Preparation and characterization of nanoparticles of carboxymethyl cellulose acetate butyrate containing acyclovir

NASA Astrophysics Data System (ADS)

Vedula, Venkata Bharadwaz; Chopra, Maulick; Joseph, Emil; Mazumder, Sonal

2016-02-01

Nanoparticles of carboxymethyl cellulose acetate butyrate complexed with the poorly soluble antiviral drug acyclovir (ACV) were produced by precipitation process and the formulation process and properties of nanoparticles were investigated. Two different particle synthesis methods were explored—a conventional precipitation method and a rapid precipitation in a multi-inlet vortex mixer. The particles were processed by rotavap followed by freeze-drying. Particle diameters as measured by dynamic light scattering were dependent on the synthesis method used. The conventional precipitation method did not show desired particle size distribution, whereas particles prepared by the mixer showed well-defined particle size ~125-450 nm before and after freeze-drying, respectively, with narrow polydispersity indices. Fourier transform infrared spectroscopy showed chemical stability and intactness of entrapped drug in the nanoparticles. Differential scanning calorimetry showed that the drug was in amorphous state in the polymer matrix. ACV drug loading was around 10 wt%. The release studies showed increase in solution concentration of drug from the nanoparticles compared to the as-received crystalline drug.

Combinatorial synthesis of phosphors using arc-imaging furnace

PubMed Central

Ishigaki, Tadashi; Toda, Kenji; Yoshimura, Masahiro; Uematsu, Kazuyoshi; Sato, Mineo

2011-01-01

We have applied a novel ‘melt synthesis technique’ rather than a conventional solid-state reaction to rapidly synthesize phosphor materials. During a synthesis, the mixture of oxides or their precursors is melted by light pulses (10–60 s) in an arc-imaging furnace on a water-cooled copper hearth to form a globule of 1–5 mm diameter, which is then rapidly cooled by turning off the light. Using this method, we synthesized several phosphor compounds including Y3Al5O12:Ce(YAG) and SrAl2O4:Eu,Dy. Complex phosphor oxides are difficult to produce by conventional solid-state reaction techniques because of the slow reaction rates among solid oxides; as a result, the oxides form homogeneous compounds or solid solutions. On the other hand, melt reactions are very fast (10–60 s) and result in homogeneous compounds owing to rapid diffusion and mixing in the liquid phase. Therefore, melt synthesis techniques are suitable for preparing multi component homogeneous compounds and solid solutions. PMID:27877432

Combinatorial synthesis of phosphors using arc-imaging furnace

NASA Astrophysics Data System (ADS)

Ishigaki, Tadashi; Toda, Kenji; Yoshimura, Masahiro; Uematsu, Kazuyoshi; Sato, Mineo

2011-10-01

We have applied a novel 'melt synthesis technique' rather than a conventional solid-state reaction to rapidly synthesize phosphor materials. During a synthesis, the mixture of oxides or their precursors is melted by light pulses (10-60 s) in an arc-imaging furnace on a water-cooled copper hearth to form a globule of 1-5 mm diameter, which is then rapidly cooled by turning off the light. Using this method, we synthesized several phosphor compounds including Y3Al5O12:Ce(YAG) and SrAl2O4:Eu,Dy. Complex phosphor oxides are difficult to produce by conventional solid-state reaction techniques because of the slow reaction rates among solid oxides; as a result, the oxides form homogeneous compounds or solid solutions. On the other hand, melt reactions are very fast (10-60 s) and result in homogeneous compounds owing to rapid diffusion and mixing in the liquid phase. Therefore, melt synthesis techniques are suitable for preparing multi component homogeneous compounds and solid solutions.

Rapid and accurate synthesis of TALE genes from synthetic oligonucleotides.

PubMed

Wang, Fenghua; Zhang, Hefei; Gao, Jingxia; Chen, Fengjiao; Chen, Sijie; Zhang, Cuizhen; Peng, Gang

2016-01-01

Custom synthesis of transcription activator-like effector (TALE) genes has relied upon plasmid libraries of pre-fabricated TALE-repeat monomers or oligomers. Here we describe a novel synthesis method that directly incorporates annealed synthetic oligonucleotides into the TALE-repeat units. Our approach utilizes iterative sets of oligonucleotides and a translational frame check strategy to ensure the high efficiency and accuracy of TALE-gene synthesis. TALE arrays of more than 20 repeats can be constructed, and the majority of the synthesized constructs have perfect sequences. In addition, this novel oligonucleotide-based method can readily accommodate design changes to the TALE repeats. We demonstrated an increased gene targeting efficiency against a genomic site containing a potentially methylated cytosine by incorporating non-conventional repeat variable di-residue (RVD) sequences.

Soft context clustering for F0 modeling in HMM-based speech synthesis

NASA Astrophysics Data System (ADS)

Khorram, Soheil; Sameti, Hossein; King, Simon

2015-12-01

This paper proposes the use of a new binary decision tree, which we call a soft decision tree, to improve generalization performance compared to the conventional `hard' decision tree method that is used to cluster context-dependent model parameters in statistical parametric speech synthesis. We apply the method to improve the modeling of fundamental frequency, which is an important factor in synthesizing natural-sounding high-quality speech. Conventionally, hard decision tree-clustered hidden Markov models (HMMs) are used, in which each model parameter is assigned to a single leaf node. However, this `divide-and-conquer' approach leads to data sparsity, with the consequence that it suffers from poor generalization, meaning that it is unable to accurately predict parameters for models of unseen contexts: the hard decision tree is a weak function approximator. To alleviate this, we propose the soft decision tree, which is a binary decision tree with soft decisions at the internal nodes. In this soft clustering method, internal nodes select both their children with certain membership degrees; therefore, each node can be viewed as a fuzzy set with a context-dependent membership function. The soft decision tree improves model generalization and provides a superior function approximator because it is able to assign each context to several overlapped leaves. In order to use such a soft decision tree to predict the parameters of the HMM output probability distribution, we derive the smoothest (maximum entropy) distribution which captures all partial first-order moments and a global second-order moment of the training samples. Employing such a soft decision tree architecture with maximum entropy distributions, a novel speech synthesis system is trained using maximum likelihood (ML) parameter re-estimation and synthesis is achieved via maximum output probability parameter generation. In addition, a soft decision tree construction algorithm optimizing a log-likelihood measure is developed. Both subjective and objective evaluations were conducted and indicate a considerable improvement over the conventional method.

Method and apparatus for producing synthesis gas

DOEpatents

Hemmings, John William; Bonnell, Leo; Robinson, Earl T.

2010-03-03

A method and apparatus for reacting a hydrocarbon containing feed stream by steam methane reforming reactions to form a synthesis gas. The hydrocarbon containing feed is reacted within a reactor having stages in which the final stage from which a synthesis gas is discharged incorporates expensive high temperature materials such as oxide dispersed strengthened metals while upstream stages operate at a lower temperature allowing the use of more conventional high temperature alloys. Each of the reactor stages incorporate reactor elements having one or more separation zones to separate oxygen from an oxygen containing feed to support combustion of a fuel within adjacent combustion zones, thereby to generate heat to support the endothermic steam methane reforming reactions.

Energy efficient room temperature synthesis of cardanol-based novolac resin using acoustic cavitation.

PubMed

Jadhav, Nilesh L; Sastry, Sai Krishna C; Pinjari, Dipak V

2018-04-01

The present study deals with synthesis of cardanol-cased novolac (CBN) resin by the condensation reaction between cardanol and formaldehyde using acoustic cavitation. It is a step-growth polymerization which occurs in the presence of an acid catalyst such as adipic acid, citric acid, oxalic acid, sulphuric acid and hydrochloric acid. CBN was also synthesised by a conventional method for the sake of comparison of techniques. The effect of molar ratio, effect of catalyst, effect of different catalyst and effect of power on the conversion to CBN has been studied. The synthesised CBN was characterized using the Fourier Transform Infra Red Spectroscopy (FTIR), Gel Permeation Chromatography (GPC), Nuclear Magnetic Resonance (NMR) Spectroscopy and Thermogravimetric Analysis (TGA). The reaction was monitored by the Acid value, free formaldehyde content and viscosity of the synthesised product. The reaction time required for the conventionally synthesised CBN was 5 h (300 min) with 120 °C as an operating temperature while sonochemically the time reduced to 30 min at room temperature. The amount of time and energy saved can be quantified. Ultrasound facilitated synthesis was found to be an energy efficient and time-saving method for the synthesis of novolac resin. Copyright © 2017 Elsevier B.V. All rights reserved.

Properties of TiNi intermetallic compound industrially produced by combustion synthesis

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

Kaieda, Yoshinari

Most TiNi shape memory intermetallic compounds are conventionally produced by the process including high frequency induction vacuum melting and casting. A gravity segregation occurs in a cast TiNi ingot because of the big difference in the specific gravity between Ti and Ni. It is difficult to control accurately the phase transformation temperature of TiNi shape memory intermetallic compound produced by the conventional process, because the martensitic transformation temperature shifts by 10K due to the change in 0.1 % of Ni content. Homogeneous TiNi intermetallic compound is produced by the industrial process including combustion synthesis method, which is a newly developedmore » manufacturing process. In the new process, phase transformation temperatures of TiNi can be controlled accurately by controlling the ratio of Ti and Ni elemental starting powders. The chemical component, the impurities and the phase transformation temperatures of the TiNi products industrially produced by the process are revealed. These properties are vitally important when combustion synthesis method is applied to an industrial mass production process for producing TiNi shape memory intermetallic compounds. TiNi shape memory products are industrially and commercially produced today the industrial process including combustion synthesis. The total production weight in a year is 30 tins in 1994.« less

Microwave-assisted synthesis of sensitive silver substrate for surface-enhanced Raman scattering spectroscopy

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

Xia Lixin; Wang Haibo; Wang Jian

A sensitive silver substrate for surface-enhanced Raman scattering (SERS) spectroscopy is synthesized under multimode microwave irradiation. The microwave-assisted synthesis of the SERS-active substrate was carried out in a modified domestic microwave oven of 2450 MHz, and the reductive reaction was conducted in a polypropylene container under microwave irradiation with a power of 100 W for 5 min. Formaldehyde was employed as both the reductant and microwave absorber in the reductive process. The effects of different heating methods (microwave dielectric and conventional) on the properties of the SERS-active substrates were investigated. Samples obtained with 5 min of microwave irradiation at amore » power of 100 W have more well-defined edges, corners, and sharper surface features, while the samples synthesized with 1 h of conventional heating at 40 deg. C consist primarily of spheroidal nanoparticles. The SERS peak intensity of the {approx}1593 cm{sup -1} band of 4-mercaptobenzoic acid adsorbed on silver nanoparticles synthesized with 5 min of microwave irradiation at a power of 100 W is about 30 times greater than when it is adsorbed on samples synthesized with 1 h of conventional heating at 40 deg. C. The results of quantum chemical calculations are in good agreement with our experimental data. This method is expected to be utilized for the synthesis of other metal nanostructural materials.« less

Facile method for the synthesis of gold nanoparticles using an ion coater

NASA Astrophysics Data System (ADS)

Lee, Seung Han; Jung, Hyun Kyu; Kim, Tae Cheol; Kim, Chang Hee; Shin, Chang Hwan; Yoon, Tae-Sik; Hong, A.-Ra; Jang, Ho Seong; Kim, Dong Hun

2018-03-01

Herein we report a metal nanoparticle synthesis method based on a physical vapor deposition process instead of the conventional wet process of chemical reactions in liquids. A narrow size distribution of synthesized gold nanoparticles was obtained using an ion coater on glycerin at low vapor pressure. The nanoparticle size could be modulated by controlling the sputtering conditions especially the discharge current. Due to the formation of gold nanoparticles, a surface plasmon resonance peak appeared at ∼530 nm in the absorption spectrum. The surface plasmon resonance peak exhibited red-shift with increasing size of the gold nanoparticles. Our results provide a simple, environmental friendly method for the synthesis of metal nanoparticles by combine low-cost deposition apparatus and a liquid medium, which is free from toxic reagents.

Effect of mechanical alloying synthesis process on the dielectric properties of (Bi{sub 0.5}Na{sub 0.5}){sub 0.94}Ba{sub 0.06}TiO{sub 3} piezoceramics

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

Ghazanfari, Mohammad Reza, E-mail: Ghazanfari.mr@gmail.com; Amini, Rasool; Shams, Seyyedeh Fatemeh

Highlights: • MA samples show higher dielectric permittivity and Curie temperature. • In MA samples, dielectric loss is almost 27% less than conventional ones. • In MA samples, sintering time and temperature are lower than conventional ones. • In MA samples, particle morphology is more homogeneous conventional ones. • In MA samples, crystallite size is smaller conventional ones. - Abstract: In present work, in order to study the effects of synthesis techniques on dielectric properties, the BNBT lead-free piezoceramics with (Bi{sub 0.5}Na{sub 0.5}){sub 0.94}Ba{sub 0.06}TiO{sub 3} stoichiometry (called as BNBT6) were synthesized by mechanical alloying (MA) and conventional mixed oxidesmore » methods. The structural, microstructural, and dielectric properties were carried out by X-ray diffractometer (XRD), scanning electron microscope (SEM), and impedance analyzer LCR meter, respectively. Based on results, the density of MA samples is considerably higher than conventional samples owning to smaller particles size and more uniformity of particle shape of MA samples. Moreover, the dielectric properties of MA samples are comparatively improved in which the dielectric loss of these samples is almost 27% less than conventional ones. Furthermore, MA samples exhibit obviously higher dielectric permittivity and Curie temperature compared to the conventional samples.« less

One-pot and efficient synthesis of triazolo[1,2-a]indazole-triones via reaction of arylaldehydes with urazole and dimedone catalyzed by silica nanoparticles prepared from rice husk.

PubMed

Hamidian, Hooshang; Fozooni, Samieh; Hassankhani, Asadollah; Mohammadi, Sayed Zia

2011-10-26

A novel synthesis of triazolo[1,2-a]indazole-1,3,8-trione derivatives by reaction of urazole, dimedone and aromatic aldehydes under conventional heating and microwave irradiation and solvent-free conditions using silica nanoparticles prepared from rice husk ash as catalyst is described. The new method features high yields, multicomponent reactions and environmental friendliness.

Metal‐Catalysed Azidation of Organic Molecules

PubMed Central

Goswami, Monalisa

2016-01-01

The azide moiety is a desirable functionality in organic molecules, useful in a variety of transformations such as olefin aziridination, C–H bond amination, isocyanate synthesis, the Staudinger reaction and the formation of azo compounds. To harness the versatility of the azide functionality fully it is important that these compounds be easy to prepare, in a clean and cost‐effective manner. Conventional (non‐catalysed) methods to synthesise azides generally require quite harsh reaction conditions that are often not tolerant of functional groups. In the last decade, several metal‐catalysed azidations have been developed in attempts to circumvent this problem. These methods are generally faster, cleaner and more functional‐group‐tolerant than conventional methods to prepare azides, and can sometimes even be conveniently combined with one‐pot follow‐up transformations of the installed azide moiety. This review highlights metal‐catalysed approaches to azide synthesis, with a focus on the substrate scopes and mechanisms, as well as on advantages and disadvantages of the methods. Overall, metal‐catalysed azidation reactions provide shorter routes to a variety of potentially useful organic molecules containing the azide moiety. PMID:28344503

Combustion synthesis of ceramic-metal composite materials in microgravity

NASA Technical Reports Server (NTRS)

Moore, John

1995-01-01

Combustion synthesis, self-propagating high temperature synthesis (SHS) or reactive synthesis provides an attractive alternative to conventional methods of producing advanced materials since this technology is based on the ability of highly exothermic reactions to be self sustaining and, therefore, energetically efficient. The exothermic SHS reaction is initiated at the ignition temperature, T(sub ig), and generates heat which is manifested in a maximum or combustion temperature, T(sub c), which can exceed 3000 K . Such high combustion temperatures are capable of melting and/or volatilizing reactant and product species and, therefore, present an opportunity for producing structure and property modification and control through liquid-solid, vapor-liquid-solid, and vapor-solid transformations.

Unifying Gate Synthesis and Magic State Distillation.

PubMed

Campbell, Earl T; Howard, Mark

2017-02-10

The leading paradigm for performing a computation on quantum memories can be encapsulated as distill-then-synthesize. Initially, one performs several rounds of distillation to create high-fidelity magic states that provide one good T gate, an essential quantum logic gate. Subsequently, gate synthesis intersperses many T gates with Clifford gates to realize a desired circuit. We introduce a unified framework that implements one round of distillation and multiquibit gate synthesis in a single step. Typically, our method uses the same number of T gates as conventional synthesis but with the added benefit of quadratic error suppression. Because of this, one less round of magic state distillation needs to be performed, leading to significant resource savings.

Novel route for rapid sol-gel synthesis of hydroxyapatite, avoiding ageing and using fast drying with a 50-fold to 200-fold reduction in process time.

PubMed

Ben-Arfa, Basam A E; Salvado, Isabel M Miranda; Ferreira, José M F; Pullar, Robert C

2017-01-01

We have developed an innovative, rapid sol-gel method of producing hydroxyapatite nanopowders that avoids the conventional lengthy ageing and drying processes (over a week), being 200 times quicker in comparison to conventional aqueous sol-gel preparation, and 50 times quicker than ethanol based sol-gel synthesis. Two different sets of experimental conditions, in terms of pH value (5.5 and 7.5), synthesis temperature (45 and 90°C), drying temperature (60 and 80°C) and calcination temperature (400 and 700°C) were explored. The products were characterised by X-ray diffraction (XRD) Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and specific surface area (SSA) measurements. Pure hydroxyapatite (Ca 10 (PO 4 ) 6 (OH) 2 , HAp) was obtained for the powders synthesised at pH7.5 and calcined at 400°C, while biphasic mixtures of HAp/β-tricalcium phosphate (β-Ca 3 (PO 4 ) 2 , TCP) were produced at pH5.5 and (pH7.5 at elevated temperature). The novel rapid drying was up to 200 times faster than conventional drying, only needing 1h with no prior ageing step, and favoured the formation of smaller/finer nanopowders, while producing pure HAp or phase mixtures virtually identical to those obtained from the slow conventional drying method, despite the absence of a slow ageing process. The products of this novel rapid process were actually shown to have smaller crystallite sizes and larger SSA, which should result in increased bioactivity. Copyright © 2016 Elsevier B.V. All rights reserved.

Photonic Crystal Biosensor with In-Situ Synthesized DNA Probes for Enhanced Sensitivity

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

Hu, Shuren; Zhao, Y.; Retterer, Scott T

2013-01-01

We report on a nearly 8-fold increase in multi-hole defect photonic crystal biosensor response by incorporating in-situ synthesis of DNA probes, as compared to the conventional functionalization method employing pre-synthesized DNA probe immobilization.

Difunctionalization of alkenes with iodine and tert-butyl hydroperoxide (TBHP) at room temperature for the synthesis of 1-(tert-butylperoxy)-2-iodoethanes.

PubMed

Wang, Hao; Chen, Cui; Liu, Weibing; Zhu, Zhibo

2017-01-01

We developed a direct vicinal difunctionalization of alkenes with iodine and TBHP at room temperature. This iodination and peroxidation in a one-pot synthesis produces 1-( tert -butylperoxy)-2-iodoethanes, which are inaccessible through conventional synthetic methods. This method generates multiple radical intermediates in situ and has excellent regioselectivity, a broad substrate scope and mild conditions. The iodine and peroxide groups of 1-( tert -butylperoxy)-2-iodoethanes have several potential applications and allow further chemical modifications, enabling the preparation of synthetically valuable molecules.

A general strategy toward the rational synthesis of metal tungstate nanostructures using plasma electrolytic oxidation method

NASA Astrophysics Data System (ADS)

Jiang, Yanan; Liu, Baodan; Zhai, Zhaofeng; Liu, Xiaoyuan; Yang, Bing; Liu, Lusheng; Jiang, Xin

2015-11-01

A new method based on conventional plasma electrolytic oxidation (PEO) technology has been developed for the rational synthesis of metal tungstate nanostructures. Using this method, ZnWO4 and NiWO4 nanostructures with controllable morphologies (nanorods, nanosheets and microsheets) and superior crystallinity have been synthesized. It has been found that the morphology diversity of ZnWO4 nanostructures can be selectively tailored through tuning the electrolyte concentration and annealing temperatures, showing obvious advantages in comparison to traditional hydrothermal and sol-gel methods. Precise microscopy analyses on the cross section of the PEO coating and ZnWO4 nanostructures confirmed that the precursors initially precipitated in the PEO coating and its surface during plasma discharge process are responsible for the nucleation and subsequent growth of metal tungstate nanostructures by thermal annealing. The method developed in this work represents a general strategy toward the rational synthesis of metal oxide nanostructures and the formation mechanism of metal tungstate nanostructures fabricated by the PEO method is finally discussed.

Multifrequency synthesis and extraction using square wave projection patterns for quantitative tissue imaging.

PubMed

Nadeau, Kyle P; Rice, Tyler B; Durkin, Anthony J; Tromberg, Bruce J

2015-11-01

We present a method for spatial frequency domain data acquisition utilizing a multifrequency synthesis and extraction (MSE) method and binary square wave projection patterns. By illuminating a sample with square wave patterns, multiple spatial frequency components are simultaneously attenuated and can be extracted to determine optical property and depth information. Additionally, binary patterns are projected faster than sinusoids typically used in spatial frequency domain imaging (SFDI), allowing for short (millisecond or less) camera exposure times, and data acquisition speeds an order of magnitude or more greater than conventional SFDI. In cases where sensitivity to superficial layers or scattering is important, the fundamental component from higher frequency square wave patterns can be used. When probing deeper layers, the fundamental and harmonic components from lower frequency square wave patterns can be used. We compared optical property and depth penetration results extracted using square waves to those obtained using sinusoidal patterns on an in vivo human forearm and absorbing tube phantom, respectively. Absorption and reduced scattering coefficient values agree with conventional SFDI to within 1% using both high frequency (fundamental) and low frequency (fundamental and harmonic) spatial frequencies. Depth penetration reflectance values also agree to within 1% of conventional SFDI.

Multifrequency synthesis and extraction using square wave projection patterns for quantitative tissue imaging

PubMed Central

Nadeau, Kyle P.; Rice, Tyler B.; Durkin, Anthony J.; Tromberg, Bruce J.

2015-01-01

Abstract. We present a method for spatial frequency domain data acquisition utilizing a multifrequency synthesis and extraction (MSE) method and binary square wave projection patterns. By illuminating a sample with square wave patterns, multiple spatial frequency components are simultaneously attenuated and can be extracted to determine optical property and depth information. Additionally, binary patterns are projected faster than sinusoids typically used in spatial frequency domain imaging (SFDI), allowing for short (millisecond or less) camera exposure times, and data acquisition speeds an order of magnitude or more greater than conventional SFDI. In cases where sensitivity to superficial layers or scattering is important, the fundamental component from higher frequency square wave patterns can be used. When probing deeper layers, the fundamental and harmonic components from lower frequency square wave patterns can be used. We compared optical property and depth penetration results extracted using square waves to those obtained using sinusoidal patterns on an in vivo human forearm and absorbing tube phantom, respectively. Absorption and reduced scattering coefficient values agree with conventional SFDI to within 1% using both high frequency (fundamental) and low frequency (fundamental and harmonic) spatial frequencies. Depth penetration reflectance values also agree to within 1% of conventional SFDI. PMID:26524682

Kinematic synthesis of adjustable robotic mechanisms

NASA Astrophysics Data System (ADS)

Chuenchom, Thatchai

1993-01-01

Conventional hard automation, such as a linkage-based or a cam-driven system, provides high speed capability and repeatability but not the flexibility required in many industrial applications. The conventional mechanisms, that are typically single-degree-of-freedom systems, are being increasingly replaced by multi-degree-of-freedom multi-actuators driven by logic controllers. Although this new trend in sophistication provides greatly enhanced flexibility, there are many instances where the flexibility needs are exaggerated and the associated complexity is unnecessary. Traditional mechanism-based hard automation, on the other hand, neither can fulfill multi-task requirements nor are cost-effective mainly due to lack of methods and tools to design-in flexibility. This dissertation attempts to bridge this technological gap by developing Adjustable Robotic Mechanisms (ARM's) or 'programmable mechanisms' as a middle ground between high speed hard automation and expensive serial jointed-arm robots. This research introduces the concept of adjustable robotic mechanisms towards cost-effective manufacturing automation. A generalized analytical synthesis technique has been developed to support the computational design of ARM's that lays the theoretical foundation for synthesis of adjustable mechanisms. The synthesis method developed in this dissertation, called generalized adjustable dyad and triad synthesis, advances the well-known Burmester theory in kinematics to a new level. While this method provides planar solutions, a novel patented scheme is utilized for converting prescribed three-dimensional motion specifications into sets of planar projections. This provides an analytical and a computational tool for designing adjustable mechanisms that satisfy multiple sets of three-dimensional motion specifications. Several design issues were addressed, including adjustable parameter identification, branching defect, and mechanical errors. An efficient mathematical scheme for identification of adjustable member was also developed. The analytical synthesis techniques developed in this dissertation were successfully implemented in a graphic-intensive user-friendly computer program. A physical prototype of a general purpose adjustable robotic mechanism has been constructed to serve as a proof-of-concept model.

PlenoPatch: Patch-Based Plenoptic Image Manipulation.

PubMed

Zhang, Fang-Lue; Wang, Jue; Shechtman, Eli; Zhou, Zi-Ye; Shi, Jia-Xin; Hu, Shi-Min

2017-05-01

Patch-based image synthesis methods have been successfully applied for various editing tasks on still images, videos and stereo pairs. In this work we extend patch-based synthesis to plenoptic images captured by consumer-level lenselet-based devices for interactive, efficient light field editing. In our method the light field is represented as a set of images captured from different viewpoints. We decompose the central view into different depth layers, and present it to the user for specifying the editing goals. Given an editing task, our method performs patch-based image synthesis on all affected layers of the central view, and then propagates the edits to all other views. Interaction is done through a conventional 2D image editing user interface that is familiar to novice users. Our method correctly handles object boundary occlusion with semi-transparency, thus can generate more realistic results than previous methods. We demonstrate compelling results on a wide range of applications such as hole-filling, object reshuffling and resizing, changing object depth, light field upscaling and parallax magnification.

Effectiveness of en masse versus two-step retraction: a systematic review and meta-analysis.

PubMed

Rizk, Mumen Z; Mohammed, Hisham; Ismael, Omar; Bearn, David R

2018-01-05

This review aims to compare the effectiveness of en masse and two-step retraction methods during orthodontic space closure regarding anchorage preservation and anterior segment retraction and to assess their effect on the duration of treatment and root resorption. An electronic search for potentially eligible randomized controlled trials and prospective controlled trials was performed in five electronic databases up to July 2017. The process of study selection, data extraction, and quality assessment was performed by two reviewers independently. A narrative review is presented in addition to a quantitative synthesis of the pooled results where possible. The Cochrane risk of bias tool and the Newcastle-Ottawa Scale were used for the methodological quality assessment of the included studies. Eight studies were included in the qualitative synthesis in this review. Four studies were included in the quantitative synthesis. En masse/miniscrew combination showed a statistically significant standard mean difference regarding anchorage preservation - 2.55 mm (95% CI - 2.99 to - 2.11) and the amount of upper incisor retraction - 0.38 mm (95% CI - 0.70 to - 0.06) when compared to a two-step/conventional anchorage combination. Qualitative synthesis suggested that en masse retraction requires less time than two-step retraction with no difference in the amount of root resorption. Both en masse and two-step retraction methods are effective during the space closure phase. The en masse/miniscrew combination is superior to the two-step/conventional anchorage combination with regard to anchorage preservation and amount of retraction. Limited evidence suggests that anchorage reinforcement with a headgear produces similar results with both retraction methods. Limited evidence also suggests that en masse retraction may require less time and that no significant differences exist in the amount of root resorption between the two methods.

A review on radiation-induced nucleation and growth of colloidal metallic nanoparticles

PubMed Central

2013-01-01

This review presents an introduction to the synthesis of metallic nanoparticles by radiation-induced method, especially gamma irradiation. This method offers some benefits over the conventional methods because it provides fully reduced and highly pure nanoparticles free from by-products or chemical reducing agents, and is capable of controlling the particle size and structure. The nucleation and growth mechanism of metallic nanoparticles are also discussed. The competition between nucleation and growth process in the formation of nanoparticles can determine the size of nanoparticles which is influenced by certain parameters such as the choice of solvents and stabilizer, the precursor to stabilizer ratio, pH during synthesis, and absorbed dose. PMID:24225302

Synthesis of Monodisperse Chitosan Nanoparticles and in Situ Drug Loading Using Active Microreactor.

PubMed

Kamat, Vivek; Marathe, Ila; Ghormade, Vandana; Bodas, Dhananjay; Paknikar, Kishore

2015-10-21

Chitosan nanoparticles are promising drug delivery vehicles. However, the conventional method of unregulated mixing during ionic gelation limits their application because of heterogeneity in size and physicochemical properties. Therefore, a detailed theoretical analysis of conventional and active microreactor models was simulated. This led to design and fabrication of a polydimethylsiloxane microreactor with magnetic micro needles for the synthesis of monodisperse chitosan nanoparticles. Chitosan nanoparticles synthesized conventionally, using 0.5 mg/mL chitosan, were 250 ± 27 nm with +29.8 ± 8 mV charge. Using similar parameters, the microreactor yielded small size particles (154 ± 20 nm) at optimized flow rate of 400 μL/min. Further optimization at 0.4 mg/mL chitosan concentration yielded particles (130 ± 9 nm) with higher charge (+39.8 ± 5 mV). The well-controlled microreactor-based mixing generated highly monodisperse particles with tunable properties including antifungal drug entrapment (80%), release rate, and effective activity (MIC, 1 μg/mL) against Candida.

A Three-Dimensional Hydrodynamic Focusing Method for Polyplex Synthesis

PubMed Central

Lu, Mengqian; Ho, Yi-Ping; Grigsby, Christopher L.; Nawaz, Ahmad Ahsan; Leong, Kam W.; Huang, Tony Jun

2014-01-01

Successful intracellular delivery of nucleic acid therapeutics relies on multi-aspect optimization, one of which is formulation. While there has been ample innovation on chemical design of polymeric gene carriers, the same cannot be said for physical processing of polymer-DNA nanocomplexes (polyplexes). Conventional synthesis of polyplexes by bulk mixing depends on the operators’ experience. The poorly controlled bulk-mixing process may also lead to batch-to-batch variation and consequent irreproducibility. Here, we synthesize polyplexes by using a three-dimensional hydrodynamic focusing (3D-HF) technique in a single-layered, planar microfluidic device. Without any additional chemical treatment or post processing, the polyplexes prepared by the 3D-HF method show smaller size, slower aggregation rate, and higher transfection efficiency, while exhibiting reduced cytotoxicity compared to the ones synthesized by conventional bulk mixing. In addition, by introducing external acoustic perturbation, mixing can be further enhanced, leading to even smaller nanocomplexes. The 3D-HF method provides a simple and reproducible process for synthesizing high-quality polyplexes, addressing a critical barrier in the eventual translation of nucleic acid therapeutics. PMID:24341632

Highly effective synthesis of a cobalt(ii) metal-organic coordination polymer by using continuous flow chemistry.

PubMed

Gong, Chunhua; Zhang, Junyong; Zeng, Xianghua; Xie, Jingli

2016-12-20

The coordination polymer [Co 2 L 4 (H 2 O) 2 ]·CH 3 CN·H 2 O (HL = (E)-2-[2-(4-chlorophenyl)vinyl]-8-hydroxyquinoline) has been achieved with 95% yield by using an Asia flow synthesis system (chip reactor). Compared with the conventional batch-type methods such as diffusion, reflux and solvothermal reactions, higher yielding reactions carried out in a flow reactor have demonstrated that this technique is a powerful strategy to obtain coordination compounds.

The integrated manual and automatic control of complex flight systems

NASA Technical Reports Server (NTRS)

Schmidt, D. K.

1983-01-01

Development of a unified control synthesis methodology for complex and/or non-conventional flight vehicles, and prediction techniques for the handling characteristics of such vehicles are reported. Identification of pilot dynamics and objectives, using time domain and frequency domain methods is proposed.

Aerobic method for the synthesis of nearly size-monodisperse bismuth nanoparticles from a redox non-innocent precursor

NASA Astrophysics Data System (ADS)

Winter, H.; Christopher-Allison, E.; Brown, A. L.; Goforth, A. M.

2018-04-01

Herein, we report an aerobic synthesis method to produce bismuth nanoparticles (Bi NPs) with average diameters in the range 40-80 nm using commercially available bismuth triiodide (BiI3) as the starting material; the method uses only readily available chemicals and conventional laboratory equipment. Furthermore, size data from replicates of the synthesis under standard reaction conditions indicate that this method is highly reproducible in achieving Bi NP populations with low standard deviations in the mean diameters. We also investigated the mechanism of the reaction, which we determined results from the reduction of a soluble alkylammonium iodobismuthate precursor species formed in situ. Under appropriate concentration conditions of iodobismuthate anion, we demonstrate that burst nucleation of Bi NPs results from reduction of Bi3+ by the coordinated, redox non-innocent iodide ligands when a threshold temperature is exceeded. Finally, we demonstrate phase transfer and silica coating of the Bi NPs, which results in stable aqueous colloids with retention of size, morphology, and colloidal stability. The resultant, high atomic number, hydrophilic Bi NPs prepared using this synthesis method have potential for application in emerging x-ray contrast and x-ray therapeutic applications.

What Synthesis Methodology Should I Use? A Review and Analysis of Approaches to Research Synthesis

PubMed Central

Schick-Makaroff, Kara; MacDonald, Marjorie; Plummer, Marilyn; Burgess, Judy; Neander, Wendy

2016-01-01

Background When we began this process, we were doctoral students and a faculty member in a research methods course. As students, we were facing a review of the literature for our dissertations. We encountered several different ways of conducting a review but were unable to locate any resources that synthesized all of the various synthesis methodologies. Our purpose is to present a comprehensive overview and assessment of the main approaches to research synthesis. We use ‘research synthesis’ as a broad overarching term to describe various approaches to combining, integrating, and synthesizing research findings. Methods We conducted an integrative review of the literature to explore the historical, contextual, and evolving nature of research synthesis. We searched five databases, reviewed websites of key organizations, hand-searched several journals, and examined relevant texts from the reference lists of the documents we had already obtained. Results We identified four broad categories of research synthesis methodology including conventional, quantitative, qualitative, and emerging syntheses. Each of the broad categories was compared to the others on the following: key characteristics, purpose, method, product, context, underlying assumptions, unit of analysis, strengths and limitations, and when to use each approach. Conclusions The current state of research synthesis reflects significant advancements in emerging synthesis studies that integrate diverse data types and sources. New approaches to research synthesis provide a much broader range of review alternatives available to health and social science students and researchers. PMID:29546155

In situ synthesis-gelation at room temperature vs. heating-cooling procedure. Fine tuning of molecular gels derived from succinic acid and L-valine.

PubMed

Fontanillo, Miriam; Angulo-Pachón, César A; Escuder, Beatriu; Miravet, Juan F

2013-12-15

The reaction between succinic anhydride and a diamine derived from L-valine should afford efficiently a molecular gelator. Based on this reaction, it should be feasible to prepare molecular gels at room temperature, avoiding the conventional thermal treatment required for the solubilization of the gelator, by in situ, simultaneous, synthesis and gelation. The gels prepared by in situ and conventional heating-cooling protocols could present important differences relevant for potential practical applications of these materials. The gelator was synthesized by reaction of succinic anhydride and a diamine derived from L-valine, affording two new amide bonds. The molecular gels were studied by IR, NMR, electron microscopy, X-ray diffraction and DSC. The results indicate that different polymorphic fibrillar networks are formed depending on the gel preparation method, highlighting how the properties of molecular gels can be tuned in this way. Significant differences between thermal and in situ gels were found in properties such as thermal stability, thixotropic behavior or release of an entrapped dye. In situ synthesis-gelation has also been shown to provide gels in media such as oleic acid which cannot be jellified by conventional heating-cooling procedures. Copyright © 2013 Elsevier Inc. All rights reserved.

A Review of Microwave-Assisted Reactions for Biodiesel Production

PubMed Central

Nomanbhay, Saifuddin; Ong, Mei Yin

2017-01-01

The conversion of biomass into chemicals and biofuels is an active research area as trends move to replace fossil fuels with renewable resources due to society’s increased concern towards sustainability. In this context, microwave processing has emerged as a tool in organic synthesis and plays an important role in developing a more sustainable world. Integration of processing methods with microwave irradiation has resulted in a great reduction in the time required for many processes, while the reaction efficiencies have been increased markedly. Microwave processing produces a higher yield with a cleaner profile in comparison to other methods. The microwave processing is reported to be a better heating method than the conventional methods due to its unique thermal and non-thermal effects. This paper provides an insight into the theoretical aspects of microwave irradiation practices and highlights the importance of microwave processing. The potential of the microwave technology to accomplish superior outcomes over the conventional methods in biodiesel production is presented. A green process for biodiesel production using a non-catalytic method is still new and very costly because of the supercritical condition requirement. Hence, non-catalytic biodiesel conversion under ambient pressure using microwave technology must be developed, as the energy utilization for microwave-based biodiesel synthesis is reported to be lower and cost-effective. PMID:28952536

A Review of Microwave-Assisted Reactions for Biodiesel Production.

PubMed

Nomanbhay, Saifuddin; Ong, Mei Yin

2017-06-15

The conversion of biomass into chemicals and biofuels is an active research area as trends move to replace fossil fuels with renewable resources due to society's increased concern towards sustainability. In this context, microwave processing has emerged as a tool in organic synthesis and plays an important role in developing a more sustainable world. Integration of processing methods with microwave irradiation has resulted in a great reduction in the time required for many processes, while the reaction efficiencies have been increased markedly. Microwave processing produces a higher yield with a cleaner profile in comparison to other methods. The microwave processing is reported to be a better heating method than the conventional methods due to its unique thermal and non-thermal effects. This paper provides an insight into the theoretical aspects of microwave irradiation practices and highlights the importance of microwave processing. The potential of the microwave technology to accomplish superior outcomes over the conventional methods in biodiesel production is presented. A green process for biodiesel production using a non-catalytic method is still new and very costly because of the supercritical condition requirement. Hence, non-catalytic biodiesel conversion under ambient pressure using microwave technology must be developed, as the energy utilization for microwave-based biodiesel synthesis is reported to be lower and cost-effective.

Obstacles to Using Prior Research and Evaluations.

ERIC Educational Resources Information Center

Orwin, Robert G.

1985-01-01

The manner in which results and methods are reported influences the ability of the synthesis of prior studies for planning new evaluations. Confidence ratings, coding conventions, and supplemental evidence can partially overcome the difficulties. Planners must acknowledge the influence of their own judgement in using prior research. (Author)

What Synthesis Methodology Should I Use? A Review and Analysis of Approaches to Research Synthesis.

PubMed

Schick-Makaroff, Kara; MacDonald, Marjorie; Plummer, Marilyn; Burgess, Judy; Neander, Wendy

2016-01-01

When we began this process, we were doctoral students and a faculty member in a research methods course. As students, we were facing a review of the literature for our dissertations. We encountered several different ways of conducting a review but were unable to locate any resources that synthesized all of the various synthesis methodologies. Our purpose is to present a comprehensive overview and assessment of the main approaches to research synthesis. We use 'research synthesis' as a broad overarching term to describe various approaches to combining, integrating, and synthesizing research findings. We conducted an integrative review of the literature to explore the historical, contextual, and evolving nature of research synthesis. We searched five databases, reviewed websites of key organizations, hand-searched several journals, and examined relevant texts from the reference lists of the documents we had already obtained. We identified four broad categories of research synthesis methodology including conventional, quantitative, qualitative, and emerging syntheses. Each of the broad categories was compared to the others on the following: key characteristics, purpose, method, product, context, underlying assumptions, unit of analysis, strengths and limitations, and when to use each approach. The current state of research synthesis reflects significant advancements in emerging synthesis studies that integrate diverse data types and sources. New approaches to research synthesis provide a much broader range of review alternatives available to health and social science students and researchers.

Mechanism of plant-mediated synthesis of silver nanoparticles - A review on biomolecules involved, characterisation and antibacterial activity.

PubMed

Rajeshkumar, S; Bharath, L V

2017-08-01

Engineering a reliable and eco-accommodating methodology for the synthesis of metal nanoparticles is a crucial step in the field of nanotechnology. Plant-mediated synthesis of metal nanoparticles has been developed as a substitute to defeat the limitations of conventional synthesis approaches such as physical and chemical methods. Biomolecules, such as proteins, amino acids, enzymes, flavonoids, and terpenoids from several plant extracts have been used as a stabilising and reducing agents for the synthesis of AgNPs. Regardless of an extensive range of biomolecules assistance in the synthesis procedure, researchers are facing a significant challenge to synthesise stable and geometrically controlled AgNPs. In the past decade, several efforts were made to develop Plant-mediated synthesis methods to produce stable, cost effective and eco-friendly AgNPs. More than hundred different plants extract sources for synthesising AgNPs were described in the last decade by several researchers. Most of the reviews were focused on various plant sources for synthesis, various characterization techniques for characteristic analysis, and antibacterial activity against bacterial. There are many reviews are available for the plant-mediated synthesis of AgNPs as well as antibacterial activity of AgNPs but this is the first review article mainly focused on biomolecules of plants and its various parts and operating conditions involved in the synthesis. Apart from, this review includes the characterisation of AgNPs and antibacterial activity of such nanoparticles with size, shape and method used for this study. Copyright © 2017 Elsevier B.V. All rights reserved.

Ultrafast synthesis of LTA nanozeolite using a two-phase segmented fluidic microreactor.

PubMed

Zhou, Jianhai; Jiang, Hao; Xu, Jian; Hu, Jun; Liu, Honglai; Hu, Ying

2013-08-01

Fast synthesis of nanosized zeolite is desirable for many industrial applications. An ultrafast synthesis of LTA nanozeolite by the organic-additive-free method in a two-phase segmented fluidic microreactor has been realized. The results reveal that the obtained LTA nanozeolites through microreactor are much smaller and higher crystallinity than those under similar conditions through conventional macroscale batch reactor. By investing various test conditions, such as the crystallization temperature, the flow rate, the microchannel length, and the aging time of gel solution, this two-phase segmented fluidic microreactor system enables us to develop an ultrafast method for nanozeolite production. Particularly, when using a microreactor with the microchannel length of 20 m, it only takes 10 min for the crystallization and no aging process to successfully produce the crystalline LTA nanozeolites at 95 degrees C.

Development of a Test Facility for Air Revitalization Technology Evaluation

NASA Technical Reports Server (NTRS)

Lu, Sao-Dung; Lin, Amy; Campbell, Melissa; Smith, Frederick

2006-01-01

An active fault tolerant control (FTC) law is generally sensitive to false identification since the control gain is reconfigured for fault occurrence. In the conventional FTC law design procedure, dynamic variations due to false identification are not considered. In this paper, an FTC synthesis method is developed in order to consider possible variations of closed-loop dynamics under false identification into the control design procedure. An active FTC synthesis problem is formulated into an LMI optimization problem to minimize the upper bound of the induced-L2 norm which can represent the worst-case performance degradation due to false identification. The developed synthesis method is applied for control of the longitudinal motions of FASER (Free-flying Airplane for Subscale Experimental Research). The designed FTC law of the airplane is simulated for pitch angle command tracking under a false identification case.

Gain-Scheduled Fault Tolerance Control Under False Identification

NASA Technical Reports Server (NTRS)

Shin, Jong-Yeob; Belcastro, Christine (Technical Monitor)

2006-01-01

An active fault tolerant control (FTC) law is generally sensitive to false identification since the control gain is reconfigured for fault occurrence. In the conventional FTC law design procedure, dynamic variations due to false identification are not considered. In this paper, an FTC synthesis method is developed in order to consider possible variations of closed-loop dynamics under false identification into the control design procedure. An active FTC synthesis problem is formulated into an LMI optimization problem to minimize the upper bound of the induced-L2 norm which can represent the worst-case performance degradation due to false identification. The developed synthesis method is applied for control of the longitudinal motions of FASER (Free-flying Airplane for Subscale Experimental Research). The designed FTC law of the airplane is simulated for pitch angle command tracking under a false identification case.

Flow chemistry to control the synthesis of nano and microparticles for biomedical applications.

PubMed

Hassan, Natalia; Oyarzun-Ampuero, Felipe; Lara, Pablo; Guerrero, Simón; Cabuil, Valérie; Abou-Hassan, Ali; Kogan, Marcelo J

2014-03-01

In this article we review the flow chemistry methodologies for the controlled synthesis of different kind of nano and microparticles for biomedical applications. Injection mechanism has emerged as new alternative for the synthesis of nanoparticles due to this strategy allows achieving superior levels of control of self-assemblies, leading to higher-ordered structures and rapid chemical reactions. Self-assembly events are strongly dependent on factors such as the local concentration of reagents, the mixing rates, and the shear forces, which can be finely tuned, as an example, in a microfluidic device. Injection methods have also proved to be optimal to elaborate microsystems comprising polymer solutions. Concretely, extrusion based methods can provide controlled fluid transport, rapid chemical reactions, and cost-saving advantages over conventional reactors. We provide an update of synthesis of nano and microparticles such as core/shell, Janus, nanocrystals, liposomes, and biopolymeric microgels through flow chemistry, its potential bioapplications and future challenges in this field are discussed.

Impact Assessment and Environmental Evaluation of Various Ammonia Production Processes

NASA Astrophysics Data System (ADS)

Bicer, Yusuf; Dincer, Ibrahim; Vezina, Greg; Raso, Frank

2017-05-01

In the current study, conventional resources-based ammonia generation routes are comparatively studied through a comprehensive life cycle assessment. The selected ammonia generation options range from mostly used steam methane reforming to partial oxidation of heavy oil. The chosen ammonia synthesis process is the most common commercially available Haber-Bosch process. The essential energy input for the methods are used from various conventional resources such as coal, nuclear, natural gas and heavy oil. Using the life cycle assessment methodology, the environmental impacts of selected methods are identified and quantified from cradle to gate. The life cycle assessment outcomes of the conventional resources based ammonia production routes show that nuclear electrolysis-based ammonia generation method yields the lowest global warming and climate change impacts while the coal-based electrolysis options bring higher environmental problems. The calculated greenhouse gas emission from nuclear-based electrolysis is 0.48 kg CO2 equivalent while it is 13.6 kg CO2 per kg of ammonia for coal-based electrolysis method.

Impact Assessment and Environmental Evaluation of Various Ammonia Production Processes.

PubMed

Bicer, Yusuf; Dincer, Ibrahim; Vezina, Greg; Raso, Frank

2017-05-01

In the current study, conventional resources-based ammonia generation routes are comparatively studied through a comprehensive life cycle assessment. The selected ammonia generation options range from mostly used steam methane reforming to partial oxidation of heavy oil. The chosen ammonia synthesis process is the most common commercially available Haber-Bosch process. The essential energy input for the methods are used from various conventional resources such as coal, nuclear, natural gas and heavy oil. Using the life cycle assessment methodology, the environmental impacts of selected methods are identified and quantified from cradle to gate. The life cycle assessment outcomes of the conventional resources based ammonia production routes show that nuclear electrolysis-based ammonia generation method yields the lowest global warming and climate change impacts while the coal-based electrolysis options bring higher environmental problems. The calculated greenhouse gas emission from nuclear-based electrolysis is 0.48 kg CO 2 equivalent while it is 13.6 kg CO 2 per kg of ammonia for coal-based electrolysis method.

15 CFR Supplement No. 2 to Part 710 - Definitions of Production

Code of Federal Regulations, 2010 CFR

2010-01-01

... reaction Produced by synthesis* Formation through chemical synthesis.Processing to extract and isolate... (Continued) BUREAU OF INDUSTRY AND SECURITY, DEPARTMENT OF COMMERCE CHEMICAL WEAPONS CONVENTION REGULATIONS GENERAL INFORMATION AND OVERVIEW OF THE CHEMICAL WEAPONS CONVENTION REGULATIONS (CWCR) Pt. 710, Supp. 2...

Synthesis of ammonia directly from air and water at ambient temperature and pressure

NASA Astrophysics Data System (ADS)

Lan, Rong; Irvine, John T. S.; Tao, Shanwen

2013-01-01

The N≡N bond (225 kcal mol-1) in dinitrogen is one of the strongest bonds in chemistry therefore artificial synthesis of ammonia under mild conditions is a significant challenge. Based on current knowledge, only bacteria and some plants can synthesise ammonia from air and water at ambient temperature and pressure. Here, for the first time, we report artificial ammonia synthesis bypassing N2 separation and H2 production stages. A maximum ammonia production rate of 1.14 × 10-5 mol m-2 s-1 has been achieved when a voltage of 1.6 V was applied. Potentially this can provide an alternative route for the mass production of the basic chemical ammonia under mild conditions. Considering climate change and the depletion of fossil fuels used for synthesis of ammonia by conventional methods, this is a renewable and sustainable chemical synthesis process for future.

Synthesis of ammonia directly from air and water at ambient temperature and pressure

PubMed Central

Lan, Rong; Irvine, John T. S.; Tao, Shanwen

2013-01-01

The N≡N bond (225 kcal mol−1) in dinitrogen is one of the strongest bonds in chemistry therefore artificial synthesis of ammonia under mild conditions is a significant challenge. Based on current knowledge, only bacteria and some plants can synthesise ammonia from air and water at ambient temperature and pressure. Here, for the first time, we report artificial ammonia synthesis bypassing N2 separation and H2 production stages. A maximum ammonia production rate of 1.14 × 10−5 mol m−2 s−1 has been achieved when a voltage of 1.6 V was applied. Potentially this can provide an alternative route for the mass production of the basic chemical ammonia under mild conditions. Considering climate change and the depletion of fossil fuels used for synthesis of ammonia by conventional methods, this is a renewable and sustainable chemical synthesis process for future. PMID:23362454

Synthesis of ammonia directly from air and water at ambient temperature and pressure.

PubMed

Lan, Rong; Irvine, John T S; Tao, Shanwen

2013-01-01

The N≡N bond (225 kcal mol⁻¹) in dinitrogen is one of the strongest bonds in chemistry therefore artificial synthesis of ammonia under mild conditions is a significant challenge. Based on current knowledge, only bacteria and some plants can synthesise ammonia from air and water at ambient temperature and pressure. Here, for the first time, we report artificial ammonia synthesis bypassing N₂ separation and H₂ production stages. A maximum ammonia production rate of 1.14 × 10⁻⁵ mol m⁻² s⁻¹ has been achieved when a voltage of 1.6 V was applied. Potentially this can provide an alternative route for the mass production of the basic chemical ammonia under mild conditions. Considering climate change and the depletion of fossil fuels used for synthesis of ammonia by conventional methods, this is a renewable and sustainable chemical synthesis process for future.

Ultrasound-assisted synthesis of novel 4-(2-phenyl-1,2,3-triazol-4-yl)-3,4-dihydropyrimidin-(1H)-(thio)ones catalyzed by Sm(ClO(4))(3).

PubMed

Liu, Chen-Jiang; Wang, Ji-De

2010-03-24

An efficient synthesis of novel 4-(2-phenyl-1,2,3-triazol-4-yl)-3,4-dihydro-pyrimidin-2(1H)-(thio)ones from 1,3-dicarbonyl compounds, 2-phenyl-1,2,3-triazole-4-carbaldehyde and urea or thiourea under ultrasound irradiation and using samarium perchlorate as catalyst is described. Compared with conventional methods, the main advantages of the present methodology are milder conditions, shorter reaction times and higher yields.

Replacement solvents for use in chemical synthesis

DOEpatents

Molnar, Linda K.; Hatton, T. Alan; Buchwald, Stephen L.

2001-05-15

Replacement solvents for use in chemical synthesis include polymer-immobilized solvents having a flexible polymer backbone and a plurality of pendant groups attached onto the polymer backbone, the pendant groups comprising a flexible linking unit bound to the polymer backbone and to a terminal solvating moiety. The polymer-immobilized solvent may be dissolved in a benign medium. Replacement solvents for chemical reactions for which tetrahydrofuran or diethyl may be a solvent include substituted tetrahydrofurfuryl ethers and substituted tetrahydro-3-furan ethers. The replacement solvents may be readily recovered from the reaction train using conventional methods.

Low-redundancy linear arrays in mirrored interferometric aperture synthesis.

PubMed

Zhu, Dong; Hu, Fei; Wu, Liang; Li, Jun; Lang, Liang

2016-01-15

Mirrored interferometric aperture synthesis (MIAS) is a novel interferometry that can improve spatial resolution compared with that of conventional IAS. In one-dimensional (1-D) MIAS, antenna array with low redundancy has the potential to achieve a high spatial resolution. This Letter presents a technique for the direct construction of low-redundancy linear arrays (LRLAs) in MIAS and derives two regular analytical patterns that can yield various LRLAs in short computation time. Moreover, for a better estimation of the observed scene, a bi-measurement method is proposed to handle the rank defect associated with the transmatrix of those LRLAs. The results of imaging simulation demonstrate the effectiveness of the proposed method.

Synthesis of Bi0.9Nd0.1FeO3 multiferroic nanoceramic by sol-gel method and its structural, surface morphology and dielectric analysis

NASA Astrophysics Data System (ADS)

Das, S.; Bera, K. P.; Nath, T. K.

2017-05-01

Synthesis of Nd-doped BFO multiferroic nanoceramic by the conventional sol-gel method has been carried out. HRXRD and FESEM have been used for the structural analysis to confirm the triclinic structure and to obtain the surface morphology showing agglomeration and to find out the size of the nanoparticles. A high precision LCR meter has been used to record the dielectric constants at various temperatures. Several anomalies are observed whose physical explanations have been given. Space charge polarization effect and magnetoelectric coupling have been confirmed in the synthesized Bi0.9Nd0.1FeO3 nanoceramic sample.

Red tea leaves infusion as a reducing and stabilizing agent in silver nanoparticles synthesis

NASA Astrophysics Data System (ADS)

Pluta, K.; Tryba, A. M.; Malina, D.; Sobczak-Kupiec, A.

2017-12-01

Due to the unique properties of silver nanoparticles there is growing interest in their applications. Current trends in nanotechnology are focused on developing a new technique to synthesize nanoparticles using biological methods associated with the use of plant extracts, fungi, bacteria or essential oils. These methods are a promising alternative to conventional approaches which can minimize the use of hazardous substances. The silver nanoparticles synthesis using red tea infusion as a reducing and stabilizing agent and their characteristics have been described. Total antioxidant capacity using DPPH radical and total content of phenolic compounds by Folin-Ciocalteau method were measured in tea infusion. Synthesis of silver nanoparticles was carried out using chemical reduction at various temperatures. Furthermore, the effect of tea infusion volume added to reaction mixture on nanoparticles’ properties was investigated. Finally, nanosilver suspensions were characterized by UV-vis spectrophotometer, dynamic light scattering (DLS) scanning electron microscope (SEM) and transmission electron microscope (TEM). Moreover, phytotoxicity of silver nanoparticles was determined using Phytotestkit microbiotest.

A review on biogenic synthesis of ZnO nanoparticles using plant extracts and microbes: A prospect towards green chemistry.

PubMed

Ahmed, Shakeel; Annu; Chaudhry, Saif Ali; Ikram, Saiqa

2017-01-01

Nanotechnology is emerging as an important area of research with its tremendous applications in all fields of science, engineering, medicine, pharmacy, etc. It involves the materials and their applications having one dimension in the range of 1-100nm. Generally, various techniques are used for syntheses of nanoparticles (NPs) viz. laser ablation, chemical reduction, milling, sputtering, etc. These conventional techniques e.g. chemical reduction method, in which various hazardous chemicals are used for the synthesis of NPs later become liable for innumerable health risks due to their toxicity and endangering serious concerns for environment, while other approaches are expensive, need high energy for the synthesis of NPs. However, biogenic synthesis method to produce NPs is eco-friendly and free of chemical contaminants for biological applications where purity is of concerns. In biological method, different biological entities such as extract, enzymes or proteins of a natural product are used to reduce and stabilised formation of NPs. The nature of these biological entities also influence the structure, shape, size and morphology of synthesized NPs. In this review, biogenic synthesis of zinc oxide (ZnO) NPs, procedures of syntheses, mechanism of formation and their various applications have been discussed. Various entities such as proteins, enzymes, phytochemicals, etc. available in the natural reductants are responsible for synthesis of ZnO NPs. Copyright © 2016 Elsevier B.V. All rights reserved.

Promoted Iron Nanocrystals Obtained via Ligand Exchange as Active and Selective Catalysts for Synthesis Gas Conversion

PubMed Central

2017-01-01

Colloidal synthesis routes have been recently used to fabricate heterogeneous catalysts with more controllable and homogeneous properties. Herein a method was developed to modify the surface composition of colloidal nanocrystal catalysts and to purposely introduce specific atoms via ligands and change the catalyst reactivity. Organic ligands adsorbed on the surface of iron oxide catalysts were exchanged with inorganic species such as Na2S, not only to provide an active surface but also to introduce controlled amounts of Na and S acting as promoters for the catalytic process. The catalyst composition was optimized for the Fischer–Tropsch direct conversion of synthesis gas into lower olefins. At industrially relevant conditions, these nanocrystal-based catalysts with controlled composition were more active, selective, and stable than catalysts with similar composition but synthesized using conventional methods, possibly due to their homogeneity of properties and synergic interaction of iron and promoters. PMID:28824820

Pb(core)/ZnO(shell) nanowires obtained by microwave-assisted method

PubMed Central

2011-01-01

In this study, Pb-filled ZnO nanowires [Pb(core)/ZnO(shell)] were synthesized by a simple and novel one-step vapor transport and condensation method by microwave-assisted decomposition of zinc ferrite. The synthesis was performed using a conventional oven at 1000 W and 5 min of treatment. After synthesis, a spongy white cotton-like material was obtained in the condensation zone of the reaction system. HRTEM analysis revealed that product consists of a Pb-(core) with (fcc) cubic structure that preferentially grows in the [111] direction and a hexagonal wurtzite ZnO-(Shell) that grows in the [001] direction. Nanowire length was more than 5 μm and a statistical analysis determined that the shell and core diameters were 21.00 ± 3.00 and 4.00 ± 1.00 nm, respectively. Experimental, structural details, and synthesis mechanism are discussed in this study. PMID:21985637

A rapid microwave-assisted synthesis of a sodium-cadmium metal-organic framework having improved performance as a CO2 adsorbent for CCS.

PubMed

Palomino Cabello, Carlos; Arean, Carlos Otero; Parra, José B; Ania, Conchi O; Rumori, P; Turnes Palomino, G

2015-06-07

We report on a facile and rapid microwave-assisted method for preparing a sodium-cadmium metal-organic framework (having coordinatively unsaturated sodium ions) that considerably shortens the conventional synthesis time from 5 days to 1 hour. The obtained (Na,Cd)-MOF showed an excellent volumetric CO2 adsorption capacity (5.2 mmol cm(-3) at 298 K and 1 bar) and better CO2 adsorption properties than those shown by the same metal-organic framework when synthesized following a more conventional procedure. Moreover, the newly prepared material was found to display high selectivity for adsorption of carbon dioxide over nitrogen, and good regenerability and stability during repeated CO2 adsorption-desorption cycles, which are the required properties for any adsorbent intended for carbon dioxide capture and sequestration (CSS) from the post-combustion flue gas of fossil fuelled power stations.

Converting Wind Energy to Ammonia at Lower Pressure

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

Malmali, Mahdi; Reese, Michael; McCormick, Alon V.

Renewable wind energy can be used to make ammonia. However, wind-generated ammonia costs about twice that made from a traditional fossil-fuel driven process. To reduce the production cost, we replace the conventional ammonia condensation with a selective absorber containing metal halides, e.g., calcium chloride, operating at near synthesis temperatures. With this reaction-absorption process, ammonia can be synthesized at 20 bar from air, water, and wind-generated electricity, with rates comparable to the conventional process running at 150–300 bar. In our reaction-absorption process, the rate of ammonia synthesis is now controlled not by the chemical reaction but largely by the pump usedmore » to recycle the unreacted gases. The results suggest an alternative route to distributed ammonia manufacture which can locally supply nitrogen fertilizer and also a method to capture stranded wind energy as a carbon-neutral liquid fuel.« less

Converting Wind Energy to Ammonia at Lower Pressure

DOE PAGES

Malmali, Mahdi; Reese, Michael; McCormick, Alon V.; ...

2017-11-07

Renewable wind energy can be used to make ammonia. However, wind-generated ammonia costs about twice that made from a traditional fossil-fuel driven process. To reduce the production cost, we replace the conventional ammonia condensation with a selective absorber containing metal halides, e.g., calcium chloride, operating at near synthesis temperatures. With this reaction-absorption process, ammonia can be synthesized at 20 bar from air, water, and wind-generated electricity, with rates comparable to the conventional process running at 150–300 bar. In our reaction-absorption process, the rate of ammonia synthesis is now controlled not by the chemical reaction but largely by the pump usedmore » to recycle the unreacted gases. The results suggest an alternative route to distributed ammonia manufacture which can locally supply nitrogen fertilizer and also a method to capture stranded wind energy as a carbon-neutral liquid fuel.« less

Synthesis of metal-organic framework films by pore diffusion method

NASA Astrophysics Data System (ADS)

Murayama, Naohiro; Nishimura, Yuki; Kajiro, Hiroshi; Kishida, Satoru; Kinoshita, Kentaro; Tottori Univ Team; Nippon Steel; Sumitomo Metal Co. Collaboration; Tottori Integrated Frontier Resaerch Center (Tifrec) Collaboration; Tottori University Electronic Display Resaerch Center (Tedrec) Collaboration

Metal-organic frameworks (MOFs) presents high controllability in designing the nano-scale pore, and this enable molecular storages, catalysts, gas sensors, gas separation membranes, and electronic devices for next-generation. Therefore, a simple method for film synthesis of MOFs compared with conventional methods [1] is strongly required. In this paper, we provide pore diffusion method, in which a substrate containing constituent metals of MOF is inserted in solution that includes only linker molecules of MOF. As a result, 2D growth of MOF was effectively enhanced, and the formation of flat and dense MOF films was attained. The growth time, t, dependence of film thickness, d, can be expressed by the relation of d = Aln(t + 1) + B, where A and B are constants. It means that ionized coppers diffuse through the pores of MOFs and the synthesis reaction proceeds at the MOF/solvent interface. We demonstrated the fabrication of a HKUST-1/Cu-TPA hetero structure by synthesizing a Cu-TPA film continuously after the growth of a HKUST-1 film on the CuOx substrate.

Rapid and direct synthesis of complex perovskite oxides through a highly energetic planetary milling

PubMed Central

Lee, Gyoung-Ja; Park, Eun-Kwang; Yang, Sun-A; Park, Jin-Ju; Bu, Sang-Don; Lee, Min-Ku

2017-01-01

The search for a new and facile synthetic route that is simple, economical and environmentally safe is one of the most challenging issues related to the synthesis of functional complex oxides. Herein, we report the expeditious synthesis of single-phase perovskite oxides by a high-rate mechanochemical reaction, which is generally difficult through conventional milling methods. With the help of a highly energetic planetary ball mill, lead-free piezoelectric perovskite oxides of (Bi, Na)TiO3, (K, Na)NbO3 and their modified complex compositions were directly synthesized with low contamination. The reaction time necessary to fully convert the micron-sized reactant powder mixture into a single-phase perovskite structure was markedly short at only 30–40 min regardless of the chemical composition. The cumulative kinetic energy required to overtake the activation period necessary for predominant formation of perovskite products was ca. 387 kJ/g for (Bi, Na)TiO3 and ca. 580 kJ/g for (K, Na)NbO3. The mechanochemically derived powders, when sintered, showed piezoelectric performance capabilities comparable to those of powders obtained by conventional solid-state reaction processes. The observed mechanochemical synthetic route may lead to the realization of a rapid, one-step preparation method by which to create other promising functional oxides without time-consuming homogenization and high-temperature calcination powder procedures. PMID:28387324

Ultrasound promoted one-pot synthesis of 2-amino-4,8-dihydropyrano[3,2-b]pyran-3-carbonitrile scaffolds in aqueous media: a complementary 'green chemistry' tool to organic synthesis.

PubMed

Banitaba, Sayed Hossein; Safari, Javad; Khalili, Shiva Dehghan

2013-01-01

A green and simple approach to assembling of 2-amino-4,8-dihydropyrano[3,2-b]pyran-3-carbonitrile scaffolds via three-component reaction of kojic acid, malononitrile, and aromatic aldehydes in aqueous media under ultrasound irradiation is described. The combinatorial synthesis was achieved for this methodology with applying ultrasound irradiation while making use of water as green solvent. In comparison to conventional methods, experimental simplicity, good functional group tolerance, excellent yields, short routine, and selectivity without the need for a transition metal or base catalyst are prominent features of this green procedure. Copyright © 2012 Elsevier B.V. All rights reserved.

Harnessing Thin-Film Continuous-Flow Assembly Lines.

PubMed

Britton, Joshua; Castle, Jared W; Weiss, Gregory A; Raston, Colin L

2016-07-25

Inspired by nature's ability to construct complex molecules through sequential synthetic transformations, an assembly line synthesis of α-aminophosphonates has been developed. In this approach, simple starting materials are continuously fed through a thin-film reactor where the intermediates accrue molecular complexity as they progress through the flow system. Flow chemistry allows rapid multistep transformations to occur via reaction compartmentalization, an approach not amenable to using conventional flasks. Thin film processing can also access facile in situ solvent exchange to drive reaction efficiency, and through this method, α-aminophosphonate synthesis requires only 443 s residence time to produce 3.22 g h(-1) . Assembly-line synthesis allows unprecedented reaction flexibility and processing efficiency. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effects of ultrasonic treatment on zeolite NaA synthesized from by-product silica.

PubMed

Vaičiukynienė, Danutė; Kantautas, Aras; Vaitkevičius, Vitoldas; Jakevičius, Leonas; Rudžionis, Žymantas; Paškevičius, Mantas

2015-11-01

The synthesis of zeolite NaA from silica by-product was carried out in the presence of 20 kHz ultrasound at room temperature. Zeolites obtained in this type of synthesis were compared to zeolites obtained by performing conventional static syntheses under similar conditions. The sonication effects on zeolite NaA synthesis were characterized by phase identification, crystallinity etc. The effects of different parameters such as crystallization time and initial materials preparation methods on the crystallinity and morphology of the synthesized zeolites were investigated. The final products were characterized by XRD and FT-IR. It was possible to obtain crystalline zeolite NaA from by-product silica in the presence of ultrasound. Copyright © 2015 Elsevier B.V. All rights reserved.

Multi-atlas-based CT synthesis from conventional MRI with patch-based refinement for MRI-based radiotherapy planning

NASA Astrophysics Data System (ADS)

Lee, Junghoon; Carass, Aaron; Jog, Amod; Zhao, Can; Prince, Jerry L.

2017-02-01

Accurate CT synthesis, sometimes called electron density estimation, from MRI is crucial for successful MRI-based radiotherapy planning and dose computation. Existing CT synthesis methods are able to synthesize normal tissues but are unable to accurately synthesize abnormal tissues (i.e., tumor), thus providing a suboptimal solution. We propose a multiatlas- based hybrid synthesis approach that combines multi-atlas registration and patch-based synthesis to accurately synthesize both normal and abnormal tissues. Multi-parametric atlas MR images are registered to the target MR images by multi-channel deformable registration, from which the atlas CT images are deformed and fused by locally-weighted averaging using a structural similarity measure (SSIM). Synthetic MR images are also computed from the registered atlas MRIs by using the same weights used for the CT synthesis; these are compared to the target patient MRIs allowing for the assessment of the CT synthesis fidelity. Poor synthesis regions are automatically detected based on the fidelity measure and refined by a patch-based synthesis. The proposed approach was tested on brain cancer patient data, and showed a noticeable improvement for the tumor region.

Multi-atlas-based CT synthesis from conventional MRI with patch-based refinement for MRI-based radiotherapy planning.

PubMed

Lee, Junghoon; Carass, Aaron; Jog, Amod; Zhao, Can; Prince, Jerry L

2017-02-01

Accurate CT synthesis, sometimes called electron density estimation, from MRI is crucial for successful MRI-based radiotherapy planning and dose computation. Existing CT synthesis methods are able to synthesize normal tissues but are unable to accurately synthesize abnormal tissues (i.e., tumor), thus providing a suboptimal solution. We propose a multi-atlas-based hybrid synthesis approach that combines multi-atlas registration and patch-based synthesis to accurately synthesize both normal and abnormal tissues. Multi-parametric atlas MR images are registered to the target MR images by multi-channel deformable registration, from which the atlas CT images are deformed and fused by locally-weighted averaging using a structural similarity measure (SSIM). Synthetic MR images are also computed from the registered atlas MRIs by using the same weights used for the CT synthesis; these are compared to the target patient MRIs allowing for the assessment of the CT synthesis fidelity. Poor synthesis regions are automatically detected based on the fidelity measure and refined by a patch-based synthesis. The proposed approach was tested on brain cancer patient data, and showed a noticeable improvement for the tumor region.

Detonation Synthesis of Alpha-Variant Silicon Carbide

NASA Astrophysics Data System (ADS)

Langenderfer, Martin; Johnson, Catherine; Fahrenholtz, William; Mochalin, Vadym

2017-06-01

A recent research study has been undertaken to develop facilities for conducting detonation synthesis of nanomaterials. This process involves a familiar technique that has been utilized for the industrial synthesis of nanodiamonds. Developments through this study have allowed for experimentation with the concept of modifying explosive compositions to induce synthesis of new nanomaterials. Initial experimentation has been conducted with the end goal being synthesis of alpha variant silicon carbide (α-SiC) in the nano-scale. The α-SiC that can be produced through detonation synthesis methods is critical to the ceramics industry because of a number of unique properties of the material. Conventional synthesis of α-SiC results in formation of crystals greater than 100 nm in diameter, outside nano-scale. It has been theorized that the high temperature and pressure of an explosive detonation can be used for the formation of α-SiC in the sub 100 nm range. This paper will discuss in detail the process development for detonation nanomaterial synthesis facilities, optimization of explosive charge parameters to maximize nanomaterial yield, and introduction of silicon to the detonation reaction environment to achieve first synthesis of nano-sized alpha variant silicon carbide.

