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Sample records for microwave-assisted mcmurry polymerization

  1. Microwave-assisted cationic ring-opening polymerization of 2-oxazolines

    PubMed Central

    Luef, Klaus P.; Hoogenboom, Richard; Schubert, Ulrich S.; Wiesbrock, Frank

    2017-01-01

    Unlike any other polymer class, the (co-)poly(2-oxazoline)s have tremendously benefited from the introduction of microwave reactors into chemical laboratories. This review focuses on the research activities in the area of (co-)poly(2-oxazoline)s prepared by microwave-assisted syntheses and, correspondingly, summarizes the current-state-of the-art of the microwave-assisted synthesis of 2-oxazoline monomers and the microwave-assisted ring-opening (co-)polymerization of 2-oxazolines as well as prominent examples of post-polymerization modification of (co-)poly(2-oxazoline)s. Special attention is attributed to the kinetic analysis of the microwave-assisted polymerization of 2-oxazolines and the discussion of non-thermal microwave effects. PMID:28239203

  2. Fabrication of Vertical Array CNTs/Polyaniline Composite Membranes by Microwave-Assisted In Situ Polymerization.

    PubMed

    Ding, Jie; Li, Xiaoyan; Wang, Xia; Zhang, Jinrui; Yu, Dengguang; Qiu, Biwei

    2015-12-01

    A vertical array carbon nanotubes (VACNTs)/polyaniline (PANi) composite membrane was prepared by microwave-assisted in situ polymerization. With microwave assistance, the morphology of PANi revealed a smaller diameter and denser connection. Meanwhile, thermogravimetric analysis showed improved thermal stability of microwave-assisted PANi for higher molecular weight. Focused ion beam thinning method was used to cut the VACNTs/PANi membrane into dozen-nanometer thin strips along the cross-sectional direction, and transmission electron microscopy observation showed seamless deposition of PANi between VACNT gaps, without damaging the vertical status of CNTs. Meanwhile, stronger conjugate interaction between the quinoid ring of PANi and VACNTs of the composite membrane were prompted by microwave-assisted in situ polymerization. By using nanoindentation technology, the VACNTs/PANi composite membrane showed exponential increasing of modulus and hardness. Meanwhile, the elasticity was also improved, which was proved by the calculated plastic index. The results can provide helpful guidance for seamlessly infiltrating matrix into CNT array and also demonstrate the importance of structural hierarchy for getting proper behavior of nanostructures.

  3. Fabrication of Vertical Array CNTs/Polyaniline Composite Membranes by Microwave-Assisted In Situ Polymerization

    NASA Astrophysics Data System (ADS)

    Ding, Jie; Li, Xiaoyan; Wang, Xia; Zhang, Jinrui; Yu, Dengguang; Qiu, Biwei

    2015-12-01

    A vertical array carbon nanotubes (VACNTs)/polyaniline (PANi) composite membrane was prepared by microwave-assisted in situ polymerization. With microwave assistance, the morphology of PANi revealed a smaller diameter and denser connection. Meanwhile, thermogravimetric analysis showed improved thermal stability of microwave-assisted PANi for higher molecular weight. Focused ion beam thinning method was used to cut the VACNTs/PANi membrane into dozen-nanometer thin strips along the cross-sectional direction, and transmission electron microscopy observation showed seamless deposition of PANi between VACNT gaps, without damaging the vertical status of CNTs. Meanwhile, stronger conjugate interaction between the quinoid ring of PANi and VACNTs of the composite membrane were prompted by microwave-assisted in situ polymerization. By using nanoindentation technology, the VACNTs/PANi composite membrane showed exponential increasing of modulus and hardness. Meanwhile, the elasticity was also improved, which was proved by the calculated plastic index. The results can provide helpful guidance for seamlessly infiltrating matrix into CNT array and also demonstrate the importance of structural hierarchy for getting proper behavior of nanostructures.

  4. Polymerization of tellurophene derivatives via microwave-assisted palladium-catalyzed ipso-arylative polymerization**

    PubMed Central

    Park, Young S.; Wu, Qin; Nam, Chang-Yong; Grubbs, Robert B.

    2014-01-01

    We report the synthesis of a tellurophene-containing low bandgap polymer, PDPPTe2T, via microwave-assisted palladium-catalyzed ipso-arylative polymerization of 2,5-bis[(α-hydroxy-α,α-diphenyl)methyl]tellurophene with a diketopyrrolopyrrole (DPP) monomer. Compared with the corresponding thiophene analog, PDPPTe2T absorbs light of longer wavelengths and has a smaller bandgap. Bulk heterojunction solar cells prepared from PDPPTe2T and PC71BM show PCE values of up to 4.4%. External quantum efficiency measurements show that PDPPTe2T produces photocurrent at wavelengths up to 1 μm. DFT calculations suggest that the atomic substitution from sulfur to tellurium increases electronic coupling to decrease the length of the carbon-carbon bonds between the tellurophene and thiophene rings, which results in the red-shift in absorption upon substitution of tellurium for sulfur. PMID:25145499

  5. Microwave-assisted radical polymerization of dialkyl fumarates

    NASA Astrophysics Data System (ADS)

    Cortizo, M. Susana; Laurella, Sergio; Alessandrini, José Luis

    2007-07-01

    Free radical polymerization of dialkyl fumarates (R:isopropyl, cyclohexyl, 2-ethylhexyl, 2-phenylethyl) under microwave irradiation was investigated. The polymerizations were carried out at different powers of irradiation and initiator concentrations (benzoyl peroxide, BP) and the effect of the monomer structure on the conversion, average molecular weights and the polydispersity index ( Mw/ Mn) was analyzed. A significant enhancement of the rates of polymerization was found, as compared with those obtained under thermal conditions.

  6. Microwave assisted synthesis of polyacrylamide grafted dextrin (Dxt-g-PAM): Development and application of a novel polymeric flocculant.

    PubMed

    Pal, Sagar; Nasim, T; Patra, A; Ghosh, S; Panda, A B

    2010-12-01

    An efficient polymeric flocculant was synthesized by microwave assisted grafting of polyacrylamide to dextrin. By varying the reaction conditions, various grades of graft copolymers were synthesized to obtain the optimized one. Viscometry, elemental analysis, FTIR spectroscopy, (13)C NMR spectroscopy, determination of molecular weight and radius of gyration using SLS analysis, thermal analysis and SEM analysis were employed to confirm that polyacrylamide has been grafted onto the dextrin backbone. The flocculation efficiency of the grafted products in kaolin suspension was dependent on the molecular weight, radius of gyration and length of the grafted polyacrylamide chains. The flocculant obtained by microwave assisted grafting method was superior to dextrin and polyacrylamide-based commercial flocculant (Rishfloc 226 LV) in flocculation tests.

