate to the practical operating conditions of IP-SOFC. In addition, characteristics of carbon deposition on surface of catalyst were discussed under various operating conditions and configuration parameters of the porous support. The present works provided some theoretical explanations to the numerous experimental observations and engineered practices

Break-down of Losses in High Performing Metal-Supported Solid Oxide Fuel Cells

DEFF Research Database (Denmark)

Kromp, Alexander; Nielsen, Jimmi; Blennow Tullmar, Peter

2012-01-01

Metal supported SOFC designs offer competitive advantages such as reduced material costs and improved mechanical robustness. On the other hand, disadvantages might arise due to possible corrosion of the porous metal parts during processing and operation at high fuel utilization. In this paper we...... in hydrogen. The electrochemically active parts were applied by infiltrating CGO-Ni precursor solution into the porous metal and anode backbone and screenprinting (La,Sr)(Co,Fe)O3-based cathodes. To prevent a solid state reaction between cathode and zirconia electrolyte, CGO buffer layers were applied...... in between cathode and electrolyte. The detailed electrochemical characterization by means of impedance spectroscopy and a subsequent data analysis by the distribution of relaxation times enabled us to separate the different loss contributions in the cell. Based on an appropriate equivalent circuit model...

Manufacturing Demonstration Facility: Low Temperature Materials Synthesis

International Nuclear Information System (INIS)

Graham, David E.; Moon, Ji-Won; Armstrong, Beth L.; Datskos, Panos G.; Duty, Chad E.; Gresback, Ryan; Ivanov, Ilia N.; Jacobs, Christopher B.; Jellison, Gerald Earle; Jang, Gyoung Gug; Joshi, Pooran C.; Jung, Hyunsung; Meyer, Harry M.; Phelps, Tommy

2015-01-01

The Manufacturing Demonstration Facility (MDF) low temperature materials synthesis project was established to demonstrate a scalable and sustainable process to produce nanoparticles (NPs) for advanced manufacturing. Previous methods to chemically synthesize NPs typically required expensive, high-purity inorganic chemical reagents, organic solvents and high temperatures. These processes were typically applied at small laboratory scales at yields sufficient for NP characterization, but insufficient to support roll-to-roll processing efforts or device fabrication. The new NanoFermentation processes described here operated at a low temperature (~60 C) in low-cost, aqueous media using bacteria that produce extracellular NPs with controlled size and elemental stoichiometry. Up-scaling activities successfully demonstrated high NP yields and quality in a 900-L pilot-scale reactor, establishing this NanoFermentation process as a competitive biomanufacturing strategy to produce NPs for advanced manufacturing of power electronics, solid-state lighting and sensors.

Manufacturing Demonstration Facility: Low Temperature Materials Synthesis

Energy Technology Data Exchange (ETDEWEB)

Graham, David E. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Moon, Ji-Won [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Armstrong, Beth L. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Datskos, Panos G. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Duty, Chad E. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Gresback, Ryan [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Ivanov, Ilia N. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jacobs, Christopher B. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jellison, Gerald Earle [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jang, Gyoung Gug [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Joshi, Pooran C. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jung, Hyunsung [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Meyer, III, Harry M. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Phelps, Tommy [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

2015-06-30

The Manufacturing Demonstration Facility (MDF) low temperature materials synthesis project was established to demonstrate a scalable and sustainable process to produce nanoparticles (NPs) for advanced manufacturing. Previous methods to chemically synthesize NPs typically required expensive, high-purity inorganic chemical reagents, organic solvents and high temperatures. These processes were typically applied at small laboratory scales at yields sufficient for NP characterization, but insufficient to support roll-to-roll processing efforts or device fabrication. The new NanoFermentation processes described here operated at a low temperature (~60 C) in low-cost, aqueous media using bacteria that produce extracellular NPs with controlled size and elemental stoichiometry. Up-scaling activities successfully demonstrated high NP yields and quality in a 900-L pilot-scale reactor, establishing this NanoFermentation process as a competitive biomanufacturing strategy to produce NPs for advanced manufacturing of power electronics, solid-state lighting and sensors.

Cation exchange assisted binding-elution strategy for enzymatic synthesis of human milk oligosaccharides (HMOs).

Science.gov (United States)

Zhu, Hailiang; Wu, Zhigang; Gadi, Madhusudhan Reddy; Wang, Shuaishuai; Guo, Yuxi; Edmunds, Garrett; Guan, Wanyi; Fang, Junqiang

2017-09-15

A cation exchange assisted binding-elution (BE) strategy for enzymatic synthesis of human milk oligosaccharides (HMOs) was developed. An amino linker was used to provide the cation ion under acidic condition which can be readily bound to cation exchange resin and then eluted off by saturated ammonium bicarbonate. Ammonium bicarbonate in the collections was easily removed by vacuum evaporation. This strategy circumvented the incompatible issue between glycosyltransferases and solid support or large polymers, and no purification was needed for intermediate products. With current approach, polyLacNAc backbones of HMOs and fucosylated HMOs were synthesized smoothly. Copyright © 2017 Elsevier Ltd. All rights reserved.