DNA-Compatible Nitro Reduction and Synthesis of Benzimidazoles.

PubMed

Du, Huang-Chi; Huang, Hongbing

2017-10-18

DNA-encoded chemical libraries have emerged as a cost-effective alternative to high-throughput screening (HTS) for hit identification in drug discovery. A key factor for productive DNA-encoded libraries is the chemical diversity of the small molecule moiety attached to an encoding DNA oligomer. The library structure diversity is often limited to DNA-compatible chemical reactions in aqueous media. Herein, we describe a facile process for reducing aryl nitro groups to aryl amines. The new protocol offers simple operation and circumvents the pyrophoric potential of the conventional method (Raney nickel). The reaction is performed in aqueous solution and does not compromise DNA structural integrity. The utility of this method is demonstrated by the versatile synthesis of benzimidazoles on DNA.

Synthesis gas method and apparatus

DOEpatents

Kelly, Sean M.; Kromer, Brian R.; Litwin, Michael M.; Rosen, Lee J.; Christie, Gervase Maxwell; Wilson, Jamie; Kosowski, Lawrence W; Robinson, Charles

2015-11-06

A method and apparatus for producing a synthesis gas product having one or more oxygen transport membrane elements thermally coupled to one or more catalytic reactors such that heat generated from the oxygen transport membrane element supplies endothermic heating requirements for steam methane reforming reactions occurring within the catalytic reactor through radiation and convention heat transfer. A hydrogen containing stream containing no more than 20 percent methane is combusted within the oxygen transport membrane element to produce the heat and a heated combustion product stream. The heated combustion product stream is combined with a reactant stream to form a combined stream that is subjected to the reforming within the catalytic reactor. The apparatus may include modules in which tubular membrane elements surround a central reactor tube.

Synthesis gas method and apparatus

DOEpatents

Kelly, Sean M.; Kromer, Brian R.; Litwin, Michael M.; Rosen, Lee J.; Christie, Gervase Maxwell; Wilson, Jamie R.; Kosowski, Lawrence W.; Robinson, Charles

2013-01-08

A method and apparatus for producing a synthesis gas product having one or more oxygen transport membrane elements thermally coupled to one or more catalytic reactors such that heat generated from the oxygen transport membrane element supplies endothermic heating requirements for steam methane reforming reactions occurring within the catalytic reactor through radiation and convention heat transfer. A hydrogen containing stream containing no more than 20 percent methane is combusted within the oxygen transport membrane element to produce the heat and a heated combustion product stream. The heated combustion product stream is combined with a reactant stream to form a combined stream that is subjected to the reforming within the catalytic reactor. The apparatus may include modules in which tubular membrane elements surround a central reactor tube.

Synthesis of nanosized (<20 nm) polymer particles by radical polymerization in miniemulsion employing in situ surfactant formation.

PubMed

Guo, Yi; Zetterlund, Per B

2011-10-18

A novel method for synthesis of ultrafine polymeric nanoparticles of diameters less than 20 nm has been developed. The method is based on miniemulsion polymerization exploiting combination of the in situ surfactant generation approach (whereby the surfactant is formed at the oil-water interface by reaction between an organic acid and a base) and ultrasonication. Conventional radical polymerization and nitroxide-mediated radical polymerization of styrene have been conducted in miniemulsion using oleic acid/potassium hydroxide, demonstrating that particles with diameters less than 20 nm can be obtained by this approach at surfactant contents much lower than traditionally required in microemulsion polymerizations. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

In situ synthesis of nanocomposite membranes: comprehensive improvement strategy for direct methanol fuel cells.

PubMed

Rao, Siyuan; Xiu, Ruijie; Si, Jiangju; Lu, Shanfu; Yang, Meng; Xiang, Yan

2014-03-01

In situ synthesis is a powerful approach to control nanoparticle formation and consequently confers extraordinary properties upon composite membranes relative to conventional doping methods. Herein, uniform nanoparticles of cesium hydrogen salts of phosphotungstic acid (CsPW) are controllably synthesized in situ in Nafion to form CsPW–Nafion nanocomposite membranes with both improved proton conductivity and methanol-crossover suppression. A 101.3% increase of maximum power density has been achieved relative to pristine Nafion in a direct methanol fuel cell (DMFC), indicating a potential pathway for large-scale fabrication of DMFC alternative membranes.

Ultrasound-accelerated synthesis of biphenyl compounds using novel Pd(0) nanoparticles immobilized on bio-composite.

PubMed

Baran, Talat

2018-07-01

This study describes (i) an eco-friendly approach for design of Pd(0) nanoparticles on a natural composite, which is composed of carboxymethyl cellulose/agar polysaccharides (CMC/AG), without using any toxic reducing agents and (ii) development of ultrasound assisted simple protocol for synthesis of biphenyl compounds. Chemical characterization studies of Pd(0) nanoparticles (Pd NPs@CMC/AG) revealed that size of the particles were in the range of 37-55 nm. Catalytic performance of Pd NPs@CMC/AG was evaluated in synthesis of various biphenyl compounds by using the ultrasound-assisted method that was developed in this study. Pd NPs@CMC/AG exhibited excellent catalytic performance by producing high reaction yields. In addition, Pd NPs@CMC/AG was successfully used up to six reaction cycles without losing its catalytic activity, indicating high reproducibility of Pd NPs@CMC/AG. Additionally, compared to conventional the methods, new ultrasound-assisted synthesis technique that was followed in this study exhibited some advantages such as shorter reaction time, greener reaction conditions, higher yields and easier work-up. Copyright © 2018 Elsevier B.V. All rights reserved.

Novel Magnetic Nanomaterials Inspired by Magnetotactic Baterial: Topical Review

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

Prozorov, Tanya; Bazylinki, Dennis A.; Mallapragada, Surya K.

2013-05-14

Magnetotactic bacteria, known to produce magnetic nanocrystals with uniform shapes and sizes at physiological conditions, serve as an inspiration and source of a number of biological macromolecules used for the biomimetic synthesis of a variety of magnetic nanomaterials. This review discusses the current state of understanding of magnetosome biomineralization in magnetotactic bacteria, as well as the ways in which iron biomineralization processes can be utilized for tailored in vivo formation of complex magnetic nanomaterials, not occurring in magnetotactic bacteria naturally. The review assesses the current efforts on in vitro synthesis of a variety of magnetic nanoparticles using bioinspired approaches bymore » utilizing mineralization proteins from magnetotactic bacteria, and surveys biomimetic strategies for the rational synthesis of various magnetic nanomaterials under ambient conditions. Finally, this review presents magnetic characterization of nanoparticles, highlighting differences in magnetic behavior between magnetic nanoparticles produced using bioinspired in vivo and in vitro strategies, compared to those produced using conventional methods. This in turn impacts their utility in a wide range of applications for magnetic nanoparticles, which are examined in detail, where bioinspired synthesis methods have potentially provided added advantages.« less

Array-Based Discovery of Aptamer Pairs

DTIC Science & Technology

2014-12-11

affinities greatly exceeding either monovalent component. DNA aptamers are especially well-suited for such constructs, because they can be linked via...standard synthesis techniques without requiring chemical conjugation. Unfortunately, aptamer pairs are difficult to generate, primarily because...conventional selection methods preferentially yield aptamers that recognize a dominant “hot spot” epitope. Our 1. REPORT DATE (DD-MM-YYYY) 4. TITLE AND

A green surfactant-assisted synthesis of hierarchical TS-1 zeolites with excellent catalytic properties for oxidative desulfurization.

PubMed

Du, Shuting; Li, Fen; Sun, Qiming; Wang, Ning; Jia, Mingjun; Yu, Jihong

2016-02-25

Hierarchical TS-1 zeolites with uniform intracrystalline mesopores have been successfully synthesized through the hydrothermal method by using the green and cheap surfactant Triton X-100 as the mesoporous template. The resultant materials exhibit remarkably enhanced catalytic activity in oxidative desulfurization reactions compared to the conventional TS-1 zeolite.

Synthesis of hydroxyapatite nanorods for application in water defluoridation and optimization of process variables: Advantage of ultrasonication with precipitation method over conventional method.

PubMed

Mehta, Dhiraj; Mondal, Poonam; Saharan, Virendra Kumar; George, Suja

2017-07-01

This research work presents the synthesis of hydroxyapatite (Hap) nanorods for defluoridation of drinking water by using both conventional (CM) and ultrasonication with precipitation (USPM) methods. Calcium nitrate was reacted with potassium phosphate in presence of ammonia for controlled pH to synthesize Hap nanorods, which was characterized using FTIR, XRD, SEM, TG-DTA, and TEM/EDS for determining its phase composition, structural and thermal decomposition behavior. When USPM method was used for synthesis, the yield of the Hap nanorods was improved from 83.24±1.0% to 90.2±1.0%, and complete phase transformation occurred with formation of elongated Hap nanorods. Effects of process parameters such as solution pH, contact time and adsorbent dose were studied through response surface methodology (RSM). A simple quadratic model was developed using Central Composite Design (CCD) and optimum parameters for fluoride adsorption process were determined to be pH 7, contact time 3h and adsorbent dose 7g/L for maximum removal capacity. Fluoride removal efficiency was predicted to be 93.64% which was very close to the experimental value obtained at 92.86% using ultrasonically prepared Hap. Fluoride adsorption isotherms fitted the Freundlich isotherm with an adsorption capacity of 1.49mg/g, while the kinetic studies revealed that the process followed pseudo-second order model. The treated water quality parameters such as residual fluoride, calcium leached, total hardness and alkalinity was investigated, and it was observed that all these parameters were within the permissible limits as per WHO and BIS standards. Copyright © 2017 Elsevier B.V. All rights reserved.

Direct amidation of esters with nitroarenes

NASA Astrophysics Data System (ADS)

Cheung, Chi Wai; Ploeger, Marten Leendert; Hu, Xile

2017-03-01

Esters are one of the most common functional groups in natural and synthetic products, and the one-step conversion of the ester group into other functional groups is an attractive strategy in organic synthesis. Direct amidation of esters is particularly appealing due to the omnipresence of the amide moiety in biomolecules, fine chemicals, and drug candidates. However, efficient methods for direct amidation of unactivated esters are still lacking. Here we report nickel-catalysed reductive coupling of unactivated esters with nitroarenes to furnish in one step a wide range of amides bearing functional groups relevant to the development of drugs and agrochemicals. The method has been used to expedite the syntheses of bio-active molecules and natural products, as well as their post-synthetic modifications. Preliminary mechanistic study indicates a reaction pathway distinct from conventional amidation methods using anilines as nitrogen sources. The work provides a novel and efficient method for amide synthesis.

Continuous-Flow Synthesis of N-Succinimidyl 4-[18F]fluorobenzoate Using a Single Microfluidic Chip

PubMed Central

Kimura, Hiroyuki; Tomatsu, Kenji; Saiki, Hidekazu; Arimitsu, Kenji; Ono, Masahiro; Kawashima, Hidekazu; Iwata, Ren; Nakanishi, Hiroaki; Ozeki, Eiichi; Kuge, Yuji; Saji, Hideo

2016-01-01

In the field of positron emission tomography (PET) radiochemistry, compact microreactors provide reliable and reproducible synthesis methods that reduce the use of expensive precursors for radiolabeling and make effective use of the limited space in a hot cell. To develop more compact microreactors for radiosynthesis of 18F-labeled compounds required for the multistep procedure, we attempted radiosynthesis of N-succinimidyl 4-[18F]fluorobenzoate ([18F]SFB) via a three-step procedure using a microreactor. We examined individual steps for [18F]SFB using a batch reactor and microreactor and developed a new continuous-flow synthetic method with a single microfluidic chip to achieve rapid and efficient radiosynthesis of [18F]SFB. In the synthesis of [18F]SFB using this continuous-flow method, the three-step reaction was successfully completed within 6.5 min and the radiochemical yield was 64 ± 2% (n = 5). In addition, it was shown that the quality of [18F]SFB synthesized on this method was equal to that synthesized by conventional methods using a batch reactor in the radiolabeling of bovine serum albumin with [18F]SFB. PMID:27410684

Investigation on the reproduction performance versus acoustic contrast control in sound field synthesis.

PubMed

Bai, Mingsian R; Wen, Jheng-Ciang; Hsu, Hoshen; Hua, Yi-Hsin; Hsieh, Yu-Hao

2014-10-01

A sound reconstruction system is proposed for audio reproduction with extended sweet spot and reduced reflections. An equivalent source method (ESM)-based sound field synthesis (SFS) approach, with the aid of dark zone minimization is adopted in the study. Conventional SFS that is based on the free-field assumption suffers from synthesis error due to boundary reflections. To tackle the problem, the proposed system utilizes convex optimization in designing array filters with both reproduction performance and acoustic contrast taken into consideration. Control points are deployed in the dark zone to minimize the reflections from the walls. Two approaches are employed to constrain the pressure and velocity in the dark zone. Pressure matching error (PME) and acoustic contrast (AC) are used as performance measures in simulations and experiments for a rectangular loudspeaker array. Perceptual Evaluation of Audio Quality (PEAQ) is also used to assess the audio reproduction quality. The results show that the pressure-constrained (PC) method yields better acoustic contrast, but poorer reproduction performance than the pressure-velocity constrained (PVC) method. A subjective listening test also indicates that the PVC method is the preferred method in a live room.

Synthesis and Characterization of Doped ZnO Nanomaterials: Potential Application in Third Generation Solar Cells

NASA Astrophysics Data System (ADS)

Adcock Smith, Echo D.

ZnO nanomaterials are being incorporated into next-generation solar cell designs including dye-sensitized solar cells, multijunction solar cells, and quantum dot sensitized solar cells. ZnO nanorod (NR) arrays and nanoparticles (NP) used in these devices are typically fabricated using chemical vapor deposition and/or high-temperature reaction conditions. These methods are costly, require high energy, pressure or excessive time, but produce repeatable, defined growth that is capable of easily incorporating metal dopants. Less expensive methods of fabrication such as chemical bath deposition (CBD) eliminate the costly steps but can suffer from undefined growth, excessive waste and have a difficult time incorporating dopants into ZnO materials without additives or increased pH. This dissertation presents a novel method of growing cobalt and vanadium doped ZnO nanomaterials through microwave synthesis. The cobalt growth was compared to standard CBD and found to be faster, less wasteful, reproducible and better at incorporating cobalt ions into the ZnO lattice than typical oven CBD method. The vanadium doped ZnO microwave synthesis procedure was found to produce nanorods, nanorod arrays, and nanoparticles simultaneously. Neither the cobalt nor the vanadium growth required pH changes, catalysts or additives to assist in doping and therefore use less materials than traditional CBD. This research is important because it offers a simple, quick way to grow ZnO nanostructures and is the first to report on growing both cobalt and vanadium doped zinc oxide nanorod arrays using microwave synthesis. This synthesis method presented is a viable candidate for replacing conventional growth synthesis which will result in lowering the cost and time of production of photovoltaics while helping drive forward the development of next-generation solar cells.

A laser-deposition approach to compositional-spread discovery of materials on conventional sample sizes

NASA Astrophysics Data System (ADS)

Christen, Hans M.; Ohkubo, Isao; Rouleau, Christopher M.; Jellison, Gerald E., Jr.; Puretzky, Alex A.; Geohegan, David B.; Lowndes, Douglas H.

2005-01-01

Parallel (multi-sample) approaches, such as discrete combinatorial synthesis or continuous compositional-spread (CCS), can significantly increase the rate of materials discovery and process optimization. Here we review our generalized CCS method, based on pulsed-laser deposition, in which the synchronization between laser firing and substrate translation (behind a fixed slit aperture) yields the desired variations of composition and thickness. In situ alloying makes this approach applicable to the non-equilibrium synthesis of metastable phases. Deposition on a heater plate with a controlled spatial temperature variation can additionally be used for growth-temperature-dependence studies. Composition and temperature variations are controlled on length scales large enough to yield sample sizes sufficient for conventional characterization techniques (such as temperature-dependent measurements of resistivity or magnetic properties). This technique has been applied to various experimental studies, and we present here the results for the growth of electro-optic materials (SrxBa1-xNb2O6) and magnetic perovskites (Sr1-xCaxRuO3), and discuss the application to the understanding and optimization of catalysts used in the synthesis of dense forests of carbon nanotubes.

High-throughput continuous hydrothermal synthesis of nanomaterials (part II): unveiling the as-prepared CexZryYzO2-δ phase diagram.

PubMed

Quesada-Cabrera, Raul; Weng, Xiaole; Hyett, Geoff; Clark, Robin J H; Wang, Xue Z; Darr, Jawwad A

2013-09-09

High-throughput continuous hydrothermal flow synthesis was used to manufacture 66 unique nanostructured oxide samples in the Ce-Zr-Y-O system. This synthesis approach resulted in a significant increase in throughput compared to that of conventional batch or continuous hydrothermal synthesis methods. The as-prepared library samples were placed into a wellplate for both automated high-throughput powder X-ray diffraction and Raman spectroscopy data collection, which allowed comprehensive structural characterization and phase mapping. The data suggested that a continuous cubic-like phase field connects all three Ce-Zr-O, Ce-Y-O, and Y-Zr-O binary systems together with a smooth and steady transition between the structures of neighboring compositions. The continuous hydrothermal process led to as-prepared crystallite sizes in the range of 2-7 nm (as determined by using the Scherrer equation).

Towards a feasible and scalable production of bio-xerogels.

PubMed

Rey-Raap, Natalia; Szczurek, Andrzej; Fierro, Vanessa; Menéndez, J Angel; Arenillas, Ana; Celzard, Alain

2015-10-15

The synthesis process of carbon xerogels is limited, mainly due to two drawbacks that prevent their introduction onto the market: (i) the long time required for producing the material and (ii) the reagents used for the synthesis, which are costly and harmful to the environment. Microwave radiation is expected to produce a reduction in time of more than 90%, while the use of tannin instead of resorcinol will probably result in a cost-effective carbonaceous material. Resorcinol-tannin-formaldehyde xerogels containing different amounts of tannin, either with or without a surfactant (sodium dodecyl sulphate), were synthesized by means of two different heating methods: conventional and microwave heating. The effects of the surfactant, the heating method and the addition of tannin upon the porous structure and the chemical composition of the final materials were evaluated. It was found that the addition of surfactant is essential for obtaining highly porous xerogels when using tannins. The heating method also plays an important role, as conventionally synthesized samples display a greater volume of large pores. However, tannins are less sensitive to microwave radiation and their use results in tannin-formaldehyde xerogels that have a porous structure and chemical composition similar to those of resorcinol-formaldehyde xerogels. Copyright © 2015 Elsevier Inc. All rights reserved.

Sustainable synthesis of monodispersed spinel nano-ferrites

EPA Science Inventory

A sustainable approach for the synthesis of various monodispersed spinel ferrite nanoparticles has been developed that occurs at water-toluene interface under both conventional and microwave hydrothermal conditions. This general synthesis procedure utilizes readily available and ...

Supplementary search methods were more effective and offered better value than bibliographic database searching: A case study from public health and environmental enhancement.

PubMed

Cooper, Chris; Lovell, Rebecca; Husk, Kerryn; Booth, Andrew; Garside, Ruth

2018-06-01

We undertook a systematic review to evaluate the health benefits of environmental enhancement and conservation activities. We were concerned that a conventional process of study identification, focusing on exhaustive searches of bibliographic databases as the primary search method, would be ineffective, offering limited value. The focus of this study is comparing study identification methods. We compare (1) an approach led by searches of bibliographic databases with (2) an approach led by supplementary search methods. We retrospectively assessed the effectiveness and value of both approaches. Effectiveness was determined by comparing (1) the total number of studies identified and screened and (2) the number of includable studies uniquely identified by each approach. Value was determined by comparing included study quality and by using qualitative sensitivity analysis to explore the contribution of studies to the synthesis. The bibliographic databases approach identified 21 409 studies to screen and 2 included qualitative studies were uniquely identified. Study quality was moderate, and contribution to the synthesis was minimal. The supplementary search approach identified 453 studies to screen and 9 included studies were uniquely identified. Four quantitative studies were poor quality but made a substantive contribution to the synthesis; 5 studies were qualitative: 3 studies were good quality, one was moderate quality, and 1 study was excluded from the synthesis due to poor quality. All 4 included qualitative studies made significant contributions to the synthesis. This case study found value in aligning primary methods of study identification to maximise location of relevant evidence. Copyright © 2017 John Wiley & Sons, Ltd.

Porous MnCo2O4 as superior anode material over MnCo2O4 nanoparticles for rechargeable lithium ion batteries

NASA Astrophysics Data System (ADS)

Baji, Dona Susan; Jadhav, Harsharaj S.; Nair, Shantikumar V.; Rai, Alok Kumar

2018-06-01

Pyro synthesis is a method to coat nanoparticles by uniform layer of carbon without using any conventional carbon source. The resultant carbon coating can be evaporated in the form of CO or CO2 at high temperature with the creation of large number of nanopores on the sample surface. Hence, a porous MnCo2O4 is successfully synthesized here with the same above strategy. It is believed that the electrolyte can easily permeate through these nanopores into the bulk of the sample and allow rapid access of Li+ ions during charge/discharge cycling. In order to compare the superiority of the porous sample synthesized by pyro synthesis method, MnCo2O4 nanoparticles are also synthesized by sol-gel synthesis method at the same parameters. When tested as anode materials for lithium ion battery application, porous MnCo2O4 electrode shows high capacity with long lifespan at all the investigated current rates in comparison to MnCo2O4 nanoparticles electrode.

Combustion synthesis of ceramic-metal composite materials - The TiC-Al2O3-Al system

NASA Technical Reports Server (NTRS)

Feng, H. J.; Moore, John J.; Wirth, D. G.

1992-01-01

Combustion synthesis was applied for producing ceramic-metal composites with reduced levels of porosity, by allowing an excess amount of liquid metal, generated by the exothermic reaction during synthesis, to infiltrate the pores. It is shown that this method, when applied to TiC-Al2O3 system, led to a decreased level of porosity in the resulting TiC-Al2O3-Al product, as compared with that of TiC-Al2O3 system. This in situ procedure is more efficient than the two-stage conventional processes (i.e., sintering followed by liquid metal infiltration), although there are limitations with respect to total penetration of the liquid metal and maintaining a stable propagation of the combustion reaction.

Green synthesis of chalcones derivatives as intermediate of flavones and their antibacterial activities

NASA Astrophysics Data System (ADS)

VH, Elfi Susanti; Matsjeh, Sabirin; Wahyuningsih, Tutik Dwi; Mustofa, Redjeki, Tri

2016-02-01

Four chalcones derivatives have been synthesized from 3,4-dimethoxybenzaldehyde and acetophenone derivatives (2-hydroxy acetophenone, 2,4-dihydroxy acetophenone, 2,5-dihydroxy acetophenone and 2,6-dihydroxy acetophenone). The synthesis of these chalcones were conducted by Claisen-Schmidt condensation using grinding techniques at room temperature in the absence of solvents. The chalcones were prepared by grinding together equivalent amount of the approriate hydroxyacetophenone and 3,4-dimethoxybenzaldehyde in the presence of solid sodium hydroxide. Grinding techniques for synthesis of the chalcones derivatives is simple, efficient and environmentally benign compared to conventional methods. Then, the four chalcones derivatives undergo cyclization reactions to produce four flavones after reacted with iodine. The synthesized compounds were characterized by spectrometry (IR, 1H-NMR, 13C-NMR and MS).

Example-Based Automatic Music-Driven Conventional Dance Motion Synthesis

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

Xu, Songhua; Fan, Rukun; Geng, Weidong

We introduce a novel method for synthesizing dance motions that follow the emotions and contents of a piece of music. Our method employs a learning-based approach to model the music to motion mapping relationship embodied in example dance motions along with those motions' accompanying background music. A key step in our method is to train a music to motion matching quality rating function through learning the music to motion mapping relationship exhibited in synchronized music and dance motion data, which were captured from professional human dance performance. To generate an optimal sequence of dance motion segments to match with amore » piece of music, we introduce a constraint-based dynamic programming procedure. This procedure considers both music to motion matching quality and visual smoothness of a resultant dance motion sequence. We also introduce a two-way evaluation strategy, coupled with a GPU-based implementation, through which we can execute the dynamic programming process in parallel, resulting in significant speedup. To evaluate the effectiveness of our method, we quantitatively compare the dance motions synthesized by our method with motion synthesis results by several peer methods using the motions captured from professional human dancers' performance as the gold standard. We also conducted several medium-scale user studies to explore how perceptually our dance motion synthesis method can outperform existing methods in synthesizing dance motions to match with a piece of music. These user studies produced very positive results on our music-driven dance motion synthesis experiments for several Asian dance genres, confirming the advantages of our method.« less

Bulk Synthesis of Monodisperse Ferrite Nanoparticles at Water-Organic Interfaces under Conventional and Microwave Hydrothermal Treatment and Their Surface Functionalization

EPA Science Inventory

Synthesis of monodisperse MFe2O4 (M=, Ni, Co, Mn) and γ-Fe2O3 nanoparticles at a water-toluene interface under conventional as well as microwave hydrothermal conditions using readily available nitrate or chloride salts and oleic acid as the dispersing agent is described. The ens...

γ-Alumina Nanoparticle Catalyzed Efficient Synthesis of Highly Substituted Imidazoles.

PubMed

Reddy, Bandapalli Palakshi; Vijayakumar, Vijayaparthasarathi; Arasu, Mariadhas Valan; Al-Dhabi, Naif Abdullah

2015-10-21

γ-Alumina nano particle catalyzed multi component reaction of benzil, arylaldehyde and aryl amines afforded the highly substituted 1,2,4,5-tetraaryl imidazoles with good to excellent yield in less reaction time under the sonication as well as the conventional methods. Convenient operational simplicity, mild conditions and the reusability of catalyst were the other advantages of this developed protocol.

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

NASA Astrophysics Data System (ADS)

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.

Seedless Synthesis of Monodispersed Gold Nanorods with Remarkably High Yield: Synergistic Effect of Template Modification and Growth Kinetics Regulation.

PubMed

Liu, Kang; Bu, Yanru; Zheng, Yuanhui; Jiang, Xuchuan; Yu, Aibing; Wang, Huanting

2017-03-08

Gold nanorods (AuNRs) are versatile materials due to their broadly tunable optical properties associated with their anisotropic feature. Conventional seed-mediated synthesis is, however, not only limited by the operational complexity and over-sensitivity towards subtle changes of experimental conditions but also suffers from low yield (≈15 %). A facile seedless method is reported to overcome these challenges. Monodispersed AuNRs with high yield (≈100 %) and highly adjustable longitudinal surface plasmon resonance (LSPR) are reproducibly synthesized. The parameters that influence the AuNRs growth were thoroughly investigated in terms of growth kinetics and soft-template regulation, offering a better understanding of the template-based mechanism. The facile synthesis, broad tunability of LSRP, high reproducibility, high yield, and ease of scale-up make this method promising for the future mass production of monodispersed AuNRs for applications in catalysis, sensing, and biomedicine. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Shock-induced synthesis of high temperature superconducting materials

DOEpatents

Ginley, D.S.; Graham, R.A.; Morosin, B.; Venturini, E.L.

1987-06-18

It has now been determined that the unique features of the high pressure shock method, especially the shock-induced chemical synthesis technique, are fully applicable to high temperature superconducting materials. Extraordinarily high yields are achievable in accordance with this invention, e.g., generally in the range from about 20% to about 99%, often in the range from about 50% to about 90%, lower and higher yields, of course, also being possible. The method of this invention involves the application of a controlled high pressure shock compression pulse which can be produced in any conventional manner, e.g., by detonation of a high explosive material, the impact of a high speed projectile or the effect of intense pulsed radiation sources such as lasers or electron beams. Examples and a discussion are presented.

Techno-economic assessment of integrating methanol or Fischer-Tropsch synthesis in a South African sugar mill.

PubMed

Petersen, Abdul M; Farzad, Somayeh; Görgens, Johann F

2015-05-01

This study considered an average-sized sugar mill in South Africa that crushes 300 wet tonnes per hour of cane, as a host for integrating methanol and Fischer-Tropsch synthesis, through gasification of a combined flow of sugarcane trash and bagasse. Initially, it was shown that the conversion of biomass to syngas is preferably done by catalytic allothermal gasification instead of catalytic autothermal gasification. Thereafter, conventional and advanced synthesis routes for both Methanol and Fischer-Tropsch products were simulated with Aspen Plus® software and compared by technical and economic feasibility. Advanced FT synthesis satisfied the overall energy demands, but was not economically viable for a private investment. Advanced methanol synthesis is also not viable for private investment since the internal rate of return was 21.1%, because it could not provide the steam that the sugar mill required. The conventional synthesis routes had less viability than the corresponding advanced synthesis routes. Copyright © 2015 Elsevier Ltd. All rights reserved.

Highly efficient preparation of sphingoid bases from glucosylceramides by chemoenzymatic method[S

PubMed Central

Gowda, Siddabasave Gowda B.; Usuki, Seigo; Hammam, Mostafa A. S.; Murai, Yuta; Igarashi, Yasuyuki; Monde, Kenji

2016-01-01

Sphingoid base derivatives have attracted increasing attention as promising chemotherapeutic candidates against lifestyle diseases such as diabetes and cancer. Natural sphingoid bases can be a potential resource instead of those derived by time-consuming total organic synthesis. In particular, glucosylceramides (GlcCers) in food plants are enriched sources of sphingoid bases, differing from those of animals. Several chemical methodologies to transform GlcCers to sphingoid bases have already investigated; however, these conventional methods using acid or alkaline hydrolysis are not efficient due to poor reaction yield, producing complex by-products and resulting in separation problems. In this study, an extremely efficient and practical chemoenzymatic transformation method has been developed using microwave-enhanced butanolysis of GlcCers and a large amount of readily available almond β-glucosidase for its deglycosylation reaction of lysoGlcCers. The method is superior to conventional acid/base hydrolysis methods in its rapidity and its reaction cleanness (no isomerization, no rearrangement) with excellent overall yield. PMID:26667669

Electricity generation from synthesis gas by microbial processes: CO fermentation and microbial fuel cell technology.

PubMed

Kim, Daehee; Chang, In Seop

2009-10-01

A microbiological process was established to harvest electricity from the carbon monoxide (CO). A CO fermenter was enriched with CO as the sole carbon source. The DGGE/DNA sequencing results showed that Acetobacterium spp. were enriched from the anaerobic digester fluid. After the fermenter was operated under continuous mode, the products were then continuously fed to the microbial fuel cell (MFC) to generate electricity. Even though the conversion yield was quite low, this study proved that synthesis gas (syn-gas) can be converted to electricity with the aid of microbes that do not possess the drawbacks of metal catalysts of conventional methods.

Furfural Synthesis from d-Xylose in the Presence of Sodium Chloride: Microwave versus Conventional Heating.

PubMed

Xiouras, Christos; Radacsi, Norbert; Sturm, Guido; Stefanidis, Georgios D

2016-08-23

We investigate the existence of specific/nonthermal microwave effects for the dehydration reaction of xylose to furfural in the presence of NaCl. Such effects are reported for sugars dehydration reactions in several literature reports. To this end, we adopted three approaches that compare microwave-assisted experiments with a) conventional heating experiments from the literature; b) simulated conventional heating experiments using microwave-irradiated silicon carbide (SiC) vials; and at c) different power levels but the same temperature by using forced cooling. No significant differences in the reaction kinetics are observed using any of these methods. However, microwave heating still proves advantageous as it requires 30 % less forward power compared to conventional heating (SiC vial) to achieve the same furfural yield at a laboratory scale. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microfluidic Reactors for the Controlled Synthesis of Nanoparticles

NASA Astrophysics Data System (ADS)

Erdem, Emine Yegan

Nanoparticles have attracted a lot of attention in the past few decades due to their unique, size-dependent properties. In order to use these nanoparticles in devices or sensors effectively, it is important to maintain uniform properties throughout the system; therefore nanoparticles need to have uniform sizes -- or monodisperse. In order to achieve monodispersity, an extreme control over the reaction conditions is required during their synthesis. These reaction conditions such as temperature, concentration of reagents, residence times, etc. affect the structure of nanoparticles dramatically; therefore when the conditions vary locally in the reaction vessel, different sized nanoparticles form, causing polydispersity. In widely-used batch wise synthesis techniques, large sized reaction vessels are used to mix and heat reagents. In these types of systems, it is very hard to avoid thermal gradients and to achieve rapid mixing times as well as to control residence times. Also it is not possible to make rapid changes in the reaction parameters during the synthesis. The other drawback of conventional methods is that it is not possible to separate the nucleation of nanoparticles from their growth; this leads to combined nucleation and growth and subsequently results in polydisperse size distributions. Microfluidics is an alternative method by which the limitations of conventional techniques can be addressed. Due to the small size, it is possible to control temperature and concentration of reagents precisely as well as to make rapid changes in mixing ratios of reagents or temperature of the reaction zones. There have been several microfluidic reactors -- (microreactors) in literature that were designed to improve the size distribution of nanoparticles. In this work, two novel microfluidic systems were developed for achieving controlled synthesis of nanoparticles. The first microreactor was made out of a chemically robust polymer, polyurethane, and it was used for low temperature nanoparticle synthesis. This microreactor was fabricated by using a CO 2-laser printer, which is an inexpensive method for fabricating microfluidic devices and it is a relatively fast way compared to other fabrication techniques. Iron oxide nanoparticle synthesis was demonstrated using this reactor and size distributions with a standard deviation of 10% was obtained. The second microreactor presented in this work was designed to produce monodisperse nanoparticles by utilizing thermally isolated heated and cooled regions for separating nucleation and growth processes. This microreactor was made out of silicon and it was used to demonstrate the synthesis of TiO 2 nanoparticles. Size distributions with less than 10% standard deviation were achieved. This microreactor also provides a platform for studying the effects of temperature and residence times which is very important to understand the reaction kinetics of nanoparticle synthesis. In this work, two microfluidic techniques for retrieving nanoparticles from the microreactors were also discussed. The first method was based on trapping the aqueous droplet phase inside the microchannel and the second method was utilizing a micropost array to direct droplets from the oil solution to the pure water. As a final step, a printing technique was used to print nanoparticles synthesized inside the microreactors for future applications. This ability is important for achieving smart surfaces that can utilize the properties of nanoparticles for sensing applications in the future.

Development of a New Generation of Stable, Tunable, and Catalytically Active Nanoparticles Produced by the Helium Nanodroplet Deposition Method

DOE PAGES

Wu, Qiyuan; Ridge, Claron J.; Zhao, Shen; ...

2016-07-13

Nanoparticles (NPs) are revolutionizing many areas of science and technology, often delivering unprecedented improvements to properties of the conventional materials. However, despite important advances in NPs synthesis and applications, numerous challenges still remain. Development of alternative synthetic method capable of producing very uniform, extremely clean and very stable NPs is urgently needed. If successful, such method can potentially transform several areas of nanoscience, including environmental and energy related catalysis. Here we present the first experimental demonstration of catalytically active NPs synthesis achieved by the helium nanodroplet isolation method. This alternative method of NPs fabrication and deposition produces narrowly distributed, clean,more » and remarkably stable NPs. The fabrication is achieved inside ultra-low temperature, superfluid helium nanodroplets, which can be subsequently deposited onto any substrate. Lastly, this technique is universal enough to be applied to nearly any element, while achieving high deposition rates for single element as well as composite core-shell NPs.« less

Model Updating of Complex Structures Using the Combination of Component Mode Synthesis and Kriging Predictor

PubMed Central

Li, Yan; Wang, Dejun; Zhang, Shaoyi

2014-01-01

Updating the structural model of complex structures is time-consuming due to the large size of the finite element model (FEM). Using conventional methods for these cases is computationally expensive or even impossible. A two-level method, which combined the Kriging predictor and the component mode synthesis (CMS) technique, was proposed to ensure the successful implementing of FEM updating of large-scale structures. In the first level, the CMS was applied to build a reasonable condensed FEM of complex structures. In the second level, the Kriging predictor that was deemed as a surrogate FEM in structural dynamics was generated based on the condensed FEM. Some key issues of the application of the metamodel (surrogate FEM) to FEM updating were also discussed. Finally, the effectiveness of the proposed method was demonstrated by updating the FEM of a real arch bridge with the measured modal parameters. PMID:24634612

Synthesis of carbon nanotubes by arc discharge in open air.

PubMed

Paladugu, Mohan Chand; Maneesh, K; Nair, P Kesavan; Haridoss, Prathap

2005-05-01

In this work Carbon nanotubes have been synthesized by arc discharge in open air. A TIG welding ac/dc inverter was used as the power source for arc discharge. During each run of the arc discharge based synthesis, the anode was a low purity (approximately 85% C by weight) graphite rod. The effect of varying the atmosphere on the yield of soot of the carbon nanotube containing carbon soot has been studied. Various soots were produced, purified by oxidation and characterized to confirm formation of carbon nanotubes and their relative quality, using transmission electron microscopy, Raman spectroscopy, and XRD. It was found that the yield of soot formed on the cathode is higher when synthesis is carried out in open air than when carried out in a flowing argon atmosphere. When synthesized in open air, using a 7.2-mm-diameter graphite rod as anode, the yield of soot was around 50% by weight of the graphite consumed. Current and voltage for arcing were at identical starting values in all the experiments. This modified method does not require a controlled atmosphere as in the case of a conventional arc discharge method of synthesis and hence the cost of production may be reduced.

ERTS: A multispectral image analysis contribution for the geomorphological evaluation of southern Maracaibo Lake Basin. [geological survey and drainage patterns

NASA Technical Reports Server (NTRS)

Salas, F.; Cabello, O.; Alarcon, F.; Ferrer, C.

1974-01-01

Multispectral analysis of ERTS-A images at scales of 1:1,000,000 and 1:500,000 has been conducted with conventional photointerpretation methods. Specific methods have been developed for the geomorphological analysis of southern Maracaibo Lake Basin which comprises part of the Venezuelan Andean Range, Perija Range, the Tachira gap and the Southern part of the Maracaibo Lake depression. A steplike analysis was conducted to separate macroforms, landscapes and relief units as well as drainage patterns and tectonic features, which permitted the delineation of tectonic provinces, stratigraphic units, geomorphologic units and geomorphologic positions. The geomorphologic synthesis obtained compares favorably with conventional analysis made on this area for accuracy of 1:100,000 scale, and in some features with details obtained through conventional analysis for accuracy of 1:15,000 and field work. Geomorphological units in the mountains were identified according to changes in tone, texture, forms orientation of interfluves and tectonic characteristics which control interfluvial disimetrics.

Design and Implementation of Viterbi Decoder Using VHDL

NASA Astrophysics Data System (ADS)

Thakur, Akash; Chattopadhyay, Manju K.

2018-03-01

A digital design conversion of Viterbi decoder for ½ rate convolutional encoder with constraint length k = 3 is presented in this paper. The design is coded with the help of VHDL, simulated and synthesized using XILINX ISE 14.7. Synthesis results show a maximum frequency of operation for the design is 100.725 MHz. The requirement of memory is less as compared to conventional method.

Green synthesis of chalcones derivatives as intermediate of flavones and their antibacterial activities

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

VH, Elfi Susanti, E-mail: elsantivh@yahoo.com; Redjeki, Tri, E-mail: tri-redjeki@yahoo.com; Matsjeh, Sabirin, E-mail: sabirin-mara@yahoo.com

Four chalcones derivatives have been synthesized from 3,4-dimethoxybenzaldehyde and acetophenone derivatives (2-hydroxy acetophenone, 2,4-dihydroxy acetophenone, 2,5-dihydroxy acetophenone and 2,6-dihydroxy acetophenone). The synthesis of these chalcones were conducted by Claisen-Schmidt condensation using grinding techniques at room temperature in the absence of solvents. The chalcones were prepared by grinding together equivalent amount of the approriate hydroxyacetophenone and 3,4-dimethoxybenzaldehyde in the presence of solid sodium hydroxide. Grinding techniques for synthesis of the chalcones derivatives is simple, efficient and environmentally benign compared to conventional methods. Then, the four chalcones derivatives undergo cyclization reactions to produce four flavones after reacted with iodine. The synthesized compoundsmore » were characterized by spectrometry (IR, {sup 1}H-NMR, {sup 13}C-NMR and MS)« less

Regioisomer-Free C 4h β-Tetrakis(tert-butyl)metallo-phthalocyanines: Regioselective Synthesis and Spectral Investigations.

PubMed

Iida, Norihito; Tanaka, Kenta; Tokunaga, Etsuko; Takahashi, Hiromi; Shibata, Norio

2015-04-01

Metal β-tetrakis(tert-butyl)phthalocyanines are the most commonly used phthalocyanines due to their high solubility, stability, and accessibility. They are commonly used as a mixture of four regioisomers, which arise due to the tert-butyl substituent on the β-position, and to the best of our knowledge, their regioselective synthesis has yet to be reported. Herein, the C 4h -selective synthesis of β-tetrakis(tert-butyl)metallophthalocyanines is disclosed. Using tetramerization of α-trialkylsilyl phthalonitriles with metal salts following acid-mediated desilylation, the desired metallophthalocyanines were obtained in good yields. Upon investigation of regioisomer-free zinc β-tetrakis(tert-butyl)phthalocyanine using spectroscopy, the C 4h single isomer described here was found to be distinct in the solid state to zinc β-tetrakis(tert-butyl)phthalocyanine obtained by a conventional method.

Bacteria in Nanoparticle Synthesis: Current Status and Future Prospects

PubMed Central

2014-01-01

Microbial metal reduction can be a strategy for remediation of metal contaminations and wastes. Bacteria are capable of mobilization and immobilization of metals and in some cases, the bacteria which can reduce metal ions show the ability to precipitate metals at nanometer scale. Biosynthesis of nanoparticles (NPs) using bacteria has emerged as rapidly developing research area in green nanotechnology across the globe with various biological entities being employed in synthesis of NPs constantly forming an impute alternative for conventional chemical and physical methods. Optimization of the processes can result in synthesis of NPs with desired morphologies and controlled sizes, fast and clean. The aim of this review is, therefore, to make a reflection on the current state and future prospects and especially the possibilities and limitations of the above mentioned bio-based technique for industries. PMID:27355054

An easy access to 2-Amino-5,6-dihydro-3H-pyrimidin-4-one building blocks: the reaction under conventional and microwave conditions.

PubMed

Ostras, Konstantin S; Gorobets, Nikolay Yu; Desenko, Sergey M; Musatov, Vladimir I

2006-08-01

A new one-stage fast multicomponent synthesis of title compounds leads to products in 21-55% isolated yields under both conventional and microwave conditions. The primary amino group in the building blocks can be easily acylated by various usual electophilic agents that can be utilized in the synthesis of diverse heterocylic compounds libraries.

STUDY ON SYNTHESIS AND EVOLUTION OF NANOCRYSTALLINE Mg4Ta2O9 BY AQUEOUS SOL-GEL PROCESS

NASA Astrophysics Data System (ADS)

Wu, H. T.; Yang, C. H.; Wu, W. B.; Yue, Y. L.

2012-06-01

Nanosized and highly reactive Mg4Ta2O9 were successfully synthesized by aqueous sol-gel method compared with conventional solid-state method. Ta-Mg-citric acid solution was first formed and then evaporated resulting in a dry gel for calcination in the temperature ranging from 600°C to 800°C for crystallization in oxygen atmosphere. The crystallization process from the gel to crystalline Mg4Ta2O9 was identified by thermal analysis and phase evolution of powders was studied using X-ray diffraction (XRD) technique during calcinations. Particle size and morphology were examined by transmission electron microscopy (TEM) and high resolution scanning electron microscopy (HR-SEM). The results revealed that sol-gel process showed great advantages over conventional solid-state method and Mg4Ta2O9 nanopowders with the size of 20-30 nm were obtained at 800°C.

Low temperature synthesis of hierarchical TiO 2 nanostructures for high performance perovskite solar cells by pulsed laser deposition

DOE PAGES

Yang, Bin; Mahjouri-Samani, Masoud; Rouleau, Christopher M.; ...

2016-06-10

A promising way to advance perovskite solar cells is to improve the quality of the electron transport material e.g., titanium dioxide (TiO 2) in a direction that increases electron transport and extraction. Although dense TiO 2 films are easily grown in solution, efficient electron extraction suffers due to a lack of interfacial contact area with the perovskite. Conversely, mesoporous films do offer high surface-area-to-volume ratios, thereby promoting efficient electron extraction, but their morphology is relatively difficult to control via conventional solution synthesis methods. Here, a pulsed laser deposition method was used to assemble TiO 2 nanoparticles into TiO 2 hierarchicalmore » nanoarchitectures having the anatase crystal structure, and prototype solar cells employing these structures yielded power conversion efficiencies of ~ 14%. Our approach demonstrates a way to grow high aspect-ratio TiO 2 nanostructures for improved interfacial contact between TiO 2 and perovskite materials, leading to high electron-hole pair separation and electron extraction efficiencies for superior photovoltaic performance. In addition, compared to conventional solution-processed TiO 2 films that require 500 °C to obtain a good crystallinity, our relatively low temperature (300 °C) TiO 2 processing method may promote reduced energy-consumption during device fabrication as well as enable compatibility with various flexible polymer substrates.« less

Low temperature synthesis & characterization of lead-free BCZT ceramics using molten salt method

NASA Astrophysics Data System (ADS)

Jai Shree, K.; Chandrakala, E.; Das, Dibakar

2018-04-01

Piezoelectric properties are greatly influenced by the synthesis route, microstructure, stoichiometry of the chemical composition, purity of the starting materials. In this study, molten salt method was used to prepare lead-free BCZT ceramics. Molten salt method is one of the simplestmethods to prepare chemically-purified, single phase powders in high yield often at lower temperatures and shorten reaction time. Calcination of the molten salt synthesized powders resulted in asingle-phase perovskite structure at 1000 °C which is ˜ 350 °C less than the conventional solid-sate reaction method. With increasing calcination temperature the average template size was increased (˜ 0.5-2 µm). Formation of well dispersive templates improves the sinterability at lower temperatures. Lead-free BCZT ceramics sintered at 1500 °C for 2 h resulted in homogenous and highly dense microstructure with ˜92% of the theoretical density and a grain size of ˜ 35 µm. This highly dense microstructure could enhance the piezoelectric properties of the system.

Iron Oxide Nanoparticles Employed as Seeds for the Induction of Microcrystalline Diamond Synthesis

PubMed Central

2008-01-01

Iron nanoparticles were employed to induce the synthesis of diamond on molybdenum, silicon, and quartz substrates. Diamond films were grown using conventional conditions for diamond synthesis by hot filament chemical vapor deposition, except that dispersed iron oxide nanoparticles replaced the seeding. X-ray diffraction, visible, and ultraviolet Raman Spectroscopy, energy-filtered transmission electron microscopy , electron energy-loss spectroscopy, and X-ray photoelectron spectroscopy (XPS) were employed to study the carbon bonding nature of the films and to analyze the carbon clustering around the seed nanoparticles leading to diamond synthesis. The results indicate that iron oxide nanoparticles lose the O atoms, becoming thus active C traps that induce the formation of a dense region of trigonally and tetrahedrally bonded carbon around them with the ensuing precipitation of diamond-type bonds that develop into microcrystalline diamond films under chemical vapor deposition conditions. This approach to diamond induction can be combined with dip pen nanolithography for the selective deposition of diamond and diamond patterning while avoiding surface damage associated to diamond-seeding methods.

Synthesis of Continuous Conductive PEDOT:PSS Nanofibers by Electrospinning: A Conformal Coating for Optoelectronics.

PubMed

Bessaire, Bastien; Mathieu, Maillard; Salles, Vincent; Yeghoyan, Taguhi; Celle, Caroline; Simonato, Jean-Pierre; Brioude, Arnaud

2017-01-11

A process to synthesize continuous conducting nanofibers were developed using PEDOT:PSS as a conducting polymer and an electrospinning method. Experimental parameters were carefully explored to achieve reproducible conductive nanofibers synthesis in large quantities. In particular, relative humidity during the electrospinning process was proven to be of critical importance, as well as doping post-treatment involving glycols and alcohols. The synthesized fibers were assembled as a mat on glass substrates, forming a conductive and transparent electrode and their optoelectronic have been fully characterized. This method produces a conformable conductive and transparent coating that is well-adapted to nonplanar surfaces, having very large aspect ratio features. A demonstration of this property was made using surfaces having deep trenches and high steps, where conventional transparent conductive materials fail because of a lack of conformability.

Synthesis of reference compounds related to Chemical Weapons Convention for verification and drug development purposes – a Brazilian endeavour

NASA Astrophysics Data System (ADS)

Cavalcante, S. F. A.; de Paula, R. L.; Kitagawa, D. A. S.; Barcellos, M. C.; Simas, A. B. C.; Granjeiro, J. M.

2018-03-01

This paper deals with challenges that Brazilian Army Organic Synthesis Laboratory has been going through to access reference compounds related to the Chemical Weapons Convention in order to support verification analysis and for research of novel antidotes. Some synthetic procedures to produce the chemicals, as well as Quality Assurance issues and a brief introduction of international agreements banning chemical weapons are also presented.

Synthesis and study of the synthetic hydroxyapatite doped with aluminum

NASA Astrophysics Data System (ADS)

Goldberg, M.; Smirnov, V.; Antonova, O.; Konovalov, A.; Fomina, A.; Komlev, V. S.; Barinov, S.; Rodionov, A.; Gafurov, M.; Orlinskii, S.

2018-05-01

Powders of synthetic hydroxyapatite doped with aluminium (Al) ions in concentrations 0 and 20 mol. % were synthesized by the precipitation method from the nitrate solutions and investigated by atomic emission spectrometry with inductively coupled plasma (AES-ICP), X-ray diffraction (XRD), scanning electron microscopy (SEM), gas absorption and conventional electron paramagnetic resonance (EPR). It is shown that for the chosen synthesis route an introduction of Al provokes formation of highly anisotropic phase, leads to the decrease in the crystallinity while no significant changes in the EPR spectra of the radiation-induced defects is observed. The results could be used for understanding the structural transformations with Al doping of the mineralized materials for geological and biomedical applications.

Low-Dielectric Constant Polyimide Nanoporous Films: Synthesis and Properties

NASA Astrophysics Data System (ADS)

Mehdipour-Ataei, S.; Rahimi, A.; Saidi, S.

2007-08-01

Synthesis of high temperature polyimide foams with pore sizes in the nanometer range was developed. Foams were prepared by casting graft copolymers comprising a thermally stable block as the matrix and a thermally labile material as the dispersed phase. Polyimides derived from pyromellitic dianhydride with new diamines (4BAP and BAN) were used as the matrix material and functionalized poly(propylene glycol) oligomers were used as a thermally labile constituent. Upon thermal treatment the labile blocks were subsequently removed leaving pores with the size and shape of the original copolymer morphology. The polyimides and foamed polyimides were characterized by some conventional methods including FTIR, H-NMR, DSC, TGA, SEM, TEM, and dielectric constant.

Biosynthesis of Oligomeric Anthocyanins from Grape Skin Extracts.

PubMed

Hwang, Jin-Woo; Natarajan, Sithranga Boopathy; Kim, Yon-Suk; Kim, Eun-Kyung; Lee, Jae Woong; Moon, Sang-Ho; Jeon, Byong-Tae; Park, Pyo-Jam

2017-03-21

We synthesized oligomeric anthocyanins from grape skin-derived monomeric anthocyanins such as anthocyanidin and proanthocyanidin by a fermentation technique using Aspergillus niger, crude enzymes and glucosidase. The biosyntheses of the oligomeric anthocyanins carried out by the conventional method using Aspergillus niger and crude enzymes were confirmed by ESI-MS. The molecular weight of the synthesized anthocyanin oligomers was determined using MALDI-MS. The yield of anthocyanin oligomers using crude enzymes was higher than that of the synthesis using Aspergillus fermentation. Several studies have been demonstrated that oligomeric anthocyanins have higher antioxidant activity than monomeric anthocyanins. Fermentation-based synthesis of oligomeric anthocyanins is an alternative way of producing useful anthocyanins that could support the food industry.

Ultrasound mediated, iodine catalyzed green synthesis of novel 2-amino-3-cyano-4H-pyran derivatives.

PubMed

Tabassum, Sumaiya; Govindaraju, Santhosh; Khan, Riyaz-ur-Rahaman; Pasha, Mohamed Afzal

2015-05-01

An efficient synthesis of a novel series of twelve substituted 2-amino-3-cyano-4H-pyran derivatives was achieved by a one-pot three-component cyclocondensation reaction of heteroaryl aldehydes, malononitrile and active methylene compounds catalyzed by iodine in aqueous medium under ultrasound irradiation. In comparison with conventional methods, our protocol is convenient and offers several advantages, such as shorter reaction time, higher yields, milder conditions and environmental friendliness. We have herein successfully demonstrated the synergistic outcome of multi-component reaction (MCR) and sonication to offer a facile route for the design of these derivatives. Copyright © 2014 Elsevier B.V. All rights reserved.

Lithium Assisted “Dissolution–Alloying” Synthesis of Nanoalloys from Individual Bulk Metals

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

Barkholtz, Heather M.; Gallagher, James R.; Li, Tao

2016-04-12

We report new fundamental chemistry involved in the synthesis of bimetallic nanoalloys via dissolving the pure bulk transition metals in molten lithium. It is revealed at the atomic level that when two pure bulk transition metals such as Pd and Pt are placed in molten lithium (similar to 200 degrees C), they undergo a dissolution process in which the metal-metal bonds in pure bulk transition metals are completely ruptured, which results in the existence of individual Pd and Pt atoms surrounded by lithium atoms, as is evident by synchrotron X-ray adsorption techniques. Then, upon the conversion of metal lithium tomore » LiOH in humid air, the Pd and Pt atoms undergo an alloying process to aggregate into nanoalloys. This method was further expanded to include PdZn, which is notoriously difficult to prepare via traditional nanoalloy synthesis methods due to the easily oxidizable Zn component. The constantly reducing environment of metallic Li allowed for preparation of PdZn nanoalloys with minimal Zn oxidation via dissolution-alloying of individual bulk transition metals in molten lithium. Additionally, this lithium assisted "dissolution-alloying" method bypasses many complications intrinsic to conventional ion reduction-based nanoalloy synthesis including the necessity of ligated metal ions, the use of proper reducing agents and dispersing surfactants, and the presence of segregated phases due to different reduction potentials of the constituent metal ions.« less

Lithium assisted “dissolution–alloying” synthesis of nanoalloys from individual bulk metals

DOE PAGES

Barkholtz, Heather M.; Gallagher, James R.; Li, Tao; ...

2016-03-27

Here, we report new fundamental chemistry involved in the synthesis of bimetallic nanoalloys via dissolving the pure bulk transition metals in molten lithium. It is revealed at the atomic level that when two pure bulk transition metals such as Pd and Pt are placed in molten lithium (~200°C), they undergo a dissolution process in which the metal-metal bonds in pure bulk transition metals are completely ruptured, resulting in the existence of individual Pd and Pt atoms surrounded by lithium atoms, as is evident by synchrotron Xray adsorption techniques. Then, upon the conversion of metal lithium to LiOH in humid air,more » the Pd and Pt atoms undergo an alloying process, to aggregate into nanoalloys. This method was further expanded to include PdZn, which is notoriously difficult to prepare via traditional nanoalloy synthesis methods due to the easily oxidizable Zn component. The constantly reducing environment of metallic Li allowed for preparation of PdZn nanoalloys with minimal Zn oxidation via dissolution-alloying of individual bulk transition metals in molten lithium. Additionally, this lithium assisted “dissolutionalloying” method bypasses many complications intrinsic to conventional ion reductionbased nanoalloy synthesis including the necessity of ligated metal ions, the use of proper reducing agents and dispersing surfactants, and the presence of segregated phases due to different reduction potentials of the constituent metal ions.« less

Synthesis and Characterization of Functionalized Metal-organic Frameworks

PubMed Central

Karagiaridi, Olga; Bury, Wojciech; Sarjeant, Amy A.; Hupp, Joseph T.; Farha, Omar K.

2014-01-01

Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and technological applications. Their signature property is their ultrahigh porosity, which however imparts a series of challenges when it comes to both constructing them and working with them. Securing desired MOF chemical and physical functionality by linker/node assembly into a highly porous framework of choice can pose difficulties, as less porous and more thermodynamically stable congeners (e.g., other crystalline polymorphs, catenated analogues) are often preferentially obtained by conventional synthesis methods. Once the desired product is obtained, its characterization often requires specialized techniques that address complications potentially arising from, for example, guest-molecule loss or preferential orientation of microcrystallites. Finally, accessing the large voids inside the MOFs for use in applications that involve gases can be problematic, as frameworks may be subject to collapse during removal of solvent molecules (remnants of solvothermal synthesis). In this paper, we describe synthesis and characterization methods routinely utilized in our lab either to solve or circumvent these issues. The methods include solvent-assisted linker exchange, powder X-ray diffraction in capillaries, and materials activation (cavity evacuation) by supercritical CO2 drying. Finally, we provide a protocol for determining a suitable pressure region for applying the Brunauer-Emmett-Teller analysis to nitrogen isotherms, so as to estimate surface area of MOFs with good accuracy. PMID:25225784

Lutetium-177 DOTATATE Production with an Automated Radiopharmaceutical Synthesis System.

PubMed

Aslani, Alireza; Snowdon, Graeme M; Bailey, Dale L; Schembri, Geoffrey P; Bailey, Elizabeth A; Pavlakis, Nick; Roach, Paul J

2015-01-01

Peptide Receptor Radionuclide Therapy (PRRT) with yttrium-90 ((90)Y) and lutetium-177 ((177)Lu)-labelled SST analogues are now therapy option for patients who have failed to respond to conventional medical therapy. In-house production with automated PRRT synthesis systems have clear advantages over manual methods resulting in increasing use in hospital-based radiopharmacies. We report on our one year experience with an automated radiopharmaceutical synthesis system. All syntheses were carried out using the Eckert & Ziegler Eurotope's Modular-Lab Pharm Tracer® automated synthesis system. All materials and methods used were followed as instructed by the manufacturer of the system (Eckert & Ziegler Eurotope, Berlin, Germany). Sterile, GMP-certified, no-carrier added (NCA) (177)Lu was used with GMP-certified peptide. An audit trail was also produced and saved by the system. The quality of the final product was assessed after each synthesis by ITLC-SG and HPLC methods. A total of 17 [(177)Lu]-DOTATATE syntheses were performed between August 2013 and December 2014. The amount of radioactive [(177)Lu]-DOTATATE produced by each synthesis varied between 10-40 GBq and was dependant on the number of patients being treated on a given day. Thirteen individuals received a total of 37 individual treatment administrations in this period. There were no issues and failures with the system or the synthesis cassettes. The average radiochemical purity as determined by ITLC was above 99% (99.8 ± 0.05%) and the average radiochemical purity as determined by HPLC technique was above 97% (97.3 ± 1.5%) for this period. The automated synthesis of [(177)Lu]-DOTATATE using Eckert & Ziegler Eurotope's Modular-Lab Pharm Tracer® system is a robust, convenient and high yield approach to the radiolabelling of DOTATATE peptide benefiting from the use of NCA (177)Lu and almost negligible radiation exposure of the operators.

Synthesis of high-quality libraries of long (150mer) oligonucleotides by a novel depurination controlled process

PubMed Central

LeProust, Emily M.; Peck, Bill J.; Spirin, Konstantin; McCuen, Heather Brummel; Moore, Bridget; Namsaraev, Eugeni; Caruthers, Marvin H.

2010-01-01

We have achieved the ability to synthesize thousands of unique, long oligonucleotides (150mers) in fmol amounts using parallel synthesis of DNA on microarrays. The sequence accuracy of the oligonucleotides in such large-scale syntheses has been limited by the yields and side reactions of the DNA synthesis process used. While there has been significant demand for libraries of long oligos (150mer and more), the yields in conventional DNA synthesis and the associated side reactions have previously limited the availability of oligonucleotide pools to lengths <100 nt. Using novel array based depurination assays, we show that the depurination side reaction is the limiting factor for the synthesis of libraries of long oligonucleotides on Agilent Technologies’ SurePrint® DNA microarray platform. We also demonstrate how depurination can be controlled and reduced by a novel detritylation process to enable the synthesis of high quality, long (150mer) oligonucleotide libraries and we report the characterization of synthesis efficiency for such libraries. Oligonucleotide libraries prepared with this method have changed the economics and availability of several existing applications (e.g. targeted resequencing, preparation of shRNA libraries, site-directed mutagenesis), and have the potential to enable even more novel applications (e.g. high-complexity synthetic biology). PMID:20308161

III-V nanowire synthesis by use of electrodeposited gold particles.

PubMed

Jafari Jam, Reza; Heurlin, Magnus; Jain, Vishal; Kvennefors, Anders; Graczyk, Mariusz; Maximov, Ivan; Borgström, Magnus T; Pettersson, Håkan; Samuelson, Lars

2015-01-14

Semiconductor nanowires are great candidates for building novel electronic devices. Considering the cost of fabricating such devices, substrate reuse and gold consumption are the main concerns. Here we report on implementation of high throughput gold electrodeposition for selective deposition of metal seed particles in arrays defined by lithography for nanowire synthesis. By use of this method, a reduction in gold consumption by a factor of at least 300 was achieved, as compared to conventional thermal evaporation for the same pattern. Because this method also facilitates substrate reuse, a significantly reduced cost of the final device is expected. We investigate the morphology, crystallography, and optical properties of InP and GaAs nanowires grown from electrodeposited gold seed particles and compare them with the properties of nanowires grown from seed particles defined by thermal evaporation of gold. We find that nanowire synthesis, as well as the material properties of the grown nanowires are comparable and quite independent of the gold deposition technique. On the basis of these results, electrodeposition is proposed as a key technology for large-scale fabrication of nanowire-based devices.

Nanophase materials assembled from clusters

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

Siegel, R.W.

1992-02-01

The preparation of metal and ceramic atom clusters by means of the gas-condensation method, followed by their in situ collection and consolidation under high-vacuum conditions, has recently led to the synthesis of a new class of ultrafine-grained materials. These nanophase materials, with typical average grain sizes of 5 to 50 nm and, hence, a large fraction of their atoms in interfaces, exhibit properties that are often considerably improved relative to those of conventional materials. Furthermore, their synthesis and processing characteristics should enable the design of new materials with unique properties. Some examples are ductile ceramics that can be formed andmore » sintered to full density at low temperatures without the need for binding or sintering aids, and metals with dramatically increased strength. The synthesis of these materials is briefly described along with what is presently known of their structure and properties. Their future impact on materials science and technology is also considered.« less

Advances in nanosized zeolites

NASA Astrophysics Data System (ADS)

Mintova, Svetlana; Gilson, Jean-Pierre; Valtchev, Valentin

2013-07-01

This review highlights recent developments in the synthesis of nanosized zeolites. The strategies available for their preparation (organic-template assisted, organic-template free, and alternative procedures) are discussed. Major breakthroughs achieved by the so-called zeolite crystal engineering and encompass items such as mastering and using the physicochemical properties of the precursor synthesis gel/suspension, optimizing the use of silicon and aluminium precursor sources, the rational use of organic templates and structure-directing inorganic cations, and careful adjustment of synthesis conditions (temperature, pressure, time, heating processes from conventional to microwave and sonication) are addressed. An on-going broad and deep fundamental understanding of the crystallization process, explaining the influence of all variables of this complex set of reactions, underpins an even more rational design of nanosized zeolites with exceptional properties. Finally, the advantages and limitations of these methods are addressed with particular attention to their industrial prospects and utilization in existing and advanced applications.

Self-organized synthesis of silver dendritic nanostructures via an electroless metal deposition method

NASA Astrophysics Data System (ADS)

Qiu, T.; Wu, X. L.; Mei, Y. F.; Chu, P. K.; Siu, G. G.

2005-09-01

Unique silver dendritic nanostructures, with stems, branches, and leaves, were synthesized with self-organization via a simple electroless metal deposition method in a conventional autoclave containing aqueous HF and AgNO3 solution. Their growth mechanisms are discussed in detail on the basis of a self-assembled localized microscopic electrochemical cell model. A process of diffusion-limited aggregation is suggested for the formation of the silver dendritic nanostructures. This nanostructured material is of great potential to be building blocks for assembling mini-functional devices of the next generation.

Synthesis and characterization of pyrite (FeS{sub 2}) using microwave irradiation

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

Kim, Eun Jung, E-mail: ekim229@uwo.ca; Batchelor, Bill

2009-07-01

A procedure using microwave irradiation was studied to develop a fast and reliable method for synthesizing pyrite. Pyrite was successfully synthesized within a few minutes via reaction of ferric iron and hydrogen sulfide under the influence of irradiation by a conventional microwave oven. The SEM-EDX study revealed that the nucleation and growth of pyrite occurred on the surface of elemental sulfur, where polysulfides are available. Compared to conventional heating, using microwave energy results in rapid (<1 min) formation of smaller particulates of pyrite. Higher levels of microwave power can form pyrite even faster, but faster reaction can lead to themore » formation of pyrite with defects.« less

The synthesis of cadmium sulfide nanoplatelets using a novel continuous flow sonochemical reactor

DOE PAGES

Palanisamy, Barath; Paul, Brian; Chang, Chih -hung

2015-01-21

A continuous flow sonochemical reactor was developed capable of producing metastable cadmium sulfide (CdS) nanoplatelets with thicknesses at or below 10 nm. The continuous flow sonochemical reactor included the passive in-line micromixing of reagents prior to sonochemical reaction. Synthesis results were compared with those from reactors involving batch conventional heating and batch ultrasound-induced heating. The continuous sonochemical synthesis was found to result in high aspect ratio hexagonal platelets of CdS possessing cubic crystal structures with thicknesses well below 10 nm. The unique shape and crystal structure of the nanoplatelets are suggestive of high localized temperatures within the sonochemical process. Asmore » a result, the particle size uniformity and product throughput are much higher for the continuous sonochemical process in comparison to the batch sonochemical process and conventional synthesis processes.« less

Nanoporous films: From conventional to the conformal

DOE PAGES

Allendorf, Mark D.; Stavila, Vitalie

2015-12-14

Here, thin and continuous films of porous metal-organic frameworks can now be conformally deposited on various substrates using a vapor-phase synthesis approach that departs from conventional solution-based routes.

On-chip synthesis of fine-tuned bone-seeking hybrid nanoparticles.

PubMed

Hasani-Sadrabadi, Mohammad Mahdi; Dashtimoghadam, Erfan; Bahlakeh, Ghasem; Majedi, Fatemeh S; Keshvari, Hamid; Van Dersarl, Jules J; Bertsch, Arnaud; Panahifar, Arash; Renaud, Philippe; Tayebi, Lobat; Mahmoudi, Morteza; Jacob, Karl I

2015-01-01

Here we report a one-step approach for reproducible synthesis of finely tuned targeting multifunctional hybrid nanoparticles (HNPs). A microfluidic-assisted method was employed for controlled nanoprecipitation of bisphosphonate-conjugated poly(D,L-lactide-co-glycolide) chains, while coencapsulating superparamagnetic iron oxide nanoparticles and the anticancer drug Paclitaxel. Smaller and more compact HNPs with narrower size distribution and higher drug loading were obtained at microfluidic rapid mixing regimen compared with the conventional bulk method. The HNPs were shown to have a strong affinity for hydroxyapatite, as demonstrated in vitro bone-binding assay, which was further supported by molecular dynamics simulation results. In vivo proof of concept study verified the prolonged circulation of targeted microfluidic HNPs. Biodistribution as well as noninvasive bioimaging experiments showed high tumor localization and suppression of targeted HNPs to the bone metastatic tumor. The hybrid bone-targeting nanoparticles with adjustable characteristics can be considered as promising nanoplatforms for various theragnostic applications.

Transformation of metal-organic frameworks for molecular sieving membranes

PubMed Central

Li, Wanbin; Zhang, Yufan; Zhang, Congyang; Meng, Qin; Xu, Zehai; Su, Pengcheng; Li, Qingbiao; Shen, Chong; Fan, Zheng; Qin, Lei; Zhang, Guoliang

2016-01-01

The development of simple, versatile strategies for the synthesis of metal-organic framework (MOF)-derived membranes are of increasing scientific interest, but challenges exist in understanding suitable fabrication mechanisms. Here we report a route for the complete transformation of a series of MOF membranes and particles, based on multivalent cation substitution. Through our approach, the effective pore size can be reduced through the immobilization of metal salt residues in the cavities, and appropriate MOF crystal facets can be exposed, to achieve competitive molecular sieving capabilities. The method can also be used more generally for the synthesis of a variety of MOF membranes and particles. Importantly, we design and synthesize promising MOF membranes candidates that are hard to achieve through conventional methods. For example, our CuBTC/MIL-100 membrane exhibits 89, 171, 241 and 336 times higher H2 permeance than that of CO2, O2, N2 and CH4, respectively. PMID:27090597

Design synthesis and optimization of joined-wing transports

NASA Technical Reports Server (NTRS)

Gallman, John W.; Smith, Stephen C.; Kroo, Ilan M.

1990-01-01

A computer program for aircraft synthesis using a numerical optimizer was developed to study the application of the joined-wing configuration to transport aircraft. The structural design algorithm included the effects of secondary bending moments to investigate the possibility of tail buckling and to design joined wings resistant to buckling. The structural weight computed using this method was combined with a statistically-based method to obtain realistic estimates of total lifting surface weight and aircraft empty weight. A variety of 'optimum' joined-wing and conventional aircraft designs were compared on the basis of direct operating cost, gross weight, and cruise drag. The most promising joined-wing designs were found to have a joint location at about 70 percent of the wing semispan. The optimum joined-wing transport is shown to save 1.7 percent in direct operating cost and 11 percent in drag for a 2000 nautical mile transport mission.