  7. Microwave-assisted synthesis of titania coating onto polymeric separators for improved lithium-ion battery performance

    NASA Astrophysics Data System (ADS)

    Juang, Ruey-Shin; Hsieh, Chien-Te; Chen, Po-An; Chen, Yu-Fu

    2015-07-01

    This study adopts an efficient microwave-assisted method to deposit TiO2 into tri-layered polymeric membranes, forming composite separators for Li-ion batteries (LIBs) consisted of Li4Ti5O12 (LTO) anode/Li cathode. The microwave deposition is capable of growing TiO2 crystals into the porous membranes at 40 °C in a short period of ∼8 min. Both improved thermal and dimensional stability are achieved by the deposition of TiO2 in the separators. The improvement can be attributed to the formation of robust skeleton to stabilize the separators, imparting a superior insulation and mass transport barrier against volatile compounds formed during the thermal decomposition process. After depositing an appropriate amount of TiO2, the TiO2-coated separator still features well-developed porous structure, allowing favorable liquid wettability and high mass uptake of electrolyte. The amount of TiO2 deposits plays as a crucial role in facilitating the cell performance, including high ionic conductivity, low inner resistance, high operation temperature, high energy density, and excellent cycleability. Accordingly, this low-temperature deposition method of modifying polymeric separators is attractive for application in high-performance LIBs.

  8. Selective adsorption behavior of Cd(II) ion imprinted polymers synthesized by microwave-assisted inverse emulsion polymerization: Adsorption performance and mechanism.

    PubMed

    Zhu, Fang; Li, Luwei; Xing, Junde

    2017-01-05

    Microwave-assisted inverse emulsion polymerization method was used to prepare Cd(II) imprinted polymer (IIP) by using β-cyclodextrin (β-CD) and acrylamide (AM) as functional monomer, epichlorohydrin (ECH) as crossing-linking agent, ammonium persulfate as initiator. The Cd(II) imprinted polymer was characterized by SEM, FTIR and TGA. The influences of initial concentration of Cd(II), pH values, temperature, time and competitive ions on adsorption capacity and recognition properties are investigated. Under the optimal conditions, the adsorption capacity could reach 107mg/g. Furthermore, pseudo first order kinetic model, pseudo second order kinetic model and intra-particular diffusion model were used to describe the adsorption kinetic behavior. Results showed that the pseudo-second-order model (R(2) 0.9928-0.9961) had the best agreement with the experimental data. Langmuir adsorption isotherm model described the experimental data well, which indicated that adsorption was mainly monolayer absorption. Moreover, the study of adsorption thermodynamics (ΔG(0)<0, ΔH(0)>0, ΔS(0)>0) suggested that the adsorption process was a spontaneous and endothermic process. Competitive selectivity experiment revealed that imprinted polymer could selectively recognize Cd(II). It provides a new idea for removing Cd(II) from aqueous solution.

  9. Rapid preparation of molecularly imprinted polymers by microwave-assisted emulsion polymerization for the extraction of florfenicol in milk.

    PubMed

    Chen, Haiyan; Son, Sunil; Zhang, Fengshuang; Yan, Jin; Li, Yi; Ding, Hong; Ding, Lan

    2015-03-01

    In this study, we proposed a rapid and simple method for the preparation of molecularly imprinted polymers (MIPs) by emulsion polymerization. The polymerization process was accelerated by microwave heating, and the reaction time was greatly shortened. The obtained MIPs were spherical in shape and exhibited a uniform morphology. The MIPs with selectivity and high affinity to florfenicol were successfully applied as solid-phase extraction materials to extract and clean up the florfenicol in milk, followed by liquid chromatography-tandem mass spectrometry (LC-MS) analysis. The parameters affecting the performance of extraction and LC-MS analysis were evaluated. The detection limit of the method was 4.1ngmL(-1). The relative standard deviations of intra- and inter-day were in the range of 3.5-4.7% and 3.9-7.5%, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Microwave-assisted Chemical Transformations

    EPA Science Inventory

    In recent years, there has been a considerable interest in developing sustainable chemistries utilizing green chemistry principles. Since the first published report in 1986 by Gedye and Giguere on microwave assisted synthesis in household microwave ovens, the use of microwaves as...

  11. Microwave-assisted Chemical Transformations

    EPA Science Inventory

    In recent years, there has been a considerable interest in developing sustainable chemistries utilizing green chemistry principles. Since the first published report in 1986 by Gedye and Giguere on microwave assisted synthesis in household microwave ovens, the use of microwaves as...

  12. Microwave assisted chemical vapor infiltration

    SciTech Connect

    Devlin, D.J.; Currier, R.P.; Barbero, R.S.; Espinoza, B.F.; Elliott, N.

    1991-12-31

    A microwave assisted process for production of continuous fiber reinforced ceramic matrix composites is described. A simple apparatus combining a chemical vapor infiltration reactor with a conventional 700 W multimode oven is described. Microwave induced inverted thermal gradients are exploited with the ultimate goal of reducing processing times on complex shapes. Thermal gradients in stacks of SiC (Nicalon) cloths have been measured using optical thermometry. Initial results on the ``inside out`` deposition of SiC via decomposition of methyltrichlorosilane in hydrogen are presented. Several key processing issues are identified and discussed. 5 refs.

  13. MICROWAVE-ASSISTED SYNTHESIS OF NOBLE NANOSTRUCTURES

    EPA Science Inventory

    Microwave-assisted (MW) spontaneous reduction of noble metal salts, silver (Ag), gold (Au), platinum (Pt) and palladium (Pd) is reported using sugar solutions such as -D glucose, sucrose and maltose, etc. to generate nanomaterials. These MW-assisted reactions, conducted in aqueo...

  14. MICROWAVE-ASSISTED SYNTHESIS OF NOBLE NANOSTRUCTURES

    EPA Science Inventory

    Microwave-assisted (MW) spontaneous reduction of noble metal salts, silver (Ag), gold (Au), platinum (Pt) and palladium (Pd) is reported using sugar solutions such as -D glucose, sucrose and maltose, etc. to generate nanomaterials. These MW-assisted reactions, conducted in aqueo...

  15. Microwave-assisted synthesis of cyclodextrin polyurethanes

    USDA-ARS?s Scientific Manuscript database

    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 alpha-, ß-, and gamma-CD and thr...

  16. Ultrafast microwave-assisted in-tip digestion of proteins.

    PubMed

    Hahn, Hans W; Rainer, Matthias; Ringer, Thomas; Huck, Christian W; Bonn, Günther K

    2009-09-01

    Trypsin was immobilized on glycidylmethacrylate-co-divinylbenzene (GMA/DVB) polymerized in pipet tips for online enzymatic digestion of proteins. The major advantages of in-tip digestion are easy handling and small sample amount required for analysis. Microwave-assisted digestion was applied for highly efficient and time saving proteolysis. Adaption to an automated robotic system allowed fast and reproducible sample treatment. Investigations with matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF/MS) and liquid chromatography coupled with electrospray-ionization mass spectrometry (LC-ESI/MS) attested high sequence coverages (SCs) for the three standard proteins, myoglobin (Myo, 89%), bovine serum albumin (BSA, 78%) and alpha-casein (alpha-Cas, 83%). Compared to commercially available trypsin tips, clear predominance concerning the digestion performance was achieved. Storageability was tested over a period of several weeks and results showed only little decrease (<5%) of protein sequence coverages. The application of microwave-assisted in-tip digestion (2 min) with full automation by a robotic system allows high-throughput analysis (96 samples within 80 min) and highly effective proteolysis.