Solid waste burial grounds interim safety analysis

International Nuclear Information System (INIS)

Saito, G.H.

1994-01-01

This Interim Safety Analysis document supports the authorization basis for the interim operation and restrictions on interim operations for the near-surface land disposal of solid waste in the Solid Waste Burial Grounds. The Solid Waste Burial Grounds Interim Safety Basis supports the upgrade progress for the safety analysis report and the technical safety requirements for the operations in the Solid Waste Burial Grounds. Accident safety analysis scenarios have been analyzed based on the significant events identified in the preliminary hazards analysis. The interim safety analysis provides an evaluation of the operations in the Solid Waste Burial Grounds to determine if the radiological and hazardous material exposures will be acceptable from an overall health and safety standpoint to the worker, the onsite personnel, the public, and the environment

Solid waste burial grounds interim safety analysis

Energy Technology Data Exchange (ETDEWEB)

Saito, G.H.

1994-10-01

This Interim Safety Analysis document supports the authorization basis for the interim operation and restrictions on interim operations for the near-surface land disposal of solid waste in the Solid Waste Burial Grounds. The Solid Waste Burial Grounds Interim Safety Basis supports the upgrade progress for the safety analysis report and the technical safety requirements for the operations in the Solid Waste Burial Grounds. Accident safety analysis scenarios have been analyzed based on the significant events identified in the preliminary hazards analysis. The interim safety analysis provides an evaluation of the operations in the Solid Waste Burial Grounds to determine if the radiological and hazardous material exposures will be acceptable from an overall health and safety standpoint to the worker, the onsite personnel, the public, and the environment.

Supervision, support and mentoring interventions for health practitioners in rural and remote contexts: an integrative review and thematic synthesis of the literature to identify mechanisms for successful outcomes

Science.gov (United States)

2014-01-01

Objective To identify mechanisms for the successful implementation of support strategies for health-care practitioners in rural and remote contexts. Design This is an integrative review and thematic synthesis of the empirical literature that examines support interventions for health-care practitioners in rural and remote contexts. Results This review includes 43 papers that evaluated support strategies for the rural and remote health workforce. Interventions were predominantly training and education programmes with limited evaluations of supervision and mentoring interventions. The mechanisms associated with successful outcomes included: access to appropriate and adequate training, skills and knowledge for the support intervention; accessible and adequate resources; active involvement of stakeholders in programme design, implementation and evaluation; a needs analysis prior to the intervention; external support, organisation, facilitation and/or coordination of the programme; marketing of the programme; organisational commitment; appropriate mode of delivery; leadership; and regular feedback and evaluation of the programme. Conclusion Through a synthesis of the literature, this research has identified a number of mechanisms that are associated with successful support interventions for health-care practitioners in rural and remote contexts. This research utilised a methodology developed for studying complex interventions in response to the perceived limitations of traditional systematic reviews. This synthesis of the evidence will provide decision-makers at all levels with a collection of mechanisms that can assist the development and implementation of support strategies for staff in rural and remote contexts. PMID:24521004

Synthesis and characterization of bulk Cu2ZnSnX4 (X: S, Se) via thermodynamically supported mechano-chemical process

International Nuclear Information System (INIS)

Pareek, Devendra; Balasubramaniam, K.R.; Sharma, Pratibha

2015-01-01

Materials with the general formula, Cu 2 ZnSnX 4 (CZTX; X: Group 16 elements), with X being S/Se, have been receiving considerable attention due to their utility as an absorber layer in solar photovoltaics (PV). This paper reports on the synthesis of CZTSe and CZTS nanocrystalline powders at low temperatures, starting from elemental metal and chalcogen powders, via the low cost, scalable technique of ball milling. The prepared samples were well characterized using the different characterization tools. XRD, Raman, SEM and TEM studies confirm the formation of single-phase, stoichiometric, nano-crystalline kesterite CZTS and CZTSe powders. The low temperature phase selection of the complex quaternary compound in this system is seen as a direct consequence of the thermodynamic facilitation, coupled with the capability of mechano-chemical synthesis to aid in overcoming kinetic constraints. The optical bandgap of the various samples of CZTS was observed in the range of 1.4–1.6 eV and corresponding values for CZTSe was observed to be in the range of 1.08–1.18 eV. Our work provides a pathway for developing cheap, scalable, and ink-based techniques for low cost solar PV. - Graphical abstract: Display Omitted - Highlights: • A scalable route for synthesis of near phase pure CZTS/Se nano-crystals has been demonstrated. • Stoichiometric CZTS and CZTSe were synthesized via mechano-chemical synthesis route. • Synthesis at near room temperature is supported by thermodynamic calculations