A liquid metal reaction environment for the room-temperature synthesis of atomically thin metal oxides

NASA Astrophysics Data System (ADS)

Zavabeti, Ali; Ou, Jian Zhen; Carey, Benjamin J.; Syed, Nitu; Orrell-Trigg, Rebecca; Mayes, Edwin L. H.; Xu, Chenglong; Kavehei, Omid; O'Mullane, Anthony P.; Kaner, Richard B.; Kalantar-zadeh, Kourosh; Daeneke, Torben

2017-10-01

Two-dimensional (2D) oxides have a wide variety of applications in electronics and other technologies. However, many oxides are not easy to synthesize as 2D materials through conventional methods. We used nontoxic eutectic gallium-based alloys as a reaction solvent and co-alloyed desired metals into the melt. On the basis of thermodynamic considerations, we predicted the composition of the self-limiting interfacial oxide. We isolated the surface oxide as a 2D layer, either on substrates or in suspension. This enabled us to produce extremely thin subnanometer layers of HfO2, Al2O3, and Gd2O3. The liquid metal-based reaction route can be used to create 2D materials that were previously inaccessible with preexisting methods. The work introduces room-temperature liquid metals as a reaction environment for the synthesis of oxide nanomaterials with low dimensionality.

Nano-formulations of drugs: Recent developments, impact and challenges.

PubMed

Jeevanandam, Jaison; Chan, Yen San; Danquah, Michael K

2016-01-01

Nano-formulations of medicinal drugs have attracted the interest of many researchers for drug delivery applications. These nano-formulations enhance the properties of conventional drugs and are specific to the targeted delivery site. Dendrimers, polymeric nanoparticles, liposomes, nano-emulsions and micelles are some of the nano-formulations that are gaining prominence in pharmaceutical industry for enhanced drug formulation. Wide varieties of synthesis methods are available for the preparation of nano-formulations to deliver drugs in biological system. The choice of synthesis methods depend on the size and shape of particulate formulation, biochemical properties of drug, and the targeted site. This article discusses recent developments in nano-formulation and the progressive impact on pharmaceutical research and industries. Additionally, process challenges relating to consistent generation of nano-formulations for drug delivery are discussed. Copyright © 2016 Elsevier B.V. and Société Française de Biochimie et Biologie Moléculaire (SFBBM). All rights reserved.

Benzene construction via organocatalytic formal [3+3] cycloaddition reaction.

PubMed

Zhu, Tingshun; Zheng, Pengcheng; Mou, Chengli; Yang, Song; Song, Bao-An; Chi, Yonggui Robin

2014-09-25

The benzene unit, in its substituted forms, is a most common scaffold in natural products, bioactive molecules and polymer materials. Nearly 80% of the 200 best selling small molecule drugs contain at least one benzene moiety. Not surprisingly, the synthesis of substituted benzenes receives constant attentions. At present, the dominant methods use pre-existing benzene framework to install substituents by using conventional functional group manipulations or transition metal-catalyzed carbon-hydrogen bond activations. These otherwise impressive approaches require multiple synthetic steps and are ineffective from both economic and environmental perspectives. Here we report an efficient method for the synthesis of substituted benzene molecules. Instead of relying on pre-existing aromatic rings, here we construct the benzene core through a carbene-catalyzed formal [3+3] reaction. Given the simplicity and high efficiency, we expect this strategy to be of wide use especially for large scale preparation of biomedicals and functional materials.

Modelling and Simulation on Multibody Dynamics for Vehicular Cold Launch Systems Based on Subsystem Synthesis Method

NASA Astrophysics Data System (ADS)

Panyun, YAN; Guozhu, LIANG; Yongzhi, LU; Zhihui, QI; Xingdou, GAO

2017-12-01

The fast simulation of the vehicular cold launch system (VCLS) in the launch process is an essential requirement for practical engineering applications. In particular, a general and fast simulation model of the VCLS will help the designer to obtain the optimum scheme in the initial design phase. For these purposes, a system-level fast simulation model was established for the VCLS based on the subsystem synthesis method. Moreover, a comparison of the load of a seven-axis VCLS on the rigid ground through both theoretical calculations and experiments was carried out. It was found that the error of the load of the rear left outrigger is less than 7.1%, and the error of the total load of all the outriggers is less than 2.8%. Moreover, time taken for completion of the simulation model is only 9.5 min, which is 5% of the time taken by conventional algorithms.

Hydrogen generation from water/methanol under visible light using aerogel prepared strontium titanate (SrTiO3) nanomaterials doped with ruthenium and rhodium metals

NASA Astrophysics Data System (ADS)

Kuo, Yenting; Klabunde, Kenneth J.

2012-07-01

Nanostructured strontium titanate visible-light-driven photocatalysts containing rhodium and ruthenium were synthesized by a modified aerogel synthesis using ruthenium chloride and rhodium nitrate as dopant precursors, and titanium isopropoxide and strontium metal as the metal sources. The well-defined crystalline SrTiO3 structure was confirmed by means of x-ray diffraction. After calcination at 500 °C, diffuse reflectance spectroscopy shows an increase in light absorption at 370 nm due to the presence of Rh3 + ; however an increase of the calcination temperature to 600 °C led to a decrease in intensity, probably due to a loss of surface area. An increase in the rhodium doping level also led to an increase in absorption at 370 nm however, the higher amounts of dopant lowered the photocatalytic activity. The modified aerogel synthesis allows greatly enhanced H2 production performance from an aqueous methanol solution under visible light irradiation compared with lower surface area conventional materials. We believe that this enhanced activity is due to the higher surface areas while high quality nanocrystalline materials are still obtained. Furthermore, the surface properties of these nanocrystalline aerogel materials are different, as exhibited by the higher activities in alkaline solutions, while conventional materials (obtained via high temperature solid-state synthesis methods) only exhibit reasonable hydrogen production in acidic solutions. Moreover, an aerogel synthesis approach gives the possibility of thin-film formation and ease of incorporation into practical solar devices.

Precursor-Based Synthesis of Porous Colloidal Particles towards Highly Efficient Catalysts.

PubMed

Zheng, Yun; Geng, Hongbo; Zhang, Yufei; Chen, Libao; Li, Cheng Chao

2018-04-02

In recent years, porous colloidal particles have found promising applications in catalytic fields, such as photocatalysis, electrocatalysis, industrial and automotive byproducts removal, as well as biomass upgrading. These applications are critical for alleviating the energy crisis and environmental pollution. Porous colloidal particles have remarkable specific areas and abundant reactive sites, which can significantly improve the mass/charge transport and reaction rate in catalysis. Precursor-based synthesis is among the most facile and widely-adopted methods to achieve monodisperse and homogeneous porous colloidal particles. In the current review, we briefly introduce the general catalytic applications of porous colloidal particles. The conventional precursor-based methods are reviewed to design state-of-the-art porous colloidal particles as highly efficient catalysts. The recent development of porous colloidal particles derived from metal-organic frameworks (MOFs), glycerates, carbonate precursors, and ion exchange methods are reviewed. In the end, the current concerns and future development of porous colloidal particles are outlined. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Environmentally friendly ultrosound synthesis and antibacterial activity of cellulose/Ag/AgCl hybrids.

PubMed

Dong, Yan-Yan; Deng, Fu; Zhao, Jin-Jin; He, Jing; Ma, Ming-Guo; Xu, Feng; Sun, Run-Cang

2014-01-01

This study aims to investigate the fabrication and property of cellulose/Ag/AgCl hybrids. In this article, preparation of cellulose/Ag/AgCl hybrids was reported using the cellulose solution, AgNO₃, AlCl₃·6H₂O with ultrasound agitation method. The cellulose solution was synthesized by the dissolution of the microcrystalline cellulose in NaOH/urea aqueous solution. Influences of the experimental parameters of ultrasound treatment time and ultrasonic intermittent on the hybrids were investigated. The phase, microstructure, thermal stability, and morphology of the hybrids were characterized by X-ray powder diffraction (XRD), Fourier transform infrared (FTIR) spectrometry, thermogravimetric analysis (TGA), differential thermal analysis (DTA), and scanning electron microscopy (SEM). Results showed the successful synthesis of cellulose/Ag/AgCl hybrids with good thermal stability. Moreover, the hybrids displayed desirable antimicrobial activities. Compared with other conventional methods, the rapid, green, and environmentally friendly ultrasound agitation method opens a new window to the high value-added applications of biomass. Copyright © 2013 Elsevier Ltd. All rights reserved.

Hydrography synthesis using LANDSAT remote sensing and the SCS models

NASA Technical Reports Server (NTRS)

Ragan, R. M.; Jackson, T. J.

1976-01-01

The land cover requirements of the Soil Conservation Service (SCS) Model used for hydrograph synthesis in urban areas were modified to be LANDSAT compatible. The Curve Numbers obtained with these alternate land cover categories compare well with those obtained in published example problems using the conventional categories. Emergency spillway hydrographs and synthetic flood frequency flows computed for a 21.1 sq. mi. test area showed excellent agreement between the conventional aerial photo-based and the Landsat-based SCS approaches.

Efficiency, error and yield in light-directed maskless synthesis of DNA microarrays

PubMed Central

2011-01-01

Background Light-directed in situ synthesis of DNA microarrays using computer-controlled projection from a digital micromirror device--maskless array synthesis (MAS)--has proved to be successful at both commercial and laboratory scales. The chemical synthetic cycle in MAS is quite similar to that of conventional solid-phase synthesis of oligonucleotides, but the complexity of microarrays and unique synthesis kinetics on the glass substrate require a careful tuning of parameters and unique modifications to the synthesis cycle to obtain optimal deprotection and phosphoramidite coupling. In addition, unintended deprotection due to scattering and diffraction introduce insertion errors that contribute significantly to the overall error rate. Results Stepwise phosphoramidite coupling yields have been greatly improved and are now comparable to those obtained in solid phase synthesis of oligonucleotides. Extended chemical exposure in the synthesis of complex, long oligonucleotide arrays result in lower--but still high--final average yields which approach 99%. The new synthesis chemistry includes elimination of the standard oxidation until the final step, and improved coupling and light deprotection. Coupling Insertions due to stray light are the limiting factor in sequence quality for oligonucleotide synthesis for gene assembly. Diffraction and local flare are by far the largest contributors to loss of optical contrast. Conclusions Maskless array synthesis is an efficient and versatile method for synthesizing high density arrays of long oligonucleotides for hybridization- and other molecular binding-based experiments. For applications requiring high sequence purity, such as gene assembly, diffraction and flare remain significant obstacles, but can be significantly reduced with straightforward experimental strategies. PMID:22152062

The challenges and opportunities for integration of solar syngas production with liquid fuel synthesis

NASA Astrophysics Data System (ADS)

Hinkley, James T.; McNaughton, Robbie K.; Pye, John; Saw, Woei; Stechel, Ellen B.

2016-05-01

Reforming of methane is practiced on a vast scale globally for the production of syngas as a precursor for the production of many commodities, including hydrogen, ammonia and synthetic liquid fuels. Solar reforming can reduce the greenhouse gas intensity of syngas production by up to about 40% by using solar thermal energy to provide the endothermic heat of reaction, traditionally supplied by combustion of some of the feed. This has the potential to enable the production of solar derived synthetic fuels as drop in replacements for conventional fuels with significantly lower CO2 intensity than conventional gas to liquids (GTL) processes. However, the intermittent nature of the solar resource - both diurnal and seasonal - poses significant challenges for such a concept, which relies on synthesis processes that typically run continuously on very stable feed compositions. We find that the integration of solar syngas production to a GTL process is a non-trivial exercise, with the ability to turn down the capacity of the GTL synthesis section, and indeed to suspend operations for short periods without significant detriment to product quality or process operability, likely to be a key driver for the commercial implementation of solar liquid fuels. Projected costs for liquid fuel synthesis suggest that solar reforming and small scale gas to liquid synthesis can potentially compete with conventional oil derived transport fuels in the short to medium term.

A distributed finite-element modeling and control approach for large flexible structures

NASA Technical Reports Server (NTRS)

Young, K. D.

1989-01-01

An unconventional framework is described for the design of decentralized controllers for large flexible structures. In contrast to conventional control system design practice which begins with a model of the open loop plant, the controlled plant is assembled from controlled components in which the modeling phase and the control design phase are integrated at the component level. The developed framework is called controlled component synthesis (CCS) to reflect that it is motivated by the well developed Component Mode Synthesis (CMS) methods which were demonstrated to be effective for solving large complex structural analysis problems for almost three decades. The design philosophy behind CCS is also closely related to that of the subsystem decomposition approach in decentralized control.

Nanostructured materials: A novel approach to enhanced performance. Final report

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

Korth, G.E.; Froes, F.H.; Suryanarayana, C.

Nanostuctured materials are an emerging class of materials that can exhibit physical and mechanical characteristics often exceeding those exhibited by conventional course grained materials. A number of different techniques can be employed to produce these materials. In this program, the synthesis methods were (a) mechanical alloying , (b) physical vapor deposition, and (c) plasma processing. The physical vapor deposition and plasma processing were discontinued after initial testing with subsequent efforts focused on mechanical alloying. The major emphasis of the program was on the synthesis, consolidation, and characterization of nanostructured Al-Fe, Ti-Al, Ti-Al-Nb, and Fe-Al by alloying intermetallics with a viewmore » to increase their ductilities. The major findings of this project are reported.« less

A novel liquid template corrosion approach for layered silica with various morphologies and different nanolayer thicknesses

NASA Astrophysics Data System (ADS)

Yang, Wanliang; Li, Baoshan

2014-01-01

A novel liquid template corrosion (LTC) method has been developed for the synthesis of layered silica materials with a variety of morphologies, including hollow nanospheres, trilobite-like nanoparticles, spherical particles and a film resembling the van Gogh painting `Starry Night'. Lamellar micelles and microemulsion droplets are first formed in an oil-water (O/W) mixture of ethyl acetate (EA), cetyltrimethylammonium bromide (CTAB) and water. After adding aqueous ammonia the EA becomes hydrolyzed, which results in corrosion of microemulsion droplets. These droplets subsequently act as templates for the synthesis of silica formed by hydrolysis of tetraethyl orthosilicate. The morphological evolution of silica can be tuned by varying the concentration of aqueous ammonia which controls the degree of corrosion of the microemulsion droplet templates. A possible mechanism is proposed to explain why the LTC approach affords layered silica nanostructured materials with various morphologies and nanolayer thickness (2.6-4.5 nm), rather than the usual ordered mesostructures formed in the absence of EA. Our method provides a simple way to fabricate a variety of building blocks for assembling nanomaterials with novel structures and functionality, which are not available using conventional template methods.A novel liquid template corrosion (LTC) method has been developed for the synthesis of layered silica materials with a variety of morphologies, including hollow nanospheres, trilobite-like nanoparticles, spherical particles and a film resembling the van Gogh painting `Starry Night'. Lamellar micelles and microemulsion droplets are first formed in an oil-water (O/W) mixture of ethyl acetate (EA), cetyltrimethylammonium bromide (CTAB) and water. After adding aqueous ammonia the EA becomes hydrolyzed, which results in corrosion of microemulsion droplets. These droplets subsequently act as templates for the synthesis of silica formed by hydrolysis of tetraethyl orthosilicate. The morphological evolution of silica can be tuned by varying the concentration of aqueous ammonia which controls the degree of corrosion of the microemulsion droplet templates. A possible mechanism is proposed to explain why the LTC approach affords layered silica nanostructured materials with various morphologies and nanolayer thickness (2.6-4.5 nm), rather than the usual ordered mesostructures formed in the absence of EA. Our method provides a simple way to fabricate a variety of building blocks for assembling nanomaterials with novel structures and functionality, which are not available using conventional template methods. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr04733d

Synthesis of PZT powder by conventional method at various conditions

NASA Astrophysics Data System (ADS)

Necira, Z.; Boutarfaia, A.; Abba, M.; Abdessalem, N.

2012-06-01

In this work, the formation of Pb(Zr1-xTix)O3 solid solutions with composition near the morphotropic phase boundary (MPB) using the conventional ceramic method have been studied by changing the thermal conditions such as temperature ramp rate and isothermal times during the calcination treatment performed between 700 and 900 °C. The perovskite phase formation and morphology of undoped Pb(Zr0.52Ti0.48)O3 (abbreviated PZT) and doped new material Pb0.98Gd0.02[(Zr0.52Ti0.48)0.98 (Mg1/3Nb2/3)0.01 (Ni1/3Sb2/3)0.01]O3 (abbreviated PZT-PGMNNS) specimens have been examined by powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier Transform Infrared (FTIR) while the thermal evolution of the initial precursor was followed by TG-DTA. So the results of these studies have been discussed.

A novel approach for in vitro meat production.

PubMed

Pandurangan, Muthuraman; Kim, Doo Hwan

2015-07-01

The present review describes the possibility of in vitro meat production with the help of advanced co-culturing methods. In vitro meat production method could be a possible alternative for the conventional meat production. Originally, the research on in vitro meat production was initiated by the National Aeronautics and Space Administration (NASA) for space voyages. The required key qualities for accepting in vitro meat for consumption would be good efficiency ratio, increased protein synthesis rate in skeletal muscles, and mimicking the conventional meat qualities. In vitro culturing of meat is possible with the use of skeletal muscle tissue engineering, stem cell, cell co-culture, and tissue culture methods. Co-culture of myoblast and fibroblast is believed as one of the major techniques for in vitro meat production. In our lab, we have co-cultured myoblast and fibroblast. We believe that a billion pounds of in vitro meat could be produced from one animal for consumption. However, we require a great deal of research on in vitro meat production.

"Glitch Logic" and Applications to Computing and Information Security

NASA Technical Reports Server (NTRS)

Stoica, Adrian; Katkoori, Srinivas

2009-01-01

This paper introduces a new method of information processing in digital systems, and discusses its potential benefits to computing and information security. The new method exploits glitches caused by delays in logic circuits for carrying and processing information. Glitch processing is hidden to conventional logic analyses and undetectable by traditional reverse engineering techniques. It enables the creation of new logic design methods that allow for an additional controllable "glitch logic" processing layer embedded into a conventional synchronous digital circuits as a hidden/covert information flow channel. The combination of synchronous logic with specific glitch logic design acting as an additional computing channel reduces the number of equivalent logic designs resulting from synthesis, thus implicitly reducing the possibility of modification and/or tampering with the design. The hidden information channel produced by the glitch logic can be used: 1) for covert computing/communication, 2) to prevent reverse engineering, tampering, and alteration of design, and 3) to act as a channel for information infiltration/exfiltration and propagation of viruses/spyware/Trojan horses.

Synthesis of Graphite Oxide with Different Surface Oxygen Contents Assisted Microwave Radiation

PubMed Central

Ibarra-Hernández, Adriana

2018-01-01

Graphite oxide is synthesized via oxidation reaction using oxidant compounds that have lattice defects by the incorporation of unlike functional groups. Herein, we report the synthesis of the graphite oxide with diverse surface oxygen content through three (B, C, D) different modified versions of the Hummers method assisted microwave radiation compared with the conventional graphite oxide sample obtained by Hummers method (A). These methods allow not only the production of graphite oxide but also reduced graphene oxide, without undergoing chemical, thermal, or mechanical reduction steps. The values obtained of C/O ratio were ~2, 3.4, and ~8.5 for methodologies C, B, and D, respectively, indicating the presence of graphite oxide and reduced graphene oxide, according to X-ray photoelectron spectroscopy. Raman spectroscopy of method D shows the fewest structural defects compared to the other methodologies. The results obtained suggest that the permanganate ion produces reducing species during graphite oxidation. The generation of these species is attributed to a reversible reaction between the permanganate ion with π electrons, ions, and radicals produced after treatment with microwave radiation. PMID:29438280

Synthesis and structural properties of (Y, Sr)(Ti, Fe, Nb)O3-δ perovskite nanoparticles fabricated by modified polymer precursor method

NASA Astrophysics Data System (ADS)

Miruszewski, T.; Gdaniec, P.; Karczewski, J.; Bochentyn, B.; Szaniawska, K.; Kupracz, P.; Prześniak-Welenc, M.; Kusz, B.

2016-09-01

The yttrium, iron and niobium doped-SrTiO3 powders have been successfully fabricated by a modified low-temperature synthesis method from a polymer complex. The usage of strontium hydroxide precursor instead of conventional strontium nitrate or strontium carbonate provides to the possibility of significant decrease of annealing temperature. It allows to prepare a material with sphere-shape grains of nanometric size (15-70 nm). The results of thermal analysis indicate that the crystallization of precursor takes place at different stages. The product after heat treatment at 600 °C for 3 h in air was also characterized by X-Ray diffraction method (XRD) and Fourier transform - infrared spectroscopy (FT-IR). After the crystallization and the impurity removal process, a single-phase material was obtained in case of all analyzed samples. The morphology of obtained nano-powders was also studied by a scanning electron microscopy (SEM). It can be concluded, that this method allows obtaining a perovskite phase of a metal doped SrTiO3 with nanometric particles.

[Experimental research on the effect of nanophase ceramics on osteoblasts functions].

PubMed

Wen, Bo; Chen, Zhiqing; Jiang, Yinshan; Yang, Zhengwen; Xu, Yongzhong

2005-06-01

In order to study the cytocompatibility of nanophase hydroxyapatite ceramic in vitro, we prepared hydroxyapatite by use of the wet chemistry techniques. The grain size of hydroxyapatite of interest to the present study was determined by scanning electron microscopy and atomic force microscopy with image analysis software. Primary culture of osteoblast from rat calvaria was established. Protein content, synthesis of alkaline phosphatase and deposition of calcium-containing mineral by osteoblasts cultured on nanophase hydroxyapatite ceramics and on conventional hydroxyapatite ceramics for 7, 14, 21 and 28 days were examined. The results showed that the average surface grain size of the nanophase and that of the conventional HA compact formulations was 55 (nanophase) and 780 (conventional) nm, respectively. More importantly, compared to the synthesis of alkaline phosphatase and deposition of calcium-containing mineral by osteoblasts cultured on nanophase was significantly greater than that on conventional ceramics after 21 and 28 days. The cytocompatibility was significantly greater on nanophase HA than on conventional formulations of the same ceramic.

Electrically Controllable Microparticle Synthesis and Digital Microfluidic Manipulation by Electric-Field-Induced Droplet Dispensing into Immiscible Fluids

PubMed Central

Um, Taewoong; Hong, Jiwoo; Im, Do Jin; Lee, Sang Joon; Kang, In Seok

2016-01-01

The dispensing of tiny droplets is a basic and crucial process in a myriad of applications, such as DNA/protein microarray, cell cultures, chemical synthesis of microparticles, and digital microfluidics. This work systematically demonstrates droplet dispensing into immiscible fluids through electric charge concentration (ECC) method. It exhibits three main modes (i.e., attaching, uniform, and bursting modes) as a function of flow rates, applied voltages, and gap distances between the nozzle and the oil surface. Through a conventional nozzle with diameter of a few millimeters, charged droplets with volumes ranging from a few μL to a few tens of nL can be uniformly dispensed into the oil chamber without reduction in nozzle size. Based on the features of the proposed method (e.g., formation of droplets with controllable polarity and amount of electric charge in water and oil system), a simple and straightforward method is developed for microparticle synthesis, including preparation of colloidosomes and fabrication of Janus microparticles with anisotropic internal structures. Finally, a combined system consisting of ECC-induced droplet dispensing and electrophoresis of charged droplet (ECD)-driven manipulation systems is constructed. This integrated platform will provide increased utility and flexibility in microfluidic applications because a charged droplet can be delivered toward the intended position by programmable electric control. PMID:27534580

Microfluidic Synthesis and Biological Evaluation of Photothermal Biodegradable Copper Sulfide Nanoparticles.

PubMed

Ortiz de Solorzano, Isabel; Prieto, Martín; Mendoza, Gracia; Alejo, Teresa; Irusta, Silvia; Sebastian, Victor; Arruebo, Manuel

2016-08-24

The continuous synthesis of biodegradable photothermal copper sulfide nanoparticles has been carried out with the aid of a microfluidic platform. A comparative physicochemical characterization of the resulting products from the microreactor and from a conventional batch reactor has been performed. The microreactor is able to operate in a continuous manner and with a 4-fold reduction in the synthesis times compared to that of the conventional batch reactor producing nanoparticles with the same physicochemical requirements. Biodegradation subproducts obtained under simulated physiological conditions have been identified, and a complete cytotoxicological analysis on different cell lines was performed. The photothermal effect of those nanomaterials has been demonstrated in vitro as well as their ability to generate reactive oxygen species.

Plasma methods of obtainment of multifunctional composite materials, dispersion-hardened by nanoparticles

NASA Astrophysics Data System (ADS)

Sizonenko, O. N.; Grigoryev, E. G.; Zaichenko, A. D.; Pristash, N. S.; Torpakov, A. S.; Lipyan, Ye V.; Tregub, V. A.; Zholnin, A. G.; Yudin, A. V.; Kovalenko, A. A.

2016-04-01

The new approach in developed plasma methods consists in that dispersionhardening additives (TiC, TiB2 in particular) are not mechanically added to powder mixture as additional component, as in conventional methods, but are instead synthesized during high voltage electric discharges (HVED) in disperse system “hydrocarbon liquid - powder” preservation of ultrafine structure is ensured due to use of spark plasma sintering (SPS) as a consolidation method. HVED in disperse system “hydrocarbon liquid - powder” due to impact of plasma discharge channel, electromagnetic fields, shock waves mechanical impact, hydro flows and volume microcavitation leads to synthesis of nanocarbon, metal powders dispersion and synthesis of micro- (from 10-6 to 10-7 m) and nanosized (from 10-7 to 10-9 m) composite powders of hardening phases. SPS is the passage of pulsed current (superposition of direct and alternating current) through powder with the simultaneous mechanical compressing. The formation of plasma is initiated in gaseous phase that fills gaps between particles. SPS allows targeted control of grain growth rate and thus allows obtainment of multifunctional composite materials dispersion hardened by nanoparticles. Processes of HVED synthesis of micro- and nanosized powders of new compositions from elemental metal powders and their mixtures with the subsequent application of high-speed SPS of obtained powders create conditions for increase of strength (by 10 - 20%), hardness and wear-resistance (by 30 - 60%) of obtained materials.

MX Siting Investigation Geotechnical Evaluation Verification Study - Cave Valley, Nevada. Volume I. Synthesis.

DTIC Science & Technology

1981-10-26

areas of non- rippable materials may be encountered throughout the northwestern portion of the valley. Laboratory test results and field observations...non- rippable at shallow depths, thereby classifying them in this instance as areas of rock and/or shallow rock. When this occurs, these areas may...OCCUR- Rock is defined as any earth material which is not rippable RING WITHIN 50 FEET 015m) AND by conventional excavation methods. Where available

Micelle-templated, poly(lactic-co-glycolic acid) nanoparticles for hydrophobic drug delivery

PubMed Central

Nabar, Gauri M; Mahajan, Kalpesh D; Calhoun, Mark A; Duong, Anthony D; Souva, Matthew S; Xu, Jihong; Czeisler, Catherine; Puduvalli, Vinay K; Otero, José Javier; Wyslouzil, Barbara E; Winter, Jessica O

2018-01-01

Purpose Poly(lactic-co-glycolic acid) (PLGA) is widely used for drug delivery because of its biocompatibility, ability to solubilize a wide variety of drugs, and tunable degradation. However, achieving sub-100 nm nanoparticles (NPs), as might be desired for delivery via the enhanced permeability and retention effect, is extremely difficult via typical top-down emulsion approaches. Methods Here, we present a bottom-up synthesis method yielding PLGA/block copolymer hybrids (ie, “PolyDots”), consisting of hydrophobic PLGA chains entrapped within self-assembling poly(styrene-b-ethylene oxide) (PS-b-PEO) micelles. Results PolyDots exhibit average diameters <50 nm and lower polydispersity than conventional PLGA NPs. Drug encapsulation efficiencies of PolyDots match conventional PLGA NPs (ie, ~30%) and are greater than those obtained from PS-b-PEO micelles (ie, ~7%). Increasing the PLGA:PS-b-PEO weight ratio alters the drug release mechanism from chain relaxation to erosion controlled. PolyDots are taken up by model glioma cells via endocytotic mechanisms within 24 hours, providing a potential means for delivery to cytoplasm. PolyDots can be lyophilized with minimal change in morphology and encapsulant functionality, and can be produced at scale using electrospray. Conclusion Encapsulation of PLGA within micelles provides a bottom-up route for the synthesis of sub-100 nm PLGA-based nanocarriers with enhanced stability and drug-loading capacity, and tunable drug release, suitable for potential clinical applications. PMID:29391794

Synthesis and fabrication of porous activated carbon/nano ZnO composite electrode for supercapacitor

NASA Astrophysics Data System (ADS)

P, Shabeeba; Thayyil, Mohammed Shahin; Pillai, M. P.

2017-05-01

Supercapacitors, also called as ultracapacitors, are electrochemical energy-storage devices that exploit the electrostatic interaction between high-surface-area nanoporous electrodes and electrolyte ions that combine properties of conventional batteries and conventional capacitors. A symmetrical ZnO-Activated Carbon (ZAC) electrode supercapacitor have been fabricated in a simple and inexpensive manner. The electrochemical characteristics of fabricated supercapacitor was analyzed using Cyclic Voltammetry (CV), galvanostatic charge discharge technique, and impedance spectroscopy methods. Capacitance of fabricated ZAC electrode were showed capacitance in the range of 60-70 F/g respectively. It has been found that the cells have excellent electro chemical reversibility, capacitive characteristics in electrolyte and stable in cyclings, which is promising for energy storage applications.

Total chemical synthesis of proteins without HPLC purification† †Electronic supplementary information (ESI) available. See DOI: 10.1039/c6sc01883a Click here for additional data file.

PubMed Central

Loibl, S. F.; Harpaz, Z.; Zitterbart, R.

2016-01-01

The total chemical synthesis of proteins is a tedious and time-consuming endeavour. The typical steps involve solid phase synthesis of peptide thioesters and cysteinyl peptides, native chemical ligation (NCL) in solution, desulfurization or removal of ligation auxiliaries in the case of extended NCL as well as many intermediary and final HPLC purification steps. With an aim to facilitate and improve the throughput of protein synthesis we developed the first method for the rapid chemical total on-resin synthesis of proteins that proceeds without a single HPLC-purification step. The method relies on the combination of three orthogonal protein tags that allow sequential immobilization (via the N-terminal and C-terminal ends), extended native chemical ligation and release reactions. The peptide fragments to be ligated are prepared by conventional solid phase synthesis and used as crude materials in the subsequent steps. An N-terminal His6 unit permits selective immobilization of the full length peptide thioester onto Ni-NTA agarose beads. The C-terminal peptide fragment carries a C-terminal peptide hydrazide and an N-terminal 2-mercapto-2-phenyl-ethyl ligation auxiliary, which serves as a reactivity tag for the full length peptide. As a result, only full length peptides, not truncation products, react in the subsequent on-bead extended NCL. After auxiliary removal the ligation product is liberated into solution upon treatment with mild acid, and is concomitantly captured by an aldehyde-modified resin. This step allows the removal of the most frequently observed by-product in NCL chemistry, i.e. the hydrolysed peptide thioester (which does not contain a C-terminal peptide hydrazide). Finally, the target protein is released with diluted hydrazine or acid. We applied the method in the synthesis of 46 to 126 amino acid long MUC1 proteins comprising 2–6 copies of a 20mer tandem repeat sequence. Only three days were required for the parallel synthesis of 9 MUC1 proteins which were obtained in 8–33% overall yield with 90–98% purity despite the omission of HPLC purification. PMID:28451120

Mechanistic Studies Of Combustion And Structure Formation During Combustion Synthesis Of Advanced Materials: Phase Separation Mechanism For Bio-Alloys

NASA Technical Reports Server (NTRS)

Varma, A.; Lau, C.; Mukasyan, A.

2003-01-01

Among all implant materials, Co-Cr-Mo alloys demonstrate perhaps the most useful balance of resistance to corrosion, fatigue and wear, along with strength and biocompatibility [1]. Currently, these widely used alloys are produced by conventional furnace technology. Owing to high melting points of the main alloy elements (e.g. Tm.p.(Co) 1768 K), high-temperature furnaces and long process times (several hours) are required. Therefore, attempts to develop more efficient and flexible methods for production of such alloys with superior properties are of great interest. The synthesis of materials using combustion phenomena is an advanced approach in powder metallurgy [2]. The process is characterized by unique conditions involving extremely fast heating rates (up to 10(exp 6 K/s), high temperatures (up to 3500 K), and short reaction times (on the order of seconds). As a result, combustion synthesis (CS) offers several attractive advantages over conventional metallurgical processing and alloy development technologies. The foremost is that solely the heat of chemical reaction (instead of an external source) supplies the energy for the synthesis. Also, simple equipment, rather than energy-intensive high-temperature furnaces, is sufficient. This work was devoted to experiments on CS of Co-based alloys by utilizing thermite (metal oxide-reducing metal) reactions, where phase separation subsequently produces materials with tailored compositions and properties. Owing to high reaction exothermicity, the CS process results in a significant increase of temperature (up to 3000 C), which is higher than melting points of all products. Since the products differ in density, phase separation may be a gravitydriven process: the heavy (metallic phase) settles while the light (slag) phase floats. The goal was to determine if buoyancy is indeed the major mechanism that controls phase segregation.

Soft chemical synthesis of silicon nanosheets and their applications

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

Nakano, Hideyuki; Ikuno, Takashi

2016-12-15

Two-dimensional silicon nanomaterials are expected to show different properties from those of bulk silicon materials by virtue of surface functionalization and quantum size effects. Since facile fabrication processes of large area silicon nanosheets (SiNSs) are required for practical applications, a development of soft chemical synthesis route without using conventional vacuum processes is a challenging issue. We have recently succeeded to prepare SiNSs with sub-nanometer thicknesses by exfoliating layered silicon compounds, and they are found to be composed of crystalline single-atom-thick silicon layers. In this review, we present the synthesis and modification methods of SiNSs. These SiNSs have atomically flat andmore » smooth surfaces due to dense coverage of organic moieties, and they are easily self-assembled in a concentrated state to form a regularly stacked structure. We have also characterized the electron transport properties and the electronic structures of SiNSs. Finally, the potential applications of these SiNSs and organic modified SiNSs are also reviewed.« less

Synthesis of photochromic oligophenylenimines: optical and computational studies.

PubMed

Pérez, Armando I Martínez; Alonso, Oscar Coreño; Borbolla, Julián Cruz; Vásquez-Pérez, José M; Alonso, Juan Coreño; Ayala, Karina Alemán; Luna-Bárcenas, Gabriel; Pandiyan, Thangarasu; García, Rosa A Vázquez

2015-03-27

Phenyleneimine oligomers 4,4'-(((1E,1'E)-(((1E,1'E)-(1,4-phenylenebis-(azanylylidene))bis(methanylylidene))bis(2,5-bis(octyloxy)-4,1-phenylene))bis(methanylyl-idene))-bis(azanylylidene))dianiline (OIC1MS) and 7,7'-(((1E,1'E)-(((1E,1'E)-((9H-fluorene-2,7-diyl)bis(azanylylidene))bis(methanylylidene))bis(2,5-bis(octyloxy)-4,1phenylene))bis- (methanylylidene))bis(azanylylidene))bis(9H-fluoren-2-amine) (OIC2MS) were prepared by means of conventional and mechanochemical synthesis and characterized by FT-IR, 1H- and 13C-NMR techniques. The optical properties of the compounds were studied in solution by using UV-visible spectroscopy, and the optical effects were analyzed as a function of solvent. The results show that OIC2MS exhibits interesting photochromic properties. Furthermore, the structural and electronic properties of the compounds were analyzed by TD-DFT. It was found that the mechanosynthesis is an efficient method for the synthesis of both tetraimines.

Synthesis and characterization of TiO₂ and TiO₂/Ag for use in photodegradation of methylviologen, with kinetic study by laser flash photolysis.

PubMed

Ramos, Dayana Doffinger; Bezerra, Paula C S; Quina, Frank H; Dantas, Renato F; Casagrande, Gleison A; Oliveira, Silvio C; Oliveira, Márcio R S; Oliveira, Lincoln C S; Ferreira, Valdir S; Oliveira, Samuel L; Machulek, Amilcar

2015-01-01

This paper reports the synthesis, characterization, and application of TiO2 and TiO2/Ag nanoparticles for use in photocatalysis, employing the herbicide methylviologen (MV) as a substrate for photocatalytic activity testing. At suitable metal to oxide ratios, increases in silver surface coating on TiO2 enhanced the efficiency of heterogeneous photocatalysis by increasing the electron transfer constant. The sol-gel method was used for TiO2 synthesis. P25 TiO2 was the control material. Both oxides were subjected to the same silver incorporation process. The materials were characterized by conventional spectroscopy, SEM micrography, X-ray diffraction, calculation of surface area per mass of catalyst, and thermogravimetry. Also, electron transfers between TiO2 or TiO2/Ag and MV in the absence and presence of sodium formate were investigated using laser flash photolysis. Oxides synthesized with 2.0 % silver exhibited superior photocatalytic activity for MV degradation.

Novel Rubidium Poly-Nitrogen Energetic Materials

NASA Astrophysics Data System (ADS)

Huff, Ashley; Steele, Brad; Oleynik, Ivan

High-nitrogen content compounds are being actively explored with the goal of discovering new high-energy density materials with performance surpassing the conventional energetic materials such as HMX or RDX. Although pure polynitrogen compounds such as cg-N are predicted to deliver 10-fold increase in detonation pressure and detonation velocity of 30 km/s, their synthesis and recovery at ambient conditions is problematic. Doping polynitrogens with other elements is a viable route to promote metastability while reducing synthesis pressure. In this work, rubidium poly-nitrides are being investigated as candidates for high energy density materials. Using first principles evolutionary structure search methods performed at varying stoichiometries and several pressures ranging from 0 to 100 GPa, several new polynitrogen compounds have been discovered. The phase diagrams containing thermodynamically stable and lowest metastable phases are calculated and the dynamical stability of the promising materials is investigated at various pressures. Raman spectra and XRD patterns are also calculated to provide experimentally relevant information useful for identification of these compounds during their synthesis.

Catalytic enantioselective synthesis of atropisomeric biaryls by a cation-directed O-alkylation

NASA Astrophysics Data System (ADS)

Jolliffe, John D.; Armstrong, Roly J.; Smith, Martin D.

2017-06-01

Axially chiral biaryls, as exemplified by 1,1‧-bi-2-naphthol (BINOL), are key components of catalysts, natural products and medicines. These materials are synthesized conventionally in enantioenriched form through metal-mediated cross coupling, de novo construction of an aromatic ring, point-to-axial chirality transfer or an atropselective transformation of an existing biaryl. Here, we report a highly enantioselective organocatalytic method for the synthesis of atropisomeric biaryls by a cation-directed O-alkylation. Treatment of racemic 1-aryl-2-tetralones with a chiral quinidine-derived ammonium salt under basic conditions in the presence of an alkylating agent leads to atropselective O-alkylation with e.r. up to 98:2. Oxidation with DDQ gives access to C2-symmetric and non-symmetric BINOL derivatives without compromising e.r. We propose that the chiral ammonium counterion differentiates between rapidly equilibrating atropisomeric enolates, leading to highly atropselective O-alkylation. This dynamic kinetic resolution process offers a general approach to the synthesis of enantioenriched atropisomeric materials.

Microwave-Assisted Rapid Enzymatic Synthesis of Nucleic Acids.

PubMed

Hari Das, Rakha; Ahirwar, Rajesh; Kumar, Saroj; Nahar, Pradip

2016-07-02

Herein we report microwave-induced enhancement of the reactions catalyzed by Escherichia coli DNA polymerase I and avian myeloblastosis virus-reverse transcriptase. The reactions induced by microwaves result in a highly selective synthesis of nucleic acids in 10-50 seconds. In contrast, same reactions failed to give desired reaction products when carried out in the same time periods, but without microwave irradiation. Each of the reactions was carried out for different duration of microwave exposure time to find the optimum reaction time. The products produced by the respective enzyme upon microwave irradiation of the reaction mixtures were identical to that produced by the conventional procedures. As the microwave-assisted reactions are rapid, microwave could be a useful alternative to the conventional and time consuming procedures of enzymatic synthesis of nucleic acids.

Making MgO/SiO2 Glasses By The Sol-Gel Process

NASA Technical Reports Server (NTRS)

Bansal, Narottam P.

1989-01-01

Silicon dioxide glasses containing 15 mole percent magnesium oxide prepared by sol-gel process. Not made by conventional melting because ingredients immiscible liquids. Synthesis of MgO/SiO2 glass starts with mixing of magnesium nitrate hexahydrate with silicon tetraethoxide, both in alcohol. Water added, and transparent gel forms. Subsequent processing converts gel into glass. Besides producing glasses of new composition at lower processing temperatures, sol-gel method leads to improved homogeneity and higher purity.

An efficient synthesis strategy for metal-organic frameworks: Dry-gel synthesis of MOF-74 framework with high yield and improved performance

DOE PAGES

Das, Atanu Kumar; Vemuri, Rama Sesha; Kutnyakov, Igor; ...

2016-06-16

Here, vapor-assisted dry-gel synthesis of MOF-74 structure, specifically NiMOF-74 from its synthetic precursors, was conducted with high yield and improved performance showing promise for gas (CO 2) and water adsorption applications. Unlike conventional synthesis, which takes 72 h, this kinetic study showed that NiMOF-74 forms within 12 h under dry-gel conditions with similar performance characteristics and exhibits the best performance characteristics after 48 h of heating.

Molten salt synthesis of nanocrystalline phase of high dielectric constant material CaCu3Ti4O12.

PubMed

Prakash, B Shri; Varma, K B R

2008-11-01

Nanocrystalline powders of giant dielectric constant material, CaCu3Ti4O12 (CCTO), have been prepared successfully by the molten salt synthesis (MSS) using KCl at 750 degrees C/10 h, which is significantly lower than the calcination temperature (approximately 1000 degrees C) that is employed to obtain phase pure CCTO in the conventional solid-state reaction route. The water washed molten salt synthesized powder, characterized by X-ray powder diffraction (XRD), Scanning electron microscopy (SEM), and Transmission electron microscopy (TEM) confirmed to be a phase pure CCTO associated with approximately 150 nm sized crystallites of nearly spherical shape. The decrease in the formation temperature/duration of CCTO in MSS method was attributed to an increase in the diffusion rate or a decrease in the diffusion length of reacting ions in the molten salt medium. As a consequence of liquid phase sintering, pellets of as-synthesized KCl containing CCTO powder exhibited higher sinterability and grain size than that of KCl free CCTO samples prepared by both MSS method and conventional solid-state reaction route. The grain size and the dielectric constant of KCl containing CCTO ceramics increased with increasing sintering temperature (900 degrees C-1050 degrees C). Indeed the dielectric constants of these ceramics were higher than that of KCl free CCTO samples prepared by both MSS method and those obtained via the solid-state reaction route and sintered at the same temperature. Internal barrier layer capacitance (IBLC) model was invoked to correlate the observed dielectric constant with the grain size in these samples.

Use of collagen hydrolysate as a complex nitrogen source for the synthesis of penicillin by Penicillium chrysogenum.

PubMed

Leonhartsberger, S; Lafferty, R M; Korneti, L

1993-09-01

Optimal conditions for both biomass formation and penicillin synthesis by a strain of Penicillium chrysogenum were determined when using a collagen-derived nitrogen source. Preliminary investigations were carried out in shaken flask cultures employing a planned experimental program termed the Graeco-Latin square technique (Auden et al., 1967). It was initially determined that up to 30% of a conventional complex nitrogen source such as cottonseed meal could be replaced by the collagen-derived nitrogen source without decreasing the productivity with respect to the penicillin yield. In the pilot scale experiments using a 30 l stirred tank type of bioreactor, higher penicillin yields were obtained when 70% of the conventional complex nitrogen source in the form of cottonseed meal was replaced by the collagen hydrolysate. Furthermore, the maximum rate of penicillin synthesis continued for over a longer period when using collagen hydrolysate as a complex nitrogen source. Penicillin synthesis rates were determined using a linear regression.

Facile synthesis of upconversion nanoparticles with high purity using lanthanide oleate compounds

NASA Astrophysics Data System (ADS)

Kang, Ning; Ai, Chao-Chao; Zhou, Ya-Ming; Wang, Zuo; Ren, Lei

2018-02-01

A novel strategy for preparing highly pure NaYF4-based upconversion nanoparticles (UCNPs) was developed using lanthanide oleate compounds [Ln(OA)3] as the precursor, denoted as the Ln-OA preparation method. Compared to the conventional solvothermal method for synthesizing UCNPs using lanthanide chloride compounds (LnCl3) as the precursor (denoted as the Ln-Cl method), the Ln-OA strategy exhibited the merits of high purity, reduced purification process and a uniform size in preparing core and core-shell UCNPs excited by a 980 or 808 nm near infrared (NIR) laser. This work sheds new insight on the preparation of UCNPs and promotes their application in biomedical fields.

Thermodynamically balanced inside-out (TBIO) PCR-based gene synthesis: a novel method of primer design for high-fidelity assembly of longer gene sequences

PubMed Central

Gao, Xinxin; Yo, Peggy; Keith, Andrew; Ragan, Timothy J.; Harris, Thomas K.

2003-01-01

A novel thermodynamically-balanced inside-out (TBIO) method of primer design was developed and compared with a thermodynamically-balanced conventional (TBC) method of primer design for PCR-based gene synthesis of codon-optimized gene sequences for the human protein kinase B-2 (PKB2; 1494 bp), p70 ribosomal S6 subunit protein kinase-1 (S6K1; 1622 bp) and phosphoinositide-dependent protein kinase-1 (PDK1; 1712 bp). Each of the 60mer TBIO primers coded for identical nucleotide regions that the 60mer TBC primers covered, except that half of the TBIO primers were reverse complement sequences. In addition, the TBIO and TBC primers contained identical regions of temperature- optimized primer overlaps. The TBC method was optimized to generate sequential overlapping fragments (∼0.4–0.5 kb) for each of the gene sequences, and simultaneous and sequential combinations of overlapping fragments were tested for their ability to be assembled under an array of PCR conditions. However, no fully synthesized gene sequences could be obtained by this approach. In contrast, the TBIO method generated an initial central fragment (∼0.4–0.5 kb), which could be gel purified and used for further inside-out bidirectional elongation by additional increments of 0.4–0.5 kb. By using the newly developed TBIO method of PCR-based gene synthesis, error-free synthetic genes for the human protein kinases PKB2, S6K1 and PDK1 were obtained with little or no corrective mutagenesis. PMID:14602936

Sequential structural and optical evolution of MoS2 by chemical synthesis and exfoliation

NASA Astrophysics Data System (ADS)

Kim, Ju Hwan; Kim, Jungkil; Oh, Si Duck; Kim, Sung; Choi, Suk-Ho

2015-06-01

Various types of MoS2 structures are successfully obtained by using economical and facile sequential synthesis and exfoliation methods. Spherically-shaped lumps of multilayer (ML) MoS2 are prepared by using a conventional hydrothermal method and were subsequently 1st-exfoliated in hydrazine while being kept in autoclave to be unrolled and separated into five-to-six-layer MoS2 pieces of several-hundred nm in size. The MoS2 MLs are 2nd-exfoliated in sodium naphthalenide under an Ar ambient to finally produce bilayer MoS2 crystals of ~100 nm. The sequential exfoliation processes downsize MoS2 laterally and reduce its number of layers. The three types of MoS2 allotropes exhibit particular optical properties corresponding to their structural differences. These results suggest that two-dimensional MoS2 crystals can be prepared by employing only chemical techniques without starting from high-pressure-synthesized bulk MoS2 crystals.

Optimization of infrared two-color multicycle field synthesis for intense-isolated-attosecond-pulse generation

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

Lan Pengfei; Takahashi, Eiji J.; Midorikawa, Katsumi

2010-11-15

We present the optimization of the two-color synthesis method for generating an intense isolated attosecond pulse (IAP) in the multicycle regime. By mixing an infrared assistant pulse with a Ti:sapphire main pulse, we show that an IAP can be produced using a multicycle two-color pulse with a duration longer than 30 fs. We also discuss the influence of the carrier-envelope phase (CEP) and the relative intensity on the generation of IAPs. By optimizing the wavelength of the assistant field, IAP generation becomes insensitive to the CEP slip. Therefore, the optimized two-color method enables us to relax the requirements of pulsemore » duration and easily produce the IAP with a conventional multicycle laser pulse. In addition, it enables us to markedly suppress the ionization of the harmonic medium. This is a major advantage for efficiently generating intense IAPs from a neutral medium by applying the appropriate phase-matching and energy-scaling techniques.« less

The Complex Sol-Gel Process for producing small ThO2 microspheres

NASA Astrophysics Data System (ADS)

Brykala, Marcin; Rogowski, Marcin

2016-05-01

Thorium based fuels offer several benefits compared to uranium based fuels thus they might be an attractive alternative to conventional fuel types. This study is devoted to the synthesis and the characterization of small thorium dioxide microspheres (Ø <50 μm). Their application involves using powder-free process, called the Complex Sol-Gel Process. The source sols used for the processes were prepared by the method where in the starting ascorbic acid solution the solid thorium nitrate was dissolved and partially neutralized by aqueous ammonia under pH control. The microspheres of thorium-ascorbate gel were obtained using the ICHTJ Process (INCT in English). Studies allowed to determine an optimal heat treatment with calcination temperature of 700 °C and temperature rate not higher than 2 °C/min which enabled us to obtain a crack-free surface of microspheres. The main parameters which have a strong influence on the synthesis method and features of the spherical particles of thorium dioxide are described in this article.

Fully Synthetic Granulocyte Colony-Stimulating Factor Enabled by Isonitrile-Mediated Coupling of Large, Side-Chain-Unprotected Peptides

PubMed Central

Roberts, Andrew G.; Johnston, Eric V.; Shieh, Jae-Hung; Sondey, Joseph P.; Hendrickson, Ronald C.; Moore, Malcolm A. S.; Danishefsky, Samuel J.

2015-01-01

Human granulocyte colony-stimulating factor (G-CSF) is an endogenous glycoprotein involved in hematopoiesis. Natively glycosylated and nonglycosylated recombinant forms, lenograstim and filgrastim, respectively, are used clinically to manage neutropenia in patients undergoing chemotherapeutic treatment. Despite their comparable therapeutic potential, the purpose of O-linked glycosylation at Thr133 remains a subject of controversy. In light of this, we have developed a synthetic platform to prepare G-CSF aglycone with the goal of enabling access to native and designed glycoforms with site-selectivity and glycan homogeneity. To address the synthesis of a relatively large, aggregation-prone sequence, we advanced an isonitrile-mediated ligation method. The chemoselective activation and coupling of C-terminal peptidyl Gly thioacids with the N-terminus of an unprotected peptide provide ligated peptides directly in a manner complementary to that with conventional native chemical ligation–desulfurization strategies. Herein, we describe the details and application of this method as it enabled the convergent total synthesis of G-CSF aglycone. PMID:26401918

Solvent and Intermediate Phase as Boosters for the Perovskite Transformation and Solar Cell Performance

PubMed Central

Kim, Jinhyun; Hwang, Taehyun; Lee, Sangheon; Lee, Byungho; Kim, Jaewon; Jang, Gil Su; Nam, Seunghoon; Park, Byungwoo

2016-01-01

High power conversion efficiency and device stabilization are two major challenges for CH3NH3PbI3 (MAPbI3) perovskite solar cells to be commercialized. Herein, we demonstrate a diffusion-engineered perovskite synthesis method using MAI/ethanol dipping, and compared it to the conventional synthesis method from MAI/iso-propanol. Diffusion of MAI/C2H5OH into the PbCl2 film was observed to be more favorable than that of MAI/C3H7OH. Facile perovskite conversion from ethanol and highly-crystalline MAPbI3 with minimized impurities boosted the efficiency from 5.86% to 9.51%. Additionally, we further identified the intermediates and thereby the reaction mechanisms of PbCl2 converting into MAPbI3. Through straightforward engineering to enhance the surface morphology as well as the crystallinity of the perovskite with even faster conversion, an initial power conversion efficiency of 11.23% was obtained, in addition to superior stability after 30 days under an ambient condition. PMID:27156481

Fe3O4 nanocubes assembled on RGO nanosheets: Ultrasound induced in-situ and eco-friendly synthesis, characterization and their excellent catalytic performance for the production of liquid fuel in Fischer-tropsch synthesis.

PubMed

Abbas, Mohamed; Zhang, Juan; Lin, Ke; Chen, Jiangang

2018-04-01

In this study, Fe 3 O 4 nanocubes (NCs) decorated on RGO nanosheets (NSs) structures were successfully synthesized through an innovative and environmentally-friendly rapid sonochemical method. More importantly, iron(II) sulfate heptahydrate and GO were employed as precursors and water as reaction medium, meanwhile, NaOH within the generated free radicals from the high intensity ultrasound were sufficient as reducing and base agent in our clean synthesis. Moreover, the hydrothermal method as a conventional approach was employed to synthesize the same catalysts for the comparison with the ultrasonocation technique. The as-synthesized Fe 3 O 4 and RGO/Fe 3 O 4 NSs catalysts were exposed to industrially relevant Fischer-tropsch synthesis (FTS) conditions at various reaction temperatures (250-290 °C), and they subjected to fully characterization before and after FTS reaction using XRD, TEM, HRTEM, EDS mapping, XPS, FTIR, BET, H 2 -TPR, H 2 -TPD and CO-TPD to understand the structure-performance relationships. Notably, the catalysts produced using the sonochemical method had a better CO conversion rate [Fe 3 O 4 (80%), RGO/Fe 3 O 4 (82%)] than the hydrothermally synthesized catalysts. However, compared to the naked-Fe 3 O 4 catalysts, the sonochemically and hydrothermally synthesized RGO-supported Fe 3 O 4 catalysts had higher long chain hydrocarbon (C5+) selectivity values (72% and 67%) and C 2 -C 4 olefin/paraffin selectivity ratio (3.2 and 2) and low CH4 selectivity values (6% and 8.5%), respectively. This can be attributed to their high surface area, the degree of reducibility, and content of Hägg iron carbide (χ-Fe 5 C 2 ) as the most active phase of the FTS reaction. Proposed reaction mechanisms for the sonochemical and hydrothermal reaction synthesis of Fe 3 O 4 and RGO/Fe 3 O 4 nanoparticles are discussed. In conclusion, our developed surfactantless-sonochemical method holds promise for the eco-friendly synthesis of highly efficient catalysts materials for FTS reaction. Copyright © 2017 Elsevier B.V. All rights reserved.

High degree reduction and restoration of graphene oxide on SiO2 at low temperature via remote Cu-assisted plasma treatment.

PubMed

Obata, Seiji; Sato, Minoru; Akada, Keishi; Saiki, Koichiro

2018-06-15

A high throughput synthesis method of graphene has been required for a long time to apply graphene to industrial applications. Of the various synthesis methods, the chemical exfoliation of graphite via graphene oxide (GO) is advantageous as far as productivity is concerned; however, the quality of the graphene produced by this method is far inferior to that synthesized by other methods, such as chemical vapor deposition on metals. Developing an effective reduction and restoration method for GO on dielectric substrates has been therefore a key issue. Here, we present a method for changing GO deposited on a dielectric substrate into high crystallinity graphene at 550 °C; this method uses CH 4 /H 2 plasma and a Cu catalyst. We found that Cu remotely catalyzed the high degree reduction and restoration of GO on SiO 2 and the effect ranged over at least 8 mm. With this method, field-effect transistor devices can be fabricated without any post treatment such as a transfer process. This plasma treatment increased electron and hole mobilities of GO to 480 cm 2 V -1 s -1 and 460 cm 2 V -1 s -1 respectively; these values were more than 50 times greater than that of conventional reduced GO. Furthermore, the on-site conversion ensured that the shape of the GO sheets remained unchanged after the treatment. This plasma treatment realizes the high throughput synthesis of a desired shaped graphene on any substrate without any residue and damage being caused by the transfer process; as such, it expands the potential applicability of graphene.

High degree reduction and restoration of graphene oxide on SiO2 at low temperature via remote Cu-assisted plasma treatment

NASA Astrophysics Data System (ADS)

Obata, Seiji; Sato, Minoru; Akada, Keishi; Saiki, Koichiro

2018-06-01

A high throughput synthesis method of graphene has been required for a long time to apply graphene to industrial applications. Of the various synthesis methods, the chemical exfoliation of graphite via graphene oxide (GO) is advantageous as far as productivity is concerned; however, the quality of the graphene produced by this method is far inferior to that synthesized by other methods, such as chemical vapor deposition on metals. Developing an effective reduction and restoration method for GO on dielectric substrates has been therefore a key issue. Here, we present a method for changing GO deposited on a dielectric substrate into high crystallinity graphene at 550 °C this method uses CH4/H2 plasma and a Cu catalyst. We found that Cu remotely catalyzed the high degree reduction and restoration of GO on SiO2 and the effect ranged over at least 8 mm. With this method, field-effect transistor devices can be fabricated without any post treatment such as a transfer process. This plasma treatment increased electron and hole mobilities of GO to 480 cm2 V‑1 s‑1 and 460 cm2 V‑1 s‑1 respectively; these values were more than 50 times greater than that of conventional reduced GO. Furthermore, the on-site conversion ensured that the shape of the GO sheets remained unchanged after the treatment. This plasma treatment realizes the high throughput synthesis of a desired shaped graphene on any substrate without any residue and damage being caused by the transfer process; as such, it expands the potential applicability of graphene.

DEXTROSE-TEMPLATED MICROWAVE-ASSISTED COMBUSTION SYNTHESIS OF SPONGY METAL OXIDES

EPA Science Inventory

Microwave-assisted combustion synthesis of porous nanocrystalline titania and carbon coated titania is reported using dextrose as template and the product was compared with the one obtained using conventional heating furnace. Out of three compositions viz., 1:1, 1:3, and 1:5 (met...

Electrically Controllable Microparticle Synthesis and Digital Microfluidic Manipulation by Electric-Field-Induced Droplet Dispensing into Immiscible Fluids

NASA Astrophysics Data System (ADS)

Um, Taewoong; Hong, Jiwoo; Kang, In Seok

2016-11-01

The dispensing of tiny droplets is a basic and crucial process in a myriad of applications, such as DNA/protein microarray, cell cultures, chemical synthesis of microparticles, and digital microfluidics. This work demonstrates the droplet dispensing into immiscible fluids through electric charge concentration (ECC) method. Three main modes (i.e., attaching, uniform and bursting modes) are exhibited as a function of flow rates, applied voltage and gap distance between the nozzle and the oil surface. Through a conventional nozzle with diameter of a few millimeters, charged droplets with volumes ranging from a few μL to a few tens of nL can be uniformly dispensed into the oil chamber without reduction in nozzle size. Based on the features of the proposed method (e.g., formation of droplets with controllable polarity and amount of electric charge in water and oil system), a simple and straightforward method is developed for microparticle synthesis, including preparation for colloidosomes and fabrication of Janus microparticles with anisotropic internal structures. Finally, a combined system consisting of ECC-induced droplet dispensing and electrophoresis of charged droplet (ECD)-driven manipulation systems is constructed. This work was supported by the BK21Plus Program for advanced education of creative chemical engineers of the National Research Foundation of Korea (NRF) Grant funded by the Korea government (MSIP).

Microwave-assisted synthesis of highly fluorescent nanoparticles of a melamine-based porous covalent organic framework for trace-level detection of nitroaromatic explosives.

PubMed

Zhang, Wang; Qiu, Ling-Guang; Yuan, Yu-Peng; Xie, An-Jian; Shen, Yu-Hua; Zhu, Jun-Fa

2012-06-30

Covalent organic frameworks (COFs) are a new generation of porous materials constructed from light elements linked by strong covalent bonds. Herein we present rapid preparation of highly fluorescent nanoparticles of a new type of COF, i.e. melamine-based porous polymeric network SNW-1, by a microwave-assisted synthesis route. Although the synthesis of SNW-1 has to be carried out at 180°C for 3d under conventional reflux conditions, SNW-1 nanoparticles could be obtained in 6h by using such a microwave-assisted method. The results obtained have clearly demonstrated that microwave-assisted synthesis is a simple yet highly efficient approach to nanoscale COFs or other porous polymeric materials. Remarkably, the as-synthesized SNW-1 nanoparticles exhibit extremely high sensitivity and selectivity, as well as fast response to nitroaromatic explosives such as 2,4,6-trinitrotoluene (TNT), 2,4,6-trinitrophenylmethylnitramine (Tetryl) and picric acid (PA) without interference by common organic solvents, which is due to the nanoscaled size and unique hierarchical porosity of such fluorescence-based sensing material. Copyright © 2012 Elsevier B.V. All rights reserved.

Polyol synthesis, functionalisation, and biocompatibility studies of superparamagnetic iron oxide nanoparticles as potential MRI contrast agents

NASA Astrophysics Data System (ADS)

Hachani, Roxanne; Lowdell, Mark; Birchall, Martin; Hervault, Aziliz; Mertz, Damien; Begin-Colin, Sylvie; Thanh, Nguy&Ecirtil; N. Thi&Cmb. B. Dot; Kim

2016-02-01

Iron oxide nanoparticles (IONPs) of low polydispersity were obtained through a simple polyol synthesis in high pressure and high temperature conditions. The control of the size and morphology of the nanoparticles was studied by varying the solvent used, the amount of iron precursor and the reaction time. Compared with conventional synthesis methods such as thermal decomposition or co-precipitation, this process yields nanoparticles with a narrow particle size distribution in a simple, reproducible and cost effective manner without the need for an inert atmosphere. For example, IONPs with a diameter of ca. 8 nm could be made in a reproducible manner and with good crystallinity as evidenced by X-ray diffraction analysis and high saturation magnetization value (84.5 emu g-1). The surface of the IONPs could be tailored post synthesis with two different ligands which provided functionality and stability in water and phosphate buffer saline (PBS). Their potential as a magnetic resonance imaging (MRI) contrast agent was confirmed as they exhibited high r1 and r2 relaxivities of 7.95 mM-1 s-1 and 185.58 mM-1 s-1 respectively at 1.4 T. Biocompatibility and viability of IONPs in primary human mesenchymal stem cells (hMSCs) was studied and confirmed.Iron oxide nanoparticles (IONPs) of low polydispersity were obtained through a simple polyol synthesis in high pressure and high temperature conditions. The control of the size and morphology of the nanoparticles was studied by varying the solvent used, the amount of iron precursor and the reaction time. Compared with conventional synthesis methods such as thermal decomposition or co-precipitation, this process yields nanoparticles with a narrow particle size distribution in a simple, reproducible and cost effective manner without the need for an inert atmosphere. For example, IONPs with a diameter of ca. 8 nm could be made in a reproducible manner and with good crystallinity as evidenced by X-ray diffraction analysis and high saturation magnetization value (84.5 emu g-1). The surface of the IONPs could be tailored post synthesis with two different ligands which provided functionality and stability in water and phosphate buffer saline (PBS). Their potential as a magnetic resonance imaging (MRI) contrast agent was confirmed as they exhibited high r1 and r2 relaxivities of 7.95 mM-1 s-1 and 185.58 mM-1 s-1 respectively at 1.4 T. Biocompatibility and viability of IONPs in primary human mesenchymal stem cells (hMSCs) was studied and confirmed. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr03867g

Graphene-supported platinum catalyst prepared with ionomer as surfactant for anion exchange membrane fuel cells

NASA Astrophysics Data System (ADS)

Zeng, L.; Zhao, T. S.; An, L.; Zhao, G.; Yan, X. H.; Jung, C. Y.

2015-02-01

In this work, we have synthesized an ionomer-coated graphene-supported platinum catalyst for anion exchange membrane fuel cells. Unlike the common surfactant stabilized colloidal method, we employ a home-made anion exchange ionomer (AEI), namely quaternary ammonia poly (2, 6-dimethyl-1, 4-phenylene oxide) (QAPPO), as the surfactant. The AEI coated on reduced graphene oxide (rGO) surfaces serves as a stabilizer to anchor the platinum precursor on rGO surfaces due to electrostatic interactions. As a result, platinum nanoparticles (Pt NPs) can be easily deposited onto rGO surfaces with a uniform distribution. The remarkable feature of the present synthesis method is that the surfactant, the coated AEI, does not need to be removed from the catalyst, but serves as hydroxide-conductive paths in the catalyst layer, leading to enhanced triple phase boundaries. It is demonstrated that the use of the catalyst obtained with the present method enables a H2/O2 AEMFC to yield a peak power density of 264.8 mW cm-2 at 60 °C, which is 30% higher than that produced from the same fuel cell but with the use of the catalyst synthesized by the conventional synthesis method.

Virtual view image synthesis for eye-contact in TV conversation system

NASA Astrophysics Data System (ADS)

Murayama, Daisuke; Kimura, Keiichi; Hosaka, Tadaaki; Hamamoto, Takayuki; Shibuhisa, Nao; Tanaka, Seiichi; Sato, Shunichi; Saito, Sakae

2010-02-01

Eye-contact plays an important role for human communications in the sense that it can convey unspoken information. However, it is highly difficult to realize eye-contact in teleconferencing systems because of camera configurations. Conventional methods to overcome this difficulty mainly resorted to space-consuming optical devices such as half mirrors. In this paper, we propose an alternative approach to achieve eye-contact by techniques of arbitrary view image synthesis. In our method, multiple images captured by real cameras are converted to the virtual viewpoint (the center of the display) by homography, and evaluation of matching errors among these projected images provides the depth map and the virtual image. Furthermore, we also propose a simpler version of this method by using a single camera to save the computational costs, in which the only one real image is transformed to the virtual viewpoint based on the hypothesis that the subject is located at a predetermined distance. In this simple implementation, eye regions are separately generated by comparison with pre-captured frontal face images. Experimental results of both the methods show that the synthesized virtual images enable the eye-contact favorably.

RNActive® Technology: Generation and Testing of Stable and Immunogenic mRNA Vaccines.

PubMed

Rauch, Susanne; Lutz, Johannes; Kowalczyk, Aleksandra; Schlake, Thomas; Heidenreich, Regina

2017-01-01

Developing effective mRNA vaccines poses certain challenges concerning mRNA stability and ability to induce sufficient immune stimulation and requires a specific panel of techniques for production and testing. Here, we describe the production of stabilized mRNA with enhanced immunogenicity, generated using conventional nucleotides only, by introducing changes to the mRNA sequence and by complexation with the nucleotide-binding peptide protamine (RNActive® technology). Methods described here include the synthesis, purification, and protamine complexation of mRNA vaccines as well as a comprehensive panel of in vitro and in vivo methods for evaluation of vaccine quality and immunogenicity.

Microwave-Assisted Synthesis of High Dielectric Constant CaCu3Ti4O12 from Sol-Gel Precursor

NASA Astrophysics Data System (ADS)

Ouyang, Xin; Cao, Peng; Huang, Saifang; Zhang, Weijun; Huang, Zhaohui; Gao, Wei

2015-07-01

CaCu3Ti4O12 (CCTO) powders derived from sol-gel precursors were calcined and sintered via microwave radiation. The obtained CCTO powders were compared with that obtained via a conventional heating method. For microwave heating, 89.1 wt.% CCTO was achieved from the sol-gel precursor, after only 17 min at 950°C. In contrast, the conventional calcination method required 3 h to generate 87.6 wt.% CCTO content at 1100°C. In addition, the CCTO powders prepared through 17 min of microwave calcination exhibited a small particle size distribution of D50 = 3.826 μm. It was found that a lengthy hold time of 1 h by microwave sintering is required to obtain a high dielectric constant (3.14 × 103 at 102 Hz) and a reasonably low dielectric loss (0.161) in the sintered CCTO ceramic. Based upon the distinct microstructures, the dielectric responses of the CCTO samples sintered by different methods are attributed to space charge polarization and internal barrier layer capacitor mechanism.

Synthesis of an integrated cockpit management system

NASA Technical Reports Server (NTRS)

Dasaro, J. A.; Elliott, C. T.

1982-01-01

The process used in the synthesis of an integrated cockpit management system was discussed. Areas covered included flight displays, subsystem management, checklists, and procedures (both normal and emergency). The process of evolving from the unintegrated conventional system to the integrated system is examined and a brief description of the results presented.

Conventional and microwave assisted synthesis of pyrazolone Mannich bases possessing anti-inflammatory, analgesic, ulcerogenic effect and antimicrobial properties.

PubMed

Sivakumar, Kullampalayam Krishnasamy; Rajasekaran, Aiyalu; Senthilkumar, Palaniappan; Wattamwar, Prasad P

2014-07-01

In the present study, an efficient synthesis of some Mannich base of 5-methyl-2-[(2-oxo-2H-chromen-3-yl)carbonyl]-2,4-dihydro-3H-pyrazol-3-one (4a-j) have been described by using conventional and non-conventional (microwave) techniques. Microwave assisted reactions showed that require shorter reaction time and good yield. The newly synthesized compounds were screened for their anti-inflammatory, analgesic activity, antioxidant, and antibacterial effects were compared with standard drug. Among the compounds studied, compound (4f) showing nearly equipotent anti-inflammatory and analgesic activity than the standard drug (indomethacin), along with minimum ulcerogenic index. Compounds (4b and 4i) showing 1.06 times more active than ciprofloxacin against tested Gram-negative bacteria. Copyright © 2014 Elsevier Ltd. All rights reserved.

Chemoselective reductive nucleophilic addition to tertiary amides, secondary amides, and N-methoxyamides.

PubMed

Nakajima, Minami; Oda, Yukiko; Wada, Takamasa; Minamikawa, Ryo; Shirokane, Kenji; Sato, Takaaki; Chida, Noritaka

2014-12-22

As the complexity of targeted molecules increases in modern organic synthesis, chemoselectivity is recognized as an important factor in the development of new methodologies. Chemoselective nucleophilic addition to amide carbonyl centers is a challenge because classical methods require harsh reaction conditions to overcome the poor electrophilicity of the amide carbonyl group. We have successfully developed a reductive nucleophilic addition of mild nucleophiles to tertiary amides, secondary amides, and N-methoxyamides that uses the Schwartz reagent [Cp2 ZrHCl]. The reaction took place in a highly chemoselective fashion in the presence of a variety of sensitive functional groups, such as methyl esters, which conventionally require protection prior to nucleophilic addition. The reaction will be applicable to the concise synthesis of complex natural alkaloids from readily available amide groups. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

N-Sulfanylethylaminooxybutyramide (SEAoxy): A Crypto-Thioester Compatible with Fmoc Solid-Phase Peptide Synthesis.