  17. Ceramic matrix composites by microwave assisted CVI

    SciTech Connect

    Currier, R.P.; Devlin, D.J.

    1993-05-01

    Chemical vapor infiltration (CVI) processes for producing continuously reinforced ceramic composites are reviewed. The potential advantages of microwave assisted CVI are noted. Recent numerical studies of microwave assisted CVI are then reviewed. These studies predict inverted thermal gradients in fibrous ceramic preforms subjected to microwave radiation and suggest processing strategies for achieving uniformly dense composites. Comparisons are made to experimental results obtained using silicon based composite systems. The importance of microwave-material interactions is stressed. In particular, emphasis is placed on the role played by the relative ability of fiber and matrix to dissipate microwave energy. Results suggest that microwave induced inverted gradients can in fact be exploited using the CVI technique to promote inside-out densification.

  18. Ceramic matrix composites by microwave assisted CVI

    SciTech Connect

    Currier, R.P.; Devlin, D.J.

    1993-01-01

    Chemical vapor infiltration (CVI) processes for producing continuously reinforced ceramic composites are reviewed. The potential advantages of microwave assisted CVI are noted. Recent numerical studies of microwave assisted CVI are then reviewed. These studies predict inverted thermal gradients in fibrous ceramic preforms subjected to microwave radiation and suggest processing strategies for achieving uniformly dense composites. Comparisons are made to experimental results obtained using silicon based composite systems. The importance of microwave-material interactions is stressed. In particular, emphasis is placed on the role played by the relative ability of fiber and matrix to dissipate microwave energy. Results suggest that microwave induced inverted gradients can in fact be exploited using the CVI technique to promote inside-out densification.

  19. Crossed McMurry Coupling Reactions for Porphycenic Macrocycles: Non-Statistical Selectivity and Rationalisation.

    PubMed

    Cowie, Thomas Y; Kennedy, Lorna; Żurek, Justyna M; Paterson, Martin J; Bebbington, Magnus W P

    2015-06-01

    Crossed McMurry reactions of bifuran- or bithiophenedicarbaldehydes with bipyrroledicarbaldehydes have been studied for the first time. Only those porphycenic macrocycles derived from homocoupled McMurry products were formed. The results are explained by using both density functional theory and electron propagator computations to model the electron affinity of the dialdehyde starting materials. It was predicted that bifuran\\bithiophene cross-coupling would indeed occur, and this was demonstrated by the first synthesis of a novel dioxa,dithio hetero-porphycenoid annulene. This approach will allow the prior identification of viable substrates for related crossed McMurry reactions.

  20. Crossed McMurry Coupling Reactions for Porphycenic Macrocycles: Non-Statistical Selectivity and Rationalisation

    PubMed Central

    Cowie, Thomas Y; Kennedy, Lorna; Żurek, Justyna M; Paterson, Martin J; Bebbington, Magnus W P

    2015-01-01

    Crossed McMurry reactions of bifuran- or bithiophenedicarbaldehydes with bipyrroledicarbaldehydes have been studied for the first time. Only those porphycenic macrocycles derived from homocoupled McMurry products were formed. The results are explained by using both density functional theory and electron propagator computations to model the electron affinity of the dialdehyde starting materials. It was predicted that bifuran\\bithiophene cross-coupling would indeed occur, and this was demonstrated by the first synthesis of a novel dioxa,dithio hetero-porphycenoid annulene. This approach will allow the prior identification of viable substrates for related crossed McMurry reactions. PMID:26213484

  1. 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.

  2. Microwave-assisted synthesis of organics and nanomaterials

    EPA Science Inventory

    Microwave-assisted chemistry techniques and greener reaction media are dramatically reducing chemical waste and reaction times in several organic transformations and material synthesis. This presentation summarizes author’s own experience in developing MW-assisted chemical proces...

  3. Microwave-assisted extraction in natural products isolation.

    PubMed

    Delazar, Abbas; Nahar, Lutfun; Hamedeyazdan, Sanaz; Sarker, Satyajit D

    2012-01-01

    Microwave-assisted extraction (MAE) or simply microwave extraction is a relatively new extraction technique that combines microwave and traditional solvent extraction. Application of microwaves for heating the solvents and plant tissues in extraction process, which increases the kinetic of extraction, is called microwave-assisted extraction. MAE has a number of advantages, e.g., shorter extraction time, less solvent, higher extraction rate and lower cost, over traditional method of extraction of compounds from various matrices, especially natural products. The use of MAE in natural products extraction started in the late 1980s, and through the technological developments, it has now become one of the popular and cost-effective extraction methods available today, and several advanced MAE instrumentations and methodologies have become available, e.g., pressurized microwave-assisted extraction (PMAE) and solvent-free microwave-assisted extraction (SFMAE). This chapter provides an overview of the MAE and presents a number of specific protocols for natural products extraction.

  4. Microwave-Assisted Synthesis of Phenothiazine and Quinoline Derivatives

    PubMed Central

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

    2007-01-01

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

  5. Analytical-scale microwave-assisted extraction.

    PubMed

    Eskilsson, C S; Björklund, E

    2000-12-01

    Microwave-assisted extraction (MAE) is a process of using microwave energy to heat solvents in contact with a sample in order to partition analytes from the sample matrix into the solvent. The ability to rapidly heat the sample solvent mixture is inherent to MAE and the main advantage of this technique. By using closed vessels the extraction can be performed at elevated temperatures accelerating the mass transfer of target compounds from the sample matrix. A typical extraction procedure takes 15-30 min and uses small solvent volumes in the range of 10-30 ml. These volumes are about 10 times smaller than volumes used by conventional extraction techniques. In addition, sample throughput is increased as several samples can be extracted simultaneously. In most cases recoveries of analytes and reproducibility are improved compared to conventional techniques, as shown in several applications. This review gives a brief theoretical background of microwave heating and the basic principles of using microwave energy for extraction. It also attempts to summarize all studies performed on closed-vessel MAE until now. The influences of parameters such as solvent choice, solvent volume, temperature, time and matrix characteristics (including water content) are discussed.

  6. System to continuously produce carbon fiber via microwave assisted plasma processing

    DOEpatents

    White, Terry L [Knoxville, TN; Paulauskas, Felix L [Knoxville, TN; Bigelow, Timothy S [Knoxville, TN

    2010-11-02

    A system to continuously produce fully carbonized or graphitized carbon fibers using microwave-assisted plasma (MAP) processing comprises an elongated chamber in which a microwave plasma is excited in a selected gas atmosphere. Fiber is drawn continuously through the chamber, entering and exiting through openings designed to minimize in-leakage of air. There is a gradient of microwave power within the chamber with generally higher power near where the fiber exits and lower power near where the fiber enters. Polyacrylonitrile (PAN), pitch, or any other suitable organic/polymeric precursor fibers can be used as a feedstock for the inventive system. Oxidized or partially oxidized PAN or pitch or other polymeric fiber precursors are run continuously through a MAP reactor in an inert, non-oxidizing atmosphere to heat the fibers, drive off the unwanted elements such as oxygen, nitrogen, and hydrogen, and produce carbon or graphite fibers faster than conventionally produced carbon fibers.