A New Miniaturized Inkjet Printed Solid State Electrolyte Sensor for Applications in Life Support Systems - First Results

Science.gov (United States)

Hill, Christine; Stefanos Fasoulas, -; Eberhart, Martin; Berndt, Felix

New generations of integrated closed loop systems will combine life support systems (incl. biological components) and energy systems such as fuel cell and electrolysis systems. Those systems and their test beds also contain complex safety sensor monitoring systems. Especially in fuel cells and electrolysis systems, the hydrogen and oxygen flows and exchange into other areas due to diffusion processes or leaks need to be monitored. Knowledge of predominant gas concentrations at all times is essential to avoid explosive gas mixtures. Solid state electrolyte sensors are promising for use as safety sensors. They have already been developed and produced at various institutes, but the power consumption for heating an existing solid state electrolyte sensor element still lies between 1 to 1.5 W and the operational readiness still takes about 20 to 30 s. This is partially due to the current manufacturing process for the solid state electrolyte sensor elements that is based on screen printing technology. However this technology has strong limitations in flexibility of the layout and re-designs. It is therefore suitable for mass production, but not for a flexible development and the production of specific individual sensors, e.g. for space applications. Moreover a disadvantage is the relatively high material consumption, especially in combination with the sensors need of expensive noble metal and ceramic pastes, which leads to a high sensor unit price. The Inkjet technology however opens up completely new possibilities in terms of dimensions, geometries, structures, morphologies and materials of sensors. This new approach is capable of printing finer high-resolution layers without the necessity of meshes or masks for patterning. Using the Inkjet technology a design change is possible at any time on the CAD screen. Moreover the ink is only deposited where it is needed. Custom made sensors, as they are currently demanded in space sensor applications, are thus realized simply

Robotic synthesis of [carbon-11]methionine

International Nuclear Information System (INIS)

Korsakov, M.V.; Kisselev, M.Y.; Solovyov, D.; Horti, A.G.; Vasilev, A.; Nilsson, L.E.; Ulin, J.

1992-01-01

[ 11 C]Methionine was prepared in a fully automated robotic synthesis, using the SCANDITRONIX robotic system starting from [ 11 C]I and homocysteine thiolactone. The product was purified using solid phase extraction on anionic exchange cartridges. The decay corrected yield was 60% based on CH 3 I and 16 min synthesis time. The radiochemical purity was 98-99% and the chemical impurities were: homocysteine 0.05-0.07 mg/ml, homocystine 0.005 mg/ml, 'cold' methionine 0.03-0.05 mg/ml, and homocysteine thiolactone 0.0008-0.002 mg/ml. The total procedure takes 30 min from EOB. (author) 6 figs., 3 tabs

Synthesis of solid and hollow ATO spheres by carbothermal reduction of ATO nanoparticles

International Nuclear Information System (INIS)

Chai Chunfang; Huang Zaiyin; Liao Dankui; Tan Xuecai; Wu Jian; Yuan Aiqun

2007-01-01

Solid and hollow ATO spheres were fabricated by heating ATO nanoparticles and graphite mixture in a tube furnace. The as-synthesized samples were characterized by EDS, XRD, FE-SEM, TEM and HRTEM. The size of the solid spheres could be controlled by adjusting the rate of Ar flow and deposition positions. The hollow spheres were synthesized in an alumina tube system under conditions of a relatively high oxygen concentration. The growth mechanism of solid and hollow spheres was analysed

Synthesis, characterization, Hirshfeld surface and theoretical properties of (C.sub.7./sub.H.sub.10./sub.N).sub.4./sub.[H.sub.2./sub.P.sub.2./sub.Mo.sub.5./sub.O.sub.23./sub.]•H.sub.2./sub.O

Czech Academy of Sciences Publication Activity Database

Harchani, A.; Kučeráková, Monika; Dušek, Michal; Haddad, A.

2017-01-01

Roč. 8, Sep (2017), s. 1-9, č. článku 1361. ISSN 0974-3626 R&D Projects: GA ČR(CZ) GA15-12653S; GA MŠk LO1603 EU Projects: European Commission(XE) CZ.2.16/3.1.00/24510 Institutional support: RVO:68378271 Keywords : diphosphopentamolybdate * synthesis * crystal structure * physicochemical properties * theoretical study Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 1.235, year: 2016

Synthesis of multicomponent metallic layers during impulse plasma deposition

Directory of Open Access Journals (Sweden)