PubMed

Tsuda, Shugo; Mochizuki, Masayoshi; Sakamoto, Ken; Denda, Masaya; Nishio, Hideki; Otaka, Akira; Yoshiya, Taku

2016-11-18

An N-sulfanylethylaminooxybutyramide (SEAoxy) has been developed as a novel thioester equivalent for native chemical ligation. SEAoxy peptide was straightforwardly synthesized by conventional Fmoc solid-phase peptide synthesis without a problem. Moreover, SEAoxy peptide could be directly applied to native chemical ligation owing to the intramolecular N-to-S acyl shift that releases the peptide-thioester in situ. This methodology was successfully applied to the synthesis of two bioactive peptides.

Surface-Directed Synthesis of Erbium-Doped Yttrium Oxide Nanoparticles within Organosilane Zeptoliter Containers

PubMed Central

2015-01-01

We introduce an approach to synthesize rare earth oxide nanoparticles using high temperature without aggregation of the nanoparticles. The dispersity of the nanoparticles is controlled at the nanoscale by using small organosilane molds as reaction containers. Zeptoliter reaction vessels prepared from organosilane self-assembled monolayers (SAMs) were used for the surface-directed synthesis of rare earth oxide (REO) nanoparticles. Nanopores of octadecyltrichlorosilane were prepared on Si(111) using particle lithography with immersion steps. The nanopores were filled with a precursor solution of erbium and yttrium salts to confine the crystallization step to occur within individual zeptoliter-sized organosilane reaction vessels. Areas between the nanopores were separated by a matrix film of octadecyltrichlorosilane. With heating, the organosilane template was removed by calcination to generate a surface array of erbium-doped yttria nanoparticles. Nanoparticles synthesized by the surface-directed approach retain the periodic arrangement of the nanopores formed from mesoparticle masks. While bulk rare earth oxides can be readily prepared by solid state methods at high temperature (>900 °C), approaches for preparing REO nanoparticles are limited. Conventional wet chemistry methods are limited to low temperatures according to the boiling points of the solvents used for synthesis. To achieve crystallinity of REO nanoparticles requires steps for high-temperature processing of samples, which can cause self-aggregation and dispersity in sample diameters. The facile steps for particle lithography address the problems of aggregation and the requirement for high-temperature synthesis. PMID:25163977

Comparison studies on catalytic properties of silver nanoparticles biosynthesized via aqueous leaves extract of Hibiscus rosa sinensis and Imperata cylindrica

NASA Astrophysics Data System (ADS)

Fairuzi, Afiza Ahmad; Bonnia, Noor Najmi; Akhir, Rabiatuladawiyah Md.; Akil, Hazizan Md; Yahya, Sabrina M.; Rahman, Norafifah A.

2018-05-01

Synthesis of silver nanoparticles has been developed by using aqueous leaves extract (ALE) of Hibiscus rosa sinensis (H. rosa sinensis) and Imperata cylindrica (I. cylindrica). Both plants extract acts as reducing and capping agent. The colour change in reaction mixture (pale yellow to dark brown) was observed during the synthesis process. The formation of silver nanoparticles was confirmed by surface Plasmon Resonance (SPR) at range 300-700 nm for both leaves using UV-Vis Spectroscopy. The reduction of silver ions to silver nanoparticles was completed within 2 hour for H. rosa sinensis and 30 minutes for I. cylindrica extract. The synthesized nanoparticles were characterized using UV-Vis spectroscopy, field emission scanning electron microscope (FESEM) and Fourier transform infrared (FTIR) spectroscopy. The morphology of silver nanoparticles was found to be different when synthesized using different plant extract. In addition, this study also reported on the effect of silver nanoparticles on the degradation of organic dye by sodium borohydride (NaBH4). The silver nanoparticles synthesis by aqueous leaf extract demonstrates rapid, simple and inexpensive method compared to the conventional physical and physical methods. The efficiency of silver nanoparticles as a promising candidate for the catalysis of organic dyes by NaBH4 through the electron transfer is established in the present study.

27Al, 47,49Ti, 31P, and 13C MAS NMR Study of VX, GD, and HD Reactions with Nanosize Al2O3, Conventional Al2O3 and TiO2, and Aluminum and Titanium Metal

DTIC Science & Technology

2007-01-01

The alumina was used as received. Anatase, rutile, aluminum, and titania metal powders, titanium (IV) isopropoxide , and pinacolyl methylphosphonate...Synthesis. Titanophosphonate synthesis was adapted from Mutin et al.4 using titanium (IV) isopropoxide (TIP) and pinacolyl methylphosphonate (PMPA...REPORT 27Al, 47,49Ti, 31P, and 13C MAS NMR Study of VX, GD, and HD Reactions with Nanosize Al2O3, Conventional Al2O3 and TiO2, and Aluminum and Titanium

Synthesis of phthalide-fused indoline by microwave irradiation and preliminary binding study with metal cations

NASA Astrophysics Data System (ADS)

Ling, Sheryn Wong Shue; Latip, Jalifah; Hassan, Nurul Izzaty; Hasbullah, Siti Aishah

2018-04-01

An efficient and green method of synthesizing phthalide-fused indoline, 3-[(1,3,3-trimethylindolin-2-ylidene)methyl]isobenzofuran-1(3H)-one (3) has been developed by the coupling reaction of 1,3,3-trimethyl-2-methyleneindoline, 1 and phthalaldehydic acid, 2 under solvent-free domestic microwave irradiation. The compound was produced with an excellent yield (98 %) and at a shorter reaction time (5 min) as compared to the conventional method. Compound 3 was fully characterized by analytical and spectral methods. Preliminary binding study of 3 towards different types of metal cations was done by "naked eye" colorimetric detection and UV-vis spectrophotometer. Compound 3 exhibits good selectivity and sensitivity for Sn2+ compared to other metal cations.

Low-temperature solvothermal approach to the synthesis of La4Ni3O8 by topotactic oxygen deintercalation.

PubMed

Blakely, Colin K; Bruno, Shaun R; Poltavets, Viktor V

2011-07-18

A chimie douce solvothermal reduction method is proposed for topotactic oxygen deintercalation of complex metal oxides. Four different reduction techniques were employed to qualitatively identify the relative reduction activity of each including reduction with H(2) and NaH, solution-based reduction using metal hydrides at ambient pressure, and reduction under solvothermal conditions. The reduction of the Ruddlesden-Popper nickelate La(4)Ni(3)O(10) was used as a test case to prove the validity of the method. The completely reduced phase La(4)Ni(3)O(8) was produced via the solvothermal technique at 150 °C--a lower temperature than by other more conventional solid state oxygen deintercalation methods.

A Direction Finding Method with A 3-D Array Based on Aperture Synthesis

NASA Astrophysics Data System (ADS)

Li, Shiwen; Chen, Liangbing; Gao, Zhaozhao; Ma, Wenfeng

2018-01-01

Direction finding for electronic warfare application should provide a wider field of view as possible. But the maximum unambiguous field of view for conventional direction finding methods is a hemisphere. It cannot distinguish the direction of arrival of the signals from the back lobe of the array. In this paper, a full 3-D direction finding method based on aperture synthesis radiometry is proposed. The model of the direction finding system is illustrated, and the fundamentals are presented. The relationship between the outputs of the measurements of a 3-D array and the 3-D power distribution of the point sources can be represented by a 3-D Fourier transform, and then the 3-D power distribution of the point sources can be reconstructed by an inverse 3-D Fourier transform. And in order to display the 3-D power distribution of the point sources conveniently, the whole spherical distribution is represented by two 2-D circular distribution images, one of which is for the upper hemisphere, and the other is for the lower hemisphere. Then a numeric simulation is designed and conducted to demonstrate the feasibility of the method. The results show that the method can estimate the arbitrary direction of arrival of the signals in the 3-D space correctly.

78 FR 23738 - Monsanto Company and Forage Genetics International (FGI); Availability of Petition for...

Federal Register 2010, 2011, 2012, 2013, 2014

2013-04-22

... pathway. Suppression of the CCOMT gene expression leads to lower CCOMT protein expression resulting in reduced synthesis of G lignin subunit compared to conventional alfalfa at the same stage of growth. The reduction in G lignin subunit synthesis leads to reduced accumulation of total lignin, measured as acid...

Control of nonlinear systems using terminal sliding modes

NASA Technical Reports Server (NTRS)

Venkataraman, S. T.; Gulati, S.

1992-01-01

The development of an approach to control synthesis for robust robot operations in unstructured environments is discussed. To enhance control performance with full model information, the authors introduce the notion of terminal convergence and develop control laws based on a class of sliding modes, denoted as terminal sliders. They demonstrate that terminal sliders provide robustness to parametric uncertainty without having to resort to high-frequency control switching, as in the case of conventional sliders. It is shown that the proposed method leads to greater guaranteed precision in all control cases discussed.

The marriage of metallacycle transfer chemistry with Suzuki-Miyaura cross-coupling to give main group element-containing conjugated polymers.

PubMed

He, Gang; Kang, Le; Torres Delgado, William; Shynkaruk, Olena; Ferguson, Michael J; McDonald, Robert; Rivard, Eric

2013-04-10

A versatile and general synthetic route for the synthesis of conjugated main group element-based polymers, previously inaccessible by conventional means, is reported. These polymers contain five-membered chalcogenophene rings based on S, Se, and Te, and we demonstrate that optoelectronic properties can be readily tuned via controlled atom substitution chemistry. In addition, regioregular hybrid thiophene-selenophene-tellurophene and selenophene-fluorene copolymers were synthesized to provide a further illustration of the scope of the presented metallacycle transfer/cross-coupling polymerization method.

Enhanced oxygen storage capacity of cation-ordered cerium-zirconium oxide induced by titanium substitution.

PubMed

Goto, Yoshihiro; Morikawa, Akira; Iwasaki, Masaoki; Miura, Masahide; Tanabe, Toshitaka

2018-04-03

Herein, we report on the synthesis of Ce0.5Zr0.5-xTixO2 oxygen storage materials prepared via a solution combustion method. Ce0.5Zr0.4Ti0.1O2 showed an outstanding oxygen storage capacity (1310 μmol-O per g) at 200 °C compared to conventional κ-Ce2Zr2O8 (650 μmol-O per g) due to its cation ordering and the formation of weakly bound oxygen atoms induced by Ti substitution.

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

Ma, Ying; Li, Hong; Bridges, Denzel

We report that the continuing miniaturization of microelectronics is pushing advanced manufacturing into nanomanufacturing. Nanojoining is a bottom-up assembly technique that enables functional nanodevice fabrication with dissimilar nanoscopic building blocks and/or molecular components. Various conventional joining techniques have been modified and re-invented for joining nanomaterials. Our review surveys recent progress in nanojoining methods, as compared to conventional joining processes. Examples of nanojoining are given and classified by the dimensionality of the joining materials. At each classification, nanojoining is reviewed and discussed according to materials specialties, low dimensional processing features, energy input mechanisms and potential applications. The preparation of new intermetallicmore » materials by reactive nanoscale multilayer foils based on self-propagating high-temperature synthesis is highlighted. This review will provide insight into nanojoining fundamentals and innovative applications in power electronics packaging, plasmonic devices, nanosoldering for printable electronics, 3D printing and space manufacturing.« less

Synthesis of the zeolitic imidazolate framework ZIF-4 from the ionic liquid 1-butyl-3-methylimidazolium imidazolate

NASA Astrophysics Data System (ADS)

Hovestadt, Maximilian; Schwegler, Johannes; Schulz, Peter S.; Hartmann, Martin

2018-05-01

A new synthesis route for the zeolitic imidazolate framework ZIF-4 using imidazolium imidazolate is reported. Additionally, the ionic liquid-derived material is compared to conventional ZIF-4 with respect to the powder X-ray diffraction pattern pattern, nitrogen uptake, particle size, and separation potential for olefin/paraffin gas mixtures. Higher synthesis yields were obtained, and the different particle size affected the performance in the separation of ethane and ethylene.

Heterogeneous enantioselective hydrogenation of beta-keto esters using chirally modified supported Ni nanoparticles

NASA Astrophysics Data System (ADS)

Acharya, Sushma

Enantioselective heterogeneous catalysis is an important and rapidly expanding research area. The two most heavily researched examples of this type of catalysis are the enantioselective hydrogenation of α-keto-esters over Pt-based catalysts and the enantioselective hydrogenation of β-keto-esters over Ni-based catalysts. These enantioselective surface reactions are controlled by the presence of adsorbed chiral molecules i.e. tartaric acid on the surface of the metal component of the catalyst. The work presented in this thesis focuses on two parts, the synthesis of pure nickel nanoparticles and enantioselective behavior of the modified nickel nanoparticles. The works on the synthesis of pure nickel nanoparticles were carried out using two methods, the reverse microemulsion and the reduction method. It was discovered that the reverse microemulsion method produced nickel oxide nanoparticles, whereas the reduction method produced pure nickel nanoparticles. Chiral modifications of Raney nickel (RNi) and C-supported catalysts were studied. The catalysts were employed in enantioselective hydrogenation of methyl acetoacetate (MAA) to (R) - and (S)-enantiomers of methyl 3-hydroxybutyrate (MHB). The effects of modification and hydrogenation parameters such as concentration of modifier temperature, pressure and solvent on the enantioselectivity of MAA hydrogenation were discussed. For RNi methanol was found to be the best solvent, with tartaric acid concentration 0.2 mol/L for achieving the highest enantiomeric excess under 8 bar at 70 oC. Characteristic features of the in-situ modification of Raney nickel and C-supported Ni were also evaluated and the results obtained were compared with the conventional (pre-modification) approach. Parameters for the conventional and in-situ methods were optimised in a series of experiments for both types of catalysts. The in-situ modified catalyst was found more active for both RNi and C-supported catalysts with 98 % and 42% enantiomeric excess, respectively.

Large Marks-decahedral Pd nanoparticles synthesized by a modified hydrothermal method using a homogeneous reactor

NASA Astrophysics Data System (ADS)

Zhao, Haiqiang; Qi, Weihong; Ji, Wenhai; Wang, Tianran; Peng, Hongcheng; Wang, Qi; Jia, Yanlin; He, Jieting

2017-05-01

Fivefold symmetry appears only in small particles and quasicrystals because internal stress in the particles increases with the particle size. However, a typical Marks decahedron with five re-entrant grooves located at the ends of the twin boundaries can further reduce the strain energy. During hydrothermal synthesis, it is difficult to stir the reaction solution contained in a digestion high-pressure tank because of the relatively small size and high-temperature and high-pressure sealed environment. In this work, we optimized a hydrothermal reaction system by replacing the conventional drying oven with a homogeneous reactor to shift the original static reaction solution into a full mixing state. Large Marks-decahedral Pd nanoparticles ( 90 nm) have been successfully synthesized in the optimized hydrothermal synthesis system. Additionally, in the products, round Marks-decahedral Pd particles were also found for the first time. While it remains a challenge to understand the growth mechanism of the fivefold twinned structure, we proposed a plausible growth-mediated mechanism for Marks-decahedral Pd nanoparticles based on observations of the synthesis process.

Meta-analytical synthesis of regression coefficients under different categorization scheme of continuous covariates.

PubMed

Yoneoka, Daisuke; Henmi, Masayuki

2017-11-30

Recently, the number of clinical prediction models sharing the same regression task has increased in the medical literature. However, evidence synthesis methodologies that use the results of these regression models have not been sufficiently studied, particularly in meta-analysis settings where only regression coefficients are available. One of the difficulties lies in the differences between the categorization schemes of continuous covariates across different studies. In general, categorization methods using cutoff values are study specific across available models, even if they focus on the same covariates of interest. Differences in the categorization of covariates could lead to serious bias in the estimated regression coefficients and thus in subsequent syntheses. To tackle this issue, we developed synthesis methods for linear regression models with different categorization schemes of covariates. A 2-step approach to aggregate the regression coefficient estimates is proposed. The first step is to estimate the joint distribution of covariates by introducing a latent sampling distribution, which uses one set of individual participant data to estimate the marginal distribution of covariates with categorization. The second step is to use a nonlinear mixed-effects model with correction terms for the bias due to categorization to estimate the overall regression coefficients. Especially in terms of precision, numerical simulations show that our approach outperforms conventional methods, which only use studies with common covariates or ignore the differences between categorization schemes. The method developed in this study is also applied to a series of WHO epidemiologic studies on white blood cell counts. Copyright © 2017 John Wiley & Sons, Ltd.

Robust one pot synthesis of colloidal silver nanoparticles by simple redox method and absorbance recovered sensing.

PubMed

Salman, Muhammad; Iqbal, Mahwish; El Ashry, El Sayed H; Kanwal, Shamsa

2012-01-01

Conventional synthesis of silver nanoparticles employs a reducing agent and a capping agent. In this report water-soluble silver nanoparticles (AgNPs) were prepared facilely by chemical reduction of Ag(I) ions. 4-Amino-3-(d-gluco-pentitol-1-yl)-4,5-dihydro-1,2,4-triazole-5-thione (AGTT) was used both as reducing and stabilizing agent. Direct heating methodology was found to be more suitable for achieving particles with a hydrodynamic diameter of ~20 nm. AGTT exists as tautomer in solution form and our studies indicate that -NH(2) group is involved in the reduction and stabilization of Ag(+) and thione (Δ=S) group of AGTT is possibly involved in stabilizing the nanoparticles via coordinate covalent linkage. Characterization of synthesized silver nanoparticles was performed by UV-vis, FT-IR and by FESEM. Based on the absorption properties of synthesized AgNPs, we used AgNPs to detect bovine serum albumin (BSA) and AgNPs-BSA composite nanoprobe was further applied to detect Cu(2+) based on absorbance recovery. The proposed method has advantages over existing methods in terms of rapid synthesis and stability of AgNPs and their applications. Analysis is reproducible, cost effective and highly sensitive. The lowest detectable concentration of BSA in this approach is 3 nM, and for Cu(2+) it can detect upto 200 pM. Copyright © 2012 Elsevier B.V. All rights reserved.

Tapping the potential of trioctylphosphine (TOP) in the realization of highly luminescent blue-emitting colloidal indium phosphide (InP) quantum dots

NASA Astrophysics Data System (ADS)

Singh, Akanksha; Chawla, Parul; Jain, Shefali; Sharma, Shailesh Narain

2017-06-01

In this work, extremely small blue emitting colloidal InP-based quantum dots (size 2-5 nm) have been synthesized using trioctylphosphine (TOP) as a source of phosphorus. The method reported here is unconventional, quite rapid ( 90 min), more viable, less expensive and relatively greener as compared to other conventional methods that employ tristrimethylsilyylphosphine(P(SiMe3)3) which is scarce, expensive, flammable, highly toxic and even banned in a few countries. Highly luminescent InP QDs having bluish-green emission (λ 490 nm) can be synthesized using this method without resorting to any post-synthesis etching to tune the emission to the blue region. Besides being the source of phosphorus and the particle size regulating agent, the efficacy of TOP is further realized during synthesis via its reduction of indium salt, which aids in the formation of indium metal and then subsequently in the development of InP QDs. The PL intensity of as-synthesized InP QDs is further enhanced by growing a shell of wide band gap material, i.e. ZnS resulting in a concurrent increment in quantum yield from 25% to 38% respectively.

ZnO-Ag core shell nanocomposite formed by green method using essential oil of wild ginger and their bactericidal and cytotoxic effects

NASA Astrophysics Data System (ADS)

Azizi, Susan; Mohamad, Rosfarizan; Rahim, Raha Abdul; Moghaddam, Amin Boroumand; Moniri, Mona; Ariff, Arbakariya; Saad, Wan Zuhainis; Namvab, Farideh

2016-10-01

In this paper, a novel green method for fabrication of zinc oxide-silver (ZnO-Ag) core-shell nanocomposite using essential oil of ginger (EO-G) is reported. The EO-G played two significant roles in the synthesis process: it could act as a reaction media for the formation of ZnO and reduce Ag+ to Ag0. The bioformed ZnO-Ag nanocomposite was compared with pure biosynthesized ZnO-NPs and characterized by UV-vis spectroscopy, TEM, EDX, XRD and FTIR. The characterization results confirmed that Ag-NPs had been embedded in ZnO hexagonal nanoparticles. Six Gram positive and negative pathogens were used to investigate the antibacterial effects of these samples. Ag-doping improves the bactericidal activity of ZnO-NPs. In vitro cytotoxicity studies on Vero cells, a dose dependent toxicity with non-toxic effect of concentration below 100 μg/mL was shown for ZnO-Ag nanocomposite. The biosynthesized ZnO-Ag nanocomposites were found to be comparable to those obtained from the conventional methods using hazardous materials which can be an excellent alternative for the synthesis of ZnO-Ag using biomass.

Magnetic agglomeration method for size control in the synthesis of magnetic nanoparticles

DOEpatents

Huber, Dale L [Albuquerque, NM

2011-07-05

A method for controlling the size of chemically synthesized magnetic nanoparticles that employs magnetic interaction between particles to control particle size and does not rely on conventional kinetic control of the reaction to control particle size. The particles are caused to reversibly agglomerate and precipitate from solution; the size at which this occurs can be well controlled to provide a very narrow particle size distribution. The size of particles is controllable by the size of the surfactant employed in the process; controlling the size of the surfactant allows magnetic control of the agglomeration and precipitation processes. Agglomeration is used to effectively stop particle growth to provide a very narrow range of particle sizes.

Electronic conductivity studies on oxyhalide glasses containing TMO

NASA Astrophysics Data System (ADS)

Vijayatha, D.; Viswanatha, R.; Sujatha, B.; Narayana Reddy, C.

2016-05-01

Microwave-assisted synthesis is cleaner, more economical and much faster than conventional methods. The development of new routes for the synthesis of solid materials is an integral part of material science and technology. The electronic conductivity studies on xPbCl2 - 60 PbO - (40-x) V2O5 (1 ≥ x ≤ 10) glass system has been carried out over a wide range of composition and temperature (300 K to 423 K). X-ray diffraction study confirms the amorphous nature of the samples. The Scanning electron microscopic studies reveal the formation of cluster like morphology in PbCl2 containing glasses. The d.c conductivity exhibits Arrhenius behaviour and increases with V2O5 concentration. Analysis of the results is interpreted in view Austin-Mott's small polaron model of electron transport. Activation energies calculated using regression analysis exhibit composition dependent trend and the variation is explained in view of the structure of lead-vanadate glass.

Facile and one-pot synthesis of uniform PtRu nanoparticles on polydopamine-modified multiwalled carbon nanotubes for direct methanol fuel cell application.

PubMed

Chen, Fengxia; Ren, Junkai; He, Qian; Liu, Jun; Song, Rui

2017-07-01

A facile, environment-friendly and one-pot synthesis method for the preparation of high performance PtRu electrocatalysts on the multiwalled carbon nanotubes (MWCNTs) is reported. Herein, bimetallic PtRu electrocatalysts are deposited onto polydopamine (Pdop) - functionalized MWCNTs by mildly stirring at room temperature. Without the use of expensive chemicals or corrosive acids, this noncovalent functionalization of MWCNTs by Pdop is simple, facile and eco-friendly, and thus preserving the integrity and electronic structure of MWCNTs. Due to the well improved dispersion and the decreased size of alloy nanoparticles, the PtRu electrocatalysts on Pdop-functionalized MWCNTs show much better dispersion, higher electrochemically active surface area, and higher electrocatalytic activity for the electrooxidation of methanol in direct methanol fuel cells, compared with the conventional acid-treated MWCNTs. Copyright © 2017 Elsevier Inc. All rights reserved.

One-pot synthesis of hierarchical FeZSM-5 zeolites from natural aluminosilicates for selective catalytic reduction of NO by NH3

PubMed Central

Yue, Yuanyuan; Liu, Haiyan; Yuan, Pei; Yu, Chengzhong; Bao, Xiaojun

2015-01-01

Iron-modified ZSM-5 zeolites (FeZSM-5s) have been considered to be a promising catalyst system to reduce nitrogen oxide emissions, one of the most important global environmental issues, but their synthesis faces enormous economic and environmental challenges. Herein we report a cheap and green strategy to fabricate hierarchical FeZSM-5 zeolites from natural aluminosilicate minerals via a nanoscale depolymerization-reorganization method. Our strategy is featured by neither using any aluminum-, silicon-, or iron-containing inorganic chemical nor involving any mesoscale template and any post-synthetic modification. Compared with the conventional FeZSM-5 synthesized from inorganic chemicals with the similar Fe content, the resulting hierarchical FeZSM-5 with highly-dispersed iron species showed superior catalytic activity in the selective catalytic reduction of NO by NH3. PMID:25791958

Synthesis of thoria nano-particles at low temperature through base electrogeneration on steel 316L surface: Effect of current density

NASA Astrophysics Data System (ADS)

Yousefi, Taher; Torab-Mostaedi, Meisam; Mobtaker, Hossein Ghasemi; Keshtkar, Ali Reza

2016-10-01

The strategy developed in this study, offers significant advantages (simplicity and cleanness of method and also a product purity and new morphology of the product) over the conventional routes for the synthesis of ThO2 nanostructure. The effect of current density on morphology was studied. The synthesized powder was characterized by means of Powder X-ray Diffraction (PXRD), Transmission Electron Microscopy (TEM, Phillips EM 2085) Brunauer-Emmett-Teller (BET) and Fourier Transform Infrared (FT-IR) spectroscopy. The results show that the current density has a great effect on the morphology of the samples. The average size of the particles decreases as the applied current density increases and the average size of the samples decreases from 50 to 15 nm when the current density increases from 2 to 5 mA cm-2.

A general procedure to synthesize highly crystalline metal oxide and mixed oxidenanocrystals in aqueous medium and photocatalytic activity of metal/oxide nanohybrids

NASA Astrophysics Data System (ADS)

Nguyen, Thanh-Dinh; Dinh, Cao-Thang; Do, Trong-On

2011-04-01

A conventional and general route has been exploited to the high yield synthesis of many kinds of highly crystalline metal oxide and mixed oxidenanocrystals with different morphologies including belt, rod, truncated-octahedron, cubic, sphere, sheet via the hydrothermal reaction of inorganic precursors in aqueous solution in the presence of bifunctional 6-aminohexanoic acid (AHA) molecules as a capping agent. This method is a simple, reproducible and general route for the preparation of a variety of high-crystalline inorganic nanocrystals in scale-up. The shape of inorganic nanocrystals such as CoWO4, La2(MoO4)3 can be controlled by simply adjusting the synthesis conditions including pH solution and reaction temperature. Further, by tuning precursor monomer concentration, the mesocrystal hierarchical aggregated microspheres (e.g., MnWO4, La2(MoO4)3) can be achieved, due to the spontaneous assembly of individual AHA-capped nanoparticles. These obtained AHA-capped nanocrystals are excellent supports for the synthesis of a variety of hybrid metal/oxidenanocrystals in which noble metal particles are uniformly deposited on the surface of each individual nanosupport. The photocatalytic activity of Ag/TiO2 nanobelts as a typical hybrid photocatalyst sample for Methylene Blue degradation was also studied.A conventional and general route has been exploited to the high yield synthesis of many kinds of highly crystalline metal oxide and mixed oxidenanocrystals with different morphologies including belt, rod, truncated-octahedron, cubic, sphere, sheet via the hydrothermal reaction of inorganic precursors in aqueous solution in the presence of bifunctional 6-aminohexanoic acid (AHA) molecules as a capping agent. This method is a simple, reproducible and general route for the preparation of a variety of high-crystalline inorganic nanocrystals in scale-up. The shape of inorganic nanocrystals such as CoWO4, La2(MoO4)3 can be controlled by simply adjusting the synthesis conditions including pH solution and reaction temperature. Further, by tuning precursor monomer concentration, the mesocrystal hierarchical aggregated microspheres (e.g., MnWO4, La2(MoO4)3) can be achieved, due to the spontaneous assembly of individual AHA-capped nanoparticles. These obtained AHA-capped nanocrystals are excellent supports for the synthesis of a variety of hybrid metal/oxidenanocrystals in which noble metal particles are uniformly deposited on the surface of each individual nanosupport. The photocatalytic activity of Ag/TiO2 nanobelts as a typical hybrid photocatalyst sample for Methylene Blue degradation was also studied. Electronic supplementary information (ESI) available: Additional TEM, XRD, XPS, FTIR, UV-vis and photoluminescence results of the nanocrystals. See DOI: 10.1039/c1nr10109a

Parametric study of waste chicken fat catalytic chemical vapour deposition for controlled synthesis of vertically aligned carbon nanotubes

NASA Astrophysics Data System (ADS)

Suriani, A. B.; Dalila, A. R.; Mohamed, A.; Rosmi, M. S.; Mamat, M. H.; Malek, M. F.; Ahmad, M. K.; Hashim, N.; Isa, I. M.; Soga, T.; Tanemura, M.

2016-12-01

High-quality vertically aligned carbon nanotubes (VACNTs) were synthesised using ferrocene-chicken oil mixture utilising a thermal chemical vapour deposition (TCVD) method. Reaction parameters including vaporisation temperature, catalyst concentration and synthesis time were examined for the first time to investigate their influence on the growth of VACNTs. Analysis via field emission scanning electron microscopy and micro-Raman spectroscopy revealed that the growth rate, diameter and crystallinity of VACNTs depend on the varied synthesis parameters. Vaporisation temperature of 570°C, catalyst concentration of 5.33 wt% and synthesis time of 60 min were considered as optimum parameters for the production of VACNTs from waste chicken fat. These parameters are able to produce VACNTs with small diameters in the range of 15-30 nm and good quality (ID/IG 0.39 and purity 76%) which were comparable to those synthesised using conventional carbon precursor. The low turn on and threshold fields of VACNTs synthesised using optimum parameters indicated that the VACNTs synthesised using waste chicken fat are good candidate for field electron emitter. The result of this study therefore can be used to optimise the growth and production of VACNTs from waste chicken fat in a large scale for field emission application.

Facile and green synthesis of mesoporous Co3O4 nanocubes and their applications for supercapacitors

NASA Astrophysics Data System (ADS)

Liu, Xiangmei; Long, Qing; Jiang, Chunhui; Zhan, Beibei; Li, Chen; Liu, Shujuan; Zhao, Qiang; Huang, Wei; Dong, Xiaochen

2013-06-01

Nanostructured Co3O4 materials attracted significant attention due to their exceptional electrochemical (pseudo-capacitive) properties. However, rigorous preparation conditions are needed to control the size (especially nanosize), morphology and size distribution of the products obtained by conventional methods. Herein, we describe a novel one step shape-controlled synthesis of uniform Co3O4 nanocubes with a size of 50 nm with the existence of mesoporous carbon nanorods (meso-CNRs). In this synthesis process, meso-CNRs not only act as a heat receiver to directly obtain Co3O4 eliminating the high-temperature post-calcination, but also control the morphology of the resulting Co3O4 to form nanocubes with uniform distribution. More strikingly, mesoporous Co3O4 nanocubes are obtained by further thermal treatment. The structure and morphology of the samples were characterized by scanning electron microscopy, transmission electron microscopy and X-ray diffraction. A possible formation mechanism of mesoporous Co3O4 nanocubes is proposed here. Electrochemical tests have revealed that the prepared mesoporous Co3O4 nanocubes demonstrate a remarkable performance in supercapacitor applications due to the porous structure, which endows fast ion and electron transfer.Nanostructured Co3O4 materials attracted significant attention due to their exceptional electrochemical (pseudo-capacitive) properties. However, rigorous preparation conditions are needed to control the size (especially nanosize), morphology and size distribution of the products obtained by conventional methods. Herein, we describe a novel one step shape-controlled synthesis of uniform Co3O4 nanocubes with a size of 50 nm with the existence of mesoporous carbon nanorods (meso-CNRs). In this synthesis process, meso-CNRs not only act as a heat receiver to directly obtain Co3O4 eliminating the high-temperature post-calcination, but also control the morphology of the resulting Co3O4 to form nanocubes with uniform distribution. More strikingly, mesoporous Co3O4 nanocubes are obtained by further thermal treatment. The structure and morphology of the samples were characterized by scanning electron microscopy, transmission electron microscopy and X-ray diffraction. A possible formation mechanism of mesoporous Co3O4 nanocubes is proposed here. Electrochemical tests have revealed that the prepared mesoporous Co3O4 nanocubes demonstrate a remarkable performance in supercapacitor applications due to the porous structure, which endows fast ion and electron transfer. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr00495c

Solar-assisted synthesis of ZnO nanoparticles using lime juice: a green approach

NASA Astrophysics Data System (ADS)

Hinge, Shruti P.; Pandit, Aniruddha B.

2017-12-01

Zinc oxide (ZnO) nanoparticles are those nanoparticles which have been synthesized in various morphologies and shapes. Their size and shape dependent properties and their applications in vivid sectors of science and technology make them interesting to synthesize. Present work reports a green method for ZnO nanoparticle synthesis using lime juice and sunlight. ZnO nanoparticles were also synthesized by conventionally used methods like heating, stirring or no heating and/or stirring. The nanoparticles were characterized using different techniques like UV-vis spectroscopy, scanning electron microscopy (SEM), x-ray diffraction (XRD) and dynamic light scattering (DLS). Thermo gravimetric analysis (TGA) was also carried out for the intermediate product to select the calcination temperature. Stoichiometric study reveals that the intermediate product formed is zinc citrate dihydrate. The synthesized calcined nanoparticles have good crystallinity, uniform shape, and high purity and were in the size range of 20-30 nm. These nanoparticles formed agglomerates of various shapes in the size range of 200-750 nm. This process is ecofriendly and is amiable for easy scale up.

A Generalizable Top-Down Nanostructuring Method of Bulk Oxides: Sequential Oxygen-Nitrogen Exchange Reaction.

PubMed

Lee, Lanlee; Kang, Byungwuk; Han, Suyoung; Kim, Hee-Eun; Lee, Moo Dong; Bang, Jin Ho

2018-05-27

A thermal reaction route that induces grain fracture instead of grain growth is devised and developed as a top-down approach to prepare nanostructured oxides from bulk solids. This novel synthesis approach, referred to as the sequential oxygen-nitrogen exchange (SONE) reaction, exploits the reversible anion exchange between oxygen and nitrogen in oxides that is driven by a simple two-step thermal treatment in ammonia and air. Internal stress developed by significant structural rearrangement via the formation of (oxy)nitride and the creation of oxygen vacancies and their subsequent combination into nanopores transforms bulk solid oxides into nanostructured oxides. The SONE reaction can be applicable to most transition metal oxides, and when utilized in a lithium-ion battery, the produced nanostructured materials are superior to their bulk counterparts and even comparable to those produced by conventional bottom-up approaches. Given its simplicity and scalability, this synthesis method could open a new avenue to the development of high-performance nanostructured electrode materials that can meet the industrial demand of cost-effectiveness for mass production. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Sulfur, selenium and tellurium pseudopeptides: synthesis and biological evaluation.

PubMed

Shaaban, Saad; Sasse, Florenz; Burkholz, Torsten; Jacob, Claus

2014-07-15

A new series of sulfur, selenium and tellurium peptidomimetic compounds was prepared employing the Passerini and Ugi isocyanide based multicomponent reactions (IMCRs). These reactions were clearly superior to conventional methods traditionally used for organoselenium and organotellurium synthesis, such as classical nucleophilic substitution and coupling methods. From the biological point of view, these compounds are of considerable interest because of suspected anticancer and antimicrobial activities. While the sulfur and selenium containing compounds generally did not show either anticancer or antimicrobial activities, their tellurium based counterparts frequently exhibited antimicrobial activity and were also cytotoxic. Some of the compounds synthesized even showed selective activity against certain cancer cells in cell culture. These compounds induced a cell cycle delay in the G0/G1 phase. At closer inspection, the ER and the actin cytoskeleton appeared to be the primary cellular targets of these tellurium compounds, in line with some of our previous studies. As most of these peptidomimetic compounds also comply with Lipinski's Rule of Five, they promise good bioavailability, which needs to be studied as part of future investigations. Copyright © 2014 Elsevier Ltd. All rights reserved.

Low cost hydrogen/novel membrane technology for hydrogen separation from synthesis gas

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

Not Available

1986-02-01

To make the coal-to-hydrogen route economically attractive, improvements are being sought in each step of the process: coal gasification, water-carbon monoxide shift reaction, and hydrogen separation. This report addresses the use of membranes in the hydrogen separation step. The separation of hydrogen from synthesis gas is a major cost element in the manufacture of hydrogen from coal. Separation by membranes is an attractive, new, and still largely unexplored approach to the problem. Membrane processes are inherently simple and efficient and often have lower capital and operating costs than conventional processes. In this report current ad future trends in hydrogen productionmore » and use are first summarized. Methods of producing hydrogen from coal are then discussed, with particular emphasis on the Texaco entrained flow gasifier and on current methods of separating hydrogen from this gas stream. The potential for membrane separations in the process is then examined. In particular, the use of membranes for H{sub 2}/CO{sub 2}, H{sub 2}/CO, and H{sub 2}/N{sub 2} separations is discussed. 43 refs., 14 figs., 6 tabs.« less

Synthesis and magnetic properties of cobalt-iron/cobalt-ferrite soft/hard magnetic core/shell nanowires

NASA Astrophysics Data System (ADS)

Leandro Londoño-Calderón, César; Moscoso-Londoño, Oscar; Muraca, Diego; Arzuza, Luis; Carvalho, Peterson; Pirota, Kleber Roberto; Knobel, Marcelo; Pampillo, Laura Gabriela; Martínez-García, Ricardo

2017-06-01

A straightforward method for the synthesis of CoFe2.7/CoFe2O4 core/shell nanowires is described. The proposed method starts with a conventional pulsed electrodeposition procedure on alumina nanoporous template. The obtained CoFe2.7 nanowires are released from the template and allowed to oxidize at room conditions over several weeks. The effects of partial oxidation on the structural and magnetic properties were studied by x-ray spectrometry, magnetometry, and scanning and transmission electron microscopy. The results indicate that the final nanowires are composed of 5 nm iron-cobalt alloy nanoparticles. Releasing the nanowires at room conditions promoted surface oxidation of the nanoparticles and created a CoFe2O4 shell spinel-like structure. The shell avoids internal oxidation and promotes the formation of bi-magnetic soft/hard magnetic core/shell nanowires. The magnetic properties of both the initial single-phase CoFe2.7 nanowires and the final core/shell nanowires, reveal that the changes in the properties from the array are due to the oxidation more than effects associated with released processes (disorder and agglomeration).

Synthesis and magnetic properties of cobalt-iron/cobalt-ferrite soft/hard magnetic core/shell nanowires.

PubMed

Londoño-Calderón, César Leandro; Moscoso-Londoño, Oscar; Muraca, Diego; Arzuza, Luis; Carvalho, Peterson; Pirota, Kleber Roberto; Knobel, Marcelo; Pampillo, Laura Gabriela; Martínez-García, Ricardo

2017-06-16

A straightforward method for the synthesis of CoFe 2.7 /CoFe 2 O 4 core/shell nanowires is described. The proposed method starts with a conventional pulsed electrodeposition procedure on alumina nanoporous template. The obtained CoFe 2.7 nanowires are released from the template and allowed to oxidize at room conditions over several weeks. The effects of partial oxidation on the structural and magnetic properties were studied by x-ray spectrometry, magnetometry, and scanning and transmission electron microscopy. The results indicate that the final nanowires are composed of 5 nm iron-cobalt alloy nanoparticles. Releasing the nanowires at room conditions promoted surface oxidation of the nanoparticles and created a CoFe 2 O 4 shell spinel-like structure. The shell avoids internal oxidation and promotes the formation of bi-magnetic soft/hard magnetic core/shell nanowires. The magnetic properties of both the initial single-phase CoFe 2.7 nanowires and the final core/shell nanowires, reveal that the changes in the properties from the array are due to the oxidation more than effects associated with released processes (disorder and agglomeration).

Synthesis and characterization of nanocrystalline mesoporous zirconia using supercritical drying.

PubMed

Tyagi, Beena; Sidhpuria, Kalpesh; Shaik, Basha; Jasra, Raksh Vir

2006-06-01

Synthesis of nano-crystalline zirconia aerogel was done by sol-gel technique and supercritical drying using n-propanol solvent at and above supercritical temperature (235-280 degrees C) and pressure (48-52 bar) of n-propanol. Zirconia xerogel samples have also been prepared by conventional thermal drying method to compare with the super critically dried samples. Crystalline phase, crystallite size, surface area, pore volume, and pore size distribution were determined for all the samples in detail to understand the effect of gel drying methods on these properties. Supercritical drying of zirconia gel was observed to give thermally stable, nano-crystalline, tetragonal zirconia aerogels having high specific surface area and porosity with narrow and uniform pore size distribution as compared to thermally dried zirconia. With supercritical drying, zirconia samples show the formation of only mesopores whereas in thermally dried samples, substantial amount of micropores are observed along with mesopores. The samples prepared using supercritical drying yield nano-crystalline zirconia with smaller crystallite size (4-6 nm) as compared to higher crystallite size (13-20 nm) observed with thermally dried zirconia.

A generalized method for high throughput in-situ experiment data analysis: An example of battery materials exploration

NASA Astrophysics Data System (ADS)

Aoun, Bachir; Yu, Cun; Fan, Longlong; Chen, Zonghai; Amine, Khalil; Ren, Yang

2015-04-01

A generalized method is introduced to extract critical information from series of ranked correlated data. The method is generally applicable to all types of spectra evolving as a function of any arbitrary parameter. This approach is based on correlation functions and statistical scedasticity formalism. Numerous challenges in analyzing high throughput experimental data can be tackled using the herein proposed method. We applied this method to understand the reactivity pathway and formation mechanism of a Li-ion battery cathode material during high temperature synthesis using in-situ high-energy X-ray diffraction. We demonstrate that Pearson's correlation function can easily unravel all major phase transition and, more importantly, the minor structural changes which cannot be revealed by conventionally inspecting the series of diffraction patterns. Furthermore, a two-dimensional (2D) reactivity pattern calculated as the scedasticity along all measured reciprocal space of all successive diffraction pattern pairs unveils clearly the structural evolution path and the active areas of interest during the synthesis. The methods described here can be readily used for on-the-fly data analysis during various in-situ operando experiments in order to quickly evaluate and optimize experimental conditions, as well as for post data analysis and large data mining where considerable amount of data hinders the feasibility of the investigation through point-by-point inspection.

A generalized method for high throughput in-situ experiment data analysis: An example of battery materials exploration

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

Aoun, Bachir; Yu, Cun; Fan, Longlong

A generalized method is introduced to extract critical information from series of ranked correlated data. The method is generally applicable to all types of spectra evolving as a function of any arbitrary parameter. This approach is based on correlation functions and statistical scedasticity formalism. Numerous challenges in analyzing high throughput experimental data can be tackled using the herein proposed method. We applied this method to understand the reactivity pathway and formation mechanism of a Li-ion battery cathode material during high temperature synthesis using in-situ highenergy X-ray diffraction. We demonstrate that Pearson's correlation function can easily unravel all major phase transitionmore » and, more importantly, the minor structural changes which cannot be revealed by conventionally inspecting the series of diffraction patterns. Furthermore, a two-dimensional (2D) reactivity pattern calculated as the scedasticity along all measured reciprocal space of all successive diffraction pattern pairs unveils clearly the structural evolution path and the active areas of interest during the synthesis. The methods described here can be readily used for on-the-fly data analysis during various in-situ operando experiments in order to quickly evaluate and optimize experimental conditions, as well as for post data analysis and large data mining where considerable amount of data hinders the feasibility of the investigation through point-by-point inspection.« less

A review on plants extract mediated synthesis of silver nanoparticles for antimicrobial applications: A green expertise

PubMed Central

Ahmed, Shakeel; Ahmad, Mudasir; Swami, Babu Lal; Ikram, Saiqa

2015-01-01

Metallic nanoparticles are being utilized in every phase of science along with engineering including medical fields and are still charming the scientists to explore new dimensions for their respective worth which is generally attributed to their corresponding small sizes. The up-and-coming researches have proven their antimicrobial significance. Among several noble metal nanoparticles, silver nanoparticles have attained a special focus. Conventionally silver nanoparticles are synthesized by chemical method using chemicals as reducing agents which later on become accountable for various biological risks due to their general toxicity; engendering the serious concern to develop environment friendly processes. Thus, to solve the objective; biological approaches are coming up to fill the void; for instance green syntheses using biological molecules derived from plant sources in the form of extracts exhibiting superiority over chemical and/or biological methods. These plant based biological molecules undergo highly controlled assembly for making them suitable for the metal nanoparticle syntheses. The present review explores the huge plant diversity to be utilized towards rapid and single step protocol preparatory method with green principles over the conventional ones and describes the antimicrobial activities of silver nanoparticles. PMID:26843966

Application of Palladium-Mediated 18F-Fluorination to PET Radiotracer Development: Overcoming Hurdles to Translation

PubMed Central

Kamlet, Adam S.; Neumann, Constanze N.; Lee, Eunsung; Carlin, Stephen M.; Moseley, Christian K.; Stephenson, Nickeisha; Hooker, Jacob M.; Ritter, Tobias

2013-01-01

New chemistry methods for the synthesis of radiolabeled small molecules have the potential to impact clinical positron emission tomography (PET) imaging, if they can be successfully translated. However, progression of modern reactions from the stage of synthetic chemistry development to the preparation of radiotracer doses ready for use in human PET imaging is challenging and rare. Here we describe the process of and the successful translation of a modern palladium-mediated fluorination reaction to non-human primate (NHP) baboon PET imaging–an important milestone on the path to human PET imaging. The method, which transforms [18F]fluoride into an electrophilic fluorination reagent, provides access to aryl–18F bonds that would be challenging to synthesize via conventional radiochemistry methods. PMID:23554994

Ultrasound assisted co-precipitation of nanostructured CuO-ZnO-Al2O3 over HZSM-5: effect of precursor and irradiation power on nanocatalyst properties and catalytic performance for direct syngas to DME.

PubMed

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

2014-03-01

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

A simple and cost-effective molecular diagnostic system and DNA probes synthesized by light emitting diode photolithography

NASA Astrophysics Data System (ADS)

Oleksandrov, Sergiy; Kwon, Jung Ho; Lee, Ki-chang; Sujin-Ku; Paek, Mun Cheol

2014-09-01

This work introduces a novel chip to be used in the future as a simple and cost-effective method for creating DNA arrays using light emission diode (LED) photolithography. The DNA chip platform contains 24 independent reaction sites, which allows for the testing of a corresponding amount of patients' samples in hospital. An array of commercial UV LEDs and lens systems was combined with a microfluidic flow system to provide patterning of 24 individual reaction sites, each with 64 independent probes. Using the LED array instead of conventional laser exposure systems or micro-mirror systems significantly reduces the cost of equipment. The microfluidic system together with microfluidic flow cells drastically reduces the amount of used reagents, which is important due to the high cost of commercial reagents. The DNA synthesis efficiency was verified by fluorescence labeling and conventional hybridization.

Zero-dimensional to three-dimensional nanojoining: current status and potential applications

DOE PAGES

Ma, Ying; Li, Hong; Bridges, Denzel; ...

2016-08-01

We report that the continuing miniaturization of microelectronics is pushing advanced manufacturing into nanomanufacturing. Nanojoining is a bottom-up assembly technique that enables functional nanodevice fabrication with dissimilar nanoscopic building blocks and/or molecular components. Various conventional joining techniques have been modified and re-invented for joining nanomaterials. Our review surveys recent progress in nanojoining methods, as compared to conventional joining processes. Examples of nanojoining are given and classified by the dimensionality of the joining materials. At each classification, nanojoining is reviewed and discussed according to materials specialties, low dimensional processing features, energy input mechanisms and potential applications. The preparation of new intermetallicmore » materials by reactive nanoscale multilayer foils based on self-propagating high-temperature synthesis is highlighted. This review will provide insight into nanojoining fundamentals and innovative applications in power electronics packaging, plasmonic devices, nanosoldering for printable electronics, 3D printing and space manufacturing.« less

Suppression of copper thin film loss during graphene synthesis.

PubMed

Lee, Alvin L; Tao, Li; Akinwande, Deji

2015-01-28

Thin metal films can be used to catalyze the growth of nanomaterials in place of the bulk metal, while greatly reducing the amount of material used. A big drawback of copper thin films (0.5-1.5 μm thick) is that, under high temperature/vacuum synthesis, the mass loss of films severely reduces the process time due to discontinuities in the metal film, thereby limiting the time scale for controlling metal grain and film growth. In this work, we have developed a facile method, namely "covered growth" to extend the time copper thin films can be exposed to high temperature/vacuum environment for graphene synthesis. The key to preventing severe mass loss of copper film during the high temperature chemical vapor deposition (CVD) process is to have a cover piece on top of the growth substrate. This new "covered growth" method enables the high-temperature annealing of the copper film upward of 4 h with minimal mass loss, while increasing copper film grain and graphene domain size. Graphene was then successfully grown on the capped copper film with subsequent transfer for device fabrication. Device characterization indicated equivalent physical, chemical, and electrical properties to conventional CVD graphene. Our "covered growth" provides a convenient and effective solution to the mass loss issue of thin films that serve as catalysts for a variety of 2D material syntheses.

Phytosynthesis of intracellular and extracellular gold nanoparticles by living peanut plant (Arachis hypogaea L.).

PubMed

Raju, Dugyala; Mehta, Urmil J; Ahmad, Absar

2012-01-01

Inorganic nanomaterials of different chemical compositions are conventionally synthesized under harsh environments such as extremes of temperature, pressure, and pH. Moreover, these methods are eco-unfriendly and cumbersome, yield bigger particles, and agglomerate because of not being capped by capping agents. In contrast, biological synthesis of inorganic nanomaterials occurs under ambient conditions, namely room temperature, atmospheric pressure, and physiological pH. These methods are reliable, eco-friendly, and cheap. In this paper, we report for the first time the extracellular and intracellular synthesis of gold nanoparticles (GNPs) using living peanut seedlings. The formed GNPs were highly stable in solution and inside the plant tissue. Transmission electron microscopy revealed that extracellular GNPs distributions were in the form of monodispersed nanoparticles. The nanoparticles ranged from 4 to 6 nm in size. The intercellular nanoparticles were of oval shape and size ranged from 5 to 50 nm. Both extracellular and intracellular nanoparticles were further characterized by standard techniques. The formed GNPs inside the plant tissue were estimated by inductively coupled plasma spectrometry. This opens up an exciting possibility of a plant-based nanoparticle synthesis strategy, wherein the nanoparticles may be entrapped in the biomass in the form of a film or produced in the solution, both of which have interesting applications. © 2012 International Union of Biochemistry and Molecular Biology, Inc.

Self-ligating versus conventional metallic brackets on Streptococcus mutans retention: A systematic review

PubMed Central

Longoni, Juliano N.; Lopes, Beatriz M.; Freires, Irlan A.; Dutra, Kamile L.; Franco, Ademir; Paranhos, Luiz R.

2017-01-01

Objective: The present study aimed to review the literature systematically and assess comparatively whether self-ligating metallic brackets accumulate less Streptococcus mutans biofilm than conventional metallic brackets. Material and methods: The systematic search was performed following PRISMA guidelines and registration in PROSPERO. Seven electronic databases (Google Scholar, LILACS, Open Grey, PubMed, SciELO, ScienceDirect, and Scopus) were consulted until April 2016, with no restriction of language and time of publication. Only randomized clinical studies verifying S. mutans colonization in metallic brackets (self-ligating and conventional) were included. All steps were performed independently by two operators. Results: The search resulted in 546 records obtained from the electronic databases. Additionally, 216 references obtained from the manual search of eligible articles were assessed. Finally, a total of 5 studies were included in the qualitative synthesis. In 1 study, the total bacterial count was not different among self-ligating and conventional brackets, whereas in 2 studies the amount was lower for self-ligating brackets. Regarding the specific count of S. mutans, 2 studies showed less accumulation in self-ligating than in conventional brackets. Conclusion: Based on the limited evidence, self-ligating metallic brackets accumulate less S. mutans than conventional ones. However, these findings must be interpreted in conjunction with particularities individual for each patient – such as hygiene and dietary habits, which are components of the multifactorial environment that enables S. Mutans to proliferate and keep retained in the oral cavity. PMID:29279684

Rapid crystallization and morphological adjustment of zeolite ZSM-5 in nonionic emulsions

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

Zhang Ying, E-mail: yingzh1977@163.co; Jin Chao; Research Institute of Petroleum Processing, Beijing 100083

2011-01-15

Zeolite ZSM-5 was synthesized for the first time in a nonionic emulsion composed of polyoxyethylated alkylphenol, butanol, cyclohexane and tetraethylammonium hydroxide (TEAOH)-containing zeolite synthesis mixture. The crystallization kinetics in the emulsion was investigated and the ZSM-5 product was characterized in detail by XRD, SEM, FT-IR, TG, N{sub 2} adsorption and CHN analysis techniques. Compared with the conventionally hydrothermal synthesis with the same structure directing agent TEAOH, the emulsion system allows rapid crystallization of ZSM-5. The ZSM-5 product exhibits unusual agglomerated structure and possesses larger specific surface area. The FT-IR, TG results plus CHN analysis show the encapsulation of a tracemore » of emulsion components in the emulsion ZSM-5. Control experiments show the emulsion system exerts the crystallization induction and morphological adjustment effects mainly during the aging period. The effects are tentatively attributed to the confined space domains, surfactant-water interaction as well as surfactant-growing crystals interaction existing in the emulsion. -- Graphical abstract: The nonionic emulsion synthesis allows rapid crystallization and morphological adjustment of zeolite ZSM-5 compared with the conventional hydrothermal synthesis. Display Omitted« less

Unveiling the mystery of mitochondrial DNA replication in yeasts.

PubMed

Chen, Xin Jie; Clark-Walker, George Desmond

2018-01-01

Conventional DNA replication is initiated from specific origins and requires the synthesis of RNA primers for both the leading and lagging strands. In contrast, the replication of yeast mitochondrial DNA is origin-independent. The replication of the leading strand is likely primed by recombinational structures and proceeded by a rolling circle mechanism. The coexistent linear and circular DNA conformers facilitate the recombination-based initiation. The replication of the lagging strand is poorly understood. Re-evaluation of published data suggests that the rolling circle may also provide structures for the synthesis of the lagging-strand by mechanisms such as template switching. Thus, the coupling of recombination with rolling circle replication and possibly, template switching, may have been selected as an economic replication mode to accommodate the reductive evolution of mitochondria. Such a replication mode spares the need for conventional replicative components, including those required for origin recognition/remodelling, RNA primer synthesis and lagging-strand processing. Copyright © 2017 Elsevier B.V. and Mitochondria Research Society. All rights reserved.

Selection of Lipases for the Synthesis of Biodiesel from Jatropha Oil and the Potential of Microwave Irradiation to Enhance the Reaction Rate

PubMed Central

2016-01-01

The present study deals with the enzymatic synthesis of biodiesel by transesterification of Jatropha oil (Jatropha curcas L.) with ethanol in a solvent-free system. Seven commercial lipase preparations immobilized by covalent attachment on epoxy-polysiloxane-polyvinyl alcohol composite (epoxy-SiO2-PVA) were tested as biocatalysts. Among them, immobilized lipases from Pseudomonas fluorescens (lipase AK) and Burkholderia cepacia (lipase PS) were the most active biocatalysts in biodiesel synthesis, reaching ethyl ester yields (FAEE) of 91.1 and 98.3% at 72 h of reaction, respectively. The latter biocatalyst exhibited similar performance compared to Novozym® 435. Purified biodiesel was characterized by different techniques. Transesterification reaction carried out under microwave irradiation exhibited higher yield and productivity than conventional heating. The operational stability of immobilized lipase PS was determined in repeated batch runs under conventional and microwave heating systems, revealing half-life times of 430.4 h and 23.5 h, respectively. PMID:27868060

A simple single-step approach towards synthesis of nanofluids containing cuboctahedral cuprous oxide particles using glucose reduction

NASA Astrophysics Data System (ADS)

Shenoy, U. Sandhya; Shetty, A. Nityananda

2018-03-01

Enhancement of thermal properties of conventional heat transfer fluids has become one of the important technical challenges. Since nanofluids offer a promising help in this regard, development of simpler and hassle free routes for their synthesis is of utmost importance. Synthesis of nanofluids using a hassle free route with greener chemicals has been reported. The single-step chemical approach reported here overcomes the drawbacks of the two-step procedures in the synthesis of nanofluids. The resulting Newtonian nanofluids prepared contained cuboctahedral particles of cuprous oxide and exhibited a thermal conductivity of 2.852 W·m-1·K-1. Polyvinylpyrrolidone (PVP) used during the synthesis acted as a stabilizing agent rendering the nanofluid a stability of 9 weeks.

Microwave Assisted Synthesis of Biorelevant Benzazoles.

PubMed

Seth, Kapileswar; Purohit, Priyank; Chakraborti, Asit K

2017-01-01

The benzazole scaffolds are present in various therapeutic agents and have been recognized as the essential pharmacophore for diverse biological activities. These have generated interest and necessity to develop efficient synthetic methods of these privileged classes of compounds to generate new therapeutic leads for various diseases. The biological activities of the benzazoles and efforts towards their synthesis have been summarized in a few review articles. In view of these, the aim of this review is to provide an account of the developments that have taken place in the synthesis of biorelevant benzazoles under microwave irradiation as the application of microwave heating has long been recognized as a green chemistry tool for speedy generation of synthetic targets. Attention has been focused to those literature reports wherein the use of microwave irradiation is the key step in the formation of the heterocyclic ring system or in functionalization of the benzazole ring system to generate the essential pharmacophoric feature. The convenient and economic way to synthesize these privileged class of heterocycles through the use of microwave irradiation that would be beneficial for the drug discovery scientist to synthesize biologically active benzazoles and provide access to wide range of reactions for the synthesis of benzazoles constitute the theme of this review. Examples have been drawn wherein the use of microwave heating offers distinct advantage in terms of improved product yields and reduction of reaction time as compared to those observed for the synthesis under conventional heating. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Ecobody technology: rapid monoclonal antibody screening method from single B cells using cell-free protein synthesis for antigen-binding fragment formation.

PubMed

Ojima-Kato, Teruyo; Nagai, Satomi; Nakano, Hideo

2017-10-25

We report a rapid and cost-effective monoclonal antibody screening method from single animal B cells using reverse transcription (RT)-PCR and Escherichia coli cell-free protein synthesis (CFPS), which allows evaluation of antibodies within 2 working days. This process is named "Ecobody technology". The method includes strategies to isolate B cells that specifically bind an antigen from the peripheral blood of immunised animals, and single-cell RT-PCR to generate DNA fragments of the V H and V L genes, followed by CFPS for production of fragments of antigen binding (Fab). In the CFPS step, we employed our techniques: 1) 'Zipbody' as a method for producing Fab, in which the association of heavy and light chains is facilitated by adhesive leucine zipper peptides fused at the C-termini of the Fab; and 2) an N-terminal SKIK peptide tag that can increase protein expression levels. Using Ecobody technology, we obtained highly-specific monoclonal antibodies for the antigens Vibrio parahaemolyticus and E. coli O26. The anti-V. parahaemolyticus Zipbody mAb was further produced in E. coli strain SHuffle T7 Express in inclusion bodies and refolded by a conventional method, resulting in significant antigen-binding activity (K D  = 469 pM) and productivity of 8.5 mg purified antibody/L-culture.

Virtual interface substructure synthesis method for normal mode analysis of super-large molecular complexes at atomic resolution.

PubMed

Chen, Xuehui; Sun, Yunxiang; An, Xiongbo; Ming, Dengming

2011-10-14

Normal mode analysis of large biomolecular complexes at atomic resolution remains challenging in computational structure biology due to the requirement of large amount of memory space and central processing unit time. In this paper, we present a method called virtual interface substructure synthesis method or VISSM to calculate approximate normal modes of large biomolecular complexes at atomic resolution. VISSM introduces the subunit interfaces as independent substructures that join contacting molecules so as to keep the integrity of the system. Compared with other approximate methods, VISSM delivers atomic modes with no need of a coarse-graining-then-projection procedure. The method was examined for 54 protein-complexes with the conventional all-atom normal mode analysis using CHARMM simulation program and the overlap of the first 100 low-frequency modes is greater than 0.7 for 49 complexes, indicating its accuracy and reliability. We then applied VISSM to the satellite panicum mosaic virus (SPMV, 78,300 atoms) and to F-actin filament structures of up to 39-mer, 228,813 atoms and found that VISSM calculations capture functionally important conformational changes accessible to these structures at atomic resolution. Our results support the idea that the dynamics of a large biomolecular complex might be understood based on the motions of its component subunits and the way in which subunits bind one another. © 2011 American Institute of Physics

Multiphase organic synthesis in microchannel reactors.

PubMed

Kobayashi, Juta; Mori, Yuichiro; Kobayashi, Shū

2006-07-17

"Miniaturization" is one of the most important aspects in today's technology. Organic chemistry is no exception. The search for highly effective, controllable, environmentally friendly methods for preparing products is of prime importance. The development of multiphase organic reactions in microchannel reactors has gained significant importance in recent years to allow novel reactivity, and has led to many fruitful results that are not attainable in conventional reactors. This Focus Review aims to shed light on how effectively multiphase organic reactions can be conducted with microchannel reactors by providing examples of recent remarkable studies, which have been grouped on the basis of the phases involved.

Nucleic acid amplification using modular branched primers

DOEpatents

Ulanovsky, Levy; Raja, Mugasimangalam C.

2001-01-01

Methods and compositions expand the options for making primers for use in amplifying nucleic acid segments. The invention eliminates the step of custom synthesis of primers for Polymerase Chain Reactions (PCR). Instead of being custom-synthesized, a primer is replaced by a combination of several oligonucleotide modules selected from a pre-synthesized library. A modular combination of just a few oligonucleotides essentially mimics the performance of a conventional, custom-made primer by matching the sequence of the priming site in the template. Each oligonucleotide module has a segment that matches one of the stretches within the priming site.

Palladium-catalyzed hydroaminocarbonylation of alkenes with amines: a strategy to overcome the basicity barrier imparted by aliphatic amines.

PubMed

Zhang, Guoying; Gao, Bao; Huang, Hanmin

2015-06-22

A novel and efficient palladium-catalyzed hydroaminocarbonylation of alkenes with aminals has been developed under mild reaction conditions, and allows the synthesis of a wide range of N-alkyl linear amides in good yields with high regioselectivity. On the basis of this method, a cooperative catalytic system operating by the synergistic combination of palladium, paraformaldehyde, and acid was established for promoting the hydroaminocarbonylation of alkenes with both aromatic and aliphatic amines, which do not react well under conventional palladium-catalyzed hydroaminocarbonylation. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Sensory and metabolic profiles of "Fuji" apples (Malus domestica Borkh.) grown without synthetic agrochemicals: the role of ethylene production.

PubMed

Tanaka, Fukuyo; Miyazawa, Toshio; Okazaki, Keiki; Tatsuki, Miho; Ito, Tsutae

2015-01-01

Flavors of "Fuji" apple cultivated with or without synthetic agrochemicals were compared using quantitative descriptive analyses (QDA) and metabolite profiling for 3 seasons. Experimental plots included conventional crops (with agrochemicals) and organic crops (without agrochemicals) at our institute and organic and conventional farms. Additionally, mass market samples were analyzed. Organic apples were weak in sweetness and floral characteristics and had enhanced green and sour flavors. Most esters and sugars were present in lower concentrations in organic than in conventional apples. Close relation of principal component 1 of QDA and metabolite profiles, to ethylene production suggested that ethylene is considerably involved in flavor synthesis. Reduced ethylene associated with immaturity accounted for insufficient flavor synthesis and weak aroma and flavor attributes of organic apples. Furthermore, organic apples from the farm were more flavorsome than those from the institute in 2012, suggesting possible recovery of ethylene production after a long organic cultivation period.

Sodium hydroxide catalyzed monodispersed high surface area silica nanoparticles.

PubMed

Bhakta, Snehasis; Dixit, Chandra K; Bist, Itti; Jalil, Karim Abdel; Suib, Steven L; Rusling, James F

2016-07-01

Understanding of the synthesis kinetics and our ability to modulate medium conditions allowed us to generate nanoparticles via an ultra-fast process. The synthesis medium is kept quite simple with tetraethyl orthosilicate (TEOS) as precursor and 50% ethanol and sodium hydroxide catalyst. Synthesis is performed under gentle conditions at 20 °C for 20 min Long synthesis time and catalyst-associated drawbacks are most crucial in silica nanoparticle synthesis. We have addressed both these bottlenecks by replacing the conventional Stober catalyst, ammonium hydroxide, with sodium hydroxide. We have reduced the overall synthesis time from 20 to 1/3 h, ~60-fold decrease, and obtained highly monodispersed nanoparticles with 5-fold higher surface area than Stober particles. We have demonstrated that the developed NPs with ~3-fold higher silane can be used as efficient probes for biosensor applications.

Micelle-templated, poly(lactic-co-glycolic acid) nanoparticles for hydrophobic drug delivery.

PubMed

Nabar, Gauri M; Mahajan, Kalpesh D; Calhoun, Mark A; Duong, Anthony D; Souva, Matthew S; Xu, Jihong; Czeisler, Catherine; Puduvalli, Vinay K; Otero, José Javier; Wyslouzil, Barbara E; Winter, Jessica O

2018-01-01

Poly(lactic- co -glycolic acid) (PLGA) is widely used for drug delivery because of its biocompatibility, ability to solubilize a wide variety of drugs, and tunable degradation. However, achieving sub-100 nm nanoparticles (NPs), as might be desired for delivery via the enhanced permeability and retention effect, is extremely difficult via typical top-down emulsion approaches. Here, we present a bottom-up synthesis method yielding PLGA/block copolymer hybrids (ie, "PolyDots"), consisting of hydrophobic PLGA chains entrapped within self-assembling poly(styrene- b -ethylene oxide) (PS- b -PEO) micelles. PolyDots exhibit average diameters <50 nm and lower polydispersity than conventional PLGA NPs. Drug encapsulation efficiencies of PolyDots match conventional PLGA NPs (ie, ~30%) and are greater than those obtained from PS- b -PEO micelles (ie, ~7%). Increasing the PLGA:PS- b -PEO weight ratio alters the drug release mechanism from chain relaxation to erosion controlled. PolyDots are taken up by model glioma cells via endocytotic mechanisms within 24 hours, providing a potential means for delivery to cytoplasm. PolyDots can be lyophilized with minimal change in morphology and encapsulant functionality, and can be produced at scale using electrospray. Encapsulation of PLGA within micelles provides a bottom-up route for the synthesis of sub-100 nm PLGA-based nanocarriers with enhanced stability and drug-loading capacity, and tunable drug release, suitable for potential clinical applications.

3' rapid amplification of cDNA ends (RACE) walking for rapid structural analysis of large transcripts.

PubMed

Ozawa, Tatsuhiko; Kondo, Masato; Isobe, Masaharu

2004-01-01

The 3' rapid amplification of cDNA ends (3' RACE) is widely used to isolate the cDNA of unknown 3' flanking sequences. However, the conventional 3' RACE often fails to amplify cDNA from a large transcript if there is a long distance between the 5' gene-specific primer and poly(A) stretch, since the conventional 3' RACE utilizes 3' oligo-dT-containing primer complementary to the poly(A) tail of mRNA at the first strand cDNA synthesis. To overcome this problem, we have developed an improved 3' RACE method suitable for the isolation of cDNA derived from very large transcripts. By using the oligonucleotide-containing random 9mer together with the GC-rich sequence for the suppression PCR technology at the first strand of cDNA synthesis, we have been able to amplify the cDNA from a very large transcript, such as the microtubule-actin crosslinking factor 1 (MACF1) gene, which codes a transcript of 20 kb in size. When there is no splicing variant, our highly specific amplification allows us to perform the direct sequencing of 3' RACE products without requiring cloning in bacterial hosts. Thus, this stepwise 3' RACE walking will help rapid characterization of the 3' structure of a gene, even when it encodes a very large transcript.

Applying reliability analysis to design electric power systems for More-electric aircraft

NASA Astrophysics Data System (ADS)

Zhang, Baozhu

The More-Electric Aircraft (MEA) is a type of aircraft that replaces conventional hydraulic and pneumatic systems with electrically powered components. These changes have significantly challenged the aircraft electric power system design. This thesis investigates how reliability analysis can be applied to automatically generate system topologies for the MEA electric power system. We first use a traditional method of reliability block diagrams to analyze the reliability level on different system topologies. We next propose a new methodology in which system topologies, constrained by a set reliability level, are automatically generated. The path-set method is used for analysis. Finally, we interface these sets of system topologies with control synthesis tools to automatically create correct-by-construction control logic for the electric power system.