  7. Electrical detection of microwave assisted magnetization reversal by spin pumping

    SciTech Connect

    Rao, Siddharth; Subhra Mukherjee, Sankha; Elyasi, Mehrdad; Singh Bhatia, Charanjit; Yang, Hyunsoo

    2014-03-24

    Microwave assisted magnetization reversal has been investigated in a bilayer system of Pt/ferromagnet by detecting a change in the polarity of the spin pumping signal. The reversal process is studied in two material systems, Pt/CoFeB and Pt/NiFe, for different aspect ratios. The onset of the switching behavior is indicated by a sharp transition in the spin pumping voltage. At a threshold value of the external field, the switching process changes from partial to full reversal with increasing microwave power. The proposed method provides a simple way to detect microwave assisted magnetization reversal.

  8. Microwave-Assisted Synthesis of "N"-Phenylsuccinimide

    ERIC Educational Resources Information Center

    Shell, Thomas A.; Shell, Jennifer R.; Poole, Kathleen A.; Guetzloff, Thomas F.

    2011-01-01

    A microwave-assisted synthesis of "N"-phenylsuccinimide has been developed for the second-semester organic teaching laboratory. Utilizing this procedure, "N"-phenylsuccinimide can be synthesized in moderate yields (40-60%) by heating a mixture of aniline and succinic anhydride in a domestic microwave oven for four minutes. This technique reduces…

  9. Microwave assisted synthesis of technologically important transition metal silicides

    SciTech Connect

    Vaidhyanathan, B.; Rao, K.J.

    1997-12-01

    A novel, simple, clean and fast microwave assisted method of preparing important transition metal silicides (MoSi{sub 2}, WSi{sub 2}, CoSi{sub 2}, and TiSi{sub 2}) has been described. Amorphous carbon is used both as a microwave susceptor and as a preventer of oxidation. {copyright} {ital 1997 Materials Research Society.}

  10. Microwave-Assisted Synthesis of "N"-Phenylsuccinimide

    ERIC Educational Resources Information Center

    Shell, Thomas A.; Shell, Jennifer R.; Poole, Kathleen A.; Guetzloff, Thomas F.

    2011-01-01

    A microwave-assisted synthesis of "N"-phenylsuccinimide has been developed for the second-semester organic teaching laboratory. Utilizing this procedure, "N"-phenylsuccinimide can be synthesized in moderate yields (40-60%) by heating a mixture of aniline and succinic anhydride in a domestic microwave oven for four minutes. This technique reduces…

  11. Adding value to ethanol production byproducts through microwave assisted pyrolysis

    USDA-ARS?s Scientific Manuscript database

    The aim of this project is to increase the value of distillers grain by utilizing it as a feedstock for microwave assisted pyrolysis (MAP). Pyrolysis is the chemical/thermal conversion of biomass without the presence of oxygen into newly formed products: gases, liquids and solids. This conversion pr...

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

    NASA Astrophysics Data System (ADS)

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

    2015-04-01

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

  13. Determination of fructooligosaccharides in burdock using HPLC and microwave-assisted extraction.

    PubMed

    Li, Jing; Liu, Xiaomei; Zhou, Bin; Zhao, Jing; Li, Shaoping

    2013-06-19

    The root of burdock ( Arctium lappa L.) is a commonly used vegetable in Asia. Fructooligosaccharides (FOS) are usually considered as its main bioactive components. Thus, quantitative analysis of these components is very important for the quality control of burdock. In this study, an HPLC-ELSD and microwave-assisted extraction method was developed for the simultaneous determination of seven FOS with degrees of polymerization (DP) between 3 and 9, as well as fructose, glucose, and sucrose in burdock from different regions. The separation was performed on a Waters XBridge Amide column (4.6 × 250 mm i.d., 3.5 μm) with gradient elution. All calibration curves for investigated analytes showed good linear regression (r > 0.9990). Their LODs and LOQs were lower than 3.63 and 24.82 μg/mL, respectively. The recoveries ranged from 99.2 to 102.6%. The developed method was successfully applied to determination of ten sugars in burdock from different locations of Asia. The results showed that the contents of FOS in different samples of burdock collected at appropriate times were similar, and the developed HPLC-ELSD with microwave-assisted extraction method is helpful to control the quality of burdock.

  14. Amphiphilic block copolymer modified magnetic nanoparticles for microwave-assisted extraction of polycyclic aromatic hydrocarbons in environmental water.

    PubMed

    Li, Nan; Qi, Li; Shen, Ying; Li, Yaping; Chen, Yi

    2013-11-05

    In this work, amphiphilic block copolymer poly(tert-butyl methacrylate)-block-poly(glycidyl methacrylate) (PtBMA-b-PGMA) modified Fe3O4 magnetic nanoparticles (Fe3O4 MNPs) were synthesized, and served as an adsorbent for microwave-assisted extraction of polycyclic aromatic hydrocarbons (PAHs). The PtBMA-b-PGMA block copolymers with different block ratios were prepared by two-step atom transfer radical polymerization (ATRP) and the extraction abilities of their corresponding Fe3O4@PtBMA-b-PGMA were investigated. The key factors affecting the extraction efficiency of the adsorbent, including microwave conditions, amount of adsorbent, type and volume of desorption solvent, were studied in detail. In comparison with vortex, which is a conventional method used for assisting extraction, the proposed microwave-assisted method allowed better extraction efficiency and required a shorter extraction time. The calibration curves of PAHs were obtained in the range of 0.05-120 μg/L (r>0.9985) and the limits of detection (S/N=3) were in the range of 2.4-6.3 ng/L. The recoveries of PAHs spiked in environmental water samples were between 62.5% and 104% with relative standard deviations (RSDs) ranging from 0.84% to 9.02%. The proposed technique combining microwave-assisted extraction and magnetic separation was demonstrated to be a fast, convenient and sensitive pretreating method for PAHs.