Nowakowska-Langier Katarzyna

2015-12-01

Full Text Available Pulsed plasma in the impulse plasma deposition (IPD synthesis is generated in a coaxial accelerator by strong periodic electrical pulses, and it is distributed in a form of energetic plasma packets. A nearly complete ionization of gas, in these conditions of plasma generation, favors the nucleation of new phase of ions and synthesis of metastable materials in a form of coatings which are characterized by amorphous and/or nanocrystalline structure. In this work, the Fe–Cu alloy, which is immiscible in the state of equilibrium, was selected as a model system to study the possibility of formation of a non-equilibrium phase during the IPD synthesis. Structural characterization of the layers was done by means of X-ray diffraction and conversion-electron Mössbauer spectroscopy. It was found that supersaturated solid solutions were created as a result of mixing and/or alloying effects between the layer components delivered to the substrate independently and separately in time. Therefore, the solubility in the Fe–Cu system was largely extended in relation to the equilibrium conditions, as described by the equilibrium phase diagram in the solid state.

Combinatorial synthesis of oxazol-thiazole bis-heterocyclic compounds.

Science.gov (United States)

Murru, Siva; Nefzi, Adel

2014-01-13

A combinatorial library of novel oxazol-thiazole bis-heterocycles was synthesized in good to excellent overall yields with high purity using a solution and solid-phase parallel synthesis approach. Oxazole amino acids, prepared from serine methyl ester and amino acids via coupling and cyclodehydration, were treated with Fmoc-NCS and α-haloketones for the parallel synthesis of diverse bis-heterocycles. Fmoc-isothiocyanate is used as a traceless reagent for thiazole formation. Oxazole diversity can be achieved by using variety of amino acids, whereas thiazole diversity is produced with various haloketones.

Monodisperse metal nanoparticle catalysts on silica mesoporous supports: synthesis, characterizations, and catalytic reactions

Energy Technology Data Exchange (ETDEWEB)

Somorjai, G.A.

2009-09-14

The design of high performance catalyst achieving near 100% product selectivity at maximum activity is one of the most important goals in the modern catalytic science research. To this end, the preparation of model catalysts whose catalytic performances can be predicted in a systematic and rational manner is of significant importance, which thereby allows understanding of the molecular ingredients affecting the catalytic performances. We have designed novel 3-dimensional (3D) high surface area model catalysts by the integration of colloidal metal nanoparticles and mesoporous silica supports. Monodisperse colloidal metal NPs with controllable size and shape were synthesized using dendrimers, polymers, or surfactants as the surface stabilizers. The size of Pt, and Rh nanoparticles can be varied from sub 1 nm to 15 nm, while the shape of Pt can be controlled to cube, cuboctahedron, and octahedron. The 3D model catalysts were generated by the incorporation of metal nanoparticles into the pores of mesoporous silica supports via two methods: capillary inclusion (CI) and nanoparticle encapsulation (NE). The former method relies on the sonication-induced inclusion of metal nanoparticles into the pores of mesoporous silica, whereas the latter is performed by the encapsulation of metal nanoparticles during the hydrothermal synthesis of mesoporous silica. The 3D model catalysts were comprehensively characterized by a variety of physical and chemical methods. These catalysts were found to show structure sensitivity in hydrocarbon conversion reactions. The Pt NPs supported on mesoporous SBA-15 silica (Pt/SBA-15) displayed significant particle size sensitivity in ethane hydrogenolysis over the size range of 1-7 nm. The Pt/SBA-15 catalysts also exhibited particle size dependent product selectivity in cyclohexene hydrogenation, crotonaldehyde hydrogenation, and pyrrole hydrogenation. The Rh loaded SBA-15 silica catalyst showed structure sensitivity in CO oxidation reaction. In

Synthesis of new water-soluble metal-binding polymers: Combinatorial chemistry approach. 1998 annual progress report

International Nuclear Information System (INIS)

Kurth, M.J.; Miller, R.B.; Sawan, S.; Smith, B.F.

1998-01-01

'(1) Develop rapid discovery and optimization approaches to new water-soluble chelating polymers for use in Polymer Filtration (PF) systems, and (2) evaluate the concept of using water and organic soluble polymers as new solid supports for combinatorial synthesis. Polymer Filtration (PF), which uses water-soluble metal-binding polymers to sequester metal ions in dilute solution with ultrafiltration (UF) to separate the polymers, is a new technology to selectively remove or recover hazardous and valuable metal ions. Future directions in PF must include rapid development, testing, and characterization of new metal-binding polymers. Thus, the authors are building upon and adapting the combinatorial chemistry approach developed for rapid molecule generation for the drug industry to the rapid development of new chelating polymers. The authors have focused on four areas including the development of: (1) synthetic procedures, (2) small ultrafiltration equipment compatible with organic- and aqueous-based combinatorial synthesis, (3) rapid assay techniques, and (4) polymer characterization techniques.'

Fischer-Tropsch synthesis. Development and perspectives