Two-Dimensional Self-Assembly and Chemical Synthesis of Charged Gold Nanoparticles in Non-Polar Solvents

NASA Astrophysics Data System (ADS)

Martin, Matthew Nichols

Gold nanoparticles between 1 and 10 nm in diameter exhibit size-dependent electronic and optical properties that cannot be explained by molecular science and which deviate significantly from their bulk counterparts. For example, the melting temperature of gold nanoparticles less than 5 nm in diameter is around 300 °C [1], whereas bulk gold melts at over 1000 °C [2]. Gold nanoparticles require precise control over particle diameter in order to exploit and tailor their unique properties; however, tuning the size reproducibly and predictably has proved to be a challenge. One of the most difficult obstacles to overcome is nanoparticle aggregation, since nanoparticles flocculate at room temperature quite readily. In 1994, Brust et al. solved the aggregation problem by introducing monolayer protection coatings on gold nanoparticles, in which organic ligand molecules are attached to the nanoparticle surface and create a physical barrier between the gold core and solvent. This was a definitive solution to size stability, since nanoparticles never aggregate, however the synthesis method does not generate monodisperse nanoparticles and has poor size-tuning capabilities. We developed a synthesis method for gold nanoparticles that improves greatly upon the Brust method. Starting from scratch, we discovered a "sweet zone" for aqueous gold nanoparticles, revealing how to make "naked" (stabilizer-free) gold nanoparticles which are continuously and precisely controlled between 3.2 and 5.2 nm in diameter, both reproducibly and predictably. Naked nanoparticles are then coated with organic 1-dodecanethiol ligand molecules, and transferred to hexane. Since all reaction byproducts remain in the water-phase, no postsynthesis cleaning or size-filtering is necessary, reducing the total synthesis time from ~24 hours in the Brust method, to less than 10 minutes. Surprisingly, our nanoparticles are highly negatively charged in nonpolar solvents. This unexpectedly caused nanoparticles to be unstable in toluene but stable in hexane. Consequently, nanoparticles float to the air-toluene interface, and after evaporation of toluene, form large 2D monolayer films of nanoparticle that are uniform at nanometer, micrometer, and millimeter length scales. This facile 2D self-assembly method also displays extremely size-dependent features in the 3.2 -- 5.2 nm range. Additionally, we managed to expand our synthesis method to include smaller gold nanoparticles. Since small gold clusters less than 2 nm in diameter are exponentially more efficient than other conventional catalysts, we labored to synthesize nanoclusters with diameters less than 2 nm, and fortunately, reduced the synthesis time to 2 minutes. With complete size control of gold nanoparticles between 1 and 5 nm, we have developed a truly novel synthesis method that forms a strong basis for many interesting studies. We have also discovered a novel method for place exchange reactions of organic molecular coatings. Ligand exchange of water-soluble thiols for alkylamines was performed at room temperature and occurred in less than 10 seconds, and allowed for the phase-transfer of nanoparticles from nonpolar solvents back to water. This method is extremely useful for the biological nanoparticle community as they are already using nanoparticles for drug delivery, DNA sensing, and molecular recognition.

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

Das, Atanu Kumar; Vemuri, Rama Sesha; Kutnyakov, Igor

Here, vapor-assisted dry-gel synthesis of MOF-74 structure, specifically NiMOF-74 from its synthetic precursors, was conducted with high yield and improved performance showing promise for gas (CO 2) and water adsorption applications. Unlike conventional synthesis, which takes 72 h, this kinetic study showed that NiMOF-74 forms within 12 h under dry-gel conditions with similar performance characteristics and exhibits the best performance characteristics after 48 h of heating.

Facile and green synthesis of mesoporous Co3O4 nanocubes and their applications for supercapacitors.

PubMed

Liu, Xiangmei; Long, Qing; Jiang, Chunhui; Zhan, Beibei; Li, Chen; Liu, Shujuan; Zhao, Qiang; Huang, Wei; Dong, Xiaochen

2013-07-21

Nanostructured Co3O4 materials attracted significant attention due to their exceptional electrochemical (pseudo-capacitive) properties. However, rigorous preparation conditions are needed to control the size (especially nanosize), morphology and size distribution of the products obtained by conventional methods. Herein, we describe a novel one step shape-controlled synthesis of uniform Co3O4 nanocubes with a size of 50 nm with the existence of mesoporous carbon nanorods (meso-CNRs). In this synthesis process, meso-CNRs not only act as a heat receiver to directly obtain Co3O4 eliminating the high-temperature post-calcination, but also control the morphology of the resulting Co3O4 to form nanocubes with uniform distribution. More strikingly, mesoporous Co3O4 nanocubes are obtained by further thermal treatment. The structure and morphology of the samples were characterized by scanning electron microscopy, transmission electron microscopy and X-ray diffraction. A possible formation mechanism of mesoporous Co3O4 nanocubes is proposed here. Electrochemical tests have revealed that the prepared mesoporous Co3O4 nanocubes demonstrate a remarkable performance in supercapacitor applications due to the porous structure, which endows fast ion and electron transfer.

A novel magnetic core-shell nanocomposite Fe3O4@chitosan@ZnO for the green synthesis of 2-benzimidazoles

NASA Astrophysics Data System (ADS)

Tian, Fei; Niu, Libo; Chen, Bo; Gao, Xuejia; Lan, Xingwang; Huo, Li; Bai, Guoyi

2017-10-01

A novel magnetic core-shell nanocomposite Fe3O4@Chitosan@ZnO was successfully prepared by in situ chemical precipitation method. It has a clear core-shell structure with magnetic Fe3O4 (about 160 nm in diameter) as core, chitosan as the inner shell, and ZnO as the outer shell, as demonstrated by the transmission electron microscopy and the related elemental mapping. Moreover, this nanocomposite has high magnetization (43.6 emu g-1) so that it can be easily separated from the reaction mixture within 4 s by an external magnetic field. The introduction of the natural chitosan shell, instead of the conventional SiO2 shell, and its combination with the active ZnO ensures this novel nanocomposite green character and good catalytic performance in the synthesis of 2-benzimidazoles with moderate to excellent isolated yields at room temperature. Notably, it can be recycled seven times without appreciable loss of its initial catalytic activity, demonstrating its good stability and making it an attractive candidate for the green synthesis of 2-benzimidazoles. [Figure not available: see fulltext.

A General Method for the Chemical Synthesis of Large-Scale, Seamless Transition Metal Dichalcogenide Electronics.

PubMed

Li, Li; Guo, Yichuan; Sun, Yuping; Yang, Long; Qin, Liang; Guan, Shouliang; Wang, Jinfen; Qiu, Xiaohui; Li, Hongbian; Shang, Yuanyuan; Fang, Ying

2018-03-01

The capability to directly build atomically thin transition metal dichalcogenide (TMD) devices by chemical synthesis offers important opportunities to achieve large-scale electronics and optoelectronics with seamless interfaces. Here, a general approach for the chemical synthesis of a variety of TMD (e.g., MoS 2 , WS 2 , and MoSe 2 ) device arrays over large areas is reported. During chemical vapor deposition, semiconducting TMD channels and metallic TMD/carbon nanotube (CNT) hybrid electrodes are simultaneously formed on CNT-patterned substrate, and then coalesce into seamless devices. Chemically synthesized TMD devices exhibit attractive electrical and mechanical properties. It is demonstrated that chemically synthesized MoS 2 -MoS 2 /CNT devices have Ohmic contacts between MoS 2 /CNT hybrid electrodes and MoS 2 channels. In addition, MoS 2 -MoS 2 /CNT devices show greatly enhanced mechanical stability and photoresponsivity compared with conventional gold-contacted devices, which makes them suitable for flexible optoelectronics. Accordingly, a highly flexible pixel array based on chemically synthesized MoS 2 -MoS 2 /CNT photodetectors is applied for image sensing. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Cost-effective single-step carbon nanotube synthesis using microwave oven

NASA Astrophysics Data System (ADS)

Algadri, Natheer A.; Ibrahim, K.; Hassan, Z.; Bououdina, M.

2017-08-01

This paper reports the characterization of carbon nanotubes (CNTs) synthesised using a conventional microwave oven method, offering several advantages including fast, simple, low cost, and solvent free growth process. The procedure involves flattening of graphite/ferrocene mixture catalyst inside the microwave oven under ambient conditions for a very short duration of 5 s, which inhibits the loss factor of graphite and ferrocene. The effect of graphite/ferrocene mixture ratio for the synthesis of CNTs is investigated by transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), x-ray diffraction (XRD), Raman spectroscopy and UV-NIR-Vis measurements. The samples produced using the different ratios contain nanotubes with an average diameter in the range 44-79 nm. The highest yield of CNTs is attained with graphite/ferrocene mixture ratio of 70:30. The lowest I D/I G ratio intensity as identified by Raman spectroscopy for 70:30 ratio indicates the improved crystallinity of CNTs. Due to the capillary effect of CNTs, Fe nanoparticles are found to be encapsulated inside the tubes at different positions along the tube length. The obtained results showed that the smaller the diameter of graphite and ferrocene favors the synthesis of graphene oxide upon microwave radiation.

Microwave-assisted chemistry: synthetic applications for rapid assembly of nanomaterials and organics.

PubMed

Gawande, Manoj B; Shelke, Sharad N; Zboril, Radek; Varma, Rajender S

2014-04-15

The magic of microwave (MW) heating technique, termed the Bunsen burner of the 21st century, has emerged as a valuable alternative in the synthesis of organic compounds, polymers, inorganic materials, and nanomaterials. Important innovations in MW-assisted chemistry now enable chemists to prepare catalytic materials or nanomaterials and desired organic molecules, selectively, in almost quantitative yields and with greater precision than using conventional heating. By controlling the specific MW parameters (temperature, pressure, and ramping of temperature) and choice of solvents, researchers can now move into the next generation of advanced nanomaterial design and development. Microwave-assisted chemical reactions are now well-established practices in the laboratory setting although some controversy lingers as to how MW irradiation is able to enhance or influence the outcome of chemical reactions. Much of the discussion has focused on whether the observed effects can, in all instances, be rationalized by purely thermal Arrhenius-based phenomena (thermal microwave effects), that is, the importance of the rapid heating and high bulk reaction temperatures that are achievable using MW dielectric heating in sealed reaction vessels, or whether these observations can be explained by so-called "nonthermal" or "specific microwave" effects. In recent years, innovative and significant advances have occurred in MW hardware development to help delineate MW effects, especially the use of silicon carbide (SiC) reaction vessels and the accurate measurement of temperature using fiber optic (FO) temperature probes. SiC reactors appear to be good alternatives to MW transparent borosilicate glass, because of their high microwave absorptivity, and as such they serve as valuable tools to demystify the claimed magical MW effects. This enables one to evaluate the influence of the electromagnetic field on the specific chemical reactions, under truly identical conventional heating conditions, wherein temperature is measured accurately by fiber optic (FO) probe. This Account describes the current status of MW-assisted synthesis highlighting the introduction of various prototypes of equipment, classes of organic reactions pursued using nanomaterials, and the synthesis of unique and multifunctional nanomaterials; the ensuing nanomaterials possess zero-dimensional to three-dimensional shapes, such as spherical, hexagonal, nanoprisms, star shapes, and nanorods. The synthesis of well-defined nanomaterials and nanocatalysts is an integral part of nanotechnology and catalysis science, because it is imperative to control their size, shape, and compositional engineering for unique deployment in the field of nanocatalysis and organic synthesis. MW-assisted methods have been employed for the convenient and reproducible synthesis of well-defined noble and transition core-shell metallic nanoparticles with tunable shell thicknesses. Some of the distinctive attributes of MW-selective heating in the synthesis and applications of magnetic nanocatalysts in organic synthesis under benign reaction conditions are highlighted. Sustainable nanomaterials and their applications in benign media are an ideal blend for the development of greener methodologies in organic synthesis; MW heating provides superb value to the overall sustainable process development via process intensification including the flow systems.

Sol-gel processing of bioactive glass nanoparticles: A review.

PubMed

Zheng, Kai; Boccaccini, Aldo R

2017-11-01

Silicate-based bioactive glass nanoparticles (BGN) are gaining increasing attention in various biomedical applications due to their unique properties. Controlled synthesis of BGN is critical to their effective use in biomedical applications since BGN characteristics, such as morphology and composition, determining the properties of BGN, are highly related to the synthesis process. In the last decade, numerous investigations focusing on BGN synthesis have been reported. BGN can mainly be produced through the conventional melt-quench approach or by sol-gel methods. The latter approaches are drawing widespread attention, considering the convenience and versatility they offer to tune the properties of BGN. In this paper, we review the strategies of sol-gel processing of BGN, including those adopting different catalysts for initiating the hydrolysis and condensation of silicate precursors as well as those combining sol-gel chemistry with other techniques. The processes and mechanism of different synthesis approaches are introduced and discussed in detail. Considering the importance of the BGN morphology and composition to their biomedical applications, strategies put forward to control the size, shape, pore structure and composition of BGN are discussed. BGN are particularly interesting biomaterials for bone-related applications, however, they also have potential for other biomedical applications, e.g. in soft tissue regeneration/repair. Therefore, in the last part of this review, recently reported applications of BGN in soft tissue repair and wound healing are presented. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis of Engineered Zeolitic Materials: From Classical Zeolites to Hierarchical Core-Shell Materials.

PubMed

Masoumifard, Nima; Guillet-Nicolas, Rémy; Kleitz, Freddy

2018-04-01

The term "engineered zeolitic materials" refers to a class of materials with a rationally designed pore system and active-sites distribution. They are primarily made of crystalline microporous zeolites as the main building blocks, which can be accompanied by other secondary components to form composite materials. These materials are of potential importance in many industrial fields like catalysis or selective adsorption. Herein, critical aspects related to the synthesis and modification of such materials are discussed. The first section provides a short introduction on classical zeolite structures and properties, and their conventional synthesis methods. Then, the motivating rationale behind the growing demand for structural alteration of these zeolitic materials is discussed, with an emphasis on the ongoing struggles regarding mass-transfer issues. The state-of-the-art techniques that are currently available for overcoming these hurdles are reviewed. Following this, the focus is set on core-shell composites as one of the promising pathways toward the creation of a new generation of highly versatile and efficient engineered zeolitic substances. The synthesis approaches developed thus far to make zeolitic core-shell materials and their analogues, yolk-shell, and hollow materials, are also examined and summarized. Finally, the last section concisely reviews the performance of novel core-shell, yolk-shell, and hollow zeolitic materials for some important industrial applications. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Precursor Mediated Synthesis of Nanostructured Silicas: From Precursor-Surfactant Ion Pairs to Structured Materials.

PubMed

Hesemann, Peter; Nguyen, Thy Phung; Hankari, Samir El

2014-04-11

The synthesis of nanostructured anionic-surfactant-templated mesoporous silica (AMS) recently appeared as a new strategy for the formation of nanostructured silica based materials. This method is based on the use of anionic surfactants together with a co-structure-directing agent (CSDA), mostly a silylated ammonium precursor. The presence of this CSDA is necessary in order to create ionic interactions between template and silica forming phases and to ensure sufficient affinity between the two phases. This synthetic strategy was for the first time applied in view of the synthesis of surface functionalized silica bearing ammonium groups and was then extended on the formation of materials functionalized with anionic carboxylate and bifunctional amine-carboxylate groups. In the field of silica hybrid materials, the "anionic templating" strategy has recently been applied for the synthesis of silica hybrid materials from cationic precursors. Starting from di- or oligosilylated imidazolium and ammonium precursors, only template directed hydrolysis-polycondensation reactions involving complementary anionic surfactants allowed accessing structured ionosilica hybrid materials. The mechanistic particularity of this approach resides in the formation of precursor-surfactant ion pairs in the hydrolysis-polycondensation mixture. This review gives a systematic overview over the various types of materials accessed from this cooperative ionic templating approach and highlights the high potential of this original strategy for the formation of nanostructured silica based materials which appears as a complementary strategy to conventional soft templating approaches.

Linear-parameter-varying gain-scheduled control of aerospace systems

NASA Astrophysics Data System (ADS)

Barker, Jeffrey Michael

The dynamics of many aerospace systems vary significantly as a function of flight condition. Robust control provides methods of guaranteeing performance and stability goals across flight conditions. In mu-syntthesis, changes to the dynamical system are primarily treated as uncertainty. This method has been successfully applied to many control problems, and here is applied to flutter control. More recently, two techniques for generating robust gain-scheduled controller have been developed. Linear fractional transformation (LFT) gain-scheduled control is an extension of mu-synthesis in which the plant and controller are explicit functions of parameters measurable in real-time. This LFT gain-scheduled control technique is applied to the Benchmark Active Control Technology (BACT) wing, and compared with mu-synthesis control. Linear parameter-varying (LPV) gain-scheduled control is an extension of Hinfinity control to parameter varying systems. LPV gain-scheduled control directly incorporates bounds on the rate of change of the scheduling parameters, and often reduces conservatism inherent in LFT gain-scheduled control. Gain-scheduled LPV control of the BACT wing compares very favorably with the LFT controller. Gain-scheduled LPV controllers are generated for the lateral-directional and longitudinal axes of the Innovative Control Effectors (ICE) aircraft and implemented in nonlinear simulations and real-time piloted nonlinear simulations. Cooper-Harper and pilot-induced oscillation ratings were obtained for an initial design, a reference aircraft and a redesign. Piloted simulation results for the initial LPV gain-scheduled control of the ICE aircraft are compared with results for a conventional fighter aircraft in discrete pitch and roll angle tracking tasks. The results for the redesigned controller are significantly better than both the previous LPV controller and the conventional aircraft.

Conventional and microwave combustion synthesis of optomagnetic CuFe2O4 nanoparticles for hyperthermia studies

NASA Astrophysics Data System (ADS)

Kombaiah, K.; Vijaya, J. Judith; Kennedy, L. John; Bououdina, M.; Al-Najar, Basma

2018-04-01

Nanosized copper ferrite (CuFe2O4) nanoparticles have been prepared by conventional (CCM) and microwave (MCM) combustion methods using Hibiscus rosa sinensis plant extract as a fuel. XRD and rietveld analysis confirmed the formation of single cubic phase and with crystallite size varying from 25 to 62 nm owing to grain growth after calcination. FT-IR analysis confirms the modes of the cubic CuFe2O4 phase, due to the stretching and bending vibrations. Spherical shaped particles are observed by scanning electron microscopy and the average particle size is found to be in the range of 50-200 nm. The chemical composition is confirmed by energy dispersive X-ray analysis. The optical band gap energy estimated using Kubelka-Munk function with the help of UV-Visible diffused reflectance spectroscopy, is found to be 2.34 and 2.22 eV for CCM and MCM respectively. Photoluminescence analysis indicates that both samples absorb light in the UV-visible region and exhibit emissions at 360, 376, and 412 nm. Magnetic measurements indicate a ferromagnetic behavior, where both magnetic properties very much influenced by the preparation method and calcination temperature: both saturation magnetization and coercivity are found higher when using CCM and MCM; from 29.40 to 34.09 emu/g while almost double from 224.4 to 432.2 Oe. The observed changes in physical properties are mainly associated with crystallinity, particle size, better chemical homogeneity, and cations distribution among tetrahedral/octahedral sites. The maximum specific absorption rate obtained was 14.63 W/g, which can be considered suitable and favorable for magnetic hyperthermia. This study highlighted the benefits of green synthesis of CuFe2O4 nanoparticles providing better magnetic properties for the platform of hyperthermia application.

Computer synthesis of high resolution electron micrographs

NASA Technical Reports Server (NTRS)

Nathan, R.

1976-01-01

Specimen damage, spherical aberration, low contrast and noisy sensors combine to prevent direct atomic viewing in a conventional electron microscope. The paper describes two methods for obtaining ultra-high resolution in biological specimens under the electron microscope. The first method assumes the physical limits of the electron objective lens and uses a series of dark field images of biological crystals to obtain direct information on the phases of the Fourier diffraction maxima; this information is used in an appropriate computer to synthesize a large aperture lens for a 1-A resolution. The second method assumes there is sufficient amplitude scatter from images recorded in focus which can be utilized with a sensitive densitometer and computer contrast stretching to yield fine structure image details. Cancer virus characterization is discussed as an illustrative example. Numerous photographs supplement the text.

Magnetic Droplet Microfluidics as a Platform for the Concentration of [18F]Fluoride and Radiosynthesis of Sulfonyl [18F]Fluoride.

PubMed

Fiel, Somewhere A; Yang, Hua; Schaffer, Paul; Weng, Samuel; Inkster, James A H; Wong, Michael C K; Li, Paul C H

2015-06-17

The radioisotope 18F is often considered the best choice for positron emission tomography (PET) owing to its desirable chemical and radiochemical properties. However, nucleophilic 18F-fluorination of large, water-soluble biomolecules, based on C-F bond formation, has traditionally been difficult. Thus, several aqueous fluorination approaches that offer significant versatility in radiopharmaceutical synthesis with sensitive targeting vectors have been developed. Furthermore, because 18F decays rapidly, production of these 18F-labeled compounds requires an automated process to reduce production time, reduce radiation exposure, and minimize losses due to the transfer of reagents during tracer synthesis. Herein, we report the use of magnetic droplet microfluidics (MDM) as a means to concentrate [18F]fluoride from the cyclotron target solution, followed by the synthesis of an 18F-labeled compound on a microfluidic platform. Using this method, we have demonstrated 18F preconcentration in a small-volume droplet through the use of anion exchanging magnetic particles. By using MDM, the preconcentration step took approximately 5 min, and the [18F]fluoride solution was preconcentrated by 15-fold. After the preconcentration step, an 18F-labeling reaction was performed on the MDM platform using the S-F bond formation in aqueous conditions to produce an arylsulfonyl [18F]fluoride compound which can be used as a prosthetic group to label PET targeting ligands. The high radiochemical purity of 95±1% was comparable to the 96% previously reported using a conventional method. In addition, when MDM was used, the total synthesis time was improved to 15 min with lower reagent volumes (50-60 μL) used.

Development of new inorganic luminescent materials by organic-metal complex route

NASA Astrophysics Data System (ADS)

Manavbasi, Alp

The development of novel inorganic luminescent materials has provided important improvements in lighting, display, and other technologically-important optical devices. The optical characteristics of inorganic luminescent materials (phosphors) depend on their physicochemical characteristics, including the atomic structure, homogeneity in composition, microstructure, defects, and interfaces which are all controlled by thermodynamics and kinetics of synthesis from various raw materials. A large variety of technologically-important phosphors have been produced using conventional high-temperature solid-state methods. For the synthesis of functional ceramic materials with ionic dopants in a host lattice, (such as phosphors), synthesis using organic-metal complex methods and other wet chemistry routes have been found to be excellent techniques. These methods have inherent advantages such as good control of stoichiometry by molecular level of mixing, product homogeneity, simpler synthesis procedures, and use of relatively-low calcination temperatures. Supporting evidence for this claim is accomplished by a comparison of photoluminescence characteristics of a commercially available green phosphor, Zn2SiO4:Mn, with the same material system synthesized by organic-metal synthesis route. In this study, new inorganic luminescent materials were produced using rare-earth elements (Eu3+, Ce3+, Tb3+ ) and transition metals (Cu+, Pb2+) as dopants within the crystalline host lattices; SrZnO2, Ba2YAlO 5, M3Al2O6 (M=Ca,Sr,Ba). These novel phosphors were prepared using the organic-metal complex route. Polyvinyl alcohol, sucrose, and adipic acid were used as the organic component to prepare the ceramic precursors. Materials characterization of the synthesized precursor powders and calcined phosphor samples was performed usingX-Ray Diffraction, Scanning Electron Microscopy, Photon-Correlation spectroscopy, and Fourier Transform Infrared Spectroscopy techniques. In addition to the Fluorescence Spectrometer, and Diffuse Reflectance Spectroscopy, the Time Resolved Spectroscopy technique was also used to study the photoluminescence characteristics of the synthesized phosphors. Using these characterization techniques, and through careful comparisons with related studies in the literature, the mechanisms of luminescence for each of the new phosphor materials synthesized here was discussed in a detail.

Energy efficient microwave synthesis of mesoporous Ce 0.5M 0.5O 2 (Ti, Zr, Hf) nanoparticles for low temperature CO oxidation in an ionic liquid – a comparative study

DOE PAGES

Alammar, Tarek; Chow, Ying -Kit; Mudring, Anja -Verena

2014-11-19

Ce 0.5M 0.5O 2 (M = Ti, Zr, Hf) nanoparticles have been successfully synthesized by microwave irradiation in the ionic liquid [C 4mim][Tf 2N] (1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)amide). The morphology, crystallinity, and chemical composition of the obtained materials were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX), Raman spectroscopy, and N 2–adsorption measurements. XRD and Raman spectroscopy analyses confirmed the formation of solid solutions with cubic fluorite structure. The catalytic activities of the Ce 0.5M 0.5O 2 (M = Ti, Zr, Hf) nanoparticles were investigated in the low-temperature oxidation of CO. Ce 0.5Zr 0.5O 2 nanospheresmore » exhibit the best performance (100% conversion at 350 °C), followed by Ce 0.5Hf 0.5O 2 (55% conversion at 360 °C) and Ce 0.5Ti 0.5O 2 (11% conversion at 350 °C). Heating the as-prepared Ce 0.5Zr 0.5O 2 to 600 °C for extended time leads to a decrease in surface area and, as expected decreased catalytic activity. Depending on the ionic liquid the obtained Ce 0.5Zr 0.5O 2 exhibits different morphologies, varying from nano-spheres in [C 4mim][Tf 2N] and [P 66614][Tf 2N] (P 66614 = trishexyltetradecylphosphonium) to sheet-like assemblies in [C 3mimOH][Tf 2N] (C 3mimOH = 1-(3-hydroxypropyl)-3-methylimidazolium). As a result, the microwave synthesis superiority to other heating methods like sonochemical synthesis and conventional heating was proven by comparative experiments where the catalytic activity of Ce 0.5Zr 0.5O 2 obtained by alternate methods such as conventional heating was found to be poorer than that of the microwave-synthesised material.« less

Microwave-assisted green synthesis of silver nanostructures.

PubMed

Nadagouda, Mallikarjuna N; Speth, Thomas F; Varma, Rajender S

2011-07-19

Over the past 25 years, microwave (MW) chemistry has moved from a laboratory curiosity to a well-established synthetic technique used in many academic and industrial laboratories around the world. Although the overwhelming number of MW-assisted applications today are still performed on a laboratory (mL) scale, we expect that this enabling technology may be used on a larger, perhaps even production, scale in conjunction with radio frequency or conventional heating. Microwave chemistry is based on two main principles, the dipolar mechanism and the electrical conductor mechanism. The dipolar mechanism occurs when, under a very high frequency electric field, a polar molecule attempts to follow the field in the same alignment. When this happens, the molecules release enough heat to drive the reaction forward. In the second mechanism, the irradiated sample is an electrical conductor and the charge carriers, ions and electrons, move through the material under the influence of the electric field and lead to polarization within the sample. These induced currents and any electrical resistance will heat the sample. This Account summarizes a microwave (MW)-assisted synthetic approach for producing silver nanostructures. MW heating has received considerable attention as a promising new method for the one-pot synthesis of metallic nanostructures in solutions. Researchers have successfully demonstrated the application of this method in the preparation of silver (Ag), gold (Au), platinum (Pt), and gold-palladium (Au-Pd) nanostructures. MW heating conditions allow not only for the preparation of spherical nanoparticles within a few minutes but also for the formation of single crystalline polygonal plates, sheets, rods, wires, tubes, and dendrites. The morphologies and sizes of the nanostructures can be controlled by changing various experimental parameters, such as the concentration of metallic salt precursors, the surfactant polymers, the chain length of the surfactant polymers, the solvents, and the operation reaction temperature. In general, nanostructures with smaller sizes, narrower size distributions, and a higher degree of crystallization have been obtained more consistently via MW heating than by heating with a conventional oil-bath. The use of microwaves to heat samples is a viable avenue for the greener synthesis of nanomaterials and provides several desirable features such as shorter reaction times, reduced energy consumption, and better product yields.

One-pot synthesis of iniferter-bound polystyrene core nanoparticles for the controlled grafting of multilayer shells

NASA Astrophysics Data System (ADS)

Marchyk, Nataliya; Maximilien, Jacqueline; Beyazit, Selim; Haupt, Karsten; Sum Bui, Bernadette Tse

2014-02-01

A novel approach using one-pot synthesis for the production of uniform, iniferter-bound polystyrene core nanoparticles of size 30-40 nm is described. Conventional oil-in-water emulsion polymerisation of styrene and divinylbenzene, combining a hybrid initiation system (thermal and UV), triggered sequentially, was employed to form the surface-bound thiocarbamate iniferters in situ. The iniferter cores were then used as seeds for re-initiating further polymerisation by UV irradiation to produce water-compatible core-shell nanoparticles. Grafting of various shell-types is demonstrated: linear polymers of poly(N-isopropylacrylamide) brushes, crosslinked polymers bearing different surface charges and molecularly imprinted polymers. The shell thickness was readily tuned by varying the monomers' concentration and polymerisation time. Our method is straightforward and in addition, gives access to the preparation of fluorescent seeds and the possibility of grafting nanosized multiple shells. The core-shell nanoparticles were fully characterised by dynamic light scattering, transmission electron microscopy, Fourier transform infrared spectroscopy and microelemental analysis.A novel approach using one-pot synthesis for the production of uniform, iniferter-bound polystyrene core nanoparticles of size 30-40 nm is described. Conventional oil-in-water emulsion polymerisation of styrene and divinylbenzene, combining a hybrid initiation system (thermal and UV), triggered sequentially, was employed to form the surface-bound thiocarbamate iniferters in situ. The iniferter cores were then used as seeds for re-initiating further polymerisation by UV irradiation to produce water-compatible core-shell nanoparticles. Grafting of various shell-types is demonstrated: linear polymers of poly(N-isopropylacrylamide) brushes, crosslinked polymers bearing different surface charges and molecularly imprinted polymers. The shell thickness was readily tuned by varying the monomers' concentration and polymerisation time. Our method is straightforward and in addition, gives access to the preparation of fluorescent seeds and the possibility of grafting nanosized multiple shells. The core-shell nanoparticles were fully characterised by dynamic light scattering, transmission electron microscopy, Fourier transform infrared spectroscopy and microelemental analysis. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr05295h

Discovery-Synthesis, Design, and Prediction of Chalcogenide Phases

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

Kanatzidis, Mercouri G.

The discovery of new materials and their efficient syntheses is a fundamental goal of chemistry. A related objective is to identify foundational and rational approaches to enhance the art of synthesis by combining the exquisite predictability of organic synthesis with the high yields of solid-state chemistry. In contrast to so-called solid-state methods, inorganic syntheses in liquid fluxes permit bond formation, framework assembly, and crystallization at lower temperatures because of facile diffusion and chemical reactions with and within the flux itself. The fluxes are bona fide solvents similar to conventional organic or aqueous solvents. Such reactions can produce a wide rangemore » of materials, often metastable, from oxides to intermetallics, but typically the formation mechanisms are poorly understood. This article discusses how one can design, perform, observe, understand, and engineer the formation of compounds from inorganic melts. The focus is also design concepts such as "dimensional reduction", "phase homologies", and "panoramic synthesis", and their broad applicability. When well-defined building blocks are present and stable in the reaction, prospects for increased structural diversity and product control increase substantially. Common structural motifs within these materials systems may be related to structural precursors in the melt that may be controlled by tuning reaction conditions and composition. Stabilization of a particular building block is often accomplished with tuning of the flux composition, which controls the Lewis basicity and redox potential. In such tunable and dynamic fluxes, the synthesis can be directed toward new materials. Using complementary techniques of in situ X-ray diffraction, we can create time-dependent maps of reaction space and probe the mobile species present in melts. Lastly, certain thoughts toward the ultimate goal of targeted materials synthesis by controlling inorganic melt chemistry are discussed.« less

Discovery-Synthesis, Design, and Prediction of Chalcogenide Phases

DOE PAGES

Kanatzidis, Mercouri G.

2017-03-09

The discovery of new materials and their efficient syntheses is a fundamental goal of chemistry. A related objective is to identify foundational and rational approaches to enhance the art of synthesis by combining the exquisite predictability of organic synthesis with the high yields of solid-state chemistry. In contrast to so-called solid-state methods, inorganic syntheses in liquid fluxes permit bond formation, framework assembly, and crystallization at lower temperatures because of facile diffusion and chemical reactions with and within the flux itself. The fluxes are bona fide solvents similar to conventional organic or aqueous solvents. Such reactions can produce a wide rangemore » of materials, often metastable, from oxides to intermetallics, but typically the formation mechanisms are poorly understood. This article discusses how one can design, perform, observe, understand, and engineer the formation of compounds from inorganic melts. The focus is also design concepts such as "dimensional reduction", "phase homologies", and "panoramic synthesis", and their broad applicability. When well-defined building blocks are present and stable in the reaction, prospects for increased structural diversity and product control increase substantially. Common structural motifs within these materials systems may be related to structural precursors in the melt that may be controlled by tuning reaction conditions and composition. Stabilization of a particular building block is often accomplished with tuning of the flux composition, which controls the Lewis basicity and redox potential. In such tunable and dynamic fluxes, the synthesis can be directed toward new materials. Using complementary techniques of in situ X-ray diffraction, we can create time-dependent maps of reaction space and probe the mobile species present in melts. Lastly, certain thoughts toward the ultimate goal of targeted materials synthesis by controlling inorganic melt chemistry are discussed.« less

Combining Sustainable Synthesis of a Versatile Ruthenium Dihydride Complex with Structure Determination Using Group Theory and Spectroscopy

ERIC Educational Resources Information Center

Armstrong, Christopher; Burnham, Jennifer A. J.; Warminski, Edward E.

2017-01-01

A good-yielding two-step synthesis of RuH[subscript 2](CO)(PPh[subscript 3])[subscript 3] using conventional or microwave-assisted reflux techniques is described for use in undergraduate teaching laboratories. RuH[subscript 2](CO)(PPh[subscript 3])[subscript 3] is synthesized from RuCl[subscript 3]·xH[subscript 2]O, PPh[subscript 3], and KOH in…

Synthesis of Cesium Lead Halide Perovskite Nanocrystals in a Droplet-Based Microfluidic Platform: Fast Parametric Space Mapping.

PubMed

Lignos, Ioannis; Stavrakis, Stavros; Nedelcu, Georgian; Protesescu, Loredana; deMello, Andrew J; Kovalenko, Maksym V

2016-03-09

Prior to this work, fully inorganic nanocrystals of cesium lead halide perovskite (CsPbX3, X = Br, I, Cl and Cl/Br and Br/I mixed halide systems), exhibiting bright and tunable photoluminescence, have been synthesized using conventional batch (flask-based) reactions. Unfortunately, our understanding of the parameters governing the formation of these nanocrystals is still very limited due to extremely fast reaction kinetics and multiple variables involved in ion-metathesis-based synthesis of such multinary halide systems. Herein, we report the use of a droplet-based microfluidic platform for the synthesis of CsPbX3 nanocrystals. The combination of online photoluminescence and absorption measurements and the fast mixing of reagents within such a platform allows the rigorous and rapid mapping of the reaction parameters, including molar ratios of Cs, Pb, and halide precursors, reaction temperatures, and reaction times. This translates into enormous savings in reagent usage and screening times when compared to analogous batch synthetic approaches. The early-stage insight into the mechanism of nucleation of metal halide nanocrystals suggests similarities with multinary metal chalcogenide systems, albeit with much faster reaction kinetics in the case of halides. Furthermore, we show that microfluidics-optimized synthesis parameters are also directly transferrable to the conventional flask-based reaction.

Novel high pressure hexagonal OsB2 by mechanochemistry

NASA Astrophysics Data System (ADS)

Xie, Zhilin; Graule, Moritz; Orlovskaya, Nina; Andrew Payzant, E.; Cullen, David A.; Blair, Richard G.

2014-07-01

Hexagonal OsB2, a theoretically predicted high-pressure phase, has been synthesized for the first time by a mechanochemical method, i.e., high energy ball milling. X-ray diffraction indicated that formation of hexagonal OsB2 begins after 2.5 h of milling, and the reaction reaches equilibrium after 18 h of milling. Rietveld refinement of the powder data indicated that hexagonal OsB2 crystallizes in the P63/mmc space group (No. 194) with lattice parameters of a=2.916 Å and c=7.376 Å. Transmission electron microscopy confirmed the appearance of the hexagonal OsB2 phase after high energy ball milling. in situ X-ray diffraction experiments showed that the phase is stable from -225 °C to 1050 °C. The hexagonal OsB2 powder was annealed at 1050 °C for 6 days in vacuo to improve crystallinity and remove strain induced during the mechanochemical synthesis. The structure partially converted to the orthorhombic phase (20 wt%) after fast current assisted sintering of hexagonal OsB2 at 1500 °C for 5 min. Mechanochemical approaches to the synthesis of hard boride materials allow new phases to be produced that cannot be prepared using conventional methods.

Synthesis and structural characterization of bulk Sb2Te3 single crystal

NASA Astrophysics Data System (ADS)

Sultana, Rabia; Gahtori, Bhasker; Meena, R. S.; Awana, V. P. S.

2018-05-01

We report the growth and characterization of bulk Sb2Te3 single crystal synthesized by the self flux method via solid state reaction route from high temperature melt (850˚C) and slow cooling (2˚C/hour) of constituent elements. The single crystal X-ray diffraction pattern showed the 00l alignment and the high crystalline nature of the resultant sample. The rietveld fitted room temperature powder XRD revealed the phase purity and rhombohedral structure of the synthesized crystal. The formation and analysis of unit cell structure further verified the rhombohedral structure composed of three quintuple layers stacked one over the other. The SEM image showed the layered directional growth of the synthesized crystal carried out using the ZEISS-EVOMA-10 scanning electron microscope The electrical resistivity measurement was carried out using the conventional four-probe method on a quantum design Physical Property Measurement System (PPMS). The temperature dependent electrical resistivity plot for studied Sb2Te3 single crystal depicts metallic behaviour in the absence of any applied magnetic field. The synthesis as well as the structural characterization of as grown Sb2Te3 single crystal is reported and discussed in the present letter.

Low cost hydrogen/novel membrane technology for hydrogen separation from synthesis gas. Task 1, Literature survey

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

Not Available

1986-02-01

To make the coal-to-hydrogen route economically attractive, improvements are being sought in each step of the process: coal gasification, water-carbon monoxide shift reaction, and hydrogen separation. This report addresses the use of membranes in the hydrogen separation step. The separation of hydrogen from synthesis gas is a major cost element in the manufacture of hydrogen from coal. Separation by membranes is an attractive, new, and still largely unexplored approach to the problem. Membrane processes are inherently simple and efficient and often have lower capital and operating costs than conventional processes. In this report current ad future trends in hydrogen productionmore » and use are first summarized. Methods of producing hydrogen from coal are then discussed, with particular emphasis on the Texaco entrained flow gasifier and on current methods of separating hydrogen from this gas stream. The potential for membrane separations in the process is then examined. In particular, the use of membranes for H{sub 2}/CO{sub 2}, H{sub 2}/CO, and H{sub 2}/N{sub 2} separations is discussed. 43 refs., 14 figs., 6 tabs.« less

Hybrid Technology of Hard Coal Mining from Seams Located at Great Depths

NASA Astrophysics Data System (ADS)

Czaja, Piotr; Kamiński, Paweł; Klich, Jerzy; Tajduś, Antoni

2014-10-01

Learning to control fire changed the life of man considerably. Learning to convert the energy derived from combustion of coal or hydrocarbons into another type of energy, such as steam pressure or electricity, has put him on the path of scientific and technological revolution, stimulating dynamic development. Since the dawn of time, fossil fuels have been serving as the mankind's natural reservoir of energy in an increasingly great capacity. A completely incomprehensible refusal to use fossil fuels causes some local populations, who do not possess a comprehensive knowledge of the subject, to protest and even generate social conflicts as an expression of their dislike for the extraction of minerals. Our times are marked by the search for more efficient ways of utilizing fossil fuels by introducing non-conventional technologies of exploiting conventional energy sources. During apartheid, South Africa demonstrated that cheap coal can easily satisfy total demand for liquid and gaseous fuels. In consideration of current high prices of hydrocarbon media (oil and gas), gasification or liquefaction of coal seems to be the innovative technology convergent with contemporary expectations of both energy producers as well as environmentalists. Known mainly from literature reports, underground coal gasification technologies can be brought down to two basic methods: - shaftless method - drilling, in which the gasified seam is uncovered using boreholes drilled from the surface, - shaft method, in which the existing infrastructure of underground mines is used to uncover the seams. This paper presents a hybrid shaft-drilling approach to the acquisition of primary energy carriers (methane and syngas) from coal seams located at great depths. A major advantage of this method is the fact that the use of conventional coal mining technology requires the seams located at great depths to be placed on the off-balance sheet, while the hybrid method of underground gasification enables them to become a source of additional energy for the economy. It should be noted, however, that the shaft-drilling method cannot be considered as an alternative to conventional methods of coal extraction, but rather as a complementary and cheaper way of utilizing resources located almost beyond the technical capabilities of conventional extraction methods due to the associated natural hazards and high costs of combating them. This article presents a completely different approach to the issue of underground coal gasification. Repurposing of the already fully depreciated mining infrastructure for the gasification process may result in a large value added of synthesis gas production and very positive economic effect.

Supercritical synthesis of biodiesel.

PubMed

Bernal, Juana M; Lozano, Pedro; García-Verdugo, Eduardo; Burguete, M Isabel; Sánchez-Gómez, Gregorio; López-López, Gregorio; Pucheault, Mathieu; Vaultier, Michel; Luis, Santiago V

2012-07-23

The synthesis of biodiesel fuel from lipids (vegetable oils and animal fats) has gained in importance as a possible source of renewable non-fossil energy in an attempt to reduce our dependence on petroleum-based fuels. The catalytic processes commonly used for the production of biodiesel fuel present a series of limitations and drawbacks, among them the high energy consumption required for complex purification operations and undesirable side reactions. Supercritical fluid (SCF) technologies offer an interesting alternative to conventional processes for preparing biodiesel. This review highlights the advances, advantages, drawbacks and new tendencies involved in the use of supercritical fluids (SCFs) for biodiesel synthesis.

Flow “Fine” Synthesis: High Yielding and Selective Organic Synthesis by Flow Methods

PubMed Central

2015-01-01

Abstract The concept of flow “fine” synthesis, that is, high yielding and selective organic synthesis by flow methods, is described. Some examples of flow “fine” synthesis of natural products and APIs are discussed. Flow methods have several advantages over batch methods in terms of environmental compatibility, efficiency, and safety. However, synthesis by flow methods is more difficult than synthesis by batch methods. Indeed, it has been considered that synthesis by flow methods can be applicable for the production of simple gasses but that it is difficult to apply to the synthesis of complex molecules such as natural products and APIs. Therefore, organic synthesis of such complex molecules has been conducted by batch methods. On the other hand, syntheses and reactions that attain high yields and high selectivities by flow methods are increasingly reported. Flow methods are leading candidates for the next generation of manufacturing methods that can mitigate environmental concerns toward sustainable society. PMID:26337828

Digital Transfer Growth of Patterned 2D Metal Chalcogenides by Confined Nanoparticle Evaporation

DOE PAGES

Mahjouri-Samani, Masoud; Tian, Mengkun; Wang, Kai; ...

2014-10-19

Developing methods for the facile synthesis of two-dimensional (2D) metal chalcogenides and other layered materials is crucial for emerging applications in functional devices. Controlling the stoichiometry, number of the layers, crystallite size, growth location, and areal uniformity is challenging in conventional vapor phase synthesis. Here, we demonstrate a new route to control these parameters in the growth of metal chalcogenide (GaSe) and dichalcogenide (MoSe 2) 2D crystals by precisely defining the mass and location of the source materials in a confined transfer growth system. A uniform and precise amount of stoichiometric nanoparticles are first synthesized and deposited onto a substratemore » by pulsed laser deposition (PLD) at room temperature. This source substrate is then covered with a receiver substrate to form a confined vapor transport growth (VTG) system. By simply heating the source substrate in an inert background gas, a natural temperature gradient is formed that evaporates the confined nanoparticles to grow large, crystalline 2D nanosheets on the cooler receiver substrate, the temperature of which is controlled by the background gas pressure. Large monolayer crystalline domains (~ 100 m lateral sizes) of GaSe and MoSe 2 are demonstrated, as well as continuous monolayer films through the deposition of additional precursor materials. This novel PLD-VTG synthesis and processing method offers a unique approach for the controlled growth of large-area, metal chalcogenides with a controlled number of layers in patterned growth locations for optoelectronics and energy related applications.« less

Synthesis and structural property of Si nanosheets connected to Si nanowires using MnCl2/Si powder source

NASA Astrophysics Data System (ADS)

Meng, Erchao; Ueki, Akiko; Meng, Xiang; Suzuki, Hiroaki; Itahara, Hiroshi; Tatsuoka, Hirokazu

2016-08-01

Si nanosheets connected to Si nanowires were synthesized using a MnCl2/Si powder source with an Au catalyst. The synthesis method has benefits in terms of avoiding conventionally used air-sensitive SiH4 or SiCl4. The existence of the Si nanosheets connected to the Si<111> nanowires, like sprouts or leaves with petioles, was observed, and the surface of the nanosheets was Si{111}. The nanosheets were grown in the growth direction of <211> perpendicular to that of the Si nanowires. It was evident from these structural features of the nanosheets that the nanosheets were formed by the twin-plane reentrant-edge mechanism. The feature of the observed lattice fringes, which do not appear for Si bulk crystals, of the Si(111) nanosheets obtained by high resolution transmission electron microscopy was clearly explained due to the extra diffraction spots that arose by the reciprocal lattice streaking effect.

Developing a workstation-based, real-time simulation for rapid handling qualities evaluations during design

NASA Technical Reports Server (NTRS)

Anderson, Frederick; Biezad, Daniel J.

1994-01-01

This paper describes the Rapid Aircraft DynamIcs AssessmeNt (RADIAN) project - an integration of the Aircraft SYNThesis (ACSTNT) design code with the USAD DATCOM code that estimates stability derivatives. Both of these codes are available to universities. These programs are then linked to flight simulation and flight controller synthesis tools and resulting design is evaluated on a graphics workstation. The entire process reduces the preliminary design time by an order of magnitude and provides an initial handling qualities evaluation of the design coupled to a control law. The integrated design process is applicable to both conventional aircraft taken from current textbooks and to unconventional designs emphasizing agility and propulsive control of attitude. The interactive and concurrent nature of the design process has been well received by industry and by design engineers at NASA. The process is being implemented into the design curriculum and is being used by students who view it as a significant advance over prior methods.

Synthesis, characterization, electrical conductivity and luminescence properties of two copper(II) complexes with tridentate N2O chelating ligands containing imine bond

NASA Astrophysics Data System (ADS)

Gönül, İlyas; Ay, Burak; Karaca, Serkan; Şahin, Onur; Serin, Selahattin

2018-03-01

In the present study, we describe the synthesis and characterization of two tridentate N2O donor ligands, namely, (E)-2-(((2-(diethylamino)ethyl)imino)methyl)-6-methoxyphenol (HL1) and (E)-2-(((2-(diethylamino)ethyl)imino)methyl)-6-ethoxyphenol (HL2), and their copper(II) complexes, [Cu(L1)(CH3COO)] (1), [Cu(L2)(CH3COO)] (2). They have been synthesized under conventional methods and characterized by elemental analysis, FTIR, 1H and 13C NMR, ICP-OES, TGA and GC/MS analysis. For the morphological analysis field emission scanning electron microscopy (FESEM) was used. The geometry of the copper(II) complexes was determined by single crystal X-ray diffraction analysis. The copper(II) ions are in distorted square-pyramidal coordination environments. Complexes crystallize in monoclinic space group, P21/c. The electrical conductivity and luminescence properties of 1-2 have been investigated.

Robust Control Design for Systems With Probabilistic Uncertainty

NASA Technical Reports Server (NTRS)

Crespo, Luis G.; Kenny, Sean P.

2005-01-01

This paper presents a reliability- and robustness-based formulation for robust control synthesis for systems with probabilistic uncertainty. In a reliability-based formulation, the probability of violating design requirements prescribed by inequality constraints is minimized. In a robustness-based formulation, a metric which measures the tendency of a random variable/process to cluster close to a target scalar/function is minimized. A multi-objective optimization procedure, which combines stability and performance requirements in time and frequency domains, is used to search for robustly optimal compensators. Some of the fundamental differences between the proposed strategy and conventional robust control methods are: (i) unnecessary conservatism is eliminated since there is not need for convex supports, (ii) the most likely plants are favored during synthesis allowing for probabilistic robust optimality, (iii) the tradeoff between robust stability and robust performance can be explored numerically, (iv) the uncertainty set is closely related to parameters with clear physical meaning, and (v) compensators with improved robust characteristics for a given control structure can be synthesized.

Synthesis of magnetic composite nanoparticles enveloped in copolymers specified for scale inhibition application

NASA Astrophysics Data System (ADS)

Do, Bao Phuong Huu; Dung Nguyen, Ba; Duy Nguyen, Hoang; Nguyen, Phuong Tung

2013-12-01

We report the synthesis of magnetic iron oxide nanoparticles encapsulated in maleic acid-2-acrylamido-2-methyl-1-propanesulfonate based polymer. This composite nanoparticle is specified for the high-pressure/high-temperature (HPHT) oilfield scale inhibition application. The process includes a facile-ultrasound-supported addition reaction to obtain iron oxide nanoparticles with surface coated by oleic acid. Then via inverse microemulsion polymerization with selected monomers, the specifically designed copolymers have been formatted in nanoscale. The structure and morphology of obtained materials were characterized by transmission electron microscopy (TEM), x-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and the thermal stability. The effectiveness of synthesized compounds as a carbonate scale inhibitor was investigated by testing method NACE standard TM 03-074-95 at aging temperature of 70, 90 and 120 °C. The magnetic nanocomposite particles can be easily collected and detected demonstrating their superior monitoring ability, which is absent in the case of conventional copolymer-based scale inhibitor.

Electronic conductivity studies on oxyhalide glasses containing TMO

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

Vijayatha, D.; Department of Physics, Gurunanak Institute of Technology, Hyderabad -040; Viswanatha, R.

2016-05-06

Microwave-assisted synthesis is cleaner, more economical and much faster than conventional methods. The development of new routes for the synthesis of solid materials is an integral part of material science and technology. The electronic conductivity studies on xPbCl{sub 2} – 60 PbO – (40-x) V{sub 2}O{sub 5} (1 ≥ x ≤ 10) glass system has been carried out over a wide range of composition and temperature (300 K to 423 K). X-ray diffraction study confirms the amorphous nature of the samples. The Scanning electron microscopic studies reveal the formation of cluster like morphology in PbCl{sub 2} containing glasses. The d.c conductivity exhibitsmore » Arrhenius behaviour and increases with V{sub 2}O{sub 5} concentration. Analysis of the results is interpreted in view Austin-Mott’s small polaron model of electron transport. Activation energies calculated using regression analysis exhibit composition dependent trend and the variation is explained in view of the structure of lead-vanadate glass.« less

Agile green process design for the intensified Kolbe-Schmitt synthesis by accompanying (simplified) life cycle assessment.

PubMed

Kressirer, Sabine; Kralisch, Dana; Stark, Annegret; Krtschil, Ulrich; Hessel, Volker

2013-05-21

In order to investigate the potential for process intensification, various reaction conditions were applied to the Kolbe-Schmitt synthesis starting from resorcinol. Different CO₂ precursors such as aqueous potassium hydrogencarbonate, hydrogencarbonate-based ionic liquids, DIMCARB, or sc-CO₂, the application of microwave irradiation for fast volumetric heating of the reaction mixture, and the effect of harsh reaction conditions were investigated. The experiments, carried out in conventional batch-wise as well as in continuously operated microstructured reactors, aimed at the development of an environmentally benign process for the preparation of 2,4-dihydroxybenzoic acid. To provide decision support toward a green process design, a research-accompanying simplified life cycle assessment (SLCA) was performed throughout the whole investigation. Following this approach, it was found that convective heating methods such as oil bath or electrical heating were more beneficial than the application of microwave irradiation. Furthermore, the consideration of workup procedures was crucial for a holistic view on the environmental burdens.

Microfluidic Remote Loading for Rapid Single-Step Liposomal Drug Preparation

PubMed Central

Hood, R.R.; Vreeland, W. N.; DeVoe, D.L.

2014-01-01

Microfluidic-directed formation of liposomes is combined with in-line sample purification and remote drug loading for single step, continuous-flow synthesis of nanoscale vesicles containing high concentrations of stably loaded drug compounds. Using an on-chip microdialysis element, the system enables rapid formation of large transmembrane pH and ion gradients, followed by immediate introduction of amphipathic drug for real-time remote loading into the liposomes. The microfluidic process enables in-line formation of drug-laden liposomes with drug:lipid molar ratios of up to 1.3, and a total on-chip residence time of approximately 3 min, representing a significant improvement over conventional bulk-scale methods which require hours to days for combined liposome synthesis and remote drug loading. The microfluidic platform may be further optimized to support real-time generation of purified liposomal drug formulations with high concentrations of drugs and minimal reagent waste for effective liposomal drug preparation at or near the point of care. PMID:25003823

Green heterogeneous Pd(II) catalyst produced from chitosan-cellulose micro beads for green synthesis of biaryls.

PubMed

Baran, Talat; Sargin, Idris; Kaya, Murat; Menteş, Ayfer

2016-11-05

In green catalyst systems, both the catalyst and the technique should be environmentally safe. In this study we designed a green palladium(II) catalyst for microwave-assisted Suzuki CC coupling reactions. The catalyst support was produced from biopolymers; chitosan and cellulose. The catalytic activity of the catalyst was tested on 16 substrates in solvent-free media and compared with those of commercial palladium salts. Reusability tests were done. The catalyst was also used in conventional reflux-heating system to demonstrate the efficiency of microwave heating method. We recorded high activity, selectivity and excellent TONs (6600) and TOFs (82500) just using a small catalyst loading (1.5×10(-3)mol%) in short reaction time (5min). The catalyst exhibited a long lifetime (9 runs). The findings indicated that both green chitosan/cellulose-Pd(II) catalyst and the microwave heating are suitable for synthesis of biaryl compounds by using Suzuki CC coupling reactions. Copyright © 2016 Elsevier Ltd. All rights reserved.

Encapsulation of biomaterials in porous glass-like matrices prepared via an aqueous colloidal sol-gel process

DOEpatents

Liu, Dean-Mo; Chen, I-Wei

2001-01-01

The present invention provides a process for the encapsulation of biologically important proteins into transparent, porous silica matrices by an alcohol-free, aqueous, colloidal sol-gel process, and to the biological materials encapsulated thereby. The process is exemplified by studies involving encapsulated cytochrome c, catalase, myoglobin, and hemoglobin, although non-proteinaceous biomaterials, such as active DNA or RNA fragments, cells or even tissues, may also be encapsulated in accordance with the present methods. Conformation, and hence activity of the biomaterial, is successfully retained after encapsulation as demonstrated by optical characterization of the molecules, even after long-term storage. The retained conformation of the biomaterial is strongly correlated to both the rate of gelation and the subsequent drying speed of the encapsulatng matrix. Moreover, in accordance with this process, gelation is accelerated by the use of a higher colloidal solid concentration and a lower synthesis pH than conventional methods, thereby enhancing structural stability and retained conformation of the biomaterials. Thus, the invention also provides a remarkable improvement in retaining the biological activity of the encapsulated biomaterial, as compared with those involved in conventional alkoxide-based processes. It further provides new methods for the quantitative and qualitative detection of test substances that are reactive to, or catalyzed by, the active, encapsulated biological materials.

Control of RNA synthesis in Escherichia coli after a shift to higher temperature.

PubMed Central

Ryals, J; Little, R; Bremer, H

1982-01-01

Parameters of RNA synthesis were measured after a temperature upshift in a pair of Escherichia coli B/r strains that are isogenic except for having relA and relA+ loci, to examine the cause for a reported anomaly in the correlation between guanosine tetraphosphate (ppGpp) and stable RNA (rRNA, tRNA) synthesis under such conditions. Two main results were: (i) the specific stable RNA gene activity (stable RNA per total RNA synthesis) correlated in the conventionally expected fashion with the level of ppGpp but was obscured by a nonspecific increase in the RNA chain elongation rate due to the higher temperature; (ii) the temperature upshift caused a transient reduction in the RNA polymerase activity (transcribing per total enzyme) that accounts for the previously observed oscillating RNA synthesis rate after a temperature shift. PMID:6179925

Radar cross-section reduction based on an iterative fast Fourier transform optimized metasurface

NASA Astrophysics Data System (ADS)

Song, Yi-Chuan; Ding, Jun; Guo, Chen-Jiang; Ren, Yu-Hui; Zhang, Jia-Kai

2016-07-01

A novel polarization insensitive metasurface with over 25 dB monostatic radar cross-section (RCS) reduction is introduced. The proposed metasurface is comprised of carefully arranged unit cells with spatially varied dimension, which enables approximate uniform diffusion of incoming electromagnetic (EM) energy and reduces the threat from bistatic radar system. An iterative fast Fourier transform (FFT) method for conventional antenna array pattern synthesis is innovatively applied to find the best unit cell geometry parameter arrangement. Finally, a metasurface sample is fabricated and tested to validate RCS reduction behavior predicted by full wave simulation software Ansys HFSSTM and marvelous agreement is observed.

Organic Dye Degradation Under Solar Irradiation by Hydrothermally Synthesized ZnS Nanospheres

NASA Astrophysics Data System (ADS)

Samanta, Dhrubajyoti; Chanu, T. Inakhunbi; Basnet, Parita; Chatterjee, Somenath

2018-02-01

The green synthesis of ZnS nanospheres using Citrus limetta (sweet lime) juice as a capping agent through a conventional hydrothermal method was studied. The particle size, morphology, chemical composition, band gap, and optical properties of the synthesized ZnS nanospheres were characterized using x-ray diffraction spectroscopy, field emission scanning electron microscopy, high-resolution transmission electron microscopy, and ultraviolet-visible spectroscopy. The photocatalytic activity of the ZnS nanospheres was evaluated by degradation of rhodamine B (RhB) and methyl orange (MO) under solar irradiation. Upon 150 min of solar irradiation, the extent of degradation was 94% and 77% for RhB and MO, respectively.

Bubble template synthesis of Sn2Nb2O7 hollow spheres for enhanced visible-light-driven photocatalytic hydrogen production.

PubMed

Zhou, Chao; Zhao, Yufei; Bian, Tong; Shang, Lu; Yu, Huijun; Wu, Li-Zhu; Tung, Chen-Ho; Zhang, Tierui

2013-10-28

Hierarchical Sn2Nb2O7 hollow spheres were prepared for the first time via a facile hydrothermal route using bubbles generated in situ from the decomposition of urea as soft templates. The as-obtained hollow spheres with a large specific surface area of 58.3 m(2) g(-1) show improved visible-light-driven photocatalytic H2 production activity in lactic acid aqueous solutions, about 4 times higher than that of the bulk Sn2Nb2O7 sample prepared by a conventional high temperature solid state reaction method.

Systemic Synthesis Questions [SSynQs] as Tools to Help Students to Build Their Cognitive Structures in a Systemic Manner

NASA Astrophysics Data System (ADS)

Hrin, Tamara N.; Fahmy, Ameen F. M.; Segedinac, Mirjana D.; Milenković, Dušica D.

2016-08-01

Many studies dedicated to the teaching and learning of organic chemistry courses have emphasized that high school students have shown significant difficulties in mastering the concepts of this discipline. Therefore, the aim of our study was to help students to overcome these difficulties by applying systemic synthesis questions, [SSynQs], as the instructional method in our intervention. This work shows that students from the group exposed to the new teaching method achieved higher scores on final testing than students from the control group, who were taught by the traditional method, when students' achievements in conventional, linear questions [LQs] and in [SSynQs] were studied. These results were followed by observation of lower levels of mental effort by students from the intervention group, and higher levels of mental effort in the control group, invested during solving both types of questions. This correlation between achievement and mental effort resulted in high instructional efficiency for the applied method in the intervention group, [SSynQs], and low instructional efficiency for the traditional teaching and learning method applied in the control group. A systemic triangular relation between achievement, mental effort, and instructional efficiency, established by each group and gender, emphasized that the application of [SSynQs] was more suited to female students than for male students because of [SSynQs] characteristics as teaching and learning tools and because of learning style and ability differences between genders.

Y3Fe5O12 nanoparticulate garnet ferrites: Comprehensive study on the synthesis and characterization fabricated by various routes

NASA Astrophysics Data System (ADS)

Niaz Akhtar, Majid; Azhar Khan, Muhammad; Ahmad, Mukhtar; Murtaza, G.; Raza, Rizwan; Shaukat, S. F.; Asif, M. H.; Nasir, Nadeem; Abbas, Ghazanfar; Nazir, M. S.; Raza, M. R.

2014-11-01

The effects of synthesis methods such as sol-gel (SG), self combustion (SC) and modified conventional mixed oxide (MCMO) on the structure, morphology and magnetic properties of the (Y3Fe5O12) garnet ferrites have been studied in the present work. The samples of Y3Fe5O12 were sintered at 950 °C and 1150 °C (by SG and SC methods). For MCMO route the sintering was done at 1350 °C for 6 h. Synthesized samples prepared by various routes were investigated using X-ray diffraction (XRD) analysis, Field emission scanning electron microscopy (FESEM), Impedance network analyzer and transmission electron microscopy (TEM). The structural analysis reveals that the samples are of single phase structure and shows variations in the particle sizes and cells volumes, prepared by various routes. FESEM and TEM images depict that grain size increases with the increase of sintering temperature from 40 nm to 100 nm.Magnetic measurements reveal that garnet ferrite synthesized by sol gel method has high initial permeability (60.22) and low magnetic loss (0.0004) as compared to other garnet ferrite samples, which were synthesized by self combustion and MCMO methods. The M-H loops exhibit very low coercivity which enables the use of these materials in relays and switching devices fabrications. Thus, the garnet nanoferrites with low magnetic loss prepared by different methods may open new horizon for electronic industry for their use in high frequency applications.

Synthesis of SnS nanoparticles by SILAR method for quantum dot-sensitized solar cells.

PubMed

Tsukigase, Hiroki; Suzuki, Yoshikazu; Berger, Marie-Hélène; Sagawa, Takashi; Yoshikawa, Susumu

2011-03-01

SnS-sensitized TiO2 electrodes were applied in quantum dot-sensitized solar cells (QDSSCs) which are environmentally more favorable than conventional Cd or Pb-chalcogenide-sensitized electrodes. SnS nanoparticles were well-distributed over the surface of TiO2 nanoparticles by the successive ionic layer adsorption and reaction (SILAR) method. Deposited SnS nanoparticles had diameter about 3 nm. Under AM1.5 irradiation with 100 mW/cm2 light intensity (at 1 sun), the energy conversion efficiency of obtained cells reached a value of 0.21% (0.25 cm2) at SILAR coating cycles of 5. In addition, the photovoltaic performance was improved by additional ZnS coating on the surface of SnS-sensitized TiO2 electrodes.

Design of transmission-type phase holograms for a compact radar-cross-section measurement range at 650 GHz.

PubMed

Noponen, Eero; Tamminen, Aleksi; Vaaja, Matti

2007-07-10

A design formalism is presented for transmission-type phase holograms for use in a submillimeter-wave compact radar-cross-section (RCS) measurement range. The design method is based on rigorous electromagnetic grating theory combined with conventional hologram synthesis. Hologram structures consisting of a curved groove pattern on a 320 mmx280 mm Teflon plate are designed to transform an incoming spherical wave at 650 GHz into an output wave generating a 100 mm diameter planar field region (quiet zone) at a distance of 1 m. The reconstructed quiet-zone field is evaluated by a numerical simulation method. The uniformity of the quiet-zone field is further improved by reoptimizing the goal field. Measurement results are given for a test hologram fabricated on Teflon.

Preparation of well-defined erythromycin imprinted non-woven fabrics via radiation-induced RAFT-mediated grafting

NASA Astrophysics Data System (ADS)

Söylemez, Meshude Akbulut; Barsbay, Murat; Güven, Olgun

2018-01-01

Radiation-induced RAFT polymerization technique was applied to synthesize well-defined molecularly imprinted polymers (MIPs) of erythromycin (ERY). Methacrylic acid (MAA) was grafted onto porous polyethylene (PE)/polypropylene (PP) nonwoven fabrics, under γ-irradiation by employing 2-pheny-2-propyl benzodithioate as the RAFT agent and ethylene glycol dimethacrylate (EGDMA) as the crosslinker. MAA/erythromycin ratios of 2/1, 4/1, 6/1 were tested to optimize the synthesis of MIPs. The highest binding capacity was encountered at a MAA/ERY ratio of 4/1. Non-imprinted polymers (NIPs) were also synthesized in the absence of ERY. The MIPs synthesized by RAFT method presented a better binding capacity compared to those prepared by conventional method where no RAFT agent was employed.

Synthesis of Silver Polymer Nanocomposites and Their Antibacterial Activity

NASA Astrophysics Data System (ADS)

Gavade, Chaitali; Shah, Sunil; Singh, N. L.

2011-07-01

PVA (Polyvinyl Alcohol) silver nanocomposites of different sizes were prepared by chemical reduction method. Silver nitrate was taken as the metal precursor and amine hydrazine as a reducing agent. The formation of the silver nanoparticles was noticed using UV- visible absorption spectroscopy. The UV-visible spectroscopy revealed the formation of silver nanoparticles by exhibiting the surface plasmon resonance. The bactericidal activity due to silver release from the surface was determined by the modification of conventional diffusion method. Salmonella typhimurium, Serratia sps and Shigella sps were used as test bacteria which are gram-negative type bacteria. Effect of the different sizes of silver nano particles on antibacterial efficiency was discussed. Zones of inhibition were measured after 24 hours of incubation at 37 °C which gave 20 mm radius for high concentration of silver nanoparticles.

Metal-chelate dye-controlled organization of Cd32S14(SPh)40(4-) nanoclusters into three-dimensional molecular and covalent open architecture.

PubMed

Zheng, Nanfeng; Lu, Haiwei; Bu, Xianhui; Feng, Pingyun

2006-04-12

Chalcogenide II-VI nanoclusters are usually prepared as isolated clusters and have defied numerous efforts to join them into covalent open-framework architecture with conventional templating methods such as protonated amines or inorganic cations commonly used to direct the formation of porous frameworks. Herein, we report the first templated synthesis of II-VI covalent superlattices from large II-VI tetrahedral clusters (i.e., [Cd32S14(SPh)38]2-). Our method takes advantage of low charge density of metal-chelate dyes that is a unique match with three-dimensional II-VI semiconductor frameworks in charge density, surface hydrophilicity-hydrophobicity, and spatial organization. In addition, metal-chelate dyes also serve to tune the optical properties of resulting dye semiconductor composite materials.

Facile synthesis and antibacterial, antitubercular, and anticancer activities of novel 1,4-dihydropyridines.

PubMed

Sirisha, Kalam; Achaiah, Garlapati; Reddy, Vanga Malla

2010-06-01

A series of twenty new 4-substituted-2,6-dimethyl-3,5-bis-N-(heteroaryl)-carbamoyl-1,4-dihydropyridines have been prepared from a three-component one-pot condensation reaction of N-heteroaryl acetoacetamide, an aromatic/heteroaromatic aldehyde, and ammonium acetate under four different experimental conditions. Except for the conventional method, all the experimental conditions were simple, eco-friendly, economical, and the reactions were rapid and high-yielding. The methods employed have been compared in terms of yields, cost, and simplicity. The synthesized compounds were characterized by different spectroscopic techniques and evaluated for their in-vitro anticancer, antibacterial, and antitubercular activities. Amongst the compounds tested, compound 25 exhibited the highest anticancer activity while compounds 14 and 18 exhibited significant antibacterial and antitubercular activities.

Synthesis of Conformationally North-Locked Pyrimidine Nucleosides Built on an Oxabicyclo[3.1.0]hexane Scaffold | Center for Cancer Research

Cancer.gov

Beginning with a known 3-oxabicyclo[3.1.0]-hexane scaffold, the relocation of the fused cyclopropane ring bond and the shifting of the oxygen atom to an alternative location engendered a new 2-oxabicyclo[3.1.0]hexane template that mimics more closely the tetrahydrofuran ring of conventional nucleosides. The synthesis of this new class of locked nucleosides involved a novel

Ion beams provided by small accelerators for material synthesis and characterization

NASA Astrophysics Data System (ADS)

Mackova, Anna; Havranek, Vladimir

2017-06-01

The compact, multipurpose electrostatic tandem accelerators are extensively used for production of ion beams with energies in the range from 400 keV to 24 MeV of almost all elements of the periodic system for the trace element analysis by means of nuclear analytical methods. The ion beams produced by small accelerators have a broad application, mainly for material characterization (Rutherford Back-Scattering spectrometry, Particle Induced X ray Emission analysis, Nuclear Reaction Analysis and Ion-Microprobe with 1 μm lateral resolution among others) and for high-energy implantation. Material research belongs to traditionally progressive fields of technology. Due to the continuous miniaturization, the underlying structures are far beyond the analytical limits of the most conventional methods. Ion Beam Analysis (IBA) techniques provide this possibility as they use probes of similar or much smaller dimensions (particles, radiation). Ion beams can be used for the synthesis of new progressive functional nanomaterials for optics, electronics and other applications. Ion beams are extensively used in studies of the fundamental energetic ion interaction with matter as well as in the novel nanostructure synthesis using ion beam irradiation in various amorphous and crystalline materials in order to get structures with extraordinary functional properties. IBA methods serve for investigation of materials coming from material research, industry, micro- and nano-technology, electronics, optics and laser technology, chemical, biological and environmental investigation in general. Main research directions in laboratories employing small accelerators are also the preparation and characterization of micro- and nano-structured materials which are of interest for basic and oriented research in material science, and various studies of biological, geological, environmental and cultural heritage artefacts are provided too.

Interpenetrating Polymer Networks as Innovative Drug Delivery Systems

PubMed Central

Lohani, Alka; Singh, Garima; Bhattacharya, Shiv Sankar; Verma, Anurag

2014-01-01

Polymers have always been valuable excipients in conventional dosage forms, also have shown excellent performance into the parenteral arena, and are now capable of offering advanced and sophisticated functions such as controlled drug release and drug targeting. Advances in polymer science have led to the development of several novel drug delivery systems. Interpenetrating polymer networks (IPNs) have shown superior performances over the conventional individual polymers and, consequently, the ranges of applications have grown rapidly for such class of materials. The advanced properties of IPNs like swelling capacity, stability, biocompatibility, nontoxicity and biodegradability have attracted considerable attention in pharmaceutical field especially in delivering bioactive molecules to the target site. In the past few years various research reports on the IPN based delivery systems showed that these carriers have emerged as a novel carrier in controlled drug delivery. The present review encompasses IPNs, their types, method of synthesis, factors which affects the morphology of IPNs, extensively studied IPN based drug delivery systems, and some natural polymers widely used for IPNs. PMID:24949205

Roll-to-Roll Laser-Printed Graphene-Graphitic Carbon Electrodes for High-Performance Supercapacitors.