  15. Microwave-Assisted Ignition for Improved Internal Combustion Engine Efficiency

    NASA Astrophysics Data System (ADS)

    DeFilippo, Anthony Cesar

    The ever-present need for reducing greenhouse gas emissions associated with transportation motivates this investigation of a novel ignition technology for internal combustion engine applications. Advanced engines can achieve higher efficiencies and reduced emissions by operating in regimes with diluted fuel-air mixtures and higher compression ratios, but the range of stable engine operation is constrained by combustion initiation and flame propagation when dilution levels are high. An advanced ignition technology that reliably extends the operating range of internal combustion engines will aid practical implementation of the next generation of high-efficiency engines. This dissertation contributes to next-generation ignition technology advancement by experimentally analyzing a prototype technology as well as developing a numerical model for the chemical processes governing microwave-assisted ignition. The microwave-assisted spark plug under development by Imagineering, Inc. of Japan has previously been shown to expand the stable operating range of gasoline-fueled engines through plasma-assisted combustion, but the factors limiting its operation were not well characterized. The present experimental study has two main goals. The first goal is to investigate the capability of the microwave-assisted spark plug towards expanding the stable operating range of wet-ethanol-fueled engines. The stability range is investigated by examining the coefficient of variation of indicated mean effective pressure as a metric for instability, and indicated specific ethanol consumption as a metric for efficiency. The second goal is to examine the factors affecting the extent to which microwaves enhance ignition processes. The factors impacting microwave enhancement of ignition processes are individually examined, using flame development behavior as a key metric in determining microwave effectiveness. Further development of practical combustion applications implementing microwave-assisted

  16. New facile and rapid synthesis of polyamides and polyimides by microwave-assisted polycondensation

    SciTech Connect

    Imai, Yoshio

    1995-12-01

    The application of microwave energy using a domestic microwave oven to organic synthesis as well as to radical polymerization of vinyl monomers and curing of polymers have been known during the past decade, however, there is no report so far an the synthesis of condensation polymers under microwave irradiation. We have developed successfully a new method for the facile and rapid synthesis of aliphatic polyamides from both co-amino acids and nylon salts, aliphatic polyimides from diamine-tetra-carboxylic acid salt monomers, and aromatic polyamides with use of a condensing agent by the microwave-assisted polycondensation. In these preparations, the presence of the polar solvents having good solubility of monomers coupled with high boiling point were necessary, which facilitated the high temperature polycondensation in solution or plastisized melt state, yielding the condensation polymers with high inherent viscosities by the microwave heating for only 2-5 min.

  17. Microwave-assisted methanolysis of green coffee oil.

    PubMed

    Oigman, S S; de Souza, R O M A; Dos Santos Júnior, H M; Hovell, A M C; Hamerski, L; Rezende, C M

    2012-09-15

    Optimisation of a microwave-assisted methanolysis was performed to obtain cafestol and kahweol directly from green coffee oil (Coffea arabica). A two-factor (the methanolysis period and temperature), three-level, factorial experimental design (3(2)) was adopted. The methanolysis procedure was performed under microwave irradiation, using closed vessel and accurate fast responding internal fibre-optic temperature probe. The effects on the responses were measured by HPLC. After 3 min of microwave irradiation (hold time) at 100°C, with 500 mg of green coffee oil, a yield higher than 99% was obtained. The yield of this reaction is 26% after 2h when working under conventional heating. The methods described in the literature lead to long reaction times, poor yields and formation of side products. The microwave-assisted technique proved to be faster, avoided undesired side products and gave better conversion, when compared to conventional heating process. Copyright © 2012 Elsevier Ltd. All rights reserved.

  18. Critical damping constant of microwave-assisted magnetization switching

    NASA Astrophysics Data System (ADS)

    Yamaji, Toshiki; Arai, Hiroko; Matsumoto, Rie; Imamura, Hiroshi

    2016-02-01

    Microwave-assisted switching of magnetization in a perpendicularly magnetized disk was theoretically studied and special attention was paid to the effect of a damping constant on the switching field. We found that there exists a critical damping constant above which the switching field suddenly increases. We derived an analytical expression of the critical damping constant and showed that it decreases with increasing frequency of the microwave field, while it increases with increasing amplitude of the microwave field and the effective anisotropy field.

  19. Focused microwave-assisted Soxhlet extraction: devices and applications.

    PubMed

    Luque-García, J L; Luque de Castro, M D

    2004-10-20

    An overview of a new extraction technique called focused microwave-assisted Soxhlet extraction (FMASE) is here presented. This technique is based on the same principles as conventional Soxhlet extraction but using microwaves as auxiliary energy to accelerate the process. The different devices designed and constructed so far, their advantages and limitations as well as their main applications on environmental and food analysis are discussed in this article.

  20. Microwave-Assisted Hydrogenation of Codeine in Aqueous Media

    PubMed Central

    Taktak, F.; Bulduk, I.

    2012-01-01

    An efficient one-pot microwave-assisted hydrogenation of codeine was achieved in aqueous solution. This technique is simple, fast, environmentally friendly, and highly efficient. Structure of produced dihydrocodeine was approved by using FT-IR, 1H NMR, 13C NMR, EIMS, and elemental analysis technique. Its purity analysis was performed by using HPLC and assay analysis was performed by using potentiometric titration methods. PMID:24052836

  1. Microwave-assisted hydrogenation of codeine in aqueous media.

    PubMed

    Taktak, F; Bulduk, I

    2012-01-01

    An efficient one-pot microwave-assisted hydrogenation of codeine was achieved in aqueous solution. This technique is simple, fast, environmentally friendly, and highly efficient. Structure of produced dihydrocodeine was approved by using FT-IR, (1)H NMR, (13)C NMR, EIMS, and elemental analysis technique. Its purity analysis was performed by using HPLC and assay analysis was performed by using potentiometric titration methods.

  2. Microwave-assisted pyrolysis of biomass for liquid biofuels production.

    PubMed

    Yin, Chungen

    2012-09-01

    Production of 2nd-generation biofuels from biomass residues and waste feedstock is gaining great concerns worldwide. Pyrolysis, a thermochemical conversion process involving rapid heating of feedstock under oxygen-absent condition to moderate temperature and rapid quenching of intermediate products, is an attractive way for bio-oil production. Various efforts have been made to improve pyrolysis process towards higher yield and quality of liquid biofuels and better energy efficiency. Microwave-assisted pyrolysis is one of the promising attempts, mainly due to efficient heating of feedstock by "microwave dielectric heating" effects. This paper presents a state-of-the-art review of microwave-assisted pyrolysis of biomass. First, conventional fast pyrolysis and microwave dielectric heating is briefly introduced. Then microwave-assisted pyrolysis process is thoroughly discussed stepwise from biomass pretreatment to bio-oil collection. The existing efforts are summarized in a table, providing a handy overview of the activities (e.g., feedstock and pretreatment, reactor/pyrolysis conditions) and findings (e.g., pyrolysis products) of various investigations.