PubMed

Kang, Sangmin; Lim, Kyungmi; Park, Hyeokjun; Park, Jong Bo; Park, Seong Chae; Cho, Sung-Pyo; Kang, Kisuk; Hong, Byung Hee

2018-01-10

Carbon electrodes including graphene and thin graphite films have been utilized for various energy and sensor applications, where the patterning of electrodes is essentially included. Laser scribing in a DVD writer and inkjet printing were used to pattern the graphene-like materials, but the size and speed of fabrication has been limited for practical applications. In this work, we devise a simple strategy to use conventional laser-printer toner materials as precursors for graphitic carbon electrodes. The toner was laser-printed on metal foils, followed by thermal annealing in hydrogen environment, finally resulting in the patterned thin graphitic carbon or graphene electrodes for supercapacitors. The electrochemical cells made of the graphene-graphitic carbon electrodes show remarkably higher energy and power performance compared to conventional supercapacitors. Furthermore, considering the simplicity and scalability of roll-to-roll (R2R) electrode patterning processes, the proposed method would enable cheaper and larger-scale synthesis and patterning of graphene-graphitic carbon electrodes for various energy applications in the future.

Developing New Antimicrobial Therapies: Are Synergistic Combinations of Plant Extracts/Compounds with Conventional Antibiotics the Solution?

PubMed Central

Cheesman, Matthew J.; Ilanko, Aishwarya; Blonk, Baxter; Cock, Ian E.

2017-01-01

The discovery of penicillin nearly 90 years ago revolutionized the treatment of bacterial disease. Since that time, numerous other antibiotics have been discovered from bacteria and fungi, or developed by chemical synthesis and have become effective chemotherapeutic options. However, the misuse of antibiotics has lessened the efficacy of many commonly used antibiotics. The emergence of resistant strains of bacteria has seriously limited our ability to treat bacterial illness, and new antibiotics are desperately needed. Since the discovery of penicillin, most antibiotic development has focused on the discovery of new antibiotics derived from microbial sources, or on the synthesis of new compounds using existing antibiotic scaffolds to the detriment of other lines of discovery. Both of these methods have been fruitful. However, for a number of reasons discussed in this review, these strategies are unlikely to provide the same wealth of new antibiotics in the future. Indeed, the number of newly developed antibiotics has decreased dramatically in recent years. Instead, a reexamination of traditional medicines has become more common and has already provided several new antibiotics. Traditional medicine plants are likely to provide further new antibiotics in the future. However, the use of plant extracts or pure natural compounds in combination with conventional antibiotics may hold greater promise for rapidly providing affordable treatment options. Indeed, some combinational antibiotic therapies are already clinically available. This study reviews the recent literature on combinational antibiotic therapies to highlight their potential and to guide future research in this field. PMID:28989242

Developing New Antimicrobial Therapies: Are Synergistic Combinations of Plant Extracts/Compounds with Conventional Antibiotics the Solution?

PubMed

Cheesman, Matthew J; Ilanko, Aishwarya; Blonk, Baxter; Cock, Ian E

2017-01-01

The discovery of penicillin nearly 90 years ago revolutionized the treatment of bacterial disease. Since that time, numerous other antibiotics have been discovered from bacteria and fungi, or developed by chemical synthesis and have become effective chemotherapeutic options. However, the misuse of antibiotics has lessened the efficacy of many commonly used antibiotics. The emergence of resistant strains of bacteria has seriously limited our ability to treat bacterial illness, and new antibiotics are desperately needed. Since the discovery of penicillin, most antibiotic development has focused on the discovery of new antibiotics derived from microbial sources, or on the synthesis of new compounds using existing antibiotic scaffolds to the detriment of other lines of discovery. Both of these methods have been fruitful. However, for a number of reasons discussed in this review, these strategies are unlikely to provide the same wealth of new antibiotics in the future. Indeed, the number of newly developed antibiotics has decreased dramatically in recent years. Instead, a reexamination of traditional medicines has become more common and has already provided several new antibiotics. Traditional medicine plants are likely to provide further new antibiotics in the future. However, the use of plant extracts or pure natural compounds in combination with conventional antibiotics may hold greater promise for rapidly providing affordable treatment options. Indeed, some combinational antibiotic therapies are already clinically available. This study reviews the recent literature on combinational antibiotic therapies to highlight their potential and to guide future research in this field.

The Flight Optimization System Weights Estimation Method

NASA Technical Reports Server (NTRS)

Wells, Douglas P.; Horvath, Bryce L.; McCullers, Linwood A.

2017-01-01

FLOPS has been the primary aircraft synthesis software used by the Aeronautics Systems Analysis Branch at NASA Langley Research Center. It was created for rapid conceptual aircraft design and advanced technology impact assessments. FLOPS is a single computer program that includes weights estimation, aerodynamics estimation, engine cycle analysis, propulsion data scaling and interpolation, detailed mission performance analysis, takeoff and landing performance analysis, noise footprint estimation, and cost analysis. It is well known as a baseline and common denominator for aircraft design studies. FLOPS is capable of calibrating a model to known aircraft data, making it useful for new aircraft and modifications to existing aircraft. The weight estimation method in FLOPS is known to be of high fidelity for conventional tube with wing aircraft and a substantial amount of effort went into its development. This report serves as a comprehensive documentation of the FLOPS weight estimation method. The development process is presented with the weight estimation process.

Synthesis and Stabilization of Supported Metal Catalysts by Atomic Layer Deposition

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

Lu, Junling; Elam, Jeffrey W.; Stair, Peter C.

2013-03-12

Supported metal nanoparticles are among the most important cata-lysts for many practical reactions, including petroleum refining, automobile exhaust treatment, and Fischer–Tropsch synthesis. The catalytic performance strongly depends on the size, composition, and structure of the metal nanoparticles, as well as the underlying support. Scientists have used conventional synthesis methods including impregnation, ion exchange, and deposition–precipitation to control and tune these factors, to establish structure–performance relationships, and to develop better catalysts. Meanwhile, chemists have improved the stability of metal nanoparticles against sintering by the application of protective layers, such as polymers and oxides that encapsulate the metal particle. This often leadsmore » to decreased catalytic activity due to a lack of precise control over the thickness of the protective layer. A promising method of catalyst synthesis is atomic layer deposition (ALD). ALD is a variation on chemical vapor deposition in which metals, oxides, and other materials are deposited on surfaces by a sequence of self-limiting reactions. The self-limiting character of these reactions makes it possible to achieve uniform deposits on high-surface-area porous solids. Therefore, design and synthesis of advanced catalysts on the nanoscale becomes possible through precise control over the structure and composition of the underlying support, the catalytic active sites, and the protective layer. In this Account, we describe our advances in the synthesis and stabilization of supported metal catalysts by ALD. After a short introduction to the technique of ALD, we show several strategies for metal catalyst synthesis by ALD that take advantage of its self-limiting feature. Monometallic and bimetallic catalysts with precise control over the metal particle size, composition, and structure were achieved by combining ALD sequences, surface treatments, and deposition temperature control. Next, we describe ALD oxide overcoats applied with atomically precise thickness control that stabilize metal catalysts while preserving their catalytic function. We also discuss strategies for generation and control over the porosity of the overcoats that allow the embedded metal particles to remain accessible by reactants, and the details for ALD alumina overcoats on metal catalysts. Moreover, using methanol decomposition and oxidative dehydrogenation of ethane as probe reactions, we demonstrate that selectively blocking low coordination metal sites by oxide overcoats can provide another strategy to enhance both the durability and selectivity of metal catalysts.« less

Cavitation assisted synthesis of fatty acid methyl esters from sustainable feedstock in presence of heterogeneous catalyst using two step process.

PubMed

Dubey, Sumit M; Gole, Vitthal L; Gogate, Parag R

2015-03-01

The present work reports the intensification aspects for the synthesis of fatty acid methyl esters (FAME) from a non-edible high acid value Nagchampa oil (31 mg of KOH/g of oil) using two stage acid esterification (catalyzed by H₂SO₄) followed by transesterification in the presence of heterogeneous catalyst (CaO). Intensification aspects of both stages have been investigated using sonochemical reactors and the obtained degree of intensification has been established by comparison with the conventional approach based on mechanical agitation. It has been observed that reaction temperature for esterification reduced from 65 to 40 °C for the ultrasonic approach whereas there was a significant reduction in the optimum reaction time for transesterification from 4h for the conventional approach to 2.5h for the ultrasound assisted approach. Also the reaction temperature reduced marginally from 65 to 60 °C and yield increased from 76% to 79% for the ultrasound assisted approach. Energy requirement and activation energy for both esterification and transesterification was lower for the ultrasound based approach as compared to the conventional approach. The present work has clearly established the intensification obtained due to the use of ultrasound and also illustrated the two step approach for the synthesis of FAME from high acid value feedstock based on the use of heterogeneous catalyst for the transesterification step. Copyright © 2014 Elsevier B.V. All rights reserved.

Conventional hydrothermal synthesis of Na-A zeolite from cupola slag and aluminum sludge.

PubMed

Anuwattana, Rewadee; Khummongkol, Pojanie

2009-07-15

Na-A type zeolites were prepared from two industrial wastes: the solid by-product of cupola slag and aluminum sludge from an aluminum plating plant. Two preparation methods using the same starting material compositions were carried out. In the first method, alkaline fusion was introduced, followed by the hydrothermal treatment to obtain sodium aluminosilicate which was then crystallized in NaOH solution under the condition of 90+/-3 degrees C for 1-9h with different H(2)O/SiO2 ratios. The result shows that higher H(2)O/SiO2 ratio increases the rate of crystallization. The largest amount of crystallinity for Na-A was found at 3h. In the second method, alkaline hydrothermal treatment without fusion was carried out in the same condition as the first method. No Na-A zeolite was obtained by this method. The changes of the dissolved amounts of Si(4+) and Al(3+) in 3M NaOH were investigated during the hydrothermal reaction.

Knowledge synthesis methods for integrating qualitative and quantitative data: a scoping review reveals poor operationalization of the methodological steps.

PubMed

Tricco, Andrea C; Antony, Jesmin; Soobiah, Charlene; Kastner, Monika; MacDonald, Heather; Cogo, Elise; Lillie, Erin; Tran, Judy; Straus, Sharon E

2016-05-01

To describe and compare, through a scoping review, emerging knowledge synthesis methods for integrating qualitative and quantitative evidence in health care, in terms of expertise required, similarities, differences, strengths, limitations, and steps involved in using the methods. Electronic databases (e.g., MEDLINE) were searched, and two reviewers independently selected studies and abstracted data for qualitative analysis. In total, 121 articles reporting seven knowledge synthesis methods (critical interpretive synthesis, integrative review, meta-narrative review, meta-summary, mixed studies review, narrative synthesis, and realist review) were included after screening of 17,962 citations and 1,010 full-text articles. Common similarities among methods related to the entire synthesis process, while common differences related to the research question and eligibility criteria. The most common strength was a comprehensive synthesis providing rich contextual data, whereas the most common weakness was a highly subjective method that was not reproducible. For critical interpretive synthesis, meta-narrative review, meta-summary, and narrative synthesis, guidance was not provided for some steps of the review process. Some of the knowledge synthesis methods provided guidance on all steps, whereas other methods were missing guidance on the synthesis process. Further work is needed to clarify these emerging knowledge synthesis methods. Copyright © 2016 Elsevier Inc. All rights reserved.

Biogenic synthesis of metallic nanoparticles and prospects toward green chemistry.

PubMed

Adil, Syed Farooq; Assal, Mohamed E; Khan, Mujeeb; Al-Warthan, Abdulrahman; Siddiqui, Mohammed Rafiq H; Liz-Marzán, Luis M

2015-06-07

The immense importance of nanoparticles and their applications is a strong motivation for exploring new synthetic techniques. However, due to strict regulations that manage the potential environmental impacts greener alternatives for conventional synthesis are the focus of intense research. In the scope of this perspective, a concise discussion about the use of green reducing and stabilizing agents toward the preparation of metal nanoparticles is presented. Reports on the synthesis of noble metal nanoparticles using plant extracts, ascorbic acid and sodium citrate as green reagents are summarized and discussed, pointing toward an urgent need of understanding the mechanistic aspects of the involved reactions.

Conceptual design of single turbofan engine powered light aircraft

NASA Technical Reports Server (NTRS)

Snyder, F. S.; Voorhees, C. G.; Heinrich, A. M.; Baisden, D. N.

1977-01-01

The conceptual design of a four place single turbofan engine powered light aircraft was accomplished utilizing contemporary light aircraft conventional design techniques as a means of evaluating the NASA-Ames General Aviation Synthesis Program (GASP) as a preliminary design tool. In certain areas, disagreement or exclusion were found to exist between the results of the conventional design and GASP processes. Detail discussion of these points along with the associated contemporary design methodology are presented.

Green synthesis of silver nanoparticles via plant extracts: beginning a new era in cancer theranostics.

PubMed

Ovais, Muhammad; Khalil, Ali Talha; Raza, Abida; Khan, Muhammad Adeeb; Ahmad, Irshad; Islam, Nazar Ul; Saravanan, Muthupandian; Ubaid, Muhammad Furqan; Ali, Muhammad; Shinwari, Zabta Khan

2016-12-01

With the development of the latest technologies, scientists are looking to design novel strategies for the treatment and diagnosis of cancer. Advances in medicinal plant research and nanotechnology have attracted many researchers to the green synthesis of metallic nanoparticles due to its several advantages over conventional synthesis (simple, fast, energy efficient, one pot processes, safer, economical and biocompatibility). Medicinally active plants have proven to be the best reservoirs of diverse phytochemicals for the synthesis of biogenic silver nanoparticles (AgNPs). In this review, we discuss mechanistic advances in the synthesis and optimization of AgNPs from plant extracts. Moreover, we have thoroughly discussed the recent developments and milestones achieved in the use of biogenic AgNPs as cancer theranostic agents and their proposed mechanism of action. Anticipating all of the challenges, we hope that biogenic AgNPs may become a potential cancer theranostic agent in the near future.

Chronological protein synthesis in regenerating rat liver.

PubMed

He, Jinjun; Hao, Shuai; Zhang, Hao; Guo, Fuzheng; Huang, Lingyun; Xiao, Xueyuan; He, Dacheng

2015-07-01

Liver regeneration has been studied for decades; however, its regulation remains unclear. In this study, we report a dynamic tracing of protein synthesis in rat regenerating liver with a new proteomic technique, (35) S in vivo labeling analysis for dynamic proteomics (SiLAD). Conventional proteomic techniques typically measure protein alteration in accumulated amounts. The SiLAD technique specifically detects protein synthesis velocity instead of accumulated amounts of protein through (35) S pulse labeling of newly synthesized proteins, providing a direct way for analyzing protein synthesis variations. Consequently, protein synthesis within short as 30 min was visualized and protein regulations in the first 8 h of regenerating liver were dynamically traced. Further, the 3.5-5 h post partial hepatectomy (PHx) was shown to be an important regulatory turning point by acute regulation of many proteins in the initiation of liver regeneration. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Laser direct synthesis and patterning of silver nano/microstructures on a polymer substrate.

PubMed

Liu, Yi-Kai; Lee, Ming-Tsang

2014-08-27

This study presents a novel approach for the rapid fabrication of conductive nano/microscale metal structures on flexible polymer substrate (polyimide). Silver film is simultaneously synthesized and patterned on the polyimide substrate using an advanced continuous wave (CW) laser direct writing technology and a transparent, particle-free reactive silver ion ink. The location and shape of the resulting silver patterns are written by a laser beam from a digitally controlled micromirror array device. The silver patterns fabricated by this laser direct synthesis and patterning (LDSP) process exhibit the remarkably low electrical resistivity of 2.1 μΩ cm, which is compatible to the electrical resistivity of bulk silver. This novel LDSP process requires no vacuum chamber or photomasks, and the steps needed for preparation of the modified reactive silver ink are simple and straightforward. There is none of the complexity and instability associated with the synthesis of the nanoparticles that are encountered for the conventional laser direct writing technology which involves nanoparticle sintering process. This LDSP technology is an advanced method of nano/microscale selective metal patterning on flexible substrates that is fast and environmentally benign and shows potential as a feasible process for the roll-to-roll manufacturing of large area flexible electronic devices.

Synthesis of antiviral tetrahydrocarbazole derivatives by photochemical and acid-catalyzed C-H functionalization via intermediate peroxides (CHIPS).

PubMed

Gulzar, Naeem; Klussmann, Martin

2014-06-20

The direct functionalization of C-H bonds is an important and long standing goal in organic chemistry. Such transformations can be very powerful in order to streamline synthesis by saving steps, time and material compared to conventional methods that require the introduction and removal of activating or directing groups. Therefore, the functionalization of C-H bonds is also attractive for green chemistry. Under oxidative conditions, two C-H bonds or one C-H and one heteroatom-H bond can be transformed to C-C and C-heteroatom bonds, respectively. Often these oxidative coupling reactions require synthetic oxidants, expensive catalysts or high temperatures. Here, we describe a two-step procedure to functionalize indole derivatives, more specifically tetrahydrocarbazoles, by C-H amination using only elemental oxygen as oxidant. The reaction uses the principle of C-H functionalization via Intermediate PeroxideS (CHIPS). In the first step, a hydroperoxide is generated oxidatively using visible light, a photosensitizer and elemental oxygen. In the second step, the N-nucleophile, an aniline, is introduced by Brønsted-acid catalyzed activation of the hydroperoxide leaving group. The products of the first and second step often precipitate and can be conveniently filtered off. The synthesis of a biologically active compound is shown.

Facile chemical synthesis and equilibrium unfolding properties of CopG

PubMed Central

Wales, Thomas E.; Richardson, Jane S.; Fitzgerald, Michael C.

2004-01-01

The 45-amino acid polypeptide chain of the homodimeric transcriptional repressor, CopG, was chemically synthesized by stepwise solid phase peptide synthesis (SPPS) using a protocol based on Boc-chemistry. The product obtained from the synthesis was readily purified by reversed-phase HPLC to give a good overall yield (21% by weight). Moreover, the synthetic CopG constructs prepared in this work folded into three-dimensional structures similar to the wild-type protein prepared using conventional recombinant methods as judged by far UV-CD spectroscopy. A fluorescent CopG analog, (Y39W)CopG, was also designed and chemically synthesized to facilitate biophysical studies of CopG’s protein folding and assembly reaction. The guanidinium chloride-induced equilibrium unfolding properties of the wild-type CopG and (Y39W)CopG constructs in this work were characterized and used to develop a model for CopG’s equilibrium unfolding reaction. Our results indicate that CopG’s folding and assembly reaction is well modeled by a two-state process involving folded dimer and unfolded monomer. Using this model, ΔGf and m-values of −13.42 ± 0.04 kcal/mole dimer and 1.92 ± 0.01 kcal/(mole M) were calculated for CopG. PMID:15169951

Repetitively Coupled Chemical Reduction and Galvanic Exchange as a Synthesis Strategy for Expanding Applicable Number of Pt Atoms in Dendrimer-Encapsulated Pt Nanoparticles.

PubMed

Cho, Taehoon; Yoon, Chang Won; Kim, Joohoon

2018-06-13

In this study, we report the controllable synthesis of dendrimer-encapsulated Pt nanoparticles (Pt DENs) utilizing repetitively coupled chemical reduction and galvanic exchange reactions. The synthesis strategy allows the expansion of the applicable number of Pt atoms encapsulated inside dendrimers to more than 1000 without being limited by the fixed number of complexation sites for Pt 2+ precursor ions in the dendrimers. The synthesis of Pt DENs is achieved in a short period of time (i.e., ∼10 min) simply by the coaddition of appropriate amounts of Cu 2+ and Pt 2+ precursors into aqueous dendrimer solution and subsequent addition of reducing agents such as BH 4 - , resulting in fast and selective complexation of Cu 2+ with the dendrimers and subsequent chemical reduction of the complexed Cu 2+ while uncomplexed Pt 2+ precursors remain oxidized. Interestingly, the chemical reduction of Cu 2+ , leading to the formation of Cu nanoparticles encapsulated inside the dendrimers, is coupled with the galvanic exchange of the Cu nanoparticles with the nearby Pt 2+ . This coupling repetitively proceeds until all of the added Pt 2+ ions form into Pt nanoparticles encapsulated inside the dendrimers. In contrast to the conventional method utilizing direct chemical reduction, this repetitively coupled chemical reduction and galvanic exchange enables a substantial increase in the applicable number of Pt atoms up to 1320 in Pt DENs while maintaining the unique features of DENs.

Synthesis and Characterization of Cobalt Containing Nanoparticles on Alumina A Potential Catalyst for Gas to Liquid Fuels Production

NASA Technical Reports Server (NTRS)

Cowen, Jonathan; Hepp, Aloysius F.

2016-01-01

Fisher-Tröpsch synthesis (FTS) is a century-old gas-to-liquid (GTL) technology that commonly employs cobalt (Co, on an oxide support) or iron (supported or not) species catalysts. It has been well established that the activity of the Co catalyst depends directly upon the number of surface Co atoms. The addition of promoter (mainly noble) metals has been widely utilized to increase the fraction of Co that is available for surface catalysis. Direct synthesis of Co nanoparticles is a possible alternative approach; our preliminary synthesis and characterization efforts are described. Materials were characterized by various transmission microscopies and energy dispersive spectroscopy. Tri-n-octylphosphine oxide (TOPO) and dicobalt octacarbonyl were heated under argon to a temperature of 180 deg with constant stirring for 1 hr. Quenching the reaction in toluene produced Co-containing nanoparticles with a diameter of 5 to 10 nm. Alternatively, an alumina support (SBA-200 Al2O3) was added; the reaction was further stirred and the temperature was decreased to 140 deg to reduce the rate of further growth/ripening of the nucleated Co nanoparticles. A typical size of Co-containing NPs was also found to be in the range of 5 to 10 nm. This can be contrasted with a range of 50 to 200 nm for conventionally-produced Co-Al2O3 Fischer-Tröpsch catalysts. This method shows great potential for production of highly dispersed catalysts that are either supported or unsupported.

Precursor Mediated Synthesis of Nanostructured Silicas: From Precursor-Surfactant Ion Pairs to Structured Materials

PubMed Central

Hesemann, Peter; Nguyen, Thy Phung; Hankari, Samir El

2014-01-01

The synthesis of nanostructured anionic-surfactant-templated mesoporous silica (AMS) recently appeared as a new strategy for the formation of nanostructured silica based materials. This method is based on the use of anionic surfactants together with a co-structure-directing agent (CSDA), mostly a silylated ammonium precursor. The presence of this CSDA is necessary in order to create ionic interactions between template and silica forming phases and to ensure sufficient affinity between the two phases. This synthetic strategy was for the first time applied in view of the synthesis of surface functionalized silica bearing ammonium groups and was then extended on the formation of materials functionalized with anionic carboxylate and bifunctional amine-carboxylate groups. In the field of silica hybrid materials, the “anionic templating” strategy has recently been applied for the synthesis of silica hybrid materials from cationic precursors. Starting from di- or oligosilylated imidazolium and ammonium precursors, only template directed hydrolysis-polycondensation reactions involving complementary anionic surfactants allowed accessing structured ionosilica hybrid materials. The mechanistic particularity of this approach resides in the formation of precursor-surfactant ion pairs in the hydrolysis-polycondensation mixture. This review gives a systematic overview over the various types of materials accessed from this cooperative ionic templating approach and highlights the high potential of this original strategy for the formation of nanostructured silica based materials which appears as a complementary strategy to conventional soft templating approaches. PMID:28788602

Associative Memory Synthesis, Performance, Storage Capacity And Updating: New Heteroassociative Memory Results

NASA Astrophysics Data System (ADS)

Casasent, David; Telfer, Brian

1988-02-01

The storage capacity, noise performance, and synthesis of associative memories for image analysis are considered. Associative memory synthesis is shown to be very similar to that of linear discriminant functions used in pattern recognition. These lead to new associative memories and new associative memory synthesis and recollection vector encodings. Heteroassociative memories are emphasized in this paper, rather than autoassociative memories, since heteroassociative memories provide scene analysis decisions, rather than merely enhanced output images. The analysis of heteroassociative memories has been given little attention. Heteroassociative memory performance and storage capacity are shown to be quite different from those of autoassociative memories, with much more dependence on the recollection vectors used and less dependence on M/N. This allows several different and preferable synthesis techniques to be considered for associative memories. These new associative memory synthesis techniques and new techniques to update associative memories are included. We also introduce a new SNR performance measure that is preferable to conventional noise standard deviation ratios.

Effects of conventional and a novel colonic-release bile acid sequestrant, A3384, on fibroblast growth factor 19 and bile acid metabolism in healthy volunteers and patients with bile acid diarrhoea

PubMed Central

Bajor, A; Gillberg, P-G; Graffner, H; Simrén, M; Ung, KA; Walters, JRF

2016-01-01

Background Primary bile acid diarrhoea (BAD) is associated with increased bile acid synthesis and low fibroblast growth factor 19 (FGF19). Bile acid sequestrants are used as therapy, but are poorly tolerated and may exacerbate FGF19 deficiency. Aim The purpose of this study was to evaluate the pharmacological effects of conventional sequestrants and a colonic-release formulation preparation of colestyramine (A3384) on bile acid metabolism and bowel function in patients with BAD. Methods Patients with seven-day 75selenium-homocholic acid taurine (SeHCAT) scan retention <10% were randomised in a double-blind protocol to two weeks treatment with twice-daily A3384 250 mg (n = 6), 1 g (n = 7) or placebo (n = 6). Thirteen patients were taking conventional sequestrants at the start of the study. Symptoms were recorded and serum FGF19 and 7α-hydroxy-4-cholesten-3-one (C4) measured. Results Median serum FGF19 on conventional sequestrant treatment was 28% lower than baseline values in BAD (p < 0.05). C4 on conventional sequestrant treatment was 58% higher in BAD (p < 0.001). No changes were seen on starting or withdrawing A3384. A3384 improved diarrhoeal symptoms, with a median reduction of 2.2 points on a 0–10 Likert scale compared to placebo, p < 0.05. Conclusions Serum FGF19 was suppressed and bile acid production up-regulated on conventional bile acid sequestrants, but not with A3384. This colonic-release formulation of colestyramine produced symptomatic benefit in patients with BAD. PMID:28507750

The integrated manual and automatic control of complex flight systems

NASA Technical Reports Server (NTRS)

Schmidt, D. K.

1984-01-01

A unified control synthesis methodology for complex and/or non-conventional flight vehicles are developed. Prediction techniques for the handling characteristics of such vehicles and pilot parameter identification from experimental data are addressed.

Synthesis and photophysical characterizations of thermal-stable naphthalene benzimidazoles.

PubMed

Erten-Ela, Sule; Ozcelik, Serdar; Eren, Esin

2011-07-01

Microwave-assisted synthesis, photophysical and electrochemical properties of thermal-stable naphthalene benzimidazoles and naphthalimides are studied in this paper. Microwave-assisted synthesis of naphthalene benzimidazoles provide higher yields than the conventional thermal synthesis. Comparative photophysical properties of naphthalene benzimidazoles and naphthalimides are revealed that conjugation of electron-donating group onto naphthalimide moiety increases fluorescence quantum yields. Fluorophore-solvent interactions are also investigated using Lippert-Mataga equation for naphthalimides and naphthalene benzimidazoles. Thermal stabilities of naphthalene benzimidazoles are better than naphthalimides due to increased aromaticity. The experimental E(LUMO) levels of naphthalene benzimidazoles are found to be between 3.15 and 3.28 eV. Therefore, naphthalene benzimidazole derivatives consisting of anchoring groups are promising materials in organic dye sensitized solar cells. © Springer Science+Business Media, LLC 2011

Electrical conductivity of oxidized-graphenic nanoplatelets obtained from bamboo: effect of the oxygen content

NASA Astrophysics Data System (ADS)

Gross, K.; Prías Barragán, J. J.; Sangiao, S.; De Teresa, J. M.; Lajaunie, L.; Arenal, R.; Ariza Calderón, H.; Prieto, P.

2016-09-01

The large-scale production of graphene and reduced-graphene oxide (rGO) requires low-cost and eco-friendly synthesis methods. We employed a new, simple, cost-effective pyrolytic method to synthetize oxidized-graphenic nanoplatelets (OGNP) using bamboo pyroligneous acid (BPA) as a source. Thorough analyses via high-resolution transmission electron microscopy and electron energy-loss spectroscopy provides a complete structural and chemical description at the local scale of these samples. In particular, we found that at the highest carbonization temperature the OGNP-BPA are mainly in a sp2 bonding configuration (sp2 fraction of 87%). To determine the electrical properties of single nanoplatelets, these were contacted by Pt nanowires deposited through focused-ion-beam-induced deposition techniques. Increased conductivity by two orders of magnitude is observed as oxygen content decreases from 17% to 5%, reaching a value of 2.3 × 103 S m-1 at the lowest oxygen content. Temperature-dependent conductivity reveals a semiconductor transport behavior, described by the Mott three-dimensional variable range hopping mechanism. From the localization length, we estimate a band-gap value of 0.22(2) eV for an oxygen content of 5%. This investigation demonstrates the great potential of the OGNP-BPA for technological applications, given that their structural and electrical behavior is similar to the highly reduced rGO sheets obtained by more sophisticated conventional synthesis methods.

Microwave-assisted intramolecular dehydrogenative Diels-Alder reactions for the synthesis of functionalized naphthalenes/solvatochromic dyes.

PubMed

Kocsis, Laura S; Benedetti, Erica; Brummond, Kay M

2013-04-01

Functionalized naphthalenes have applications in a variety of research fields ranging from the synthesis of natural or biologically active molecules to the preparation of new organic dyes. Although numerous strategies have been reported to access naphthalene scaffolds, many procedures still present limitations in terms of incorporating functionality, which in turn narrows the range of available substrates. The development of versatile methods for direct access to substituted naphthalenes is therefore highly desirable. The Diels-Alder (DA) cycloaddition reaction is a powerful and attractive method for the formation of saturated and unsaturated ring systems from readily available starting materials. A new microwave-assisted intramolecular dehydrogenative DA reaction of styrenyl derivatives described herein generates a variety of functionalized cyclopenta[b]naphthalenes that could not be prepared using existing synthetic methods. When compared to conventional heating, microwave irradiation accelerates reaction rates, enhances yields, and limits the formation of undesired byproducts. The utility of this protocol is further demonstrated by the conversion of a DA cycloadduct into a novel solvatochromic fluorescent dye via a Buchwald-Hartwig palladium-catalyzed cross-coupling reaction. Fluorescence spectroscopy, as an informative and sensitive analytical technique, plays a key role in research fields including environmental science, medicine, pharmacology, and cellular biology. Access to a variety of new organic fluorophores provided by the microwave-assisted dehydrogenative DA reaction allows for further advancement in these fields.

Microwave-assisted Intramolecular Dehydrogenative Diels-Alder Reactions for the Synthesis of Functionalized Naphthalenes/Solvatochromic Dyes

PubMed Central

Kocsis, Laura S.; Benedetti, Erica; Brummond, Kay M.

2013-01-01

Functionalized naphthalenes have applications in a variety of research fields ranging from the synthesis of natural or biologically active molecules to the preparation of new organic dyes. Although numerous strategies have been reported to access naphthalene scaffolds, many procedures still present limitations in terms of incorporating functionality, which in turn narrows the range of available substrates. The development of versatile methods for direct access to substituted naphthalenes is therefore highly desirable. The Diels-Alder (DA) cycloaddition reaction is a powerful and attractive method for the formation of saturated and unsaturated ring systems from readily available starting materials. A new microwave-assisted intramolecular dehydrogenative DA reaction of styrenyl derivatives described herein generates a variety of functionalized cyclopenta[b]naphthalenes that could not be prepared using existing synthetic methods. When compared to conventional heating, microwave irradiation accelerates reaction rates, enhances yields, and limits the formation of undesired byproducts. The utility of this protocol is further demonstrated by the conversion of a DA cycloadduct into a novel solvatochromic fluorescent dye via a Buchwald-Hartwig palladium-catalyzed cross-coupling reaction. Fluorescence spectroscopy, as an informative and sensitive analytical technique, plays a key role in research fields including environmental science, medicine, pharmacology, and cellular biology. Access to a variety of new organic fluorophores provided by the microwave-assisted dehydrogenative DA reaction allows for further advancement in these fields. PMID:23609566

Integrating Cellular and Bioprocess Engineering in the Non-Conventional Yeast Yarrowia lipolytica for Biodiesel Production: A Review

PubMed Central

Xie, Dongming

2017-01-01

As one of the major biofuels to replace fossil fuel, biodiesel has now attracted more and more attention due to its advantages in higher energy density and overall less greenhouse gas generation. Biodiesel (fatty acid alkyl esters) is produced by chemically or enzymatically catalyzed transesterification of lipids from microbial cells, microalgae, oil crops, or animal fats. Currently, plant oils or waste cooking oils/fats remain the major source for biodiesel production via enzymatic route, but the production capacity is limited either by the uncertain supplement of plant oils or by the low or inconsistent quality of waste oils/fats. In the past decades, significant progresses have been made on synthesis of microalgae oils directly from CO2 via a photosynthesis process, but the production cost from any current technologies is still too high to be commercialized due to microalgae’s slow growth rate on CO2, inefficiency in photo-bioreactors, lack of efficient contamination control methods, and high cost in downstream recovery. At the same time, many oleaginous microorganisms have been studied to produce lipids via the fatty acid synthesis pathway under aerobic fermentation conditions, among them one of the most studied is the non-conventional yeast, Yarrowia lipolytica, which is able to produce fatty acids at very high titer, rate, and yield from various economical substrates. This review summarizes the recent research progresses in both cellular and bioprocess engineering in Y. lipolytica to produce lipids at a low cost that may lead to commercial-scale biodiesel production. Specific technologies include the strain engineering for using various substrates, metabolic engineering in high-yield lipid synthesis, cell morphology study for efficient substrate uptake and product formation, free fatty acid formation and secretion for improved downstream recovery, and fermentation engineering for higher productivities and less operating cost. To further improve the economics of the microbial oil-based biodiesel, production of lipid-related or -derived high-value products are also discussed. PMID:29090211

Microwave-assisted synthesis of HKUST-1 and functionalized HKUST-1-@H3PW12O40: selective adsorption of heavy metal ions in water analyzed with synchrotron radiation.

PubMed

Zou, Fang; Yu, Runhan; Li, Rongguan; Li, Wei

2013-08-26

A simple, rapid and efficient synthesis of the metal-organic framework (MOF) HKUST-1 [Cu3(1,3,5-benzene-tri-carboxilic-acid)2] by microwave irradiation is described, which afforded a homogeneous and highly selective material. The unusually short time to complete the synthesis by microwave irradiation is mainly attributable to rapid nucleation rather than to crystal growth rate. Using this method, HKUST-1-MW (MW=microwave) could be prepared within 20 min, whereas by hydrothermal synthesis, involving conventional heating, the preparation time is 8 h. Work efficiency was improved by the good performance of the obtained HKUST-1-MW which exhibited good selective adsorption of heavy metal ions, as well as a remarkably high adsorption affinity and adsorption capacity, but no adsorption of Hg(2+) under the same experimental conditions. Of particular importance is the preservation of the structure after metal-ion adsorption, which remained virtually intact, with only a few changes in X-ray diffraction intensity and a moderate decline in surface area. Synthesis of the polyoxometalate-containing HKUST-1-MW@H3PW12O40 afforded a MOF with enhanced stability in water, due to the introduced Keggin-type phosphotungstate, which systematically occluded in the cavities constituting the walls between the mesopores. Different Cu/W ratios were investigated according to the extrusion rate of cooper ions concentration, without significant structural changes after adsorption. The MOFs obtained feature particle sizes between 10-20 μm and their structures were determined using synchrotron-based X-ray diffraction. The results of this study can be considered important for potentially wider future applications of MOFs, especially to attend environmental issues. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Green synthesis of Copper nanoparticle using ionic liquid-based extraction from Polygonum minus and their applications.

PubMed

Ullah, Habib; Wilfred, Cecilia Devi; Shaharun, Maizatul Shima

2018-06-06

The present work reports the extraction of phenolic compounds from Polygonum minus using ionic liquid as extracting solvent. In this work, 1-Butyl-3-methylimidazolium hydrogen sulfate [BMIM][HSO 4 ] was used for the extraction of bioactive compounds. Accordingly, ionic liquids based microwave-assisted extraction treatment for separating of bioactive compounds from polygonum minus was first performed in the present study. The results obtained in this work have high extraction yield in comparison with conventional solvent. UV/Vis results showed that microwave synthesis was fast, well dispersed and nanosized copper nanoparticle (CuNPs) in comparison with conventional synthesis. CuNPs was characterized by X-Rays diffractometer (XRD), Fourier transform infrared (FTIR), dynamic light scattering (DLS), field emission scanning electron microscopy combined with energy dispersive x-rays (FESEM-EDX), and thermogravimetric analysis (TGA). All the instrumental analyses confirmed the particles were nanosized. Furthermore, the antibacterial activity of as-synthesized CuNPs showed effective inhibitory zone against three different bacteria. The photocatalytic degradation of copper nanoparticles was studied using methylene blue (MB) and methyl orange (MO) dyes under UV light and degraded 99.9% within short time 8 and 7 minutes.

Synthesis of biodiesel from waste cooking oil using sonochemical reactors.

PubMed

Hingu, Shishir M; Gogate, Parag R; Rathod, Virendra K

2010-06-01

Investigation into newer routes of biodiesel synthesis is a key research area especially due to the fluctuations in the conventional fuel prices and the environmental advantages of biodiesel. The present work illustrates the use of sonochemical reactors for the synthesis of biodiesel from waste cooking oil. Transesterification of used frying oil with methanol, in the presence of potassium hydroxide as a catalyst has been investigated using low frequency ultrasonic reactor (20 kHz). Effect of different operating parameters such as alcohol-oil molar ratio, catalyst concentration, temperature, power, pulse and horn position on the extent of conversion of oil have been investigated. The optimum conditions for the transesterification process have been obtained as molar ratio of alcohol to oil as 6:1, catalyst concentration of 1 wt.%, temperature as 45 degrees C and ultrasound power as 200 W with an irradiation time of 40 min. The efficacy of using ultrasound has been compared with the conventional stirring approach based on the use of a six blade turbine with diameter of 1.5 cm operating at 1000 rpm. Also the purification aspects of the final product have been investigated. (c) 2010 Elsevier B.V. All rights reserved.

IMPROVED SYNTHESIS OF ROOM TEMPERATURE IONIC LIQUIDS

EPA Science Inventory

Room temperature ionic liquids (RTILs), molten salts comprised of N-alkylimidazolium cations and various anions, have received significant attention due to their commercial potential in a variety of chemical applications especially as substitutes for conventional volatile organic...

Biomineralization of unicellular organisms: an unusual membrane biochemistry for the production of inorganic nano- and microstructures.

PubMed

Bäuerlein, Edmund

2003-02-10

With evolution, Nature has ingeniously succeeded in giving rise to an impressive variety of inorganic structures. Every organism that synthesizes biogenic minerals does so in a form that is unique to that species. This biomineralization is apparently biologically controlled. It is thus expected that both the synthesis and the form of every specific biogenic mineral is genetically determined and controlled. An investigation of the mechanism of biomineralization has only become possible with the development of modern methods in molecular biology. Unicellular organisms such as magnetic bacteria, calcareous algae, and diatoms, all of which are amongst the simplest forms of life, are particularly suited to be investigated by these methods. Crystals and composites of proteins and amorphous inorganic polymers are formed as complex structures within these organisms; these structures are not known in conventional inorganic chemistry.

Synthesis and spectroscopic characterization of gold nanobipyramids prepared by a chemical reduction method

NASA Astrophysics Data System (ADS)

Thanh Ngo, Vo Ke; Phat Huynh, Trong; Giang Nguyen, Dang; Phuong Uyen Nguyen, Hoang; Lam, Quang Vinh; Dat Huynh, Thanh

2015-12-01

Gold nanobipyramids (NBPs) have attracted much attention because they have potential for applications in smart sensing devices, such as medical diagnostic equippments. This is due to the fact that they show more advantageous plasmonic properties than other gold nanostructures. We describe a chemical reduction method for synthesizing NBPs using conventional heating with ascorbic acid reduction and cetyltrimethylamonium bromide (CTAB) + AgNO3 as capping agents. The product was characterized by ultraviolet-visible spectroscopy (UV-vis), Fourier transmission infrared spectroscopy (FTIR), transmission electron microscopy (TEM), x-ray powder diffraction (XRD). The results showed that gold nanoparticles were formed with bipyramid shape (tip-to-tip distance of 88.4 ± 9.4 nm and base length of 29.9 ± 3.2 nm) and face-centered-cubic crystalline structure. Optimum parameters for preparation of NBPs are also found.

Synthesis, characterization, and ion-exchange properties of colloidal zeolite nanocrystals

NASA Astrophysics Data System (ADS)

Jawor, Anna; Jeong, Byeong-Heon; Hoek, Eric M. V.

2009-10-01

Here, we present physical-chemical properties of Linde type A (LTA) zeolite crystals synthesized via conventional hydrothermal and microwave heating methods. Both heating methods produced LTA crystals that were sub-micron in size, highly negatively charged, super-hydrophilic, and stable when dispersed in water. However, microwave heating produced relatively narrow crystal size distributions, required much shorter heating times, and did not significantly change composition, crystallinity, or surface chemistry. Moreover, microwave heating allowed systematic variation of crystal size by varying heating temperature and time during the crystallization reaction, thus producing a continuous gradient of crystal sizes ranging from about 90 to 300 nm. In ion-exchange studies, colloidal zeolites exhibited excellent sorption kinetics and capacity for divalent metal ions, suggesting their potential for use in water softening, scale inhibition, and scavenging of toxic metal ions from water.

Microwave-assisted synthesis of cyclodextrin polyurethanes.

PubMed

Biswas, Atanu; Appell, Michael; Liu, Zengshe; Cheng, H N

2015-11-20

Cyclodextrin (CD) has often been incorporated into polyurethanes in order to facilitate its use in encapsulation or removal of organic species for various applications. In this work a microwave-assisted method has been developed to produce polyurethanes consisting of α-, β-, and γ-CD and three common diisocyanates. As compared to conventional heating, this new synthetic method saves energy, significantly reduces reaction time, and gets similar or improved yield. The reaction products have been fully characterized with (13)C, (1)H, and two-dimensional NMR spectroscopy. With suitable stoichiometry of starting CD and diisocyanate, the resulting CD polyurethane is organic-soluble and water-insoluble and is shown to remove Nile red dye and phenol from water. Possible applications include the removal of undesirable materials from process streams, toxic compounds from the environment, and encapsulation of color or fragrance molecules. Published by Elsevier Ltd.

Enhanced Imaging of Building Interior for Portable MIMO Through-the-wall Radar

NASA Astrophysics Data System (ADS)

Song, Yongping; Zhu, Jiahua; Hu, Jun; Jin, Tian; Zhou, Zhimin

2018-01-01

Portable multi-input multi-output (MIMO) radar system is able to imaging the building interior through aperture synthesis. However, significant grating lobes are invoked in the directly imaging results, which may deteriorate the imaging quality of other targets and influence the detail information extraction of imaging scene. In this paper, a two-stage coherence factor (CF) weighting method is proposed to enhance the imaging quality. After obtaining the sub-imaging results of each spatial sampling position using conventional CF approach, a window function is employed to calculate the proposed “enhanced CF” adaptive to the spatial variety effect behind the wall for the combination of these sub-images. The real data experiment illustrates the better performance of proposed method on grating lobes suppression and imaging quality enhancement compare to the traditional radar imaging approach.

Droplet microfluidics with a nanoemulsion continuous phase.

PubMed

Gu, Tonghan; Yeap, Eunice W Q; Somasundar, Ambika; Chen, Ran; Hatton, T Alan; Khan, Saif A

2016-07-05

We present the first study of a novel, generalizable method that uses a water-in-oil nanoemulsion as the continuous phase to generate uniform aqueous micro-droplets in a capillary-based microfluidic system. We first study the droplet generation mechanism in this system and compare it to the more conventional case where a simple oil/solvent (with surfactant) is used as the continuous phase. Next, we present two versatile methods - adding demulsifying chemicals and heat treatment - to allow active online chemical interaction between the continuous and dispersed phases. These methods allow each generated micro-droplet to act as a well-mixed micro-reactor with walls that are 'permeable' to the nanoemulsion droplets and their contents. Finally, we demonstrate an application of this system in the fabrication of uniform hydrogel (alginate) micro-beads with control over particle properties such as size and swelling. Our work expands the toolbox of droplet-based microfluidics, enabling new opportunities and applications involving active colloidal continuous phases carrying chemical payloads, both in advanced materials synthesis and droplet-based screening and diagnostic methods.

Transesterification of PHA to oligomers covalently bonded with (bio)active compounds containing either carboxyl or hydroxyl functionalities.

PubMed

Kwiecień, Iwona; Radecka, Iza; Kowalczuk, Marek; Adamus, Grażyna

2015-01-01

This manuscript presents the synthesis and structural characterisation of novel biodegradable polymeric controlled-release systems of pesticides with potentially higher resistance to weather conditions in comparison to conventional forms of pesticides. Two methods for the preparation of pesticide-oligomer conjugates using the transesterification reaction were developed. The first method of obtaining conjugates, which consist of bioactive compounds with the carboxyl group and polyhydroxyalkanoates (PHAs) oligomers, is "one-pot" transesterification. In the second method, conjugates of bioactive compounds with hydroxyl group and polyhydroxyalkanoates oligomers were obtained in two-step method, through cyclic poly(3-hydroxybutyrate) oligomers. The obtained pesticide-PHA conjugates were comprehensively characterised using GPC, 1H NMR and mass spectrometry techniques. The structural characterisation of the obtained products at the molecular level with the aid of mass spectrometry confirmed that both of the synthetic strategies employed led to the formation of conjugates in which selected pesticides were covalently bonded to PHA oligomers via a hydrolysable ester bond.

Protein based Block Copolymers

PubMed Central

Rabotyagova, Olena S.; Cebe, Peggy; Kaplan, David L.

2011-01-01

Advances in genetic engineering have led to the synthesis of protein-based block copolymers with control of chemistry and molecular weight, resulting in unique physical and biological properties. The benefits from incorporating peptide blocks into copolymer designs arise from the fundamental properties of proteins to adopt ordered conformations and to undergo self-assembly, providing control over structure formation at various length scales when compared to conventional block copolymers. This review covers the synthesis, structure, assembly, properties, and applications of protein-based block copolymers. PMID:21235251

A novel synthesis of a new thorium (IV) metal organic framework nanostructure with well controllable procedure through ultrasound assisted reverse micelle method.

PubMed

Sargazi, Ghasem; Afzali, Daryoush; Mostafavi, Ali

2018-03-01

Reverse micelle (RM) and ultrasound assisted reverse micelle (UARM) were applied to the synthesis of novel thorium nanostructures as metal organic frameworks (MOFs). Characterization with different techniques showed that the Th-MOF sample synthesized by UARM method had higher thermal stability (354°C), smaller mean particle size (27nm), and larger surface area (2.02×10 3 m 2 /g). Besides, in this novel approach, the nucleation of crystals was found to carry out in a shorter time. The synthesis parameters of UARM method were designed by 2 k-1 factorial and the process control was systematically studied using analysis of variance (ANOVA) and response surface methodology (RSM). ANOVA showed that various factors, including surfactant content, ultrasound duration, temperature, ultrasound power, and interaction between these factors, considerably affected different properties of the Th-MOF samples. According to the 2 k-1 factorial design, the determination coefficient (R 2 ) of the model is 0.999, with no significant lack of fit. The F value of 5432, implied that the model was highly significant and adequate to represent the relationship between the responses and the independent variables, also the large R-adjusted value indicates a good relationship between the experimental data and the fitted model. RSM predicted that it would be possible to produce Th-MOF samples with the thermal stability of 407°C, mean particle size of 13nm, and surface area of 2.20×10 3 m 2 /g. The mechanism controlling the Th-MOF properties was considerably different from the conventional mechanisms. Moreover, the MOF sample synthesized using UARM exhibited higher capacity for nitrogen adsorption as a result of larger pore sizes. It is believed that the UARM method and systematic studies developed in the present work can be considered as a new strategy for their application in other nanoscale MOF samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Robust penalty method for structural synthesis

NASA Technical Reports Server (NTRS)

Kamat, M. P.

1983-01-01

The Sequential Unconstrained Minimization Technique (SUMT) offers an easy way of solving nonlinearly constrained problems. However, this algorithm frequently suffers from the need to minimize an ill-conditioned penalty function. An ill-conditioned minimization problem can be solved very effectively by posing the problem as one of integrating a system of stiff differential equations utilizing concepts from singular perturbation theory. This paper evaluates the robustness and the reliability of such a singular perturbation based SUMT algorithm on two different problems of structural optimization of widely separated scales. The report concludes that whereas conventional SUMT can be bogged down by frequent ill-conditioning, especially in large scale problems, the singular perturbation SUMT has no such difficulty in converging to very accurate solutions.

Cation Ordering within the Perovskite Block of a Six-layer Ruddlesden-Popper Oxide from Layer-by-layer Growth

NASA Astrophysics Data System (ADS)

Yan, Lei; Niu, H. J.; Rosseinsky, M. J.

2011-03-01

The (AO)(A BO3)n Ruddlesden-Popper structure is an archetypal complex oxide consisting of two distinct structural units, an (AO) rock salt layer separating an n-octahedra thick perovskite block. Conventional high-temperature oxide synthesis methods cannot access members with n > 3 , butlowtemperaturelayer - by - layerthinfilmmethodsallowthepreparationofmaterialswiththickerperovskiteblocks , exploitinghighsurfacemobilityandlatticematchingwiththesubstrate . Thispresentationdescribesthegrowthofann = 6 memberCaO / (ABO 3)n (ABO 3 : CaMnO 3 , La 0.67 Ca 0.33 MnO 3 orCa 0.85 Sm 0.15 MnO 3) epitaxialsinglecrystalfilmsonthe (001) SrTiO 3 substrates by pulsed laser deposition with the assistance of a reflection high energy electron diffraction (RHEED).

Linear-quadratic-Gaussian synthesis with reduced parameter sensitivity

NASA Technical Reports Server (NTRS)

Lin, J. Y.; Mingori, D. L.

1992-01-01

We present a method for improving the tolerance of a conventional LQG controller to parameter errors in the plant model. The improvement is achieved by introducing additional terms reflecting the structure of the parameter errors into the LQR cost function, and also the process and measurement noise models. Adjusting the sizes of these additional terms permits a trade-off between robustness and nominal performance. Manipulation of some of the additional terms leads to high gain controllers while other terms lead to low gain controllers. Conditions are developed under which the high-gain approach asymptotically recovers the robustness of the corresponding full-state feedback design, and the low-gain approach makes the closed-loop poles asymptotically insensitive to parameter errors.

Potential of IRMS technology for tracing gamma-butyrolactone (GBL).

PubMed

Marclay, François; Pazos, Diego; Delémont, Olivier; Esseiva, Pierre; Saudan, Christophe

2010-05-20

Popularity of gamma-hydroxybutyric acid (GHB) is fairly stable among drug users, while the consumption of its chemical precursor, gamma-butyrolactone (GBL), is a growing phenomenon. Although conventional analytical methods allow to detect this substance in various matrices, linking a trace and a source is still a difficult challenge. However, as several synthesis pathways and chemical precursors exist for the production of GBL, its carbon isotopic signature may vary extensively. For that purpose, a method has been developed to determine the carbon isotopes content of GBL by means of gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS). The delta(13)C-values of 19 bulk samples purchased worldwide were in the range from -23.1 to -45.8 per thousand (SD<0.3 per thousand). Furthermore, testing on the purification of GBL by distillation has not been found to be consistent with such a large range of delta(13)C-values, which are likely to result from the isotopic composition of the organic precursors used to produce GBL together with the kinetic isotope effect associated with the synthesis routes. Finally, inter- and intra-variability measurements of the delta(13)C-values demonstrated the high potential of IRMS for discriminating between seizures of GBL and for source determination.

Practical development of continuous supercritical fluid process using high pressure and high temperature micromixer

NASA Astrophysics Data System (ADS)

Kawasaki, Shin-Ichiro; Sue, Kiwamu; Ookawara, Ryuto; Wakashima, Yuichiro; Suzuki, Akira

2015-12-01

In the synthesis of metal oxide fine particles by continuous supercritical hydrothermal method, the particle characteristics are greatly affected by not only the reaction conditions (temperature, pressure, residence time, concentration, etc.), but also the heating rate from ambient to reaction temperature. Therefore, the heating method by direct mixing of starting solution at room temperature with supercritical water is a key technology for the particle production having smaller size and narrow distribution. In this paper, mixing engineering study through comparison between conventional T-shaped mixers and recently developed swirl mixers was carried out in the hydrothermal synthesis of NiO nanoparticles from Ni(NO3)2 aqueous solution at 400 °C and 30 MPa. Inner diameter in the mixers and total flow rates were varied. Furthermore, the heating rate was calculated by computational fluid dynamics (CFD) simulation. Relationship between the heating rate and the average particle size were discussed. It was clarified that the miniaturization of mixer inner diameter and the use of the swirl flow were effective for improving mixing performance and contributed to produce small and narrow distribution particle under same experimental condition of flow rate, temperature, pressure, residence time, and concentration of the starting materials. We have focused the mixer optimization due to a difference in fluid viscosity.

Alcohols as alkylating agents in heteroarene C-H functionalization

NASA Astrophysics Data System (ADS)

Jin, Jian; MacMillan, David W. C.

2015-09-01

Redox processes and radical intermediates are found in many biochemical processes, including deoxyribonucleotide synthesis and oxidative DNA damage. One of the core principles underlying DNA biosynthesis is the radical-mediated elimination of H2O to deoxygenate ribonucleotides, an example of `spin-centre shift', during which an alcohol C-O bond is cleaved, resulting in a carbon-centred radical intermediate. Although spin-centre shift is a well-understood biochemical process, it is underused by the synthetic organic chemistry community. We wondered whether it would be possible to take advantage of this naturally occurring process to accomplish mild, non-traditional alkylation reactions using alcohols as radical precursors. Because conventional radical-based alkylation methods require the use of stoichiometric oxidants, increased temperatures or peroxides, a mild protocol using simple and abundant alkylating agents would have considerable use in the synthesis of diversely functionalized pharmacophores. Here we describe the development of a dual catalytic alkylation of heteroarenes, using alcohols as mild alkylating reagents. This method represents the first, to our knowledge, broadly applicable use of unactivated alcohols as latent alkylating reagents, achieved via the successful merger of photoredox and hydrogen atom transfer catalysis. The value of this multi-catalytic protocol has been demonstrated through the late-stage functionalization of the medicinal agents, fasudil and milrinone.

Alcohols as alkylating agents in heteroarene C-H functionalization.

PubMed

Jin, Jian; MacMillan, David W C

2015-09-03

Redox processes and radical intermediates are found in many biochemical processes, including deoxyribonucleotide synthesis and oxidative DNA damage. One of the core principles underlying DNA biosynthesis is the radical-mediated elimination of H2O to deoxygenate ribonucleotides, an example of 'spin-centre shift', during which an alcohol C-O bond is cleaved, resulting in a carbon-centred radical intermediate. Although spin-centre shift is a well-understood biochemical process, it is underused by the synthetic organic chemistry community. We wondered whether it would be possible to take advantage of this naturally occurring process to accomplish mild, non-traditional alkylation reactions using alcohols as radical precursors. Because conventional radical-based alkylation methods require the use of stoichiometric oxidants, increased temperatures or peroxides, a mild protocol using simple and abundant alkylating agents would have considerable use in the synthesis of diversely functionalized pharmacophores. Here we describe the development of a dual catalytic alkylation of heteroarenes, using alcohols as mild alkylating reagents. This method represents the first, to our knowledge, broadly applicable use of unactivated alcohols as latent alkylating reagents, achieved via the successful merger of photoredox and hydrogen atom transfer catalysis. The value of this multi-catalytic protocol has been demonstrated through the late-stage functionalization of the medicinal agents, fasudil and milrinone.

[Synthesis of hollow titania microspheres by using microfluidic droplet-template].

PubMed

Ma, Jingyun; Jiang, Lei; Qin, Jianhu

2011-09-01

Droplet-based microfluidics is of great interest due to its particular characteristics compared with the conventional methods, such as reduced reagent consumption, rapid mixing, high-throughput, shape controlled, etc. A novel method using microfluidic droplet as soft template for the synthesis of hollow titania microspheres was developed. A typical polydimethylsiloxane (PDMS) microfluidic device containing "flow-focusing" geometry was used to generate water/oil (W/O) droplet. The mechanism for the hollow structure formation was based on the interfacial hydrolysis reaction between the continuous phase containing titanium butoxide precursor and the dispersed containing water. The continuous phase mixed with butanol was added in the downstream of the channel after the hydrolysis reaction. This step was used for drawing the water out of the microgels for further hydrolysis. The microgels obtained through a glass pipe integrated were washed, dried under vacuum and calcined after aging for a certain time. The fluorescence and scanning electron microscope (SEM) image of the microspheres indicated the hollow structure and the thickness of the shell. In addition, these microspheres with thin shell (about 2 microm) were apt to rupture and collapse. Droplet-based microfluidic offered a gentle and size-controllable manner to moderate this problem. Moreover, it has potential applications in photocatalysis combined with some modification realized on the chip simultaneously.

Development of highly active and stable hybrid cathode catalyst for PEMFCs

NASA Astrophysics Data System (ADS)

Jung, Won Suk

Polymer electrolyte membrane fuel cells (PEMFCs) are attractive power sources of the future for a variety of applications including portable electronics, stationary power, and automobile application. However, sluggish cathode kinetics, high Pt cost, and durability issues inhibit the commercialization of PEMFCs. To overcome these drawbacks, research has been focused on alloying Pt with transition metals since alloy catalysts show significantly improved catalytic properties like high activity, selectivity, and durability. However, Pt-alloy catalysts synthesized using the conventional impregnation method exhibit uneven particle size and poor particle distribution resulting in poor performance and/or durability in PEMFCs. In this dissertation, a novel catalyst synthesis methodology is developed and compared with catalysts prepared using impregnation method and commercial catalysts. Two approaches are investigated for the catalyst development. The catalyst durability was studied under U. S. DRIVE Fuel Cell Tech Team suggested protocols. In the first approach, the carbon composite catalyst (CCC) having active sites for oxygen reduction reaction (ORR) is employed as a support for the synthesis of Pt/CCC catalyst. The structural and electrochemical properties of Pt/CCC catalyst are investigated using high-resolution transmission electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy, while RDE and fuel cell testing are carried out to study the electrochemical properties. The synergistic effect of CCC and Pt is confirmed by the observed high activity towards ORR for the Pt/CCC catalyst. The second approach is the synthesis of Co-doped hybrid cathode catalysts (Co-doped Pt/CCC) by diffusing the Co metal present within the CCC support into the Pt nanoparticles during heat-treatment. The optimized Co-doped Pt/CCC catalyst performed better than the commercial catalysts and the catalyst prepared using the impregnation method in PEMFCs and showed high stability under 30,000 potential cycles between 0.6 and 1.0 V. To further increase the stability of the catalyst at high potential cycles (1.0-1.5 V), high temperature treatment is used to obtain graphitized carbon having optimum BET surface area. The novel catalyst synthesis procedure developed in this study was successfully applied for the synthesis of Co-doped Pt catalysts supported on the graphitized carbon which showed high activity and enhanced stability at high potentials.

Inferring common cognitive mechanisms from brain blood-flow lateralization data: a new methodology for fTCD analysis.

PubMed

Meyer, Georg F; Spray, Amy; Fairlie, Jo E; Uomini, Natalie T

2014-01-01

Current neuroimaging techniques with high spatial resolution constrain participant motion so that many natural tasks cannot be carried out. The aim of this paper is to show how a time-locked correlation-analysis of cerebral blood flow velocity (CBFV) lateralization data, obtained with functional TransCranial Doppler (fTCD) ultrasound, can be used to infer cerebral activation patterns across tasks. In a first experiment we demonstrate that the proposed analysis method results in data that are comparable with the standard Lateralization Index (LI) for within-task comparisons of CBFV patterns, recorded during cued word generation (CWG) at two difficulty levels. In the main experiment we demonstrate that the proposed analysis method shows correlated blood-flow patterns for two different cognitive tasks that are known to draw on common brain areas, CWG, and Music Synthesis. We show that CBFV patterns for Music and CWG are correlated only for participants with prior musical training. CBFV patterns for tasks that draw on distinct brain areas, the Tower of London and CWG, are not correlated. The proposed methodology extends conventional fTCD analysis by including temporal information in the analysis of cerebral blood-flow patterns to provide a robust, non-invasive method to infer whether common brain areas are used in different cognitive tasks. It complements conventional high resolution imaging techniques.

Hynol: An economic process for methanol production from biomass and natural gas with reduced CO2 emission

NASA Astrophysics Data System (ADS)

Steinberg, M.; Dong, Yuanji

1993-10-01

The Hynol process is proposed to meet the demand for an economical process for methanol production with reduced CO2 emission. This new process consists of three reaction steps: (1) hydrogasification of biomass, (2) steam reforming of the produced gas with additional natural gas feedstock, and (3) methanol synthesis of the hydrogen and carbon monoxide produced during the previous two steps. The H2-rich gas remaining after methanol synthesis is recycled to gasify the biomass in an energy neutral reactor so that there is no need for an expensive oxygen plant as required by commercial steam gasifiers. Recycling gas allows the methanol synthesis reactor to perform at a relatively lower pressure than conventional while the plant still maintains high methanol yield. Energy recovery designed into the process minimizes heat loss and increases the process thermal efficiency. If the Hynol methanol is used as an alternative and more efficient automotive fuel, an overall 41% reduction in CO2 emission can be achieved compared to the use of conventional gasoline fuel. A preliminary economic estimate shows that the total capital investment for a Hynol plant is 40% lower than that for a conventional biomass gasification plant. The methanol production cost is $0.43/gal for a 1085 million gal/yr Hynol plant which is competitive with current U.S. methanol and equivalent gasoline prices. Process flowsheet and simulation data using biomass and natural gas as cofeedstocks are presented. The Hynol process can convert any condensed carbonaceous material, especially municipal solid waste (MSW), to produce methanol.

Comparison of the solid-phase fragment condensation and phase-change approaches in the synthesis of salmon I calcitonin.

PubMed

Gatos, D; Tzavara, C

2001-02-01

Salmon I calcitonin was synthesized using both phase-change and conventional solid-phase fragment condensation (SPFC) approaches, utilizing the Rink amide linker (Fmoc-amido-2,4-dimethoxybenzyl-4-phenoxyacetic acid) combined with 2-chlorotrityl resin and the Fmoc/tBu(Trt)-based protection scheme. Phase-change synthesis, performed by the selective detachment of the fully protected C-terminal 22-mer peptide-linker from the resin and subsequent condensation in solution with the N-terminal 1-10 fragment, gave a product of slightly less purity (85 vs. 92%) than the corresponding synthesis on the solid-phase. In both cases salmon I calcitonin was easily obtained in high purity.

Eco-friendly combination of the immobilized PGA enzyme and the S-Phacm protecting group for the synthesis of Cys-containing peptides.

PubMed

Góngora-Benítez, Miriam; Basso, Alessandra; Bruckdorfer, Thomas; Royo, Miriam; Tulla-Puche, Judit; Albericio, Fernando

2012-12-07

Enzyme-labile protecting groups have emerged as a green alternative to conventional protecting groups. These groups introduce a further orthogonal dimension and eco-friendliness into protection schemes for the synthesis of complex polyfunctional organic molecules. S-Phacm, a Cys-protecting group, can be easily removed by the action of a covalently immobilized PGA enzyme under very mild conditions. Herein, the versatility and reliability of an eco-friendly combination of the immobilized PGA enzyme and the S-Phacm protecting group has been evaluated for the synthesis of diverse Cys-containing peptides. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A review on green synthesis of silver nanoparticles and their applications.

PubMed

Rafique, Muhammad; Sadaf, Iqra; Rafique, M Shahid; Tahir, M Bilal

2017-11-01

Development of reliable and eco-accommodating methods for the synthesis of nanoparticles is a vital step in the field of nanotechnology. Silver nanoparticles are important because of their exceptional chemical, physical, and biological properties, and hence applications. In the last decade, numerous efforts were made to develop green methods of synthesis to avoid the hazardous byproducts. This review describes the methods of green synthesis for Ag-NPs and their numerous applications. It also describes the comparison of efficient synthesis methods via green routes over physical and chemical methods, which provide strong evidence for the selection of suitable method for the synthesis of Ag-NPs.

Integrated Platform for Expedited Synthesis–Purification–Testing of Small Molecule Libraries

PubMed Central

2017-01-01

The productivity of medicinal chemistry programs can be significantly increased through the introduction of automation, leading to shortened discovery cycle times. Herein, we describe a platform that consolidates synthesis, purification, quantitation, dissolution, and testing of small molecule libraries. The system was validated through the synthesis and testing of two libraries of binders of polycomb protein EED, and excellent correlation of obtained data with results generated through conventional approaches was observed. The fully automated and integrated platform enables batch-supported compound synthesis based on a broad array of chemical transformations with testing in a variety of biochemical assay formats. A library turnaround time of between 24 and 36 h was achieved, and notably, each library synthesis produces sufficient amounts of compounds for further evaluation in secondary assays thereby contributing significantly to the shortening of medicinal chemistry discovery cycles. PMID:28435537

PHOTOCATALYTIC REACTORS AND KINETICS FOR CLEAN CHEMICAL SYNTHESIS [POSTER PRESENTATION

EPA Science Inventory

Semiconductor photocatalysis has been tested at a potential technology for synthesizing alcohols, ketones and aldehydes from linear and cyclic hydrocarbons. The technology couples UV light with photocatalyst overcoming many of the drawbacks of conventional reacors. Various hydr...

Microwave Technology--Applications in Chemical Synthesis

EPA Science Inventory

Microwave heating, being specific and instantaneous, is unique and has found a place for expeditious chemical syntheses. Specifically, the solvent-free reactions are convenient to perform and have advantages over the conventional heating protocols as summarized in the previous se...

Alternative energy input: Mechanochemical, microwave and ultrasound-assisted organic synthesis

EPA Science Inventory

Microwave, ultrasound, sunlight and mechanochemical mixing can be used to augment conventional laboratory techniques. By applying these alternative means of activation, a number of chemical transformations have been achieved thereby improving many existing protocols with superi...

Low Temperature Graphene Growth and Its Applications in Electronic and Optical Devices

NASA Astrophysics Data System (ADS)

Chugh, Sunny

Graphene, a two dimensional allotrope of carbon in a honeycomb lattice, has gathered wide attention due to its excellent electrical, thermal, optical and mechanical properties. It has extremely high electron/hole mobility, very high thermal conductivity and fascinating optical properties, and combined with its mechanical strength and elasticity, graphene is believed to find commercial applications in existing as well as novel technologies. One of the biggest reasons behind the rapid development in graphene research during the last decade is the fact that laboratory procedures to obtain high quality graphene are rather cheap and simple. However, any new material market is essentially driven by the progress in its large scale commercial production with minimal costs, with properties that are suited for different applications. And it is in this aspect that graphene is still required to make a huge progress before its commercial benefits can be derived. Laboratory graphene synthesis techniques such as mechanical exfoliation, liquid phase exfoliation and SiC graphene growth pose several challenges in terms of cost, reliability and scalability. To this end, Chemical Vapor Deposition (CVD) growth of graphene has emerged as a widely used synthesis method that overcomes these problems. Unfortunately, conventional thermal CVD requires a high temperature of growth and a catalytic metal substrate, making the undesirable step of graphene transfer a necessity. Besides requiring a catalyst, the high temperature of growth also limits the range of growth substrates. In this work, I have successfully demonstrated low temperature ( 550 °C) growth of graphene directly on dielectric materials using a Plasma-Enhanced CVD (PECVD) process. The PECVD technique described here solves the issues faced by conventional CVD methods and provides a direct route for graphene synthesis on arbitrary materials at relatively low temperatures. Detailed growth studies, as described here, illustrate the difference between the PECVD and the CVD growth mechanisms. This work also provides the first experimental comparison of graphene growth rates on different substrates using PECVD. In the second part of my thesis, I have discussed some of the potential applications of PECVD graphene, including graphene as a diffusion barrier, ultra-dark graphene metamaterials, graphene-protected metal plasmonics and copper-graphene hybrids for RF transmission line applications. The experimental findings discussed here lay a solid platform for integration of graphene in damascene structures, low-loss plasmonic materials, flexible electronics and dark materials, among others.

Advancements in Research Synthesis Methods: From a Methodologically Inclusive Perspective

ERIC Educational Resources Information Center

Suri, Harsh; Clarke, David

2009-01-01

The dominant literature on research synthesis methods has positivist and neo-positivist origins. In recent years, the landscape of research synthesis methods has changed rapidly to become inclusive. This article highlights methodologically inclusive advancements in research synthesis methods. Attention is drawn to insights from interpretive,…

Metal-Organic Polyhedral Core as a Versatile Scaffold for Divergent and Convergent Star Polymer Synthesis.

PubMed

Hosono, Nobuhiko; Gochomori, Mika; Matsuda, Ryotaro; Sato, Hiroshi; Kitagawa, Susumu

2016-05-25

We herein report the divergent and convergent synthesis of coordination star polymers (CSP) by using metal-organic polyhedrons (MOPs) as a multifunctional core. For the divergent route, copper-based great rhombicuboctahedral MOPs decorated with dithiobenzoate or trithioester chain transfer groups at the periphery were designed. Subsequent reversible addition-fragmentation chain transfer (RAFT) polymerization of monomers mediated by the MOPs gave star polymers, in which 24 polymeric arms were grafted from the MOP core. On the other hand, the convergent route provided identical CSP architectures by simple mixing of a macroligand and copper ions. Isophthalic acid-terminated polymers (so-called macroligands) immediately formed the corresponding CSPs through a coordination reaction with copper(II) ions. This convergent route enabled us to obtain miktoarm CSPs with tunable chain compositions through ligand mixing alone. This powerful method allows instant access to a wide variety of multicomponent star polymers that conventionally have required highly skilled and multistep syntheses. MOP-core CSPs are a new class of star polymer that can offer a design strategy for highly processable porous soft materials by using coordination nanocages as a building component.

Multinuclear Phthalocyanine-Fused Molecular Nanoarrays: Synthesis, Spectroscopy, and Semiconducting Property.

PubMed

Shang, Hong; Xue, Zheng; Wang, Kang; Liu, Huibiao; Jiang, Jianzhuang

2017-06-27

The post-cyclization strategy rather than the conventional ante-cyclotetramerization method was employed for the synthesis of multinuclear phthalocyanine-fused molecular nanoarrays. Reaction of 2,3,9,10,16,17-hexakis(2,6-dimethylphenoxy)-23,24-diaminophthalocyaninato zinc(II) with 2,7-di-tert-butylpyrene-4,5-dione, 2,7-di-tert-butylpyrene-4,5,9,10-tetraone, and hexaketocyclohexane in refluxing acetic acid afforded the corresponding mono-, bi-, and trinuclear phthalocyanine-fused zinc complexes (Pz-pyrene){Zn[Pc(OC 8 H 9 ) 6 ]} (1), (Pz 2 -pyrene){Zn[Pc(OC 8 H 9 ) 6 ]} 2 (2), {(HAT){Zn[Pc(OC 8 H 9 ) 6 ]} 3 } (3) in 46, 13, and 25 % yield, respectively, which extend the scope of multinuclear phthalocyanine-fused nanoarrays with different molecular skeletons. The self-assembly behavior of trinuclear phthalocyanine 3 in THF/CH 3 CN was investigated by electronic absorption spectroscopy and SEM, and the fabricated nanorods showed interesting semiconducting properties, which suggest good application potential of these multinuclear phthalocyanine-fused molecular nanoarrays. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Continuous synthesis of peralkylated imidazoles and their transformation into ionic liquids with improved (electro)chemical stabilities.

PubMed

Maton, Cedric; De Vos, Nils; Roman, Bart I; Vanecht, Evert; Brooks, Neil R; Binnemans, Koen; Schaltin, Stijn; Fransaer, Jan; Stevens, Christian V

2012-09-17

A versatile and efficient method to synthesize tetrasubstituted imidazoles via a one-pot modified Debus-Radziszewski reaction and their subsequent transformation into the corresponding imidazolium ionic liquids is reported. The tetrasubstituted imidazoles were also synthesized by means of a continuous flow process. This straightforward synthetic procedure allows for a fast and selective synthesis of tetrasubstituted imidazoles on a large scale. The completely substituted imidazolium dicyanamide and bis(trifluoromethylsulfonyl)imide salts were obtained via a metathesis reaction of the imidazolium iodide salts. The melting points and viscosities are of the same order of magnitude as for their non-substituted analogues. In addition to the superior chemical stability of these novel ionic liquids, which allows them to be applied in strong alkaline media, the improved thermal and electrochemical stabilities of these compounds compared with conventional imidazolium ionic liquids is also demonstrated by thermogravimetrical analysis (TGA) and cyclic voltammetry (CV). Although increased substitution of the ionic liquids does not further increase thermal stability, a definite increase in cathodic stability is observable. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A rapid non-radioactive technique for measurement of repair synthesis in primary human fibroblasts by incorporation of ethynyl deoxyuridine (EdU).

PubMed

Limsirichaikul, Siripan; Niimi, Atsuko; Fawcett, Heather; Lehmann, Alan; Yamashita, Shunichi; Ogi, Tomoo

2009-03-01

Xeroderma pigmentosum (XP) is an autosomal recessive genetic disorder. Afflicted patients show extreme sun-sensitivity and skin cancer predisposition. XP is in most cases associated with deficient nucleotide excision repair (NER), which is the process responsible for removing photolesions from DNA. Measuring NER activity by nucleotide incorporation into repair patches, termed 'unscheduled DNA synthesis (UDS)', is one of the most commonly used assays for XP-diagnosis and NER research. We have established a rapid and accurate procedure for measuring UDS by replacement of thymidine with 5-ethynyl-2'-deoxyuridine (EdU). EdU incorporated into repair patches can be directly conjugated to fluorescent azide derivatives, thereby obviating the need for either radiolabeled thymidine or denaturation and antibody detection of incorporated bromodeoxyuridine (BrdU). We demonstrate that the EdU incorporation assay is compatible with conventional techniques such as immunofluorescent staining and labeling of cells with micro-latex beads. Importantly, we can complete the entire UDS assay within half a day from preparation of the assay coverslips; this technique may prove useful as a method for XP diagnosis.

IF-WS{sub 2} nanoparticles size design and synthesis via chemical reduction

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

Ghoreishi, S.M., E-mail: ghoreshi@cc.iut.ac.ir; Meshkat, S.S.; Dadkhah, A.A.

2010-05-15

An innovative synthesis of inorganic fullerene-like disulfide tungsten (IF-WS{sub 2}) nanoparticles was developed using a chemical reduction reaction in a horizontal quartz reactor. In this process, first tungsten trisulfide (WS{sub 3}) was formed via a chemical reaction of tetra thiotungstate ammonium ((NH{sub 4}){sub 2}WS{sub 4}), polyethylene glycol (PEG), and hydrochloric acid (HCl) at ambient temperature and pressure. Subsequently, WS{sub 3} was reacted with hydrogen (H{sub 2}) at high temperature (1173-1373 K) in a quartz tube. The produced WS{sub 2} nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray (EDAX), and transmission electron microscopy (TEM). Themore » characterization results indicated that the high-purity (100%) IF-WS{sub 2} nanoparticles were produced. Moreover, addition of surfactant (PEG) and higher operating temperature (1173-1373 K) decreased the particles agglomeration, and consequently led to the reduction of average diameter of WS{sub 2} particles in the range of 50-78 nm. The developed method is simple, environmentally compatible, and cost-effective in contrast to the conventional techniques.« less

An Eco-Friendly Ultrasound-Assisted Synthesis of Novel Fluorinated Pyridinium Salts-Based Hydrazones and Antimicrobial and Antitumor Screening

PubMed Central

Rezki, Nadjet; Al-Sodies, Salsabeel A.; Aouad, Mohamed R.; Bardaweel, Sanaa; Messali, Mouslim; El Ashry, El Sayed H.

2016-01-01

The present work reports an efficient synthesis of fluorinated pyridinium salts-based hydrazones under both conventional and eco-friendly ultrasound procedures. The synthetic approach first involves the preparation of halogenated pyridinium salts through the condensation of isonicotinic acid hydrazide (1) with p-fluorobenzaldehyde (2) followed by the nucleophilic alkylation of the resulting N-(4-fluorobenzylidene)isonicotinohydrazide (3) with a different alkyl iodide. The iodide counteranion of 5–10 was subjected to an anion exchange metathesis reaction in the presence of an excess of the appropriate metal salts to afford a new series of fluorinated pyridinium salts tethering a hydrazone linkage 11–40. Ultrasound irradiation led to higher yields in considerably less time than the conventional methods. The newly synthesized ILs were well-characterized with FT-IR, 1H NMR, 13C NMR, 11B, 19F, 31P and mass spectral analyses. The ILs were also screened for their antimicrobial and antitumor activities. Within the series, the salts tethering fluorinated counter anions 11–13, 21–23, 31–33 and 36–38 were found to be more potent against all bacterial and fungal strains at MIC 4–8 µg/mL. The in vitro antiproliferative activity was also investigated against four tumor cell lines (human ductal breast epithelial tumor T47D, human breast adenocarcinoma MCF-7, human epithelial carcinoma HeLa and human epithelial colorectal adenocarcinoma Caco-2) using the MTT assay, which revealed that promising antitumor activity was exhibited by compounds 5, 12 and 14. PMID:27213367

Ionic liquids as an electrolyte for the electro synthesis of organic compounds.

PubMed

Kathiresan, Murugavel; Velayutham, David

2015-12-25

The use of ionic liquids (ILs) as a solvent and an electrolyte for electro organic synthesis has been reviewed. To date several ILs exist, however the ILs based on tetraalkylammonium, pyrrolidinium, piperidinium and imidazolium cations with BF4(-), PF6(-), and TFSI anions have been widely used and explored the most. Electro organic synthesis in ionic liquid media leading to the synthesis of a wide range of organic compounds has been discussed. Anodic oxidation or cathodic reduction will generate radical cation or anion intermediates, respectively. These radicals can undergo self coupling or coupling with other molecules yielding organic compounds of interest. The cation of the IL is known to stabilize the radical anion extensively. This stabilization effect has a specific impact on the electrochemical CO2 reduction and coupling to various organics. The relative stability of the intermediates in IL leads to the formation of specific products in higher yields. Electrochemical reduction of imidazolium or thiazolium based ILs generates N-heterocyclic carbenes that have been shown to catalyze a wide range of base or nucleophile catalyzed organic reactions in IL media, an aspect that falls into the category of organocatalysis. Electrochemical fluorination or selective electrochemical fluorination is another fascinating area that delivers selectively fluorinated organic products in Et3N·nHF or Et4NF·nHF adducts (IL) via anodic oxidation. Oxidative polymerization in ILs has been explored the most; although morphological changes were observed compared to the conventional methods, polymers were obtained in good yields and in some cases ILs were used as dopants to improve the desired properties.

A weight of evidence framework for environmental assessments: Inferring Qualities

EPA Science Inventory

The weighing of heterogeneous evidence such as conventional laboratory toxicity tests, field tests, biomarkers, and community surveys is essential to environmental assessments. Evidence synthesis and weighing is needed to determine causes of observed effects, hazards posed by ch...

Rapid Biosynthesis of Silver Nanoparticles Using Pepino (Solanum muricatum) Leaf Extract and Their Cytotoxicity on HeLa Cells

PubMed Central

Gorbe, Mónica; Bhat, Ravishankar; Aznar, Elena; Sancenón, Félix; Marcos, M. Dolores; Herraiz, F. Javier; Prohens, Jaime; Venkataraman, Abbaraju; Martínez-Máñez, Ramón

2016-01-01

Within nanotechnology, gold and silver nanostructures have unique physical, chemical, and electronic properties [1,2], which make them suitable for a number of applications. Moreover, biosynthetic methods are considered to be a safer alternative to conventional physicochemical procedures for both the environmental and biomedical applications, due to their eco-friendly nature and the avoidance of toxic chemicals in the synthesis. For this reason, employing bio routes in the synthesis of functionalized silver nanoparticles (FAgNP) have gained importance recently in this field. In the present study, we report the rapid synthesis of FAgNP through the extract of pepino (Solanum muricatum) leaves and employing microwave oven irradiation. The core-shell globular morphology and characterization of the different shaped and sized FAgNP, with a core of 20–50 nm of diameter is established using the UV-Visible spectroscopy (UV-vis), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and Zeta potential and dynamic light scanning (DLS) studies. Moreover, cytotoxic studies employing HeLa (human cervix carcinoma) cells were undertaken to understand FAgNP interactions with cells. HeLa cells showed significant dose dependent antiproliferative activity in the presence of FAgNP at relatively low concentrations. The calculated IC50 value was 37.5 µg/mL, similar to others obtained for FAgNPs against HeLa cells. PMID:28773448

Synthesis and characterization of pore size-tunable magnetic mesoporous silica nanoparticles.

PubMed

Zhang, Jixi; Li, Xu; Rosenholm, Jessica M; Gu, Hong-chen

2011-09-01

Magnetic mesoporous silica nanoparticles (M-MSNs) are emerging as one of the most appealing candidates for theranostic carriers. Herein, a simple synthesis method of M-MSNs with a single Fe(3)O(4) nanocrystal core and a mesoporous shell with radially aligned pores was elaborated using tetraethyl orthosilicate (TEOS) as silica source, cationic surfactant CTAB as template, and 1,3,5-triisopropylbenzene (TMB)/decane as pore swelling agents. Due to the special localization of TMB during the synthesis process, the pore size was increased with added TMB amount within a limited range, while further employment of TMB lead to severe particle coalescence and not well-developed pore structure. On the other hand, when a proper amount of decane was jointly incorporated with limited amounts of TMB, effective pore expansion of M-MSNs similar to that of analogous mesoporous silica nanoparticles was realized. The resultant M-MSN materials possessed smaller particle size (about 40-70 nm in diameter), tunable pore sizes (3.8-6.1 nm), high surface areas (700-1100 m(2)/g), and large pore volumes (0.44-1.54 cm(3)/g). We also demonstrate their high potential in conventional DNA loading. Maximum loading capacity of salmon sperm DNA (375 mg/g) was obtained by the use of the M-MSN sample with the largest pore size of 6.1 nm. Copyright © 2011 Elsevier Inc. All rights reserved.

Catalysis and Sonocatalysis for the Synthesis of Biofuels

NASA Astrophysics Data System (ADS)

Deshmane, Vishwanath Ganpat

The goal of this study was to investigate the synthesis of biofuels from edible and non-edible sources using commercially available and laboratory synthesized heterogeneous catalysts with and without the aid of ultrasound. The transesterification of soybean oil using calcium methoxide as solid base catalyst and the process parameters affecting the yield of biodiesel such as the catalyst concentration, methanol/oil molar ratio and the reaction temperature were investigated in detail. The kinetics of this process with and without ultrasound was also evaluated using a previously reported kinetic and mass transfer model for heterogeneous systems. Nanocrystalline mesoporous ZrO 2 with high surface area and thermal stability was synthesized using ethylene diamine as precipitating agent. Sulfonation of obtained Zr(OH) 2 at different digestion times was carried out using sulfuric acid and chlorosulfonic acid as the sulfonating agents and the effects of process parameters including digestion time, pH, precursor concentration and calcination temperature on structural, textural and catalytic properties were studied. Parametric and optimization (Taguchi statistical methodology) studies were carried out to evaluate the effects of cellulase, cellobiase, cellulose concentration and ultrasonic power on the intensification of cellulose hydrolysis to glucose. The catalysts and cellulose were characterized by using BET, NH3-TPD, XRD, SEM, TGA-DSC, EDX and FTIR. The results of these studies suggest that synthesis of biofuels can be improved by heterogeneous catalysts and ultrasound with potential reduction in production costs compared with conventional methods.

Aqueous based synthesis of N-acetyl-L-cysteine capped ZnSe nanocrystals with intense blue emission

NASA Astrophysics Data System (ADS)

Soheyli, Ehsan; Sahraei, Reza; Nabiyouni, Gholamreza

2016-10-01

In this work a very simple reflux route for preparation of ZnSe nanocrystals with minor modification and faster preparation over conventional ones is introduced. X-ray diffraction analysis indicated that the ZnSe nanocrystals have a cubic structure. The complete disappearance of the S-H band in FT-IR spectrum of N-acetyl-L-cysteine capped ZnSe nanocrystals was an indication over formation of Zn-thiol covalent bonds at the surface of the nanocrystals which results in passivation of small nanocrystals. The strong size-quantization regime was responsible of significant blue shift in absorption/emission spectra. Using the well-known calculations, band gap and Urbach energy of the ZnSe nanocrystals were measured and their average size was estimated optically to be around 4.6 nm along with the TEM image. A dark blue emission with higher relative intensity of excitonic to trap emissions (compared to conventional method), very narrow excitonic emission peak of about 16 nm and remarkable stability was obtained from the ZnSe nanocrystals.

Hydrogen fuel - Universal energy

NASA Astrophysics Data System (ADS)

Prince, A. G.; Burg, J. A.

The technology for the production, storage, transmission, and consumption of hydrogen as a fuel is surveyed, with the physical and chemical properties of hydrogen examined as they affect its use as a fuel. Sources of hydrogen production are described including synthesis from coal or natural gas, biomass conversion, thermochemical decomposition of water, and electrolysis of water, of these only electrolysis is considered economicially and technologically feasible in the near future. Methods of production of the large quantities of electricity required for the electrolysis of sea water are explored: fossil fuels, hydroelectric plants, nuclear fission, solar energy, wind power, geothermal energy, tidal power, wave motion, electrochemical concentration cells, and finally ocean thermal energy conversion (OTEC). The wind power and OTEC are considered in detail as the most feasible approaches. Techniques for transmission (by railcar or pipeline), storage (as liquid in underwater or underground tanks, as granular metal hydride, or as cryogenic liquid), and consumption (in fuel cells in conventional power plants, for home usage, for industrial furnaces, and for cars and aircraft) are analyzed. The safety problems of hydrogen as a universal fuel are discussed, noting that they are no greater than those for conventional fuels.

Evidence synthesis for medical decision making and the appropriate use of quality scores.

PubMed

Doi, Suhail A R

2014-09-01

Meta-analyses today continue to be run using conventional random-effects models that ignore tangible information from studies such as the quality of the studies involved, despite the expectation that results of better quality studies reflect more valid results. Previous research has suggested that quality scores derived from such quality appraisals are unlikely to be useful in meta-analysis, because they would produce biased estimates of effects that are unlikely to be offset by a variance reduction within the studied models. However, previous discussions took place in the context of such scores viewed in terms of their ability to maximize their association with both the magnitude and direction of bias. In this review, another look is taken at this concept, this time asserting that probabilistic bias quantification is not possible or even required of quality scores when used in meta-analysis for redistribution of weights. The use of such a model is contrasted with the conventional random effects model of meta-analysis to demonstrate why the latter is inadequate in the face of a properly specified quality score weighting method. © 2014 Marshfield Clinic.

Photoacoustic spectroscopic studies of polycyclic aromatic hydrocarbons

NASA Astrophysics Data System (ADS)

Zaidi, Zahid H.; Kumar, Pardeep; Garg, R. K.

1999-02-01

Because of their involvement in environmental pollutants, in carcinogenic activity, plastics, pharmaceuticals, synthesis of some laser dyes and presence in interstellar space etc., Polycyclic aromatic hydrocarbons (PAHs) are important. As their structure and properties can be varied systematically, they form a beautiful class of molecules for experimental and quantum chemical investigations. These molecules are being studied for last several years by using conventional spectroscopy. In recent years, Photoacoustic (PA) spectroscopy has emerged as a new non-destructive technique with unique capability and sensitivity. The PA effect is the process of generation of acoustic waves in a sample resulting from the absorption of photons. This technique not only reveals non- radiative transitions but also provides information about forbidden singlet-triplet transitions which are not observed normally by the conventional spectroscopy. The present paper deals with the spectroscopic studies of some PAH molecules by PA spectroscopy in the region 250 - 400 nm. The CNDO/S-CI method is used to calculate the electronic transitions with the optimized geometries. A good agreement is found between the experimental and calculated results.

Morphology filter bank for extracting nodular and linear patterns in medical images.

PubMed

Hashimoto, Ryutaro; Uchiyama, Yoshikazu; Uchimura, Keiichi; Koutaki, Gou; Inoue, Tomoki

2017-04-01

Using image processing to extract nodular or linear shadows is a key technique of computer-aided diagnosis schemes. This study proposes a new method for extracting nodular and linear patterns of various sizes in medical images. We have developed a morphology filter bank that creates multiresolution representations of an image. Analysis bank of this filter bank produces nodular and linear patterns at each resolution level. Synthesis bank can then be used to perfectly reconstruct the original image from these decomposed patterns. Our proposed method shows better performance based on a quantitative evaluation using a synthesized image compared with a conventional method based on a Hessian matrix, often used to enhance nodular and linear patterns. In addition, experiments show that our method can be applied to the followings: (1) microcalcifications of various sizes in mammograms can be extracted, (2) blood vessels of various sizes in retinal fundus images can be extracted, and (3) thoracic CT images can be reconstructed while removing normal vessels. Our proposed method is useful for extracting nodular and linear shadows or removing normal structures in medical images.

A practical and catalyst-free trifluoroethylation reaction of amines using trifluoroacetic acid

NASA Astrophysics Data System (ADS)

Andrews, Keith G.; Faizova, Radmila; Denton, Ross M.

2017-06-01

Amines are a fundamentally important class of biologically active compounds and the ability to manipulate their physicochemical properties through the introduction of fluorine is of paramount importance in medicinal chemistry. Current synthesis methods for the construction of fluorinated amines rely on air and moisture sensitive reagents that require special handling or harsh reductants that limit functionality. Here we report practical, catalyst-free, reductive trifluoroethylation reactions of free amines exhibiting remarkable functional group tolerance. The reactions proceed in conventional glassware without rigorous exclusion of either moisture or oxygen, and use trifluoroacetic acid as a stable and inexpensive fluorine source. The new methods provide access to a wide range of medicinally relevant functionalized tertiary β-fluoroalkylamine cores, either through direct trifluoroethylation of secondary amines or via a three-component coupling of primary amines, aldehydes and trifluoroacetic acid. A reduction of in situ-generated silyl ester species is proposed to account for the reductive selectivity observed.

Facile electrosynthesis of silicon carbide nanowires from silica/carbon precursors in molten salt.

PubMed

Zou, Xingli; Ji, Li; Lu, Xionggang; Zhou, Zhongfu

2017-08-30

Silicon carbide nanowires (SiC NWs) have attracted intensive attention in recent years due to their outstanding performances in many applications. A large-scale and facile production of SiC NWs is critical to its successful application. Here, we report a simple method for the production of SiC NWs from inexpensive and abundantly available silica/carbon (SiO 2 /C) precursors in molten calcium chloride. The solid-to-solid electroreduction and dissolution-electrodeposition mechanisms can easily lead to the formation of homogenous SiC NWs. This template/catalyst-free approach greatly simplifies the synthesis procedure compared to conventional methods. This general strategy opens a direct electrochemical route for the conversion of SiO 2 /C into SiC NWs, and may also have implications for the electrosynthesis of other micro/nanostructured metal carbides/composites from metal oxides/carbon precursors.

Applied photo interpretation for airbrush cartography

NASA Technical Reports Server (NTRS)

Inge, J. L.; Bridges, P. M.

1976-01-01

Lunar and planetary exploration has required the development of new techniques of cartographic portrayal. Conventional photo-interpretive methods employing size, shape, shadow, tone, pattern, and texture are applied to computer-processed satellite television images. Comparative judgements are affected by illumination, resolution, variations in surface coloration, and transmission or processing artifacts. The portrayal of tonal densities in a relief illustration is performed using a unique airbrush technique derived from hill-shading of contour maps. The control of tone and line quality is essential because the mid-gray to dark tone densities must be finalized prior to the addition of highlights to the drawing. This is done with an electric eraser until the drawing is completed. The drawing density is controlled with a reflectance-reading densitometer to meet certain density guidelines. The versatility of planetary photo-interpretive methods for airbrushed map portrayals is demonstrated by the application of these techniques to the synthesis of nonrelief data.

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

Connatser, Raynella M; Prokes, Sharka M.; Glembocki, Orest

Exposure to light or heat, or simply a dearth of fingerprint material, renders some latent fingerprints undetectable using conventional methods. We begin to address such elusive fingerprints using detection targeting photo- and thermally stable fingerprint constituents: surface-enhanced Raman spectroscopy (SERS). SERS can give descriptive vibrational spectra of amino acids, among other robust fingerprint constituents, and good sensitivity can be attained by improving metal-dielectric nanoparticle substrates. With SERS chemical imaging, vibrational bands intensities recreate a visual of fingerprint topography. The impact of nanoparticle synthesis route, dispersal methodology-deposition solvent, and laser wavelength are discussed, as are data from enhanced vibrational spectra ofmore » fingerprint components. SERS and Raman chemical images of fingerprints and realistic contaminants are shown. To our knowledge, this represents the first SERS imaging of fingerprints. In conclusion, this work progresses toward the ultimate goal of vibrationally detecting latent prints that would otherwise remain undetected using traditional development methods.« less

Cobalt ferrite nanocrystals: out-performing magnetotactic bacteria.

PubMed

Prozorov, Tanya; Palo, Pierre; Wang, Lijun; Nilsen-Hamilton, Marit; Jones, DeAnna; Orr, Daniel; Mallapragada, Surya K; Narasimhan, Balaji; Canfield, Paul C; Prozorov, Ruslan

2007-10-01

Magnetotactic bacteria produce exquisitely ordered chains of uniform magnetite (Fe(3)O(4)) nanocrystals, and the use of the bacterial mms6 protein allows for the shape-selective synthesis of Fe(3)O(4) nanocrystals. Cobalt ferrite (CoFe(2)O(4)) nanoparticles, on the other hand, are not known to occur in living organisms. Here we report on the use of the recombinant mms6 protein in a templated synthesis of CoFe(2)O(4) nanocrystals in vitro. We have covalently attached the full-length mms6 protein and a synthetic C-terminal domain of mms6 protein to self-assembling polymers in order to template hierarchical CoFe(2)O(4) nanostructures. This new synthesis pathway enables facile room-temperature shape-specific synthesis of complex magnetic crystalline nanomaterials with particle sizes in the range of 40-100 nm that are difficult to produce using conventional techniques.

Low-temperature synthesis of allyl dimethylamine by selective heating under microwave irradiation used for water treatment

NASA Astrophysics Data System (ADS)

Tian, Binghui; Luan, Zhaokun; Li, Mingming

2005-08-01

Low-temperature synthesis of allyl dimethylamine (ADA) by selective heating under microwave irradiation (MI) used for water treatment is investigated. The effect of MI, ultrasound irradiation (UI) and conventional heating on yield of ADA, reaction time and the flocculation efficiency of polydiallyl dimethylammunion chloride (PDADMAC) prepared form ADA were studied. The results show that by selective heating at low temperature, MI not only increases yield of ADA and reduces reaction time, but also greatly enhances the flocculation efficiency of PDADMAC.

Integration of a code for aeroelastic design of conventional and composite wings into ACSYNT, an aircraft synthesis program. [wing aeroelastic design (WADES)

NASA Technical Reports Server (NTRS)

Mullen, J., Jr.

1976-01-01

A comparison of program estimates of wing weight, material distribution. structural loads and elastic deformations with actual Northrop F-5A/B data is presented. Correlation coefficients obtained using data from a number of existing aircraft were computed for use in vehicle synthesis to estimate wing weights. The modifications necessary to adapt the WADES code for use in the ACSYNT program are described. Basic program flow and overlay structure is outlined. An example of the convergence of the procedure in estimating wing weights during the synthesis of a vehicle to satisfy F-5 mission requirements is given. A description of inputs required for use of the WADES program is included.

Synthesis of biomass derived carbon materials for environmental engineering and energy storage applications

NASA Astrophysics Data System (ADS)

Huggins, Mitchell Tyler

Biomass derived carbon (BC) can serve as an environmentally and cost effective material for both remediation and energy production/storage applications. The use of locally derived biomass, such as unrefined wood waste, provides a renewable feedstock for carbon material production compared to conventional unrenewable resources like coal. Additionally, energy and capital cost can be reduced through the reduction in transport and processing steps and the use of spent material as a soil amendment. However, little work has been done to evaluate and compare biochar to conventional materials such as granular activated carbon or graphite in advanced applications of Environmental Engineering. In this work I evaluated the synthesis and compared the performance of biochar for different applications in wastewater treatment, nutrient recovery, and energy production and storage. This includes the use of biochar as an electrode and filter media in several bioelectrochemical systems (BES) treating synthetic and industrial wastewater. I also compared the treatment efficiency of granular biochar as a packed bed adsorbent for the primary treatment of high strength brewery wastewater. My studies conclude with the cultivation of fungal biomass to serve as a template for biochar synthesis, controlling the chemical and physical features of the feedstock and avoiding some of the limitations of waste derived materials.

Combining mutations at genes encoding key enzymes involved in starch synthesis affects the amylose content, carbohydrate allocation and hardness in the wheat grain.

PubMed

Botticella, Ermelinda; Sestili, Francesco; Sparla, Francesca; Moscatello, Stefano; Marri, Lucia; Cuesta-Seijo, Jose A; Falini, Giuseppe; Battistelli, Alberto; Trost, Paolo; Lafiandra, Domenico

2018-03-02

Modifications to the composition of starch, the major component of wheat flour, can have a profound effect on the nutritional and technological characteristics of the flour's end products. The starch synthesized in the grain of conventional wheats (Triticum aestivum) is a 3:1 mixture of the two polysaccharides amylopectin and amylose. Altering the activity of certain key starch synthesis enzymes (GBSSI, SSIIa and SBEIIa) has succeeded in generating starches containing a different polysaccharide ratio. Here, mutagenesis, followed by a conventional marker-assisted breeding exercise, has been used to generate three mutant lines that produce starch with an amylose contents of 0%, 46% and 79%. The direct and pleiotropic effects of the multiple mutation lines were identified at both the biochemical and molecular levels. Both the structure and composition of the starch were materially altered, changes which affected the functionality of the starch. An analysis of sugar and nonstarch polysaccharide content in the endosperm suggested an impact of the mutations on the carbon allocation process, suggesting the existence of cross-talk between the starch and carbohydrate synthesis pathways. © 2018 The Authors. Plant Biotechnology Journal published by Society for Experimental Biology and The Association of Applied Biologists and John Wiley & Sons Ltd.

Technique of laser chromosome welding for chromosome repair and artificial chromosome creation.

PubMed

Huang, Yao-Xiong; Li, Lin; Yang, Liu; Zhang, Yi

2018-04-01

Here we report a technique of laser chromosome welding that uses a violet pulse laser micro-beam for welding. The technique can integrate any size of a desired chromosome fragment into recipient chromosomes by combining with other techniques of laser chromosome manipulation such as chromosome cutting, moving, and stretching. We demonstrated that our method could perform chromosomal modifications with high precision, speed and ease of use in the absence of restriction enzymes, DNA ligases and DNA polymerases. Unlike the conventional methods such as de novo artificial chromosome synthesis, our method has no limitation on the size of the inserted chromosome fragment. The inserted DNA size can be precisely defined and the processed chromosome can retain its intrinsic structure and integrity. Therefore, our technique provides a high quality alternative approach to directed genetic recombination, and can be used for chromosomal repair, removal of defects and artificial chromosome creation. The technique may also have applicability on the manipulation and extension of large pieces of synthetic DNA.

Synthesis of atmospheric turbulence point spread functions by sparse and redundant representations

NASA Astrophysics Data System (ADS)

Hunt, Bobby R.; Iler, Amber L.; Bailey, Christopher A.; Rucci, Michael A.

2018-02-01

Atmospheric turbulence is a fundamental problem in imaging through long slant ranges, horizontal-range paths, or uplooking astronomical cases through the atmosphere. An essential characterization of atmospheric turbulence is the point spread function (PSF). Turbulence images can be simulated to study basic questions, such as image quality and image restoration, by synthesizing PSFs of desired properties. In this paper, we report on a method to synthesize PSFs of atmospheric turbulence. The method uses recent developments in sparse and redundant representations. From a training set of measured atmospheric PSFs, we construct a dictionary of "basis functions" that characterize the atmospheric turbulence PSFs. A PSF can be synthesized from this dictionary by a properly weighted combination of dictionary elements. We disclose an algorithm to synthesize PSFs from the dictionary. The algorithm can synthesize PSFs in three orders of magnitude less computing time than conventional wave optics propagation methods. The resulting PSFs are also shown to be statistically representative of the turbulence conditions that were used to construct the dictionary.

L-Methionine Production.

PubMed

Shim, Jihyun; Shin, Yonguk; Lee, Imsang; Kim, So Young

L-Methionine has been used in various industrial applications such as the production of feed and food additives and has been used as a raw material for medical supplies and drugs. It functions not only as an essential amino acid but also as a physiological effector, for example, by inhibiting fat accumulation and enhancing immune response. Producing methionine from fermentation is beneficial in that microorganisms can produce L-methionine selectively using eco-sustainable processes. Nevertheless, the fermentative method has not been used on an industrial scale because it is not competitive economically compared with chemical synthesis methods. Presented are efforts to develop suitable strains, engineered enzymes, and alternative process of producing L-methionine that overcomes problems of conventional fermentation methods. One of the alternative processes is a two-step process in which the L-methionine precursor is produced by fermentation and then converted to L-methionine by enzymes. Directed efforts toward strain development and enhanced enzyme engineering will advance industrial production of L-methionine based on fermentation.

Richard Schrock, Robert Grubbs, and Metathesis Method in Organic Synthesis

Science.gov Websites

Organic Synthesis Resources with Additional Information Richard R. Schrock of the Massachusetts Institute Nobel Prize in Chemistry "for the development of the metathesis method in organic synthesis" ] Chauvin, Grubbs and Schrock "for the development of the metathesis method in organic synthesis,"

Reducing the time-lag between onset of chest pain and seeking professional medical help: a theory-based review

PubMed Central

2013-01-01

Background Research suggests that there are a number of factors which can be associated with delay in a patient seeking professional help following chest pain, including demographic and social factors. These factors may have an adverse impact on the efficacy of interventions which to date have had limited success in improving patient action times. Theory-based methods of review are becoming increasingly recognised as important additions to conventional systematic review methods. They can be useful to gain additional insights into the characteristics of effective interventions by uncovering complex underlying mechanisms. Methods This paper describes the further analysis of research papers identified in a conventional systematic review of published evidence. The aim of this work was to investigate the theoretical frameworks underpinning studies exploring the issue of why people having a heart attack delay seeking professional medical help. The study used standard review methods to identify papers meeting the inclusion criterion, and carried out a synthesis of data relating to theoretical underpinnings. Results Thirty six papers from the 53 in the original systematic review referred to a particular theoretical perspective, or contained data which related to theoretical assumptions. The most frequently mentioned theory was the self-regulatory model of illness behaviour. Papers reported the potential significance of aspects of this model including different coping mechanisms, strategies of denial and varying models of treatment seeking. Studies also drew attention to the potential role of belief systems, applied elements of attachment theory, and referred to models of maintaining integrity, ways of knowing, and the influence of gender. Conclusions The review highlights the need to examine an individual’s subjective experience of and response to health threats, and confirms the gap between knowledge and changed behaviour. Interventions face key challenges if they are to influence patient perceptions regarding seriousness of symptoms; varying processes of coping; and obstacles created by patient perceptions of their role and responsibilities. A theoretical approach to review of these papers provides additional insight into the assumptions underpinning interventions, and illuminates factors which may impact on their efficacy. The method thus offers a useful supplement to conventional systematic review methods. PMID:23388093

Ultrasound assisted lipase catalyzed synthesis of poly-6-hydroxyhexanoate.

PubMed

Gumel, A M; Annuar, M S M; Chisti, Y; Heidelberg, T

2012-05-01

Ultrasonic irradiation greatly improved the Candida antarctica lipase B mediated ring opening polymerization of ε-caprolactone to poly-6-hydroxyhexanoate in the ionic liquid 1-ethyl-3-methylimidazolium tetraflouroborate. Compared to the conventional nonsonicated reaction, sonication improved the monomer conversion by 63% and afforded a polymer product of a narrower molecular weight distribution and a higher degree of crystallinity. Under sonication, the polydispersity index of the product was ~1.44 compared to a value of ~2.55 for the product of the conventional reaction. With sonication, nearly 75% of the monomer was converted to product, but the conversion was only ~16% for the reaction carried out conventionally. Compared to conventional operation, sonication enhanced the rate of polymer propagation by >2-fold and the turnover number of the lipase by >3-fold. Copyright © 2011 Elsevier B.V. All rights reserved.

Multifunctional Nanofluids with 2D Nanosheets for thermal management and tribological applications

NASA Astrophysics Data System (ADS)

Taha Tijerina, Jose Jaime

Conventional heat-transfer fluids such as water, ethylene glycol, standard oils and other lubricants are typically low-efficiency heat-transfer fluids. Thermal management plays a critical factor in many applications where these fluids can be used, such as in motors/engines, solar cells, biopharmaceuticals, fuel cells, high voltage power transmission systems, micro/nanoelectronics mechanical systems (MEMS/NEMS), and nuclear cooling among others. These insulating fluids require superb filler dispersion, high thermal conduction, and for certain applications as in electrical/electronic devices also electrical insulation. The miniaturization and high efficiency of electrical/electronic devices in these fields demand successful heat management and energy-efficient fluid-based heat-transfer systems. Recent advances in layered materials enable large scale synthesis of various two-dimensional (2D) structures. Some of these 2D materials are good choices as nanofillers in heat transfer fluids; mainly due to their inherent high thermal conductivity (TC) and high surface area available for thermal energy transport. Among various 2D-nanostructures, hexagonal boron nitride (h-BN) and graphene (G) exhibit versatile properties such as outstanding TC, excellent mechanical stability, and remarkable chemical inertness. The following research, even though investigate various conventional fluids, will focus on dielectric insulating nanofluids (mineral oil -- MO) with significant thermal performance. It is presented the plan for synthesis and characterization of stable high-thermal conductivity nanofluids using 2D-nanostructures of h-BN, which will be further incorporated at diverse filler concentrations to conventional fluids for cooling applications, without compromising its electrical insulating property. For comparison, properties of h-BN based fluids are compared with conductive fillers such as graphene; where graphene has similar crystal structure of h-BN and also has similar bulk thermal conductivity. Moreover, bot h-BN and graphene are exfoliated through the same method. In essence, this project, for the first time, unravels the behavior of the exfoliated h-BN effect on reinforced conventional fluids under the influence of atomistic scale structures (particularly, electrically insulating and lubricant/cutting fluids), thereby linking the physical, electrical and mechanical properties of these nanoscale materials. The innovative experimental approach is expected to result in de novo strategies for introducing these systems for new concepts and variables to engineer nanofluid properties suitable for very promising industrial applications.

Electrodeposition of Polymer Nanostructures using Three Diffuse Double Layers: Polymerization beyond the Liquid/Liquid Interfaces

NASA Astrophysics Data System (ADS)

Divya, Velpula; Sangaranarayanan, M. V.

2018-04-01

Nanostructured conducting polymers have received immense attention during the past few decades on account of their phenomenal usefulness in diverse contexts, while the interface between two immiscible liquids is of great interest in chemical and biological applications. Here we propose a novel Electrode(solid)/Electrolyte(aqueous)/Electrolyte(organic) Interfacial assembly for the synthesis of polymeric nanostructures using a novel concept of three diffuse double layers. There exist remarkable differences between the morphologies of the polymers synthesized using the conventional electrode/electrolyte method and that of the new approach. In contrast to the commonly employed electrodeposition at liquid/liquid interfaces, these polymer modified electrodes can be directly employed in diverse applications such as sensors, supercapacitors etc.

Synthesis of Green-Emitting (La,Gd)OBr:Tb3+ Phosphors

PubMed Central

Kim, Sun Woog; Jyoko, Kazuya; Masui, Toshiyuki; Imanaka, Nobuhito

2010-01-01

Green-emitting phosphors based on lanthanum-gadolinium oxybromide were synthesized in a single phase form by the conventional solid state reaction method, and photoluminescence properties of them were characterized. The excitation peak wavelength of (La1-xGdx)OBr:Tb3+ shifted to the shorter wavelength side with the increase in the crystal field around the Tb3+ ions by doping Gd3+ ions into the La3+ site, and, as a result, the green emission intensity was successfully enhanced. The maximum emission intensity was obtained for (La0.95Gd0.05)OBr:5%Tb3+, where the relative emission intensity was 45% of that of a commercial green-emitting LaPO4:Ce3+,Tb3+ phosphor.

Facile synthesis of PbTe nanoparticles and thin films in alkaline aqueous solution at room temperature

NASA Astrophysics Data System (ADS)

Wang, Y. Y.; Cai, K. F.; Yao, X.

2009-12-01

A novel, simple, and cost-effective route to PbTe nanoparticles and films is reported in this paper. The PbTe nanoparticles and films are fabricated by a chemical bath method, at room temperature and ambient pressure, using conventional chemicals as starting materials. The average grain size of the nanoparticles collected at the bottom of the bath is ˜25 nm. The film deposited on glass substrate is dense, smooth, and uniform with silver gray metallic luster. The film exhibits p-type conduction and has a moderate Seebeck coefficient value (˜147 μV K -1) and low electrical conductivity (˜0.017 S cm -1). The formation mechanism of the PbTe nanoparticles and films is proposed.

Synthesis of graphene nanoflakes by grinding natural graphite together with NaCl in a planetary ball mill

NASA Astrophysics Data System (ADS)

Alinejad, Babak; Mahmoodi, Korosh

Natural graphite is a soft material that conventional milling methods fail to grind into nanoparticles. We found that adding NaCl into graphite during milling allows obtaining graphene nanoflakes of about 50×200nm2 as evidenced by Transmission Electron Microscope (TEM). NaCl particles are substantially brittle and harder than graphite, serving as milling agents by both helping to chop graphite into smaller pieces and preventing graphite particles from agglomeration. After milling, NaCl can be easily washed away by water. Probable mechanism for exfoliation of graphene during the modified ball milling may be explained by NaCl and graphene slipping or sliding against and over each other, exfoliating the graphene particles into thin layers.

Amino Acid Bound Surfactants: A New Synthetic Family of Polymeric Monoliths Open Up Possibilities for Chiral Separations in Capillary Electrochromatography

PubMed Central

He, Jun; Wang, Xiaochun; Morrill, Mike; Shamsi, Shahab A.

2012-01-01

By combining a novel chiral amino-acid surfactant containing acryloyl amide tail, carbamate linker and leucine head group of different chain lengths with a conventional cross linker and a polymerization technique, a new “one-pot”, synthesis for the generation of amino-acid based polymeric monolith is realized. The method promises to open up the discovery of amino-acid based polymeric monolith for chiral separations in capillary electrochromatography (CEC). Possibility of enhanced chemoselectivity for simultaneous separation of ephedrine and pseudoephedrine containing multiple chiral centers, and the potential use of this amino-acid surfactant bound column for CEC and CEC coupled to mass spectrometric detection is demonstrated. PMID:22607448

Knowledge synthesis methods for generating or refining theory: a scoping review reveals that little guidance is available.

PubMed

Tricco, Andrea C; Antony, Jesmin; Soobiah, Charlene; Kastner, Monika; Cogo, Elise; MacDonald, Heather; D'Souza, Jennifer; Hui, Wing; Straus, Sharon E

2016-05-01

To describe and compare, through a scoping review, emerging knowledge synthesis methods for generating and refining theory, in terms of expertise required, similarities, differences, strengths, limitations, and steps involved in using the methods. Electronic databases (e.g., MEDLINE) were searched, and two reviewers independently selected studies and abstracted data for qualitative analysis. In total, 287 articles reporting nine knowledge synthesis methods (concept synthesis, critical interpretive synthesis, integrative review, meta-ethnography, meta-interpretation, meta-study, meta-synthesis, narrative synthesis, and realist review) were included after screening of 17,962 citations and 1,010 full-text articles. Strengths of the methods included comprehensive synthesis providing rich contextual data and suitability for identifying gaps in the literature, informing policy, aiding in clinical decisions, addressing complex research questions, and synthesizing patient preferences, beliefs, and values. However, many of the methods were highly subjective and not reproducible. For integrative review, meta-ethnography, and realist review, guidance was provided on all steps of the review process, whereas meta-synthesis had guidance on the fewest number of steps. Guidance for conducting the steps was often vague and sometimes absent. Further work is needed to provide direction on operationalizing these methods. Copyright © 2016 Elsevier Inc. All rights reserved.

Prenatal diagnosis of hemoglobinopathies: evaluation of techniques for analysing globin-chain synthesis in blood samples obtained by fetoscopy.

PubMed Central

Congote, L. F.; Hamilton, E. F.; Chow, J. C.; Perry, T. B.

1982-01-01

Three techniques for analysing hemoglobin synthesis in blood samples obtained by fetoscopy were evaluated. Of the fetuses studied, 12 were not at risk of genetic disorders, 10 were at risk of beta-thalassemia, 2 were at risk of sickle cell anemia and 1 was at risk of both diseases. The conventional method of prenatal diagnosis of hemoglobinopathies, involving the separation of globin chains labelled with a radioactive isotope on carboxymethyl cellulose (CMC) columns, was compared with a method involving globin-chain separation by high-pressure liquid chromatography (HPLC) and with direct analysis of labelled hemoglobin tetramers obtained from cell lysates by chromatography on ion-exchange columns. The last method is technically the simplest and can be used for diagnosing beta-thalassemia and sickle cell anemia. However, it gives spuriously high levels of adult hemoglobin in samples containing nonlabelled adult hemoglobin. HPLC is the fastest method for prenatal diagnosis of beta-thalassemia and may prove as reliable as the CMC method. Of the 13 fetuses at risk for hemoglobinopathies, 1 was predicted to be affected, and the diagnosis was confirmed in the abortus. Of 12 predicted to be unaffected, 1 was aborted spontaneously and was unavailable for confirmatory studies, as were 3 of the infants; however, the diagnosis was confirmed in seven cases and is awaiting confirmation when the infant in 6 months old in one case. Couples at risk of bearing a child with a hemoglobinopathy should be referred for genetic counselling before pregnancy or, at the latest, by the 12th week of gestation so that prenatal diagnosis can be attempted by amniocentesis, safer procedure, with restriction endonuclease analysis of the amniotic fluid cells. PMID:7139502

Non-conventional features of peripheral serotonin signalling - the gut and beyond.

PubMed

Spohn, Stephanie N; Mawe, Gary M

2017-07-01

Serotonin was first discovered in the gut, and its conventional actions as an intercellular signalling molecule in the intrinsic and extrinsic enteric reflexes are well recognized, as are a number of serotonin signalling pharmacotherapeutic targets for treatment of nausea, diarrhoea or constipation. The latest discoveries have greatly broadened our understanding of non-conventional actions of peripheral serotonin within the gastrointestinal tract and in a number of other tissues. For example, it is now clear that bacteria within the lumen of the bowel influence serotonin synthesis and release by enterochromaffin cells. Also, serotonin can act both as a pro-inflammatory and anti-inflammatory signalling molecule in the intestinal mucosa via activation of serotonin receptors (5-HT 7 or 5-HT 4 receptors, respectively). For decades, serotonin receptors have been known to exist in a variety of tissues other than the gut, but studies have now provided strong evidence for physiological roles of serotonin in several important processes, including haematopoiesis, metabolic homeostasis and bone metabolism. Furthermore, evidence for serotonin synthesis in peripheral tissues outside of the gut is emerging. In this Review, we expand the discussion beyond gastrointestinal functions to highlight the roles of peripheral serotonin in colitis, haematopoiesis, energy and bone metabolism, and how serotonin is influenced by the gut microbiota.

Acoustic cavitation induced synthesis of zirconium impregnated activated carbon for effective fluoride scavenging from water by adsorption.

PubMed

Mullick, Aditi; Neogi, Sudarsan

2018-07-01

Environmental concern associated with the side effects of high fluoride content in ground water and surface water has prompted the researchers to look for an efficient, convenient and easy method. Considering the potential of a good adsorbent, present study reports the synthesis of a composite by impregnating zirconium on powdered activated carbon (AC) using ultrasound as the tool for synthesis and applying it for fluoride adsorption from water. The nature of the composite was determined through characterization by scanning electron microscopy (SEM), energy dispersive Xray (EDX), Xray diffraction (XRD), N 2 adsorption analysis (BET) and Fourier Transform Infrared Spectroscopy (FTIR) analysis. The pH pzc (point of zero charge) of the adsorbent was found to be 5.03; with the optimum pH obtained at 4 for adsorption of strong electronegative fluoride ions. The initial fluoride concentration was varied from 2.5 up to 20 mg.L -1 and the maximum adsorption capacity of 5 mg.g -1 was obtained. A maximum fluoride removal of 94.4% was obtained for an initial concentration of 2.5 mg.L -1 within an equilibrium time of 180 min. The adsorption isotherm followed the Langmuir isotherm model indicating a monolayer adsorption process and the adsorption kinetics followed pseudo second order model. The effects of various coexisting ions (HCO 3 - , NO 3 - , SO 4 2- , Cl - ) commonly present in the water were found to have negligible impact on the process performance. Conducting the adsorption-desorption studies for five consecutive cycles for an initial fluoride concentration of 10 mg.L -1 , the removal efficiency reduced from 86.2 to 32.6%. The ultrasonic method provided an easy route to synthesize the composite in less time and significantly reduced energy consumption by more than 96% compared to the conventional method. Copyright © 2018 Elsevier B.V. All rights reserved.

Microwave assisted synthesis of cyclic carbonates from olefins with sodium bicarbonates as the C1 source.

PubMed

Yang, Xiaoqing; Wu, Jie; Mao, Xianwen; Jamison, Timothy F; Hatton, T Alan

2014-03-25

An effective transformation of alkenes into cyclic carbonates has been achieved using NaHCO3 as the C1 source in acetone-water under microwave heating, with selectivities and yields significantly surpassing those obtained using conventional heating.

Creating wavelet-based models for real-time synthesis of perceptually convincing environmental sounds

NASA Astrophysics Data System (ADS)

Miner, Nadine Elizabeth

1998-09-01

This dissertation presents a new wavelet-based method for synthesizing perceptually convincing, dynamic sounds using parameterized sound models. The sound synthesis method is applicable to a variety of applications including Virtual Reality (VR), multi-media, entertainment, and the World Wide Web (WWW). A unique contribution of this research is the modeling of the stochastic, or non-pitched, sound components. This stochastic-based modeling approach leads to perceptually compelling sound synthesis. Two preliminary studies conducted provide data on multi-sensory interaction and audio-visual synchronization timing. These results contributed to the design of the new sound synthesis method. The method uses a four-phase development process, including analysis, parameterization, synthesis and validation, to create the wavelet-based sound models. A patent is pending for this dynamic sound synthesis method, which provides perceptually-realistic, real-time sound generation. This dissertation also presents a battery of perceptual experiments developed to verify the sound synthesis results. These experiments are applicable for validation of any sound synthesis technique.

Synthesis of nonlinear control strategies from fuzzy logic control algorithms

NASA Technical Reports Server (NTRS)

Langari, Reza

1993-01-01

Fuzzy control has been recognized as an alternative to conventional control techniques in situations where the plant model is not sufficiently well known to warrant the application of conventional control techniques. Precisely what fuzzy control does and how it does what it does is not quite clear, however. This important issue is discussed and in particular it is shown how a given fuzzy control scheme can resolve into a nonlinear control law and that in those situations the success of fuzzy control hinges on its ability to compensate for nonlinearities in plant dynamics.

Physicochemical characterization of microwave assisted synthesis of silver nanoparticles using Aloe Vera (Aloe barbadensis)

NASA Astrophysics Data System (ADS)

Kuponiyi, Abiola John

Biosynthesis of silver nanoparticles (AgNP) using different biological extracts is gaining recognition for its numerous applications in different disciplines. Although different approaches (physical and chemical) have been used for the synthesis of AgNP, the green chemistry method is most preferable because of its high efficacy, cost effectiveness, and environmental benignity. Aloe Vera (AV) contains chemical compounds (anthraquinones) that are known to possess antibacterial, antivirus and anticancer properties and the extract is a good chemical reduction agent for AgNP. Hence, it was hypothesized that a microwave assisted synthesis will produce highly concentrated, homogeneous, stable and biologically active AgNP. Thus, the main objective of the study was to evaluate the effect of microwave assisted synthesis of AgNP, the effect of pulse laser treatment on size reduction of a microwave synthesized AgNP, and the physicochemical characterization of AgNP synthesized with Aloe Vera water and ethanol extract. The experiment was conducted in two phases. Phase 1 was first conducted to optimize the experimental variables, thus establishing the optimum variables to apply in the second phase. The experiment in Phase 1 was conducted using three-factor factorial experimental design comprised of the following factors: 1) Extraction Solvent, 2) Heating Methods, 3) pH; and their corresponding levels were water and ethanol, conventional and microwave, pH (7, 8, 10 and 12), respectively. All synthesis was conducted at constant temperature of 80°C. Phase II experimental treatments were Laser ablation (0, 5, and 10 min) and Storage time (Week 1, 2 & 3). The Phase I of the results showed that increased AgNP concentrations were significantly (p < 0.05) influenced by synthesis time, hence, (15 min) gave the highest concentration. The solvent type, heating methods and pH had a significant effect (p < 0.05) on the concentration AgNP. Hence, ethanol extract (99.2 ppm), microwave method (77 ppm), and pH 10 (125 ppm) are variables that exhibited the maximum contribution to the formation of AgNP. The phase II ANOVA results indicated that laser treatment has a significant effect (p < 0.01) on the concentration of AgNP during synthesis. The intensity of the absorption peak significantly (p < 0.01) increases with laser exposure time. While 214 ppm was observed at laser exposures time 0 min, 224 and 229 ppm at 5 and 10 min and at the following rates of formation 0.384, 0.408 and 0.4288 min -1 respectively. Particle sizes (hydrodynamic diameter) were approximately 37.84 nm with no laser treatment in contrast (p < 0.01) with laser treated samples at 5 and 10 min at week 1 were 10.1 and 8.72 nm, respectively. However, storability up to the maximum storage period of six weeks of the AgNP solutions does not significantly (p > 0.05) impact the particle size distribution. Hence, the Zeta potential of the particles has values typically ranging between +100 mV to -100 mV, hence indicative of colloidal stability matrix. Furthermore, the Polydispersity indexes of Week 1, 2, & 3 treatments were 0.312, 0.591 and 0.768 respectfully, indicating that the control is monodispersed while treatments week 2 & 3 indicating the laser ablation effect in further reduction of sizes to a different level of aggregation. Microwave synthesis showed significantly (p < 0.05) higher concentration of biological compounds such as aliphatic amines, alkenes (=C-H), alkanes (C-H), alcohol (O-H) and unsaturated esters(C-O).

Performance of an ultrafiltration membrane bioreactor (UF-MBR) as a processing strategy for the synthesis of galacto-oligosaccharides at high substrate concentrations.

PubMed

Córdova, Andrés; Astudillo, Carolina; Vera, Carlos; Guerrero, Cecilia; Illanes, Andrés

2016-04-10

The performance of an ultrafiltration membrane bioreactor for galacto-oligosaccharides (GOS) synthesis using high lactose concentrations (470 g/L) and β-galactosidase from Aspergillus oryzae was assessed. Tested processing variables were: transmembrane-pressure (PT), crossflow-velocity (CFV) and temperature. Results showed that processing variables had significant effect on the yield, the enzyme productivity and the flux but did not on GOS concentration and reaction conversion obtained. As expected, the use of high turbulences improved mass transfer and reduced the membrane fouling, but the use of very high crossflow-velocities caused operational instability due to vortex formation and lactose precipitation. The use of a desirability function allowed determining optimal conditions which were: PT (4.38 bar), CFV (7.35 m/s) and temperature (53.1 °C), optimizing simultaneously flux and specific enzyme productivity Under these optimal processing conditions, shear-stress and temperature did not affect the enzyme but long-term operation was limited by flux decay. In comparison to a conventional batch system, at 12.5h of processing time, the continuous GOS synthesis in the UF-MBR increased significantly the amount of processed substrate and a 2.44-fold increase in the amount of GOS produced per unit mass of catalyst was obtained with respect to a conventional batch system. Furthermore, these results can be improved by far by tuning the membranearea/reactionvolume ratio, showing that the use of an UF-MBR is an attractive alternative for the GOS synthesis at very high lactose concentrations. Copyright © 2016 Elsevier B.V. All rights reserved.

Rapid, facile microwave-assisted synthesis of xanthan gum grafted polyaniline for chemical sensor.

PubMed

Pandey, Sadanand; Ramontja, James

2016-08-01

Grafting method, through microwave radiation procedure is extremely productive in terms of time consumption, cost effectiveness and environmental friendliness. In this study, conductive and thermally stable composite (mwXG-g-PANi) was synthesized by grafting of aniline (ANi) on to xanthan gum (XG) using catalytic weight of initiator, ammonium peroxydisulfate in the process of microwave irradiation in an aqueous medium. The synthesis of mwXG-g-PANi were confirm by FTIR, XRD, TGA, and SEM. The influence of altering the microwave power, exposure time of microwave, concentration of monomer and the amount of initiator of graft polymerization were studied over the grafting parameters, for example, grafting percentage (%G) and grafting efficiency (%E). The maximum %G and %E achieved was 172 and 74.13 respectively. The outcome demonstrates that the microwave irradiation strategy can increase the reaction rate by 72 times over the conventional method. Electrical conductivity of XG and mwXG-g-PANi composite film was performed. The fabricated grafted sample film were then examined for the chemical sensor. The mwXG-g-PANi, effectively integrated and handled, are NH3 sensitive and exhibit a rapid sensing in presence of NH3 vapor. Chemiresistive NH3 sensors with superior room temperature sensing performance were produced with sensor response of 905 at 1ppb and 90% recovery within few second. Copyright © 2016 Elsevier B.V. All rights reserved.

Acidic organic compounds in beverage, food, and feed production.

PubMed

Quitmann, Hendrich; Fan, Rong; Czermak, Peter

2014-01-01

Organic acids and their derivatives are frequently used in beverage, food, and feed production. Acidic additives may act as buffers to regulate acidity, antioxidants, preservatives, flavor enhancers, and sequestrants. Beneficial effects on animal health and growth performance have been observed when using acidic substances as feed additives. Organic acids could be classified in groups according to their chemical structure. Each group of organic acids has its own specific properties and is used for different applications. Organic acids with low molecular weight (e.g. acetic acid, lactic acid, and citric acid), which are part of the primary metabolism, are often produced by fermentation. Others are produced more economically by chemical synthesis based on petrochemical raw materials on an industrial scale (e.g. formic acid, propionic and benzoic acid). Biotechnology-based production is of interest due to legislation, consumer demand for natural ingredients, and increasing environmental awareness. In the United States, for example, biocatalytically produced esters for food applications can be labeled as "natural," whereas identical conventional acid catalyst-based molecules cannot. Natural esters command a price several times that of non-natural esters. Biotechnological routes need to be optimized regarding raw materials and yield, microorganisms, and recovery methods. New bioprocesses are being developed for organic acids, which are at this time commercially produced by chemical synthesis. Moreover, new organic acids that could be produced with biotechnological methods are under investigation for food applications.

Validity and reliability of intraoral scanners compared to conventional gypsum models measurements: a systematic review.

PubMed

Aragón, Mônica L C; Pontes, Luana F; Bichara, Lívia M; Flores-Mir, Carlos; Normando, David

2016-08-01

The development of 3D technology and the trend of increasing the use of intraoral scanners in dental office routine lead to the need for comparisons with conventional techniques. To determine if intra- and inter-arch measurements from digital dental models acquired by an intraoral scanner are as reliable and valid as the similar measurements achieved from dental models obtained through conventional intraoral impressions. An unrestricted electronic search of seven databases until February 2015. Studies that focused on the accuracy and reliability of images obtained from intraoral scanners compared to images obtained from conventional impressions. After study selection the QUADAS risk of bias assessment tool for diagnostic studies was used to assess the risk of bias (RoB) among the included studies. Four articles were included in the qualitative synthesis. The scanners evaluated were OrthoProof, Lava, iOC intraoral, Lava COS, iTero and D250. These studies evaluated the reliability of tooth widths, Bolton ratio measurements, and image superimposition. Two studies were classified as having low RoB; one had moderate RoB and the remaining one had high RoB. Only one study evaluated the time required to complete clinical procedures and patient's opinion about the procedure. Patients reported feeling more comfortable with the conventional dental impression method. Associated costs were not considered in any of the included study. Inter- and intra-arch measurements from digital models produced from intraoral scans appeared to be reliable and accurate in comparison to those from conventional impressions. This assessment only applies to the intraoral scanners models considered in the finally included studies. Digital models produced by intraoral scan eliminate the need of impressions materials; however, currently, longer time is needed to take the digital images. PROSPERO (CRD42014009702). None. © The Author 2016. Published by Oxford University Press on behalf of the European Orthodontic Society. All rights reserved. For permissions, please email: journals.permissions@oup.com.

“Best fit” framework synthesis: refining the method

PubMed Central

2013-01-01

Background Following publication of the first worked example of the “best fit” method of evidence synthesis for the systematic review of qualitative evidence in this journal, the originators of the method identified a need to specify more fully some aspects of this particular derivative of framework synthesis. Methods and Results We therefore present a second such worked example in which all techniques are defined and explained, and their appropriateness is assessed. Specified features of the method include the development of new techniques to identify theories in a systematic manner; the creation of an a priori framework for the synthesis; and the “testing” of the synthesis. An innovative combination of existing methods of quality assessment, analysis and synthesis is used to complete the process. This second worked example was a qualitative evidence synthesis of employees’ views of workplace smoking cessation interventions, in which the “best fit” method was found to be practical and fit for purpose. Conclusions The method is suited to producing context-specific conceptual models for describing or explaining the decision-making and health behaviours of patients and other groups. It offers a pragmatic means of conducting rapid qualitative evidence synthesis and generating programme theories relating to intervention effectiveness, which might be of relevance both to researchers and policy-makers. PMID:23497061

A continuous-exchange cell-free protein synthesis system based on extracts from cultured insect cells.

PubMed

Stech, Marlitt; Quast, Robert B; Sachse, Rita; Schulze, Corina; Wüstenhagen, Doreen A; Kubick, Stefan

2014-01-01

In this study, we present a novel technique for the synthesis of complex prokaryotic and eukaryotic proteins by using a continuous-exchange cell-free (CECF) protein synthesis system based on extracts from cultured insect cells. Our approach consists of two basic elements: First, protein synthesis is performed in insect cell lysates which harbor endogenous microsomal vesicles, enabling a translocation of de novo synthesized target proteins into the lumen of the insect vesicles or, in the case of membrane proteins, their embedding into a natural membrane scaffold. Second, cell-free reactions are performed in a two chamber dialysis device for 48 h. The combination of the eukaryotic cell-free translation system based on insect cell extracts and the CECF translation system results in significantly prolonged reaction life times and increased protein yields compared to conventional batch reactions. In this context, we demonstrate the synthesis of various representative model proteins, among them cytosolic proteins, pharmacological relevant membrane proteins and glycosylated proteins in an endotoxin-free environment. Furthermore, the cell-free system used in this study is well-suited for the synthesis of biologically active tissue-type-plasminogen activator, a complex eukaryotic protein harboring multiple disulfide bonds.

A Continuous-Exchange Cell-Free Protein Synthesis System Based on Extracts from Cultured Insect Cells

PubMed Central

Stech, Marlitt; Quast, Robert B.; Sachse, Rita; Schulze, Corina; Wüstenhagen, Doreen A.; Kubick, Stefan

2014-01-01

In this study, we present a novel technique for the synthesis of complex prokaryotic and eukaryotic proteins by using a continuous-exchange cell-free (CECF) protein synthesis system based on extracts from cultured insect cells. Our approach consists of two basic elements: First, protein synthesis is performed in insect cell lysates which harbor endogenous microsomal vesicles, enabling a translocation of de novo synthesized target proteins into the lumen of the insect vesicles or, in the case of membrane proteins, their embedding into a natural membrane scaffold. Second, cell-free reactions are performed in a two chamber dialysis device for 48 h. The combination of the eukaryotic cell-free translation system based on insect cell extracts and the CECF translation system results in significantly prolonged reaction life times and increased protein yields compared to conventional batch reactions. In this context, we demonstrate the synthesis of various representative model proteins, among them cytosolic proteins, pharmacological relevant membrane proteins and glycosylated proteins in an endotoxin-free environment. Furthermore, the cell-free system used in this study is well-suited for the synthesis of biologically active tissue-type-plasminogen activator, a complex eukaryotic protein harboring multiple disulfide bonds. PMID:24804975

Fault tolerant control laws

NASA Technical Reports Server (NTRS)

Ly, U. L.; Ho, J. K.

1986-01-01

A systematic procedure for the synthesis of fault tolerant control laws to actuator failure has been presented. Two design methods were used to synthesize fault tolerant controllers: the conventional LQ design method and a direct feedback controller design method SANDY. The latter method is used primarily to streamline the full-state Q feedback design into a practical implementable output feedback controller structure. To achieve robustness to control actuator failure, the redundant surfaces are properly balanced according to their control effectiveness. A simple gain schedule based on the landing gear up/down logic involving only three gains was developed to handle three design flight conditions: Mach .25 and Mach .60 at 5000 ft and Mach .90 at 20,000 ft. The fault tolerant control law developed in this study provides good stability augmentation and performance for the relaxed static stability aircraft. The augmented aircraft responses are found to be invariant to the presence of a failure. Furthermore, single-loop stability margins of +6 dB in gain and +30 deg in phase were achieved along with -40 dB/decade rolloff at high frequency.

Synthesis of monolithic graphene – graphite integrated electronics

PubMed Central

Park, Jang-Ung; Nam, SungWoo; Lee, Mi-Sun; Lieber, Charles M.

2013-01-01

Encoding electronic functionality into nanoscale elements during chemical synthesis has been extensively explored over the past decade as the key to developing integrated nanosystems1 with functions defined by synthesis2-6. Graphene7-12 has been recently explored as a two-dimensional nanoscale material, and has demonstrated simple device functions based on conventional top-down fabrication13-20. However, the synthetic approach to encoding electronic functionality and thus enabling an entire integrated graphene electronics in a chemical synthesis had not previously been demonstrated. Here we report an unconventional approach for the synthesis of monolithically-integrated electronic devices based on graphene and graphite. Spatial patterning of heterogeneous catalyst metals permits the selective growth of graphene and graphite, with controlled number of graphene layers. Graphene transistor arrays with graphitic electrodes and interconnects were formed from synthesis. These functional, all-carbon structures were transferrable onto a variety of substrates. The integrated transistor arrays were used to demonstrate real-time, multiplexed chemical sensing, and more significantly, multiple carbon layers of the graphene-graphite device components were vertically assembled to form a three-dimensional flexible structure which served as a top-gate transistor array. These results represent a substantial progress towards encoding electronic functionality via chemical synthesis and suggest future promise for one-step integration of graphene-graphite based electronics. PMID:22101813

Synthesis of monolithic graphene-graphite integrated electronics.

PubMed

Park, Jang-Ung; Nam, SungWoo; Lee, Mi-Sun; Lieber, Charles M

2011-11-20

Encoding electronic functionality into nanoscale elements during chemical synthesis has been extensively explored over the past decade as the key to developing integrated nanosystems with functions defined by synthesis. Graphene has been recently explored as a two-dimensional nanoscale material, and has demonstrated simple device functions based on conventional top-down fabrication. However, the synthetic approach to encoding electronic functionality and thus enabling an entire integrated graphene electronics in a chemical synthesis had not previously been demonstrated. Here we report an unconventional approach for the synthesis of monolithically integrated electronic devices based on graphene and graphite. Spatial patterning of heterogeneous metal catalysts permits the selective growth of graphene and graphite, with a controlled number of graphene layers. Graphene transistor arrays with graphitic electrodes and interconnects were formed from the synthesis. These functional, all-carbon structures were transferable onto a variety of substrates. The integrated transistor arrays were used to demonstrate real-time, multiplexed chemical sensing and more significantly, multiple carbon layers of the graphene-graphite device components were vertically assembled to form a three-dimensional flexible structure which served as a top-gate transistor array. These results represent substantial progress towards encoding electronic functionality through chemical synthesis and suggest the future promise of one-step integration of graphene-graphite based electronics.

DNA synthesis inhibitors for the treatment of gastrointestinal cancer.

PubMed

Yasui, Hiroshi; Tsurita, Giichiro; Imai, Kohzoh

2014-11-01

Intensive laboratory, preclinical and clinical studies have identified and validated molecular targets in cancers, leading to a shift toward the development of novel, rationally designed and specific therapeutic agents. However, gastrointestinal cancers continue to have a poor prognosis, largely due to drug resistance. Here, we discuss the current understanding of DNA synthesis inhibitors and their mechanisms of action for the treatment of gastrointestinal malignancies. Conventional agents, including DNA synthesis inhibitors such as fluoropyrimidines and platinum analogs, remain the most effective therapeutics and are the standards against which new drugs are compared. Novel DNA synthesis inhibitors for the treatment of gastrointestinal malignancies include a combination of the antimetabolite TAS-102, which consists of trifluorothymidine with a thymidine phosphorylase inhibitor, and a novel micellar formulation of cisplatin NC-6004 that uses a nanotechnology-based drug delivery system. The challenges of translational cancer research using DNA synthesis inhibitors include the identification of drugs that are specific to tumor cells to reduce toxicity and increase antitumor efficacy, biomarkers to predict pharmacological responses to chemotherapeutic drugs, identification of ways to overcome drug resistance and development of novel combination therapies with DNA synthesis inhibitors and other cancer therapies, such as targeted molecular therapeutics. Here, we discuss the current understanding of DNA synthesis inhibitors and their mechanisms of action for the treatment of gastrointestinal malignancies.

Conversion of agricultural residues to carboxymethylcellulose and carboxymethylcellulose acetate

USDA-ARS?s Scientific Manuscript database

In view of continuing interest in the use of agricultural by-products, we have converted cellulose, wheat straw, barley straw, and rice hull into carboxymethylcellulose (CMC). Microwave-assisted synthesis was found to be a partly effective alternative to the conventional heating process. The CMC thu...

Novel polyurethanes from xylan and TDI: Preparation and characterization

USDA-ARS?s Scientific Manuscript database

In this work a novel polyurethane was developed involving xylan and tolylene-2,4-diisocyanate (TDI). Polymer synthesis was achieved via conventional heat or microwave-assisted reaction in dimethylsulfoxide. Because xylan has multiple OH groups on each polymer chain, the TDI/xylan molar ratio neede...

Highly parallel single-molecule amplification approach based on agarose droplet polymerase chain reaction for efficient and cost-effective aptamer selection.