  3. Microwave-assisted tissue processing for same-day EM-diagnosis of potential bioterrorism and clinical samples.

    PubMed

    Schroeder, Josef A; Gelderblom, Hans R; Hauroeder, Baerbel; Schmetz, Christel; Milios, Jim; Hofstaedter, Ferdinand

    2006-01-01

    The purpose of this study was to explore the turnaround times, section and image quality of a number of more "difficult" specimens destined for rapid diagnostic electron microscopy (EM) after microwave-assisted processing. The results were assessed and compared with those of conventionally processed samples. A variety of infectious agents, some with a potential for bioterrorism, and liver biopsies serving as an example for routine histopathology samples were studied. The samples represented virus-producing cell cultures (such as SARS-coronavirus, West Nile virus, Orthopox virus), bacteria suspensions (cultures of Escherichia coli and genetically knockout apathogenic Bacillus anthracis), suspensions of parasites (malaria Plasmodium falciparum, Leishmania major, Microsporidia cuniculi, Caenorhabditis elegans), and whole Drosophila melanogaster flies infected with microsporidia. Fresh liver samples and infected flies were fixed in Karnovsky-fixative by microwaving (20 min), all other samples were fixed in buffered glutaraldehyde or Karnovsky-fixative overnight or longer. Subsequently, all samples were divided to evaluate alternative processing protocols: one part of the sample was OsO4-postfixed, ethanol-dehydrated, Epon-infiltrated (overnight) in an automated tissue processor (LYNX, Leica), and polymerized at 60 degrees C for 48 h; in parallel the other part was microwave-assisted processed in the bench microwave device (REM, Milestone), including post-osmication and the resin block polymerization. The microwave-assisted processing protocol required at minimum 3 h 20 min: the respective epon resin blocks were uniformly polymerized allowing an easy sectioning of semi- and ultrathin sections. Sections collected on non-coated 200 mesh grids were stable in the electron beam and showed an excellent preservation of the ultrastructure and high contrast, thus allowing an easy, unequivocal and rapid assessment of specimens. Compared with conventional routine methods

  4. Analytical expression for critical frequency of microwave assisted magnetization switching

    NASA Astrophysics Data System (ADS)

    Arai, Hiroko; Imamura, Hiroshi

    2016-02-01

    The microwave-assisted switching (MAS) of magnetization in a perpendicularly magnetized circular disk is studied based on the macrospin model in a rotating frame. The analytical expression for the critical frequency of MAS is derived by analyzing the presence of a quasiperiodic mode. The critical frequency is expressed as a function of the radio frequency (rf) field Hrf and the effective anisotropy field H\\text{k}\\text{eff}. For a small rf field such that H\\text{rf} \\ll H\\text{k}\\text{eff}, the critical frequency is approximately equal to (γ /π )\\root 3 \\of{\\smash{H\\text{k}\\text{eff}H\\text{rf}2}\\mathstrut}.

  5. Microwave-Assisted Synthesis of N-Phenylsuccinimide.

    PubMed

    Shell, Thomas A; Shell, Jennifer R; Poole, Kathleen A; Guetzloff, Thomas F

    2011-10-01

    A microwave-assisted synthesis of N-phenylsuccinimide has been developed for the second-semester organic teaching laboratory. Utilizing this procedure, N-phenylsuccinimide can be synthesized by heating a mixture of aniline and succinic anhydride in a domestic microwave oven for four minutes in moderate yields (40-60%). This technique reduces the reaction time as compared to the traditional synthesis by several hours, which allows the preparation to be achieved in a single organic chemistry laboratory period. This reaction is performed in the absence of solvent, is energy efficient, and is atom economical; therefore, it represents a "greener" preparation than the traditional synthesis of N-phenylsuccinimide.

  6. Microwave-assisted extraction of polycyclic aromatic compounds from coal.

    PubMed

    Kerst, M; Andersson, J T

    2001-08-01

    Microwave-assisted extraction (MAE) of polycyclic aromatic compounds (PACs) from coal is shown to give the same pattern of compounds as Soxhlet extraction. MAE requires only 10 mL solvent and 10 min extraction time whereas Soxhlet uses 200 mL and takes 24 h. Although the yields were lower, dichloromethane (DCM) was preferred to pyridine, N-methyl-2-pyrrolidone (NMP), and NMP with CS2 because the pattern of the PACs is shown to be independent of solvent and DCM is a much more convenient solvent to work with.

  7. Microwave-Assisted Extraction of Fucoidan from Marine Algae.

    PubMed

    Mussatto, Solange I

    2015-01-01

    Microwave-assisted extraction (MAE) is a technique that can be applied to extract compounds from different natural resources. In this chapter, the use of this technique to extract fucoidan from marine algae is described. The method involves a closed MAE system, ultrapure water as extraction solvent, and suitable conditions of time, pressure, and algal biomass/water ratio. By using this procedure under the specified conditions, the penetration of the electromagnetic waves into the material structure occurs in an efficient manner, generating a distributed heat source that promotes the fucoidan extraction from the algal biomass.

  8. Tellurium nanotubes synthesized with microwave-assisted monosaccharide reduction method.

    PubMed

    Liu, Tao; Zhang, Gang; Su, Xu; Chen, Xingguo; Wang, Dahai; Qin, Jingui

    2007-07-01

    A microwave-assisted monosaccharide reducing approach has been developed in the preparation of tellurium nanotubes. The as-prepared tellurium nanotubes have the sizes of 50 - 100 nm in diameter, and a few micrometers in length. A series of contrastive experiments have illustrated that microwave-heating contributed a lot in the synthesis, and the decomposition of H2TeO3 to TeO2 and low reducibility of the monosaccharide played a key role in the process. The possible mechanism of the synthesis of the nanotubes has been preliminarily discussed.

  9. 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.

  10. Microwave-assisted extraction of phycobiliproteins from Porphyridium purpureum.

    PubMed

    Juin, Camille; Chérouvrier, Jean-René; Thiéry, Valérie; Gagez, Anne-Laure; Bérard, Jean-Baptiste; Joguet, Nicolas; Kaas, Raymond; Cadoret, Jean-Paul; Picot, Laurent

    2015-01-01

    In the present study, microwave-assisted extraction was first employed to extract the phycobiliproteins of Porphyridium purpureum (Pp). Freeze-dried Pp cells were subjected to microwave-assisted extraction (MAE) to extract phycoerythin (PE), phycocyanin (PC), and allophycocyanin (APC). MAE combined reproducibility and high extraction yields and allowed a 180- to 1,080-fold reduction of the extraction time compared to a conventional soaking process. The maximal PE extraction yield was obtained after 10-s MAE at 40 °C, and PE was thermally damaged at temperatures higher than 40 °C. In contrast, a flash irradiation for 10 s at 100 °C was the best process to efficiently extract PC and APC, as it combined a high temperature necessary to extract them from the thylakoid membrane to a short exposure to thermal denaturation. The extraction order of the three phycobiliproteins was coherent with the structure of Pp phycobilisomes. Moreover, the absorption and fluorescence properties of MAE extracted phycobiliproteins were stable for several months after the microwave treatment. Scanning electron microscopy indicated that MAE at 100 °C induced major changes in the Pp cell morphology, including fusion of the exopolysaccharidic cell walls and cytoplasmic membranes of adjacent cells. As a conclusion, MAE is a fast and high yield process efficient to extract and pre-purify phycobiliproteins, even from microalgae containing a thick exopolysaccharidic cell wall.

  11. Microwave-assisted enzymatic synthesis of beef tallow biodiesel.

    PubMed

    Rós, Patrícia C M Da; Castro, Heizir F de; Carvalho, Ana K F; Soares, Cleide M F; Moraes, Flavio F de; Zanin, Gisella M

    2012-04-01

    Optimal conditions for the microwave-assisted enzymatic synthesis of biodiesel have been developed by a full 2² factorial design leading to a set of seven runs with different combinations of molar ratio and temperature. The main goal was to reduce the reaction time preliminarily established by a process of conventional heating. Reactions yielding biodiesel, in which beef tallow and ethanol used as raw materials were catalyzed by lipase from Burkholderia cepacia immobilized on silica-PVA and microwave irradiations within the range of 8-15 W were performed to reach the reaction temperature. Under optimized conditions (1:6 molar ratio of beef tallow to ethanol molar ratio at 50°C) almost total conversion of the fatty acid presented in the original beef tallow was converted into ethyl esters in a reaction that required 8 h, i.e., a productivity of about 92 mg ethyl esters g⁻¹ h⁻¹. This represents an increase of sixfold for the process carried out under conventional heating. In general, the process promises low energy demand and higher biodiesel productivity. The microwave assistance speeds up the enzyme catalyzed reactions, decreases the destructive effects on the enzyme of the operational conditions such as, higher temperature, stability, and specificity to its substrate, and allows the entire reaction medium to be heated uniformly.

  12. Magnetic gold nanotriangles by microwave-assisted polyol synthesis

    NASA Astrophysics Data System (ADS)

    Yu, Siming; Hachtel, Jordan A.; Chisholm, Matthew F.; Pantelides, Sokrates T.; Laromaine, Anna; Roig, Anna

    2015-08-01

    Simple approaches to synthesize hybrid nanoparticles with magnetic and plasmonic functionalities, with high control of their shape and avoiding cytotoxic reactants, to target biomedical applications remain a huge challenge. Here, we report a facile, fast and bio-friendly microwave-assisted polyol route for the synthesis of a complex multi-material consisting of monodisperse gold nanotriangles around 280 nm in size uniformly decorated by superparamagnetic iron oxide nanoparticles of 5 nm. These nanotriangles are readily dispersible in water, display a strong magnetic response (10 wt% magnetic fraction) and exhibit a localized surface plasmon resonance band in the NIR region (800 nm). Moreover, these hybrid particles can be easily self-assembled at the liquid-air interfaces.Simple approaches to synthesize hybrid nanoparticles with magnetic and plasmonic functionalities, with high control of their shape and avoiding cytotoxic reactants, to target biomedical applications remain a huge challenge. Here, we report a facile, fast and bio-friendly microwave-assisted polyol route for the synthesis of a complex multi-material consisting of monodisperse gold nanotriangles around 280 nm in size uniformly decorated by superparamagnetic iron oxide nanoparticles of 5 nm. These nanotriangles are readily dispersible in water, display a strong magnetic response (10 wt% magnetic fraction) and exhibit a localized surface plasmon resonance band in the NIR region (800 nm). Moreover, these hybrid particles can be easily self-assembled at the liquid-air interfaces. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr03113c

  13. A Microwave-Assisted Reduction of Cyclohexanone Using Solid-State-Supported Sodium Borohydride

    ERIC Educational Resources Information Center

    White, Lori L.; Kittredge, Kevin W.

    2005-01-01

    The reduction of carbonyl groups by sodium borohydride though is a well-known reaction in most organic lab texts, a difficulty for an instructor adopting this reaction in a student lab is that it is too long. Using a microwave assisted organic synthesis solves this difficulty and one such reaction, which is the microwave-assisted reduction of…

  14. Bio-based products via microwave-assisted maleation of tung oil

    USDA-ARS?s Scientific Manuscript database

    A simple “green” and convenient chemical modification of tung oil for maleinized tung oil (TOMA) was developed via microwave-assisted one-step maleation. The mechanism of this microwave-assisted maleation was investigated by nuclear magnetic resonance (NMR) and gel permeation chromatography (GPC). T...

  15. A Microwave-Assisted Reduction of Cyclohexanone Using Solid-State-Supported Sodium Borohydride

    ERIC Educational Resources Information Center

    White, Lori L.; Kittredge, Kevin W.

    2005-01-01

    The reduction of carbonyl groups by sodium borohydride though is a well-known reaction in most organic lab texts, a difficulty for an instructor adopting this reaction in a student lab is that it is too long. Using a microwave assisted organic synthesis solves this difficulty and one such reaction, which is the microwave-assisted reduction of…

  16. Microwave-assisted sample preparation of coal and coal fly ash for subsequent metal determination

    SciTech Connect

    Srogi, K.

    2007-01-15

    The aim of this paper is to review microwave-assisted digestion of coal and coal fly ash. A brief description of microwave heating principles is presented. Microwave-assisted digestion appears currently to be the most popular preparation technique, possibly due to the comparatively rapid sample preparation and the reduction of contamination, compared to the conventional hot-plate digestion methods.

  17. Effect of microwave-assisted heating on chalcopyrite leaching of kinetics, interface temperature and surface energy

    NASA Astrophysics Data System (ADS)

    Wen, Tong; Zhao, Yunliang; Xiao, Qihang; Ma, Qiulin; Kang, Shichang; Li, Hongqiang; Song, Shaoxian

    The microwave-assisted leaching was a new approach to intensify the copper recovery from chalcopyrite by hydrometallurgy. In this work, the effect of microwave-assisted heating on chalcopyrite leaching of kinetics, interfacial reaction temperature and surface energy were investigated. The activation energy of chalcopyrite leaching was affected indistinctively by the microwave-assisted heating (39.1 kJ/mol) compared with the conventional heating (43.9 kJ/mol). However, the boiling point of the leaching system increased through microwave-assisted heating. Because of the improved boiling point and the selective heating of microwave, the interfacial reaction temperature increased significantly, which gave rise to the increase of the leaching recovery of copper. Moreover, the surface energy of the chalcopyrite through microwave-assisted heating was also enhanced, which was beneficial to strengthen the leaching of chalcopyrite.

  18. 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.

  19. Microwave-Assisted Synthesis of N-Phenylsuccinimide

    PubMed Central

    Shell, Thomas A.; Shell, Jennifer R.; Poole, Kathleen A.; Guetzloff, Thomas F.