PubMed

Zhang, Wei Yun; Zhang, Wenhua; Liu, Zhiyuan; Li, Cong; Zhu, Zhi; Yang, Chaoyong James

2012-01-03

We have developed a novel method for efficiently screening affinity ligands (aptamers) from a complex single-stranded DNA (ssDNA) library by employing single-molecule emulsion polymerase chain reaction (PCR) based on the agarose droplet microfluidic technology. In a typical systematic evolution of ligands by exponential enrichment (SELEX) process, the enriched library is sequenced first, and tens to hundreds of aptamer candidates are analyzed via a bioinformatic approach. Possible candidates are then chemically synthesized, and their binding affinities are measured individually. Such a process is time-consuming, labor-intensive, inefficient, and expensive. To address these problems, we have developed a highly efficient single-molecule approach for aptamer screening using our agarose droplet microfluidic technology. Statistically diluted ssDNA of the pre-enriched library evolved through conventional SELEX against cancer biomarker Shp2 protein was encapsulated into individual uniform agarose droplets for droplet PCR to generate clonal agarose beads. The binding capacity of amplified ssDNA from each clonal bead was then screened via high-throughput fluorescence cytometry. DNA clones with high binding capacity and low K(d) were chosen as the aptamer and can be directly used for downstream biomedical applications. We have identified an ssDNA aptamer that selectively recognizes Shp2 with a K(d) of 24.9 nM. Compared to a conventional sequencing-chemical synthesis-screening work flow, our approach avoids large-scale DNA sequencing and expensive, time-consuming DNA synthesis of large populations of DNA candidates. The agarose droplet microfluidic approach is thus highly efficient and cost-effective for molecular evolution approaches and will find wide application in molecular evolution technologies, including mRNA display, phage display, and so on. © 2011 American Chemical Society

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

Stair, Peter C.

The research took advantage of our capabilities to perform in-situ and operando Raman spectroscopy on complex systems along with our developing expertise in the synthesis of uniform, supported metal oxide materials to investigate relationships between the catalytically active oxide composition, atomic structure, and support and the corresponding chemical and catalytic properties. The project was organized into two efforts: 1) Synthesis of novel catalyst materials by atomic layer deposition (ALD). 2) Spectroscopic and chemical investigations of coke formation and catalyst deactivation. ALD synthesis was combined with conventional physical characterization, Raman spectroscopy, and probe molecule chemisorption to study the effect of supportedmore » metal oxide composition and atomic structure on acid-base and catalytic properties. Operando Raman spectroscopy studies of olefin polymerization leading to coke formation and catalyst deactivation clarified the mechanism of coke formation by acid catalysts.« less

A comparative study of three different synthesis routes for hydrophilic fluorophore-doped silica nanoparticles

NASA Astrophysics Data System (ADS)

Shahabi, Shakiba; Treccani, Laura; Rezwan, Kurosch

2016-01-01

The synthesis of fluorophore-doped silica nanoparticles (FDS NPs) with two conventional approaches, Stöber and microemulsion, as well as a novel amino acid-catalyzed seeds regrowth technique (ACSRT) is presented. The efficiency of each applied synthesis route toward incorporation of selected hydrophilic fluorophores, including rhodamine B isothiocyanate and fluorescein isothiocyanate, without and with an amine-containing crosslinker, into silica matrix was systematically studied. Our results clearly highlight the advantages of ACSRT to obtain FDS NPs with a remarkable encapsulation efficiency, high quantum yield, and enhanced stability against bleaching and dye leaking due to efficient embedding of the dyes inside silica network even without the amine-containing silane reagent. Moreover, evaluation of photostability of FDNPs internalized in human bone cells demonstrates the merits of ACSRT.

Fast conventional Fmoc solid-phase peptide synthesis with HCTU.

PubMed

Hood, Christina A; Fuentes, German; Patel, Hirendra; Page, Karen; Menakuru, Mahendra; Park, Jae H

2008-01-01

1H-Benzotriazolium 1-[bis(dimethyl-amino)methylene]-5-chloro-hexafluorophosphate (1-),3-oxide (HCTU) is a nontoxic, nonirritating and noncorrosive coupling reagent. Seven biologically active peptides (GHRP-6, (65-74)ACP, oxytocin, G-LHRH, C-peptide, hAmylin(1-37), and beta-amyloid(1-42)) were synthesized with reaction times reduced to deprotection times of 3 min or less and coupling times of 5 min or less using HCTU as the coupling reagent. Expensive coupling reagents or special techniques were not used. Total peptide synthesis times were dramatically reduced by as much as 42.5 h (1.8 days) without reducing the crude peptide purities. It was shown that HCTU can be used as an affordable, efficient coupling reagent for fast Fmoc solid-phase peptide synthesis.

Use of aluminum phosphate as the dehydration catalyst in single step dimethyl ether process

DOEpatents

Peng, Xiang-Dong; Parris, Gene E.; Toseland, Bernard A.; Battavio, Paula J.

1998-01-01

The present invention pertains to a process for the coproduction of methanol and dimethyl ether (DME) directly from a synthesis gas in a single step (hereafter, the "single step DME process"). In this process, the synthesis gas comprising hydrogen and carbon oxides is contacted with a dual catalyst system comprising a physical mixture of a methanol synthesis catalyst and a methanol dehydration catalyst. The present invention is an improvement to this process for providing an active and stable catalyst system. The improvement comprises the use of an aluminum phosphate based catalyst as the methanol dehydration catalyst. Due to its moderate acidity, such a catalyst avoids the coke formation and catalyst interaction problems associated with the conventional dual catalyst systems taught for the single step DME process.

Access to small size distributions of nanoparticles by microwave-assisted synthesis. Formation of Ag nanoparticles in aqueous carboxymethylcellulose solutions in batch and continuous-flow reactors

NASA Astrophysics Data System (ADS)

Horikoshi, Satoshi; Abe, Hideki; Torigoe, Kanjiro; Abe, Masahiko; Serpone, Nick

2010-08-01

This article examines the effect(s) of the 2.45-GHz microwave (MW) radiation in the synthesis of silver nanoparticles in aqueous media by reduction of the diaminesilver(i) complex, [Ag(NH3)2]+, with carboxymethylcellulose (CMC) in both batch-type and continuous-flow reactor systems with a particular emphasis on the characteristics of the microwaves in this process and the size distributions. This microwave thermally-assisted synthesis is compared to a conventional heating (CH) method, both requiring a reaction temperature of 100 °C to produce the nanoparticles, in both cases leading to the formation of silver colloids with different size distributions. Reduction of the diaminesilver(i) precursor complex, [Ag(NH3)2]+, by CMC depended on the solution temperature. Cooling the reactor during the heating process driven with 390-Watt microwaves (MW-390W/Cool protocol) yielded silver nanoparticles with sizes spanning the range 1-2 nm. By contrast, the size distribution of Ag nanoparticles with 170-Watt microwaves (no cooling; MW-170W protocol) was in the range 1.4-3.6 nm (average size ~3 nm). The overall results suggest the potential for a scale-up process in the microwave-assisted synthesis of nanoparticles. Based on the present data, a flow-through microwave reactor system is herein proposed for the continuous production of silver nanoparticles. The novel flow reactor system (flow rate, 600 mL min-1) coupled to 1200-Watt microwave radiation generated silver nanoparticles with a size distribution 0.7-2.8 nm (average size ca. 1.5 nm).

Synthesis-identification integration: One-pot hydrothermal preparation of fluorescent nitrogen-doped carbon nanodots for differentiating nucleobases with the aid of multivariate chemometrics analysis.

PubMed

Zhuang, Qianfen; Cao, Wei; Ni, Yongnian; Wang, Yong

2018-08-01

Most of the conventional multidimensional differential sensors currently need at least two-step fabrication, namely synthesis of probe(s) and identification of multiple analytes by mixing of analytes with probe(s), and were conducted using multiple sensing elements or several devices. In the study, we chose five different nucleobases (adenine, cytosine, guanine, thymine, and uracil) as model analytes, and found that under hydrothermal conditions, sodium citrate could react directly with various nucleobases to yield different nitrogen-doped carbon nanodots (CDs). The CDs synthesized from different nucleobases exhibited different fluorescent properties, leading to their respective characteristic fluorescence spectra. Hence, we combined the fluorescence spectra of the CDs with advanced chemometrics like principle component analysis (PCA), hierarchical cluster analysis (HCA), K-nearest neighbor (KNN) and soft independent modeling of class analogy (SIMCA), to present a conceptually novel "synthesis-identification integration" strategy to construct a multidimensional differential sensor for nucleobase discrimination. Single-wavelength excitation fluorescence spectral data, single-wavelength emission fluorescence spectral data, and fluorescence Excitation-Emission Matrices (EEMs) of the CDs were respectively used as input data of the differential sensor. The results showed that the discrimination ability of the multidimensional differential sensor with EEM data set as input data was superior to those with single-wavelength excitation/emission fluorescence data set, suggesting that increasing the number of the data input could improve the discrimination power. Two supervised pattern recognition methods, namely KNN and SIMCA, correctly identified the five nucleobases with a classification accuracy of 100%. The proposed "synthesis-identification integration" strategy together with a multidimensional array of experimental data holds great promise in the construction of differential sensors. Copyright © 2018 Elsevier B.V. All rights reserved.

Development of a large peptoid-DOTA combinatorial library.

PubMed

Singh, Jaspal; Lopes, Daniel; Gomika Udugamasooriya, D

2016-09-01

Conventional one-bead one-compound (OBOC) library synthesis is typically used to identify molecules with therapeutic value. The design and synthesis of OBOC libraries that contain molecules with imaging or even potentially therapeutic and diagnostic capacities (e.g. theranostic agents) has been overlooked. The development of a therapeutically active molecule with a built-in imaging component for a certain target is a daunting task, and structure-based rational design might not be the best approach. We hypothesize to develop a combinatorial library with potentially therapeutic and imaging components fused together in each molecule. Such molecules in the library can be used to screen, identify, and validate as direct theranostic candidates against targets of interest. As the first step in achieving that aim, we developed an on-bead library of 153,600 Peptoid-DOTA compounds in which the peptoids are the target-recognizing and potentially therapeutic components and the DOTA is the imaging component. We attached the DOTA scaffold to TentaGel beads using one of the four arms of DOTA, and we built a diversified 6-mer peptoid library on the remaining three arms. We evaluated both the synthesis and the mass spectrometric sequencing capacities of the test compounds and of the final library. The compounds displayed unique ionization patterns including direct breakages of the DOTA scaffold into two units, allowing clear decoding of the sequences. Our approach provides a facile synthesis method for the complete on-bead development of large peptidomimetic-DOTA libraries for screening against biological targets for the identification of potential theranostic agents in the future. © 2016 The Authors. Biopolymers Published by Wiley Periodicals, Inc. Biopolymers (Pept Sci) 106: 673-684, 2016. © 2016 The Authors. Biopolymers Published by Wiley Periodicals, Inc.

Facile green synthesis of silver nanoparticles using seed aqueous extract of Pistacia atlantica and its antibacterial activity

NASA Astrophysics Data System (ADS)

Sadeghi, Babak; Rostami, Amir; Momeni, S. S.

2015-01-01

In the present work, we describe the synthesis of silver nanoparticles (Ag-NPs) using seed aqueous extract of Pistacia atlantica (PA) and its antibacterial activity. UV-visible spectroscopy, X-ray diffraction (XRD), Fourier transform infra red spectroscopy (FTIR), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and X-ray energy dispersive spectrophotometer (EDAX) were performed to ascertain the formation of Ag-NPs. It was observed that the growths of Ag-NPs are stopped within 35 min of reaction time. The synthesized Ag-NPs were characterized by a peak at 446 nm in the UV-visible spectrum. XRD confirmed the crystalline nature of the nanoparticles of 27 nm size. The XRD peaks at 38°, 44°, 64° and 77° can be indexed to the (1 1 1), (2 0 0), (2 2 0) and (3 1 1) Bragg's reflections of cubic structure of metallic silver, respectively. The FTIR result clearly showed that the extracts containing OH as a functional group act in capping the nanoparticles synthesis. Antibacterial activities of Ag-NPs were tested against the growth of Gram-positive (S. aureus) using SEM. The inhibition was observed in the Ag-NPs against S. aureus. The results suggest that the synthesized Ag-NPs act as an effective antibacterial agent. It is confirmed that Ag-NPs are capable of rendering high antibacterial efficacy and hence has a great potential in the preparation of used drugs against bacterial diseases. The scanning electron microscopy (SEM), indicated that, the most strains of S. aureus was damaged and extensively disappeared by addition of Ag-NPs. The results confirmed that the (PA) is a very good eco friendly and nontoxic source for the synthesis of Ag-NPs as compared to the conventional chemical/physical methods.

Facile green synthesis of silver nanoparticles using seed aqueous extract of Pistacia atlantica and its antibacterial activity.

PubMed

Sadeghi, Babak; Rostami, Amir; Momeni, S S

2015-01-05

In the present work, we describe the synthesis of silver nanoparticles (Ag-NPs) using seed aqueous extract of Pistacia atlantica (PA) and its antibacterial activity. UV-visible spectroscopy, X-ray diffraction (XRD), Fourier transform infra red spectroscopy (FTIR), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and X-ray energy dispersive spectrophotometer (EDAX) were performed to ascertain the formation of Ag-NPs. It was observed that the growths of Ag-NPs are stopped within 35 min of reaction time. The synthesized Ag-NPs were characterized by a peak at 446 nm in the UV-visible spectrum. XRD confirmed the crystalline nature of the nanoparticles of 27 nm size. The XRD peaks at 38°, 44°, 64° and 77° can be indexed to the (111), (200), (220) and (311) Bragg's reflections of cubic structure of metallic silver, respectively. The FTIR result clearly showed that the extracts containing OH as a functional group act in capping the nanoparticles synthesis. Antibacterial activities of Ag-NPs were tested against the growth of Gram-positive (S. aureus) using SEM. The inhibition was observed in the Ag-NPs against S. aureus. The results suggest that the synthesized Ag-NPs act as an effective antibacterial agent. It is confirmed that Ag-NPs are capable of rendering high antibacterial efficacy and hence has a great potential in the preparation of used drugs against bacterial diseases. The scanning electron microscopy (SEM), indicated that, the most strains of S. aureus was damaged and extensively disappeared by addition of Ag-NPs. The results confirmed that the (PA) is a very good eco friendly and nontoxic source for the synthesis of Ag-NPs as compared to the conventional chemical/physical methods. Copyright © 2014 Elsevier B.V. All rights reserved.

Protocol for the Synthesis of Ortho-trifluoromethoxylated Aniline Derivatives

PubMed Central

Feng, Pengju; Ngai, Ming-Yu

2016-01-01

Molecules bearing trifluoromethoxy (OCF3) group often show desired pharmacological and biological properties. However, facile synthesis of trifluoromethoxylated aromatic compounds remains a formidable challenge in organic synthesis. Conventional approaches often suffer from poor substrate scope, or require use of highly toxic, difficult-to-handle, and/or thermally labile reagents. Herein, we report a user-friendly protocol for the synthesis of methyl 4-acetamido-3-(trifluoromethoxy)benzoate using 1-trifluoromethyl-1,2-benziodoxol-3(1H)-one (Togni reagent II). Treating methyl 4-(N-hydroxyacetamido)benzoate (1a) with Togni reagent II in the presence of a catalytic amount of cesium carbonate (Cs2CO3) in chloroform at RT afforded methyl 4-(N-(trifluoromethoxy)acetamido)benzoate (2a). This intermediate was then converted to the final product methyl 4-acetamido-3-(trifluoromethoxy)benzoate (3a) in nitromethane at 120 °C. This procedure is general and can be applied to the synthesis of a broad spectrum of ortho-trifluoromethoxylated aniline derivatives, which could serve as useful synthetic building blocks for the discovery and development of new pharmaceuticals, agrochemicals, and functional materials. PMID:26862864

Carbon nanopipettes and microtubes for electrochemical sensing and microfluidics

NASA Astrophysics Data System (ADS)

Mani, Radhika C.; Bhimarasetti, Gopinath; Lowe, Randall; Sunkara, Mahendra K.

2004-12-01

We present the synthesis of two novel morphologies for carbon tubular structures: Nanopipettes and Micropipes. The synthesis procedures for both these structures are both unique and different from each other and the conventional methods used for carbon nanotubes. Carbon nanopipettes, open at both ends, are made up of a central nanotube (~10-20 nm) surrounded by helical sheets of graphite. Thus nanopipettes have an outer conical structure, with a base size of about a micron, that narrows down to about 10-20 nm at the tip. Due to their unique morphology, the outer walls of the nanopipettes continuously expose edge planes of graphite, giving a very stable and reversible electrochemical response for detecting neurological compounds such as dopamine. The synthesis of carbon nanopipettes is based on high temperature nucleation and growth of carbon nanotubes under conditions of hydrogen etching during growth. Carbon micropipes, on the other hand, are tubular structures whose internal diameters range from a few nanometers to a few microns with a constant wall thickness of 10-20 nm. In addition to tuning the internal diameters, the conical angles of these structures could also be changed during synthesis. Due to their larger inner diameters and thin walls, both the straight and conical micro-tubular structures are suitable for microfluidic devices such as throttle valves, micro-reactors, and distribution channels. The synthesis of carbon micro-tubular structures is based on the wetting behavior of gallium with carbon during growth. The contact angle between gallium and the carbon wall determines the conical angle of the structure. By varying the contact angle, one can alter the conical angles from 400 to -150, and synthesize straight tubes using different N2/O2 dosing compositions. An 'n-step' dosing sequence at various stages of growth resulted in 'n-staged' morphologies for carbon micro-tubular structures such as funnels, tube-on-cone, Y-junctions and dumbbells.

Digital Sound Synthesis Algorithms: a Tutorial Introduction and Comparison of Methods

NASA Astrophysics Data System (ADS)

Lee, J. Robert

The objectives of the dissertation are to provide both a compendium of sound-synthesis methods with detailed descriptions and sound examples, as well as a comparison of the relative merits of each method based on ease of use, observed sound quality, execution time, and data storage requirements. The methods are classified under the general headings of wavetable-lookup synthesis, additive synthesis, subtractive synthesis, nonlinear methods, and physical modelling. The nonlinear methods comprise a large group that ranges from the well-known frequency-modulation synthesis to waveshaping. The final category explores computer modelling of real musical instruments and includes numerical and analytical solutions to the classical wave equation of motion, along with some of the more sophisticated time -domain models that are possible through the prudent combination of simpler synthesis techniques. The dissertation is intended to be understandable by a musician who is mathematically literate but who does not necessarily have a background in digital signal processing. With this limitation in mind, a brief and somewhat intuitive description of digital sampling theory is provided in the introduction. Other topics such as filter theory are discussed as the need arises. By employing each of the synthesis methods to produce the same type of sound, interesting comparisons can be made. For example, a struck string sound, such as that typical of a piano, can be produced by algorithms in each of the synthesis classifications. Many sounds, however, are peculiar to a single algorithm and must be examined independently. Psychoacoustic studies were conducted as an aid in the comparison of the sound quality of several implementations of the synthesis algorithms. Other psychoacoustic experiments were conducted to supplement the established notions of which timbral issues are important in the re -synthesis of the sounds of acoustic musical instruments.

Multifunctional Nanomaterials: Design, Synthesis and Application Properties.

PubMed

Martinelli, Marisa; Strumia, Miriam Cristina

2017-02-07

The immense scope of variation in dendritic molecules (hyper-branching, nano-sized, hydrophobicity/hydrophilicity, rigidity/flexibility balance, etc.) and their versatile functionalization, with the possibility of multivalent binding, permit the design of highly improved, novel materials. Dendritic-based materials are therefore viable alternatives to conventional polymers. The overall aim of this work is to show the advantages of dendronization processes by presenting the synthesis and characterization of three different dendronized systems: (I) microbeads of functionalized chitosan; (II) nanostructuration of polypropylene surfaces; and (III) smart dendritic nanogels. The particular properties yielded by these systems could only be achieved thanks to the dendronization process.

Mini-implants for orthodontic anchorage.

PubMed

Reynders, Reint Meursinge; Ladu, Luisa

2017-10-27

Data sourcesPubmed, Embase, Cochrane Central Register of Controlled Trials and the Web of Science databases. Hand searches of the journals European Journal of Orthodontics, Journal of Orthodontics, Journal of Clinical Orthodontics, Seminars in Orthodontics, American Journal of Orthodontics & Dentofacial Orthopaedics and Angle Orthodontist.Study selectionTwo reviewers independently selected studies. Randomised controlled trials (RCTs) and controlled clinical trials (CCTs) of orthodontic patients requiring extraction of the maxillary first premolars and closure of the spaces without anchorage loss were considered.Data extraction and synthesisData extraction and risk of bias assessment were carried out independently by two reviewers. Meta-analysis and sensitivity analysis were conducted.ResultsFourteen studies; seven RCTS and seven CCTs were included. In total 303 patients received TISADs with 313 control patients. Overall the quality of the studies was considered to be moderate. Overall the TISAD group had significantly less anchorage loss than the control group. On average, TISADs enabled 1.86mm more anchorage preservation than did conventional methods.ConclusionsThe results of the meta-analysis showed that TISADs are more effective than conventional methods of anchorage reinforcement. The average difference of 2mm seems not only statistically but also clinically significant. However, the results should be interpreted with caution because of the moderate quality of the included studies. More high-quality studies on this issue are necessary to enable drawing more reliable conclusions.

Facile and green synthesis of fluorescent carbon dots with tunable emission for sensors and cells imaging.

PubMed

Diao, Haipeng; Li, Tingting; Zhang, Rong; Kang, Yu; Liu, Wen; Cui, Yanhua; Wei, Shuangyan; Wang, Ning; Li, Lihong; Wang, Haojiang; Niu, Weifen; Sun, Tijian

2018-07-05

Most carbon dots (CDs) conventional fabrication approaches produce single colored fluorescent materials, different methods are required to synthesize distinct carbon dots for specific optical applications. Herein, using one-pot hydrothermal treatment of Syringa obtata Lindl, a facile, low-cost and green assay is achieved in the controllable synthesis of blue and green fluorescent carbon dots. The fluorescent emission of CDs can be well-tuned by adding sodium hydroxide in the precursor solution. Blue fluorescent CDs are applied to Fe 3+ sensing with a low detection limit of 0.11 μM of linear range from 0.5 to 80 μM, and then further extended to analysis river water samples. Green fluorescent CDs can be applied to pH detection, which show a remarkable linear enhancement in the green fluorescence emission region when the pH is increased from 1.98 to 8.95. Eventually, the detection of Fe 3+ and pH are applied for the living cells fluorescent images in MCF-7 cells are achieved successfully, indicating as-synthesized CDs potential toward diverse application as promising candidate. Copyright © 2018 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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.

Nanofluid Types, Their Synthesis, Properties and Incorporation in Direct Solar Thermal Collectors: A Review

PubMed Central

Chamsa-ard, Wisut; Brundavanam, Sridevi; Fung, Chun Che; Fawcett, Derek; Poinern, Gerrard

2017-01-01

The global demand for energy is increasing and the detrimental consequences of rising greenhouse gas emissions, global warming and environmental degradation present major challenges. Solar energy offers a clean and viable renewable energy source with the potential to alleviate the detrimental consequences normally associated with fossil fuel-based energy generation. However, there are two inherent problems associated with conventional solar thermal energy conversion systems. The first involves low thermal conductivity values of heat transfer fluids, and the second involves the poor optical properties of many absorbers and their coating. Hence, there is an imperative need to improve both thermal and optical properties of current solar conversion systems. Direct solar thermal absorption collectors incorporating a nanofluid offers the opportunity to achieve significant improvements in both optical and thermal performance. Since nanofluids offer much greater heat absorbing and heat transfer properties compared to traditional working fluids. The review summarizes current research in this innovative field. It discusses direct solar absorber collectors and methods for improving their performance. This is followed by a discussion of the various types of nanofluids available and the synthesis techniques used to manufacture them. In closing, a brief discussion of nanofluid property modelling is also presented. PMID:28561802

Vibrato in Singing Voice: The Link between Source-Filter and Sinusoidal Models

NASA Astrophysics Data System (ADS)

Arroabarren, Ixone; Carlosena, Alfonso

2004-12-01

The application of inverse filtering techniques for high-quality singing voice analysis/synthesis is discussed. In the context of source-filter models, inverse filtering provides a noninvasive method to extract the voice source, and thus to study voice quality. Although this approach is widely used in speech synthesis, this is not the case in singing voice. Several studies have proved that inverse filtering techniques fail in the case of singing voice, the reasons being unclear. In order to shed light on this problem, we will consider here an additional feature of singing voice, not present in speech: the vibrato. Vibrato has been traditionally studied by sinusoidal modeling. As an alternative, we will introduce here a novel noninteractive source filter model that incorporates the mechanisms of vibrato generation. This model will also allow the comparison of the results produced by inverse filtering techniques and by sinusoidal modeling, as they apply to singing voice and not to speech. In this way, the limitations of these conventional techniques, described in previous literature, will be explained. Both synthetic signals and singer recordings are used to validate and compare the techniques presented in the paper.

Mechanical instability driven self-assembly and architecturing of 2D materials

NASA Astrophysics Data System (ADS)

Cai Wang, Michael; Leem, Juyoung; Kang, Pilgyu; Choi, Jonghyun; Knapp, Peter; Yong, Keong; Nam, SungWoo

2017-06-01

Two-dimensional (2D) materials have been well studied for their diverse and impressive properties and superlative mechanical strength. Their atomic thinness and weak van der Waals interaction, while fascinating and unique, dictate their tendency to exhibit out of plane morphologies such as bending, buckling, folding, rippling, scrolling, and wrinkling, etc. In this review, we discuss the mechanisms behind these instability driven morphologies and the resultant phenomena that arise. We then survey methods to manipulate them especially in a scalable manner, and elucidate some interesting applications uniquely enabled by these structures. Contrary to conventional wisdom, the deterministic control of these features has great implications for the local and overall material properties due to heterogeneous distribution of stresses and strains. The introduction of deformable and shape memory substrates especially allow for facile and large scale synthesis of various types of out of plane morphologies. We show that a variety of exciting phenomena and applications arise, including tunable surfaces and coatings, robust devices and electronics, adaptive optoelectronics, material toughening, energy storage, and chemical sensing. This new perspective on these otherwise nuisance thin-film phenomena enable new tools for future materials discovery, design, and synthesis with the ever growing library of 2D atomically thin materials.

Nanofluid Types, Their Synthesis, Properties and Incorporation in Direct Solar Thermal Collectors: A Review.

PubMed

Chamsa-Ard, Wisut; Brundavanam, Sridevi; Fung, Chun Che; Fawcett, Derek; Poinern, Gerrard

2017-05-31

The global demand for energy is increasing and the detrimental consequences of rising greenhouse gas emissions, global warming and environmental degradation present major challenges. Solar energy offers a clean and viable renewable energy source with the potential to alleviate the detrimental consequences normally associated with fossil fuel-based energy generation. However, there are two inherent problems associated with conventional solar thermal energy conversion systems. The first involves low thermal conductivity values of heat transfer fluids, and the second involves the poor optical properties of many absorbers and their coating. Hence, there is an imperative need to improve both thermal and optical properties of current solar conversion systems. Direct solar thermal absorption collectors incorporating a nanofluid offers the opportunity to achieve significant improvements in both optical and thermal performance. Since nanofluids offer much greater heat absorbing and heat transfer properties compared to traditional working fluids. The review summarizes current research in this innovative field. It discusses direct solar absorber collectors and methods for improving their performance. This is followed by a discussion of the various types of nanofluids available and the synthesis techniques used to manufacture them. In closing, a brief discussion of nanofluid property modelling is also presented.

Cross contrast multi-channel image registration using image synthesis for MR brain images.

PubMed

Chen, Min; Carass, Aaron; Jog, Amod; Lee, Junghoon; Roy, Snehashis; Prince, Jerry L

2017-02-01

Multi-modal deformable registration is important for many medical image analysis tasks such as atlas alignment, image fusion, and distortion correction. Whereas a conventional method would register images with different modalities using modality independent features or information theoretic metrics such as mutual information, this paper presents a new framework that addresses the problem using a two-channel registration algorithm capable of using mono-modal similarity measures such as sum of squared differences or cross-correlation. To make it possible to use these same-modality measures, image synthesis is used to create proxy images for the opposite modality as well as intensity-normalized images from each of the two available images. The new deformable registration framework was evaluated by performing intra-subject deformation recovery, intra-subject boundary alignment, and inter-subject label transfer experiments using multi-contrast magnetic resonance brain imaging data. Three different multi-channel registration algorithms were evaluated, revealing that the framework is robust to the multi-channel deformable registration algorithm that is used. With a single exception, all results demonstrated improvements when compared against single channel registrations using the same algorithm with mutual information. Copyright © 2016 Elsevier B.V. All rights reserved.

Articulatory speech synthesis and speech production modelling

NASA Astrophysics Data System (ADS)

Huang, Jun

This dissertation addresses the problem of speech synthesis and speech production modelling based on the fundamental principles of human speech production. Unlike the conventional source-filter model, which assumes the independence of the excitation and the acoustic filter, we treat the entire vocal apparatus as one system consisting of a fluid dynamic aspect and a mechanical part. We model the vocal tract by a three-dimensional moving geometry. We also model the sound propagation inside the vocal apparatus as a three-dimensional nonplane-wave propagation inside a viscous fluid described by Navier-Stokes equations. In our work, we first propose a combined minimum energy and minimum jerk criterion to estimate the dynamic vocal tract movements during speech production. Both theoretical error bound analysis and experimental results show that this method can achieve very close match at the target points and avoid the abrupt change in articulatory trajectory at the same time. Second, a mechanical vocal fold model is used to compute the excitation signal of the vocal tract. The advantage of this model is that it is closely coupled with the vocal tract system based on fundamental aerodynamics. As a result, we can obtain an excitation signal with much more detail than the conventional parametric vocal fold excitation model. Furthermore, strong evidence of source-tract interaction is observed. Finally, we propose a computational model of the fricative and stop types of sounds based on the physical principles of speech production. The advantage of this model is that it uses an exogenous process to model the additional nonsteady and nonlinear effects due to the flow mode, which are ignored by the conventional source- filter speech production model. A recursive algorithm is used to estimate the model parameters. Experimental results show that this model is able to synthesize good quality fricative and stop types of sounds. Based on our dissertation work, we carefully argue that the articulatory speech production model has the potential to flexibly synthesize natural-quality speech sounds and to provide a compact computational model for speech production that can be beneficial to a wide range of areas in speech signal processing.

Nitrogen-doped graphene catalysts: High energy wet ball milling synthesis and characterizations of functional groups and particle size variation with time and speed

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

Zhuang, Shiqiang; Nunna, Bharath Babu; Boscoboinik, Jorge Anibal

Nitrogen-doped graphene (N-G) catalyst emerges as one of the promising non-platinum group metal (non-PGM) catalysts with the advantages of low cost, high oxygen reduction reaction (ORR) activity, stability, and selectivity to replace expensive PGM catalysts in electrochemical systems. This research investigated nanoscale high energy wet (NHEW) ball milling for the synthesis of N-G catalysts to make conventional problems such as sintering or localized overheating issues negligible. The successful synthesis of N-G catalysts with comparable catalytic performance to 10 wt% Pt/C by using this method has been published. This paper focuses on understanding the effect of grinding speed and grinding timemore » on the particle size and chemical state of N-G catalysts through the physical and chemical characterization. The research result shows that (1) the final particle size, nitrogen doping percentage, and nitrogen bonding composition of synthesized N-G catalysts are predictable and controllable by adjusting the grinding time, the grinding speed, and other relative experimental parameters; (2) the final particle size of N-G catalysts could be estimated from the derived relation between the cracking energy density and the particle size of ground material in the NHEW ball milling process with specified experimental parameters; and (3) the chemical composition of N-G catalysts synthesized by NHEW ball milling is controllable by adjusting the grinding time and grinding speed.« less

'Chocolate' silver nanoparticles: Synthesis, antibacterial activity and cytotoxicity.

PubMed

Chowdhury, Neelika Roy; MacGregor-Ramiasa, Melanie; Zilm, Peter; Majewski, Peter; Vasilev, Krasimir

2016-11-15

Silver nanoparticles (AgNPs) have emerged as a powerful weapon against antibiotic resistant microorganisms. However, most conventional AgNPs syntheses require the use of hazardous chemicals and generate toxic organic waste. Hence, in recent year's, plant derived and biomolecule based synthetics have has gained much attention. Cacao has been used for years for its medicinal benefits and contains a powerful reducing agent - oxalic acid. We hypothesized that, due to the presence of oxalic acid, cacao extract is capable of reducing silver nitrate (AgNO3) to produce AgNPs. In this study, AgNPs were synthesized by using natural cacao extract as a reducing and stabilizing agent. The reaction temperature, time and reactant molarity were varied to optimize the synthesis yield. UV-visible spectroscopy (UV-vis), dynamic light scattering (DLS) and transmission electron microscopy (TEM) characterization demonstrated that the synthesized AgNPs were spherical particles ranging in size from 35 to 42.5nm. The synthesized AgNPs showed significant antibacterial activity against clinically relevant pathogens such as Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus and Staphylococcus epidermidis. Importantly, these green AgNPs are not cytotoxic to human dermal fibroblasts (HDFs) at concentrations below 32μg/ml. We conclude that cacao-based synthesis is a reproducible and sustainable method for the generation of stable antimicrobial silver nanoparticles with low cytotoxicity to human cells. The AgNPs synthesized in this work have promising properties for applications in the biomedical field. Copyright © 2016 Elsevier Inc. All rights reserved.

The Microscale Synthesis and Electrochemistry of Low-Valent Mononuclear Complexes (h3-C3H5)Fe(CO)3 X (X = I, Br, Cl)

NASA Astrophysics Data System (ADS)

Mocellin, Enrico; Russell, Richard; Ravera, Mauro

1998-06-01

The experimental content of this paper will appeal to pedagogues and students who might be looking for new ideas that have an element of challenge. By combining experimental procedures which place microscale, chemical synthesis, and an inclusive, unified, product characterization in perspective, we have afforded the student the scope to obtain progressive, disciplined results and the opportunity to discuss these in the subsequent reporting. By this process, it is our experience that the students often identify with the practical work that is being undertaken, and they develop considerable empathy during their contribution to the "discovery" process that this laboratory program offers. The experimental work can be abbreviated to a single compound, subdivided into synthesis or electrochemistry, or extended to macroscale and other instrumental techniques of characterization, thus offering opportunities to accommodate time constraints, class results combination and discussion, and individual student enthusiasm. We believe that having to accept and/or constructively criticize sequential experimental results, collected by fellow students, mimics more realistically the practice of chemistry at the workplace and can build enthusiasm and elicit contagious fellowship from the class. All of these aspects can simply be achieved by utilizing the listed journals and references therein. Most importantly, it affords the students the opportunity to extricate themselves as innocent bystanders from the conventional "single experiment" practical laboratory to a path of practice and achievement in the scientific method.

Nitrogen-doped graphene catalysts: High energy wet ball milling synthesis and characterizations of functional groups and particle size variation with time and speed

DOE PAGES

Zhuang, Shiqiang; Nunna, Bharath Babu; Boscoboinik, Jorge Anibal; ...

2017-07-26

Nitrogen-doped graphene (N-G) catalyst emerges as one of the promising non-platinum group metal (non-PGM) catalysts with the advantages of low cost, high oxygen reduction reaction (ORR) activity, stability, and selectivity to replace expensive PGM catalysts in electrochemical systems. This research investigated nanoscale high energy wet (NHEW) ball milling for the synthesis of N-G catalysts to make conventional problems such as sintering or localized overheating issues negligible. The successful synthesis of N-G catalysts with comparable catalytic performance to 10 wt% Pt/C by using this method has been published. This paper focuses on understanding the effect of grinding speed and grinding timemore » on the particle size and chemical state of N-G catalysts through the physical and chemical characterization. The research result shows that (1) the final particle size, nitrogen doping percentage, and nitrogen bonding composition of synthesized N-G catalysts are predictable and controllable by adjusting the grinding time, the grinding speed, and other relative experimental parameters; (2) the final particle size of N-G catalysts could be estimated from the derived relation between the cracking energy density and the particle size of ground material in the NHEW ball milling process with specified experimental parameters; and (3) the chemical composition of N-G catalysts synthesized by NHEW ball milling is controllable by adjusting the grinding time and grinding speed.« less

Precursor-Directed Combinatorial Biosynthesis of Cinnamoyl, Dihydrocinnamoyl, and Benzoyl Anthranilates in Saccharomyces cerevisiae

DOE PAGES

Eudes, Aymerick; Teixeira Benites, Veronica; Wang, George; ...

2015-10-02

Biological synthesis of pharmaceuticals and biochemicals offers an environmentally friendly alternative to conventional chemical synthesis. These alternative methods require the design of metabolic pathways and the identification of enzymes exhibiting adequate activities. Cinnamoyl, dihydrocinnamoyl, and benzoyl anthranilates are natural metabolites which possess beneficial activities for human health, and the search is expanding for novel derivatives that might have enhanced biological activity. For example, biosynthesis in Dianthus caryophyllus is catalyzed by hydroxycinnamoyl/benzoyl-CoA:anthranilate N-hydroxycinnamoyl/ benzoyltransferase (HCBT), which couples hydroxycinnamoyl-CoAs and benzoyl-CoAs to anthranilate. We recently demonstrated the potential of using yeast (Saccharomyces cerevisiae) for the biological production of a few cinnamoyl anthranilatesmore » by heterologous co-expression of 4-coumaroyl:CoA ligase from Arabidopsis thaliana (4CL5) and HCBT. Here we report that, by exploiting the substrate flexibility of both 4CL5 and HCBT, we achieved rapid biosynthesis of more than 160 cinnamoyl, dihydrocinnamoyl, and benzoyl anthranilates in yeast upon feeding with both natural and non-natural cinnamates, dihydrocinnamates, benzoates, and anthranilates. Our results demonstrate the use of enzyme promiscuity in biological synthesis to achieve high chemical diversity within a defined class of molecules. Finally, this work also points to the potential for the combinatorial biosynthesis of diverse and valuable cinnamoylated, dihydrocinnamoylated, and benzoylated products by using the versatile biological enzyme 4CL5 along with characterized cinnamoyl-CoA- and benzoyl-CoA-utilizing transferases.« less

Eco-Efficient Synthesis of Highly Porous CoCO3 Anodes from Supercritical CO2 for Li+ and Na+ Storage.

PubMed

Li, Hui-Ying; Tseng, Chuan-Ming; Yang, Cheng-Hsien; Lee, Tai-Chou; Su, Ching-Yuan; Hsieh, Chien-Te; Chang, Jeng-Kuei

2017-06-09

An eco-efficient synthetic route for the preparation of high-performance carbonate anodes for Li + and Na + batteries is developed. With supercritical CO 2 (scCO 2 ) as the precursor, which has gas-like diffusivity, extremely low viscosity, and near-zero surface tension, CoCO 3 particles are uniformly formed and tightly connected on graphene nanosheets (GNSs). This synthesis can be conducted at 50 °C, which is considerably lower than the temperature required for conventional preparation methods, minimizing energy consumption. The obtained CoCO 3 particles (ca. 20 nm in diameter), which have a unique interpenetrating porous structure, can increase the number of electroactive sites, promote electrolyte accessibility, shorten ion diffusion length, and readily accommodate the strain generated upon charging/discharging. With a reversible capacity of 1105 mAh g -1 , the proposed CoCO 3 /GNS anode shows an excellent rate capability, as it can deliver 745 mAh g -1 in 7.5 min. More than 98 % of the initial capacity is retained after 200 cycles. These properties are clearly superior to those of previously reported CoCO 3 -based electrodes for Li + storage, indicating the merit of our scCO 2 -based synthesis, which is facile, green, and can be easily scaled up for mass production. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

A realist synthesis of the effect of social accountability interventions on health service providers' and policymakers' responsiveness.

PubMed

Lodenstein, Elsbet; Dieleman, Marjolein; Gerretsen, Barend; Broerse, Jacqueline Ew

2013-11-07

Accountability has center stage in the current post-Millennium Development Goals (MDG) debate. One of the effective strategies for building equitable health systems and providing quality health services is the strengthening of citizen-driven or social accountability processes. The monitoring of actions and decisions of policymakers and providers by citizens is regarded as a right in itself but also as an alternative to weak administrative accountability mechanisms, in particular in settings with poor governance. The effects of social accountability interventions are often based on assumptions and are difficult to evaluate because of their complex nature and context sensitivity. This study aims to review and assess the available evidence for the effect of social accountability interventions on policymakers' and providers' responsiveness in countries with medium to low levels of governance capacity and quality. For policymakers and practitioners engaged in health system strengthening, social accountability initiatives and rights-based approaches to health, the findings of this review may help when reflecting on the assumptions and theories of change behind their policies and interventions. Little is known about social accountability interventions, their outcomes and the circumstances under which they produce outcomes for particular groups or issues. In this study, social accountability interventions are conceptualized as complex social interventions for which a realist synthesis is considered the most appropriate method of systematic review. The synthesis is based on a preliminary program theory of social accountability that will be tested through an iterative process of primary study searches, data extraction, analysis and synthesis. Published and non-published (grey) quantitative and qualitative studies in English, French and Spanish will be included. Quality and validity will be enhanced by continuous peer review and team reflection among the reviewers. The authors believe the advantages of a realist synthesis for social accountability lie in the possibility of overcoming disciplinary or paradigmatic boundaries often found in public health and development. In addition, they argue that this approach fills the knowledge gap left by conventional synthesis or evaluation exercises of participatory programs. Finally, the authors describe the practical strategies adopted to address methodological challenges and validity.

The design of multirate digital control systems

NASA Technical Reports Server (NTRS)

Berg, M. C.

1986-01-01

The successive loop closures synthesis method is the only method for multirate (MR) synthesis in common use. A new method for MR synthesis is introduced which requires a gradient-search solution to a constrained optimization problem. Some advantages of this method are that the control laws for all control loops are synthesized simultaneously, taking full advantage of all cross-coupling effects, and that simple, low-order compensator structures are easily accomodated. The algorithm and associated computer program for solving the constrained optimization problem are described. The successive loop closures , optimal control, and constrained optimization synthesis methods are applied to two example design problems. A series of compensator pairs are synthesized for each example problem. The succesive loop closure, optimal control, and constrained optimization synthesis methods are compared, in the context of the two design problems.

Method of sound synthesis

DOEpatents

Miner, Nadine E.; Caudell, Thomas P.

2004-06-08

A sound synthesis method for modeling and synthesizing dynamic, parameterized sounds. The sound synthesis method yields perceptually convincing sounds and provides flexibility through model parameterization. By manipulating model parameters, a variety of related, but perceptually different sounds can be generated. The result is subtle changes in sounds, in addition to synthesis of a variety of sounds, all from a small set of models. The sound models can change dynamically according to changes in the simulation environment. The method is applicable to both stochastic (impulse-based) and non-stochastic (pitched) sounds.

Borophene as a prototype for synthetic 2D materials development.

PubMed

Mannix, Andrew J; Zhang, Zhuhua; Guisinger, Nathan P; Yakobson, Boris I; Hersam, Mark C

2018-06-01

The synthesis of 2D materials with no analogous bulk layered allotropes promises a substantial breadth of physical and chemical properties through the diverse structural options afforded by substrate-dependent epitaxy. However, despite the joint theoretical and experimental efforts to guide materials discovery, successful demonstrations of synthetic 2D materials have been rare. The recent synthesis of 2D boron polymorphs (that is, borophene) provides a notable example of such success. In this Perspective, we discuss recent progress and future opportunities for borophene research. Borophene combines unique mechanical properties with anisotropic metallicity, which complements the canon of conventional 2D materials. The multi-centre characteristics of boron-boron bonding lead to the formation of configurationally varied, vacancy-mediated structural motifs, providing unprecedented diversity in a mono-elemental 2D system with potential for electronic applications, chemical functionalization, materials synthesis and complex heterostructures. With its foundations in computationally guided synthesis, borophene can serve as a prototype for ongoing efforts to discover and exploit synthetic 2D materials.

Borophene as a prototype for synthetic 2D materials development

NASA Astrophysics Data System (ADS)

Mannix, Andrew J.; Zhang, Zhuhua; Guisinger, Nathan P.; Yakobson, Boris I.; Hersam, Mark C.

2018-06-01

The synthesis of 2D materials with no analogous bulk layered allotropes promises a substantial breadth of physical and chemical properties through the diverse structural options afforded by substrate-dependent epitaxy. However, despite the joint theoretical and experimental efforts to guide materials discovery, successful demonstrations of synthetic 2D materials have been rare. The recent synthesis of 2D boron polymorphs (that is, borophene) provides a notable example of such success. In this Perspective, we discuss recent progress and future opportunities for borophene research. Borophene combines unique mechanical properties with anisotropic metallicity, which complements the canon of conventional 2D materials. The multi-centre characteristics of boron-boron bonding lead to the formation of configurationally varied, vacancy-mediated structural motifs, providing unprecedented diversity in a mono-elemental 2D system with potential for electronic applications, chemical functionalization, materials synthesis and complex heterostructures. With its foundations in computationally guided synthesis, borophene can serve as a prototype for ongoing efforts to discover and exploit synthetic 2D materials.

Surface-Casting Synthesis of Mesoporous Zirconia with a CMK-5-Like Structure and High Surface Area.

PubMed

Gu, Dong; Schmidt, Wolfgang; Pichler, Christian M; Bongard, Hans-Josef; Spliethoff, Bernd; Asahina, Shunsuke; Cao, Zhengwen; Terasaki, Osamu; Schüth, Ferdi

2017-09-04

About 15 years ago, the Ryoo group described the synthesis of CMK-5, a material consisting of a hexagonal arrangement of carbon nanotubes. Extension of the surface casting synthesis to oxide compositions, however, was not possible so far, in spite of many attempts. Here it is demonstrated, that crystalline mesoporous hollow zirconia materials with very high surface areas up to 400 m 2  g -1 , and in selected cases in the form of CMK-5-like, are indeed accessible via such a surface casting process. The key for the successful synthesis is an increased interaction between the silica hard template surface and the zirconia precursor species by using silanol group-rich mesoporous silica as a hard template. The surface areas of the obtained zirconias exceed those of conventionally hard-templated ones by a factor of two to three. The surface casting process seems to be applicable also to other oxide materials. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Strongly coupled Sm0.2Ce0.8O2-Na2CO3 nanocomposite for low temperature solid oxide fuel cells: One-step synthesis and super interfacial proton conduction

NASA Astrophysics Data System (ADS)

Zhang, Guanghong; Li, Wenjian; Huang, Wen; Cao, Zhiqun; Shao, Kang; Li, Fengjiao; Tang, Chaoyun; Li, Cuihua; He, Chuanxin; Zhang, Qianling; Fan, Liangdong

2018-05-01

Highly conductive ceria-carbonate composite represents one type of most promising electrolyte materials for low temperature solid oxide fuel cells (SOFCs). Composites with large oxide-carbonate interface and homogeneous element/phase distribution are desirable to further enhance electrical properties and to study the ionic conduction mechanism. In this work, we report the successful synthesis of element/phase well-distributed, interfacial strongly coupled Sm0.2Ce0.8O2-Na2CO3 (NSDC) nanocomposite with different residual carbonate contents by an in-situ one-pot one-step citric acid-nitrate combustion method. Interestingly, NSDC shows distinct properties over those prepared by conventional methods and improved ionic conductivity. In particular, NSDC9010 nanocomposite displays a proton conductivity of 0.044 S cm-1 at 650 °C, which is 3-5 times higher than the oxide proton conductors. Electrolyte supported SOFCs based on the resultant nanocomposite electrolyte, NSDC9010, give the best power output of 281.5 mW cm-2 at 600 °C with LiNiO2 symmetric electro-catalysts. The excellent ionic conductivity and fuel cell performance are correlated with the unique core-shell structure, good phase distribution and large interfacial area induced by the one-step fabrication method, the strong coupling between oxide and carbonate as verified by the differential thermal and Raman spectroscopy characterization results and the optimal interfacial carbonate layer thickness by intentionally adjusting of carbonate contents.

Imprint-coating synthesis of selective functionalized ordered mesoporous sorbents for separation and sensors

DOEpatents

Dai, Sheng; Burleigh, Mark C.; Shin, Yongsoon

2001-01-01

The present invention relates generally to mesoporous sorbent materials having high capacity, high selectivity, fast kinetics, and molecular recognition capability. The invention also relates to a process for preparing these mesoporous substrates through molecular imprinting techniques which differ from convention techniques in that a template molecule is bound to one end of bifunctional ligands to form a complex prior to binding of the bifunctional ligands to the substrate. The present invention also relates to methods of using the mesoporous sorbent materials, for example, in the separation of toxic metals from process effluents, paints, and other samples; detection of target molecules, such as amino acids, drugs, herbicides, fertilizers, and TNT, in samples; separation and/or detection of substances using chromatography; imaging agents; sensors; coatings; and composites.

Multispectral Wavefronts Retrieval in Digital Holographic Three-Dimensional Imaging Spectrometry

NASA Astrophysics Data System (ADS)

Yoshimori, Kyu

2010-04-01

This paper deals with a recently developed passive interferometric technique for retrieving a set of spectral components of wavefronts that are propagating from a spatially incoherent, polychromatic object. The technique is based on measurement of 5-D spatial coherence function using a suitably designed interferometer. By applying signal processing, including aperture synthesis and spectral decomposition, one may obtains a set of wavefronts of different spectral bands. Since each wavefront is equivalent to the complex Fresnel hologram at a particular spectrum of the polychromatic object, application of the conventional Fresnel transform yields 3-D image of different spectrum. Thus, this technique of multispectral wavefronts retrieval provides a new type of 3-D imaging spectrometry based on a fully passive interferometry. Experimental results are also shown to demonstrate the validity of the method.

Polyelemental nanoparticle libraries.

PubMed

Chen, Peng-Cheng; Liu, Xiaolong; Hedrick, James L; Xie, Zhuang; Wang, Shunzhi; Lin, Qing-Yuan; Hersam, Mark C; Dravid, Vinayak P; Mirkin, Chad A

2016-06-24

Multimetallic nanoparticles are useful in many fields, yet there are no effective strategies for synthesizing libraries of such structures, in which architectures can be explored in a systematic and site-specific manner. The absence of these capabilities precludes the possibility of comprehensively exploring such systems. We present systematic studies of individual polyelemental particle systems, in which composition and size can be independently controlled and structure formation (alloy versus phase-separated state) can be understood. We made libraries consisting of every combination of five metallic elements (Au, Ag, Co, Cu, and Ni) through polymer nanoreactor-mediated synthesis. Important insight into the factors that lead to alloy formation and phase segregation at the nanoscale were obtained, and routes to libraries of nanostructures that cannot be made by conventional methods were developed. Copyright © 2016, American Association for the Advancement of Science.

Monoclinic β-Li2TiO3 nanocrystalline particles employing novel urea assisted solid state route: Synthesis, characterization and sintering behavior

NASA Astrophysics Data System (ADS)

Tripathi, Biranchi M.; Mohanty, Trupti; Prakash, Deep; Tyagi, A. K.; Sinha, P. K.

2017-07-01

Pure phase monoclinic nano-crystalline Li2TiO3 powder was synthesized by a novel urea assisted solid state synthesis method using readily available and economical precursors. A single phase and well crystalline Li2TiO3 powder has been obtained at slightly lower temperature (600-700 °C) and shorter duration (2 h) as compared to the conventional solid state method. The proposed method has significant advantages in comparison to other viable methods mainly in terms of phase purity, powder properties and sinterability. Analysis of chemical composition using inductively coupled plasma atomic emission spectroscopy (ICP-AES) shows no loss of lithium from Li2TiO3 in the proposed method. The emergence of monoclinic Li2TiO3 phase was confirmed by X-ray diffraction (XRD) pattern of as-synthesized powder. The crystallite size of Li2TiO3 powder was calculated to be in the range of 15-80 nm, which varied as a function of urea composition and temperature. The morphology of as-prepared Li2TiO3 powders was examined by scanning electron microscope (SEM). The effect of urea composition on phase and morphology was investigated so as to delineate the role of urea. Upon sintering at < 1000 °C temperature, the Li2TiO3 powder compact attained about 98% of the theoretical density with fine grained (grain size: 2-3 μm) microstructure. It indicates excellent sinter-ability of Li2TiO3 powder synthesized by the proposed method. The fine grained structure is desirable for better tritium breeding performance of Li2TiO3. Electrochemical impedance spectroscopy at variable temperature showed good electrical properties of Li2TiO3. The proposed method is simple, anticipated to be cost effective and convenient to realise for large scale production of phase pure nanocrystalline and having significantly enhanced sinter-ability Li2TiO3 powder.

A direct method for the synthesis of orthogonally protected furyl- and thienyl- amino acids.

PubMed

Hudson, Alex S; Caron, Laurent; Colgin, Neil; Cobb, Steven L

2015-04-01

The synthesis of unnatural amino acids plays a key part in expanding the potential application of peptide-based drugs and in the total synthesis of peptide natural products. Herein, we report a direct method for the synthesis of orthogonally protected 5-membered heteroaromatic amino acids.

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

Davis, B.E.; Ahner, P.F.; Singelton, A.H.

In situ gasification of steeply dipping coal beds (UCG-SDB) has significant advantages over the more conventional horizontal UCG. In fact, the UCG-SDB process appears to be both technically and operationally competitive with surface gasifiers. The results of the Rawlins UCG-SDB field test program suggest that the process can compete with more conventional sources of synthesis gas on an economic basis. The SDB process mechanism has several advantages over the horizontal process and performs in a fashion similar to surface packedbed reactors. The oxygen requirements for the process are quite low and the degree of process control observed at Rawlins ismore » very attractive.« less

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

Davis, B.E.; Ahner, P.F.

In-situ gasification of steeply dipping coal beds (UCG-SDB) has significant advantages over the more conventional horizontal UCG. In fact, the UCG-SDB process appears to be both technically and operationally competitive with surface gasifiers. The results of the Rawlins UCG-SDB field test program suggest that the process can compete with more conventional sources of synthesis gas on an economic basis. The SDB process mechanism has several advantages over the horizontal process and performs in a fashion similar to surface packed bed reactors. The oxygen requirements for the process are quite low and the degree of process control observed at Rawlins ismore » very attractive.« less

Microstructure of wave propagation during combustion synthesis of advanced materials: Experiments and theory

NASA Astrophysics Data System (ADS)

Hwang, Stephen

Combustion synthesis (CS) is an attractive method for producing advanced materials, including ceramics, intermetallics, and composites. In this process, after initiation by an external heat source, a highly exothermic reaction propagates through the sample in a self-sustained combustion wave. The process offers the possibility of producing materials with novel structures and properties. At conventional magnifications and imaging rates, the combustion wave appears to propagate in a planar, steady manner. However, using higher magnifications (>400X) and imaging rates (1000 frames/sec), fluctuations in the shape and propagation of the combustion front were observed. These variations in local conditions (i.e., the microstructure of the combustion wave) can influence the microstructure and properties of materials produced by combustion synthesis. In this work, the microstructure of wave propagation during combustion synthesis is investigated experimentally and theoretically. Using microscopic high-speed imaging, the spatial and temporal fluctuations of the combustion front shape and propagation were investigated. New image analysis methods were developed to characterize the heterogeneity of the combustion front quantitatively. The initial organization of the reaction medium was found to affect the heterogeneity of the combustion wave. Moreover, at the microscopic level, two different regimes of combustion propagation were observed. In the quasihomogeneous mechanism, the microstructure of the combustion wave resembles what is viewed macroscopically, and steady, planar propagation is observed. In the relay-race mechanism, while planar at the macroscopic level, the combustion front profiles are irregularly shaped, with arc-shaped convexities and concavities at the microscopic level. Also, the reaction front propagates as a series of rapid jumps and hesitations. Based on the combustion wave microstructure, new criteria were developed to determine the boundaries between quasihomogeneous and relay-race mechanisms, as functions of the initial organization of the reaction medium (i.e. particle size and porosity). In conjunction with the experiments, a microheterogeneous cell model was developed that simulates the local propagation of the combustion wave. Accounting for the stochastically organized medium with non-uniform properties, calculated results for the microstructural parameters of the combustion wave, and their dependence on density and reactant particle size, were in good qualitative agreement with experimental data.

Fibers innovative burning and reuse by Self-propagating High temperature Synthesis (SHS)

NASA Astrophysics Data System (ADS)

Caratto, Valentina; Belfortini, Claudio; Musi, Luigi; Gaggero, Laura; Ferretti, Maurizio

2016-04-01

The treatment of asbestos containing waste deriving from civil building and industrial applications is a social alert and an environmental problem. The project LIFE12 ENV/IT 000295 FIBERS "Fibers innovative burning and reuse by Self-propagating High temperature Synthesis (SHS)" has developed an innovative technique alternative to conventional high T processes. The University of Genoa has developed an apparatus and a technique for triggering the breakdown reaction of chrysotile by means of an alumino-thermic reaction in a process of combustion synthesis well known as Self-propagating High temperature Synthesis or SHS. This approach yielded interesting results and allowed the development of an efficient method for inerting natural asbestos fibers and man-made products carrying fibers at the scale of some grams [1]. The experiments were based on the couples Fe2O3/Mg by implementation of two prototype plants. The varying parameters were: 1) different Asbestos-Containing Waste (ACW) massive (Eternit, linoleum) and friable asbestos; 2) ACW abundance; 3) size of the pellet 4) under two triggering systems (induction by a W coil and oxyacetylene torch). The reactions were carried in two configurations: a) discontinuous, allowed us to obtain data for the development and fine-tuning of the reaction, b) continuous, was indispensable for the development and fine-tuning of the process parameters towards industrial scale up. After the combustive reaction all samples were characterized by SEM-EDS and XRPD analysis. All experiments demonstrated effective in destructing the fibrous habit of chrysotile, turning its composition to stubby olivine grains. We optimized the parameters to achieve complete conversion of the asbestos to mineral grains in all the cases. The efficiency of the SHS reaction in the discontinuous and continuous configurations was highlighted by the characterization of the post-combustion material under SEM-EDS and XRPD that verified the absence of fibers within the limits established by the regulations. The SHS process in comparison with conventional thermal treatments, due to fast reaction time, low activation energy, particularly advantages the asbestos inertization and positively reflects into time and costs of the process. Finally, the product of this transformation is liable to be re-used, e.g. as abrasive, or refractory material; this represents the end of waste status and a second life as secondary raw material. This work was carried out in the frame of LIFE12 ENV/IT/000295 FIBERS co-funded by the European Commission. [1] Gaggero L., Ferretti M., Belfortini C., Isola E. (2010) GE2010A000032

Unconventional processes for food regeneration in space - An overview

NASA Technical Reports Server (NTRS)

Stokes, B. O.; Petersen, G. R.; Schubert, W. W.; Mueller, W. A.

1981-01-01

Alternatives to conventional plant agriculture for the regeneration of food during space missions of extended duration are examined. The options considered, which may be used in combination with conventional agriculture, include the production of food from plant wastes, the chemical synthesis of food from carbon dioxide and other simple molecules or the substitution of edible chemicals, and the use of microrganisms for food and oxygen regeneration, with suitable processing. A comparison of solar energy conversion efficiencies is presented for nonphotosynthetic bacteria grown on hydrogen and algal systems photosynthetically, and it is shown that hydrogen bacteria are potentially more attractive than photosynthetic algae using artificial light. Weight-volume requirements for the conventional plant, algae and hydrogen bacteria systems are also compared to demonstrate the advantages of microbial systems.

In situ oligonucleotide synthesis on poly(dimethylsiloxane): a flexible substrate for microarray fabrication

PubMed Central

Moorcroft, Matthew J.; Meuleman, Wouter R. A.; Latham, Steven G.; Nicholls, Thomas J.; Egeland, Ryan D.; Southern, Edwin M.

2005-01-01

In this paper, we demonstrate in situ synthesis of oligonucleotide probes on poly(dimethylsiloxane) (PDMS) microchannels through use of conventional phosphoramidite chemistry. PDMS polymer was moulded into a series of microchannels using standard soft lithography (micro-moulding), with dimensions <100 μm. The surface of the PDMS was derivatized by exposure to ultraviolet/ozone followed by vapour phase deposition of glycidoxypropyltrimethoxysilane and reaction with poly(ethylene glycol) spacer, resulting in a reactive surface for oligonucleotide coupling. High, reproducible yields were achieved for both 6mer and 21mer probes as assessed by hybridization to fluorescent oligonucleotides. Oligonucleotide surface density was comparable with that obtained on glass substrates. These results suggest PDMS as a stable and flexible alternative to glass as a suitable substrate in the fabrication and synthesis of DNA microarrays. PMID:15870385

Visible light photocatalysis as a greener approach to photochemical synthesis.

PubMed

Yoon, Tehshik P; Ischay, Michael A; Du, Juana

2010-07-01

Light can be considered an ideal reagent for environmentally friendly, 'green' chemical synthesis; unlike many conventional reagents, light is non-toxic, generates no waste, and can be obtained from renewable sources. Nevertheless, the need for high-energy ultraviolet radiation in most organic photochemical processes has limited both the practicality and environmental benefits of photochemical synthesis on industrially relevant scales. This perspective describes recent approaches to the use of metal polypyridyl photocatalysts in synthetic organic transformations. Given the remarkable photophysical properties of these complexes, these new transformations, which use Ru(bpy)(3)(2+) and related photocatalysts, can be conducted using almost any source of visible light, including both store-bought fluorescent light bulbs and ambient sunlight. Transition metal photocatalysis thus represents a promising strategy towards the development of practical, scalable industrial processes with great environmental benefits.

Introduction for Design of Nanoparticle Based Drug Delivery Systems.

PubMed

Edgar, Jun Yan Chan; Wang, Hui

2017-01-01

Conventional drug delivery systems contain numerous limitations such as limited targeting, low therapeutic indices, poor water solubility, and the induction of drug resistances. In order to overcome the drawbacks of conventional pathway of drug delivery, nanoparticle delivery systems are therefore designed and used as the drug carriers. Nanoparticle based drug delivery systems have been rapidly growing and are being applied to various sections of biomedicine. Drug nanocarriers based on dendrimers, liposomes, self-assembling peptides, watersoluble polymers, and block copolymer micelles are the most extensively studied types of drug delivery systems and some of them are being used in clinical therapy. In particular for cancer therapy, antineoplastic drugs are taking advantage of nanoparticulate drug carriers to improve the cure efficacy. Nanoparticle based drug carriers are capable of improving the therapeutic effectiveness of the drugs by using active targeting for the site-specific delivery, passive targeting mechanisms such as enhanced permeability and retention (EPR), de novo synthesis and uptake of low density liposome in cancer cells or by being water-soluble to improve the suboptimal pharmacokinetics in limited water-soluble delivery methods. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Synthesis and characterization of polylactide/doxorubicin/magnetic nanoparticles composites for drug delivery

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

Mhlanga, Nikiwe; Ray, Suprakas Sinha; DST/CSIR National Centre for Nanostructured Materials, Council for Scientific and Industrial Research, Pretoria, 0001

Magnetic iron oxide nanoparticles have potential to transform conventional therapeutics, through targeted delivery by external magnetic field modulation. Conventional drug delivery lacks specificity; both normal and infected cells are exposed to toxic drugs. Consequently, the toxicity towards healthy cells leads to detrimental side effects which are formidable. However, iron oxide research in biomedicine has been hindered by their lack of stability. This study reports on the stabilization of iron oxide by polylactide (PLA). Besides affording stable iron oxide, PLA is also good for sustained delivery of the drug. PLA/doxorubicin/magnetic nanoparticles (PLA/DOX/MNPs) spheres were synthesized by solvent evaporation method and DOXmore » anticancer drug was encapsulated. The spheres were characterized using scanning electron microscope, Fourier transform infrared microscope, thermogravimetric analyzer and UV-visible spectroscopy, which ascertained formation of the anticipated spheres and incorporation of DOX. In vitro drug release studies were carried out in both phosphate buffer (pH 7.4) and acetate buffer (pH 4.6) and they showed the same trend in both mediums. Drug release kinetics followed Higuchi model, which proved drug release by diffusion via a diffusion gradient.« less

Quantum dots in biomedical applications: advances and challenges

NASA Astrophysics Data System (ADS)

Cinteza, Ludmila Otilia

2010-09-01

In the past two decades, nanotechnology has made great progress in generating novel materials with superior properties. Quantum dots (QDs) are an example of such materials. With unique optical properties, they have proven to be useful in a wide range of applications in life sciences, especially as a better alternative to overcome the shortcomings of conventional fluorophores. Current progress in the synthesis of biocompatible QDs allows for the possibility of producing a large variety of semiconductor nanocrystals in terms of size, surface functionality, bioconjugation, and targeting facilities. Strategies to enhance the water-dispersibility and biocompatibility of these nanoparticles have been developed, involving various encapsulation techniques and surface functionalization. The major obstacle in the clinical use of QDs remains their toxicity, and the systematic investigation on harmful effects of QDs both to humans and to the environment has become critical. Many examples of the experimental use of QDs prove their far-reaching potential for the study of intracellular processes at the molecular level, high resolution cellular imaging, and in vivo observation of cell trafficking. Biosensing methods based on QD bioconjugates proved to be successful in rapid detection of pathogens, and significant improvements are expected in early cancer diagnostic, non-conventional therapy of cancer and neurodegenerative diseases.

Organic-Inorganic Hybrid Halide Perovskites for Memories, Transistors, and Artificial Synapses.

PubMed

Choi, Jaeho; Han, Ji Su; Hong, Kootak; Kim, Soo Young; Jang, Ho Won

2018-05-30

Fascinating characteristics of halide perovskites (HPs), which cannot be seen in conventional semiconductors and metal oxides, have boosted the application of HPs in electronic devices beyond optoelectronics such as solar cells, photodetectors, and light-emitting diodes. Here, recent advances in HP-based memory and logic devices such as resistive-switching memories (i.e., resistive random access memory (RRAM) or memristors), transistors, and artificial synapses are reviewed, focusing on inherently exotic properties of HPs: i) tunable bandgap, ii) facile majority carrier control, iii) fast ion migration, and iv) superflexibility. Various fabrication techniques of HP thin films from solution-based methods to vacuum processes are introduced. Up-to-date work in the field, emphasizing the compositional flexibility of HPs, suggest that HPs are promising candidates for next-generation electronic devices. Taking advantages of their unique electrical properties, low-cost and low-temperature synthesis, and compositional and mechanical flexibility, HPs have enormous potential to provide a new platform for future electronic devices and explosively intensive studies will pave the way in finding new HP materials beyond conventional silicon-based semiconductors to keep up with "More-than-Moore" times. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Worked examples of alternative methods for the synthesis of qualitative and quantitative research in systematic reviews

PubMed Central

Lucas, Patricia J; Baird, Janis; Arai, Lisa; Law, Catherine; Roberts, Helen M

2007-01-01

Background The inclusion of qualitative studies in systematic reviews poses methodological challenges. This paper presents worked examples of two methods of data synthesis (textual narrative and thematic), used in relation to one review, with the aim of enabling researchers to consider the strength of different approaches. Methods A systematic review of lay perspectives of infant size and growth was conducted, locating 19 studies (including both qualitative and quantitative). The data extracted from these were synthesised using both a textual narrative and a thematic synthesis. Results The processes of both methods are presented, showing a stepwise progression to the final synthesis. Both methods led us to similar conclusions about lay views toward infant size and growth. Differences between methods lie in the way they dealt with study quality and heterogeneity. Conclusion On the basis of the work reported here, we consider textual narrative and thematic synthesis have strengths and weaknesses in relation to different research questions. Thematic synthesis holds most potential for hypothesis generation, but may obscure heterogeneity and quality appraisal. Textual narrative synthesis is better able to describe the scope of existing research and account for the strength of evidence, but is less good at identifying commonality. PMID:17224044

Multishaker modal testing

NASA Technical Reports Server (NTRS)

Craig, R. R., Jr.

1985-01-01

A component mode synthesis method for damped structures was developed and modal test methods were explored which could be employed to determine the relevant parameters required by the component mode synthesis method. Research was conducted on the following topics: (1) Development of a generalized time-domain component mode synthesis technique for damped systems; (2) Development of a frequency-domain component mode synthesis method for damped systems; and (3) Development of a system identification algorithm applicable to general damped systems. Abstracts are presented of the major publications which have been previously issued on these topics.

Microwave Synthesis of a Long-Lasting Phosphor

ERIC Educational Resources Information Center

Filhol, Jean-Sebastien; Zitoun, David; Bernaud, Laurent; Manteghetti, Alain

2009-01-01

Efficient glow-in-the-dark materials are usually difficult to synthesize and need complex experiments with long reaction times that are not appropriate for conventional lab teaching. Therefore, we describe a new experimental procedure that allows the production of one of the most efficient "glow-in-the-dark" materials (SrAl[subscript 2]O[subscript…

Synthesis of Taxol-Like Prostate Cancer Chemotherapeutic Agents

DTIC Science & Technology

2007-11-01

in Scheme 5, conventional condition utilizing n- BuLi as a base was not successful in the preparation of the desired Diels-Alder substrate 19 as only...unsuccessful. The only product obtained was n- BuLi addition to aldehyde 21. Thus, deprotonation conditions of terminal alkyne 17 or 20 are now being

The Dynamics of Climate Change: A Case Study in Organisational Learning

ERIC Educational Resources Information Center

Wasdell, David

2011-01-01

Purpose: Based in the discipline of applied consultancy-research, this paper seeks to present a synthesis-review of the social dynamics underlying the stalled negotiations of the United Nations Framework Convention on Climate Change. Its aim is to enhance understanding of the processes involved, to offer a working agenda to the organizational…

Applications of microwave-accelerated organic synthesis

NASA Astrophysics Data System (ADS)

Majetich, George; Hicks, Rodgers

1995-04-01

A comparison of microwave vs conventional heating is presented for a variety of Diels-Alder reactions, ortho-Claisen rearrangements, ene reactions, alkyl bromide preparations, Finkelstein reactions, oxidations, esterifications, hydrolyses, Williamson ether syntheses and other common organic transformations. In general, microwave-promoted reactions proceed with significant decreases in reaction times and in comparable chemical yield.

Phenanthridine synthesis through iron-catalyzed intramolecular N-arylation of O-acetyl oxime.

PubMed

Deb, Indubhusan; Yoshikai, Naohiko

2013-08-16

O-Acetyl oximes derived from 2'-arylacetophenones undergo N-O bond cleavage/intramolecular N-arylation in the presence of a catalytic amount of iron(III) acetylacetonate in acetic acid. In combination with the conventional cross-coupling or directed C-H arylation, the reaction offers a convenient route to substituted phenanthridines.