    2011-01-01

    A microwave-assisted synthesis of N-phenylsuccinimide has been developed for the second-semester organic teaching laboratory. Utilizing this procedure, N-phenylsuccinimide can be synthesized by heating a mixture of aniline and succinic anhydride in a domestic microwave oven for four minutes in moderate yields (40–60%). This technique reduces the reaction time as compared to the traditional synthesis by several hours, which allows the preparation to be achieved in a single organic chemistry laboratory period. This reaction is performed in the absence of solvent, is energy efficient, and is atom economical; therefore, it represents a “greener” preparation than the traditional synthesis of N-phenylsuccinimide. PMID:22125340

  20. Microwave-assisted synthesis and characterization of nickel ferrite nanoparticles

    NASA Astrophysics Data System (ADS)

    Carpenter, Gopal; Sen, Ravindra; Malviya, Nitin; Gupta, Nitish

    2015-08-01

    Nickel ferrite nanoparticles (NiFe2O4) were successfully prepared by microwave-assisted combustion method (MWAC) using citric Electron acid as a chelating agent. NiFe2O4 nanoparticles were characterized by X-ray diffraction (XRD) pattern, Scanning Microscopy (SEM), Fourier transform infrared (FTIR) and UV-Visible techniques. XRD analysis revealed that NiFe2O4 nanoparticles have spinel cubic structure with the average crystalline size of 26.38 nm. SEM analysis revealed random and porous structural morphology of particles and FTIR showed absorption bands related to octahedral and tetrahedral sites, in the range 400-600cm-1 which strongly favor the formation of NiFe2O4 nanoparticles. The optical band gap is determined by UV Visible method and found to be 5.4 eV.

  1. Formation of nanostructured fluorapatite via microwave assisted solution combustion synthesis.

    PubMed

    Nabiyouni, Maryam; Zhou, Huan; Luchini, Timothy J F; Bhaduri, Sarit B

    2014-04-01

    Fluorapatite (FA) has potential applications in dentistry and orthopedics, but its synthesis procedures are time consuming. The goal of the present study is to develop a quick microwave assisted solution combustion synthesis method (MASCS) for the production of FA particles. With this new processing, FA particles were successfully synthesized in minutes. Additionally, unique structures including nanotubes, hexagonal crystals, nanowhiskers, and plate agglomerates were prepared by controlling the solution composition and reaction time. In particular, the as-synthesized FA nanotubes presented a "Y" shape inner channel along the crystal axis. It is supposed that the channel formation is caused by the crystal growth and removal of water soluble salts during processing. The as-synthesized FA nanotubes showed good cytocompatibility, the cells cultured with a higher FA concentration demonstrated greater growth rate. With this new and easily applied MASCS processing application, FA nanoparticles have increased potential in dental and orthopedic applications.

  2. Microwave-assisted extraction of essential oils from herbs.

    PubMed

    Cardoso-Ugarte, Gabriel Abraham; Juárez-Becerra, Gladys Paola; Sosa-Morales, María Elena; López-Malo, Aurelio

    2013-01-01

    Microwave-assisted extraction (MAE) has been recognized as a technique with several advantages over other extraction methods, such as reduction of costs, extraction time, energy consumption, and CO2 emissions. In this study, MAE was performed to obtain essential oils from two different herbs (basil and epazote). A factorial design was conducted in order to determine the effect of solvent quantity, power, and heating time on essential oil yields. Chemical composition, physical properties and yield percentage of essential oils from MAE were compared with essential oils obtained by steam distillation (SD). Amount of solvent and heating time significantly affected the yields (p < 0.05). Chemical composition and physical properties of the essential oils from basil and epazote were not affected by the extraction method (MAE or SD), with similar yielding obtained by both methods (p < 0.05).

  3. Microwave-assisted hydrolysis of polysaccharides over polyoxometalate clusters.

    PubMed

    Tsubaki, Shuntaro; Oono, Kiriyo; Ueda, Tadaharu; Onda, Ayumu; Yanagisawa, Kazumichi; Mitani, Tomohiko; Azuma, Jun-ichi

    2013-09-01

    Polyoxometalate (POM) clusters were utilized as recyclable acid catalysts and microwave-absorbing agents for the microwave-assisted hydrolysis of corn starch and crystalline cellulose. Phosphotungstic (PW) and silicotungstic (SiW) acids showed high hydrolyzing activity, while phosphomolybdic acid (PMo) showed lower glucose stability. The PW catalyst could be recycled by ether extraction at least 4 times without changing its catalytic activity. The addition of PW could reduce the energy demand required for running the hydrolysis by 17-23%. The dielectric property of the aqueous PW solution was important for increasing the microwave-absorption capability of the reaction system and reducing the energy consumption. Copyright © 2013 Elsevier Ltd. All rights reserved.

  4. Microwave-assisted specific chemical digestion for rapid protein identification.

    PubMed

    Hua, Lin; Low, Teck Yew; Sze, Siu Kwan

    2006-01-01

    We have developed a rapid microwave-assisted protein digestion technique based on classic acid hydrolysis reaction with 2% formic acid solution. In this mild chemical environment, proteins are hydrolyzed to peptides, which can be directly analyzed by MALDI-MS or ESI-MS without prior sample purification. Dilute formic acid cleaves proteins specifically at the C-terminal of aspartyl (Asp) residues within 10 min of exposure to microwave irradiation. By adjusting the irradiation time, we found that the extent of protein fragmentation can be controlled, as shown by the single fragmentation of myoglobin at the C-terminal of any of the Asp residues. The efficacy and simplicity of this technique for protein identification are demonstrated by the peptide mass maps of in-gel digested myoglobin and BSA, as well as proteins isolated from Escherichia coli K12 cells.

  5. Microwave-assisted synthesis and characterization of nickel ferrite nanoparticles

    SciTech Connect

    Carpenter, Gopal; Sen, Ravindra; Gupta, Nitish; Malviya, Nitin

    2015-08-28

    Nickel ferrite nanoparticles (NiFe{sub 2}O{sub 4}) were successfully prepared by microwave-assisted combustion method (MWAC) using citric Electron acid as a chelating agent. NiFe{sub 2}O{sub 4} nanoparticles were characterized by X-ray diffraction (XRD) pattern, Scanning Microscopy (SEM), Fourier transform infrared (FTIR) and UV-Visible techniques. XRD analysis revealed that NiFe{sub 2}O{sub 4} nanoparticles have spinel cubic structure with the average crystalline size of 26.38 nm. SEM analysis revealed random and porous structural morphology of particles and FTIR showed absorption bands related to octahedral and tetrahedral sites, in the range 400–600cm{sup −1} which strongly favor the formation of NiFe{sub 2}O{sub 4} nanoparticles. The optical band gap is determined by UV Visible method and found to be 5.4 eV.

  6. Magnetic gold nanotriangles by microwave-assisted polyol synthesis

    SciTech Connect

    Yu, Siming; Hachtel, Jordan A.; Chisholm, Matthew F.; Pantelides, Sokrates T.; Laromaine, Anna; Roig, Anna

    2015-07-21

    Our simple approach to synthesize hybrid nanoparticles with magnetic and plasmonic functionalities, with high control of their shape and avoiding cytotoxic reactants, to target biomedical applications remains a huge challenge. We report a facile, fast and bio-friendly microwave-assisted polyol route for the synthesis of a complex multi-material consisting of monodisperse gold nanotriangles around 280 nm in size uniformly decorated by superparamagnetic iron oxide nanoparticles of 5 nm. Moreover, these nanotriangles are readily dispersible in water, display a strong magnetic response (10 wt% magnetic fraction) and exhibit a localized surface plasmon resonance band in the NIR region (800 nm). Moreover, these hybrid particles can be easily self-assembled at the liquid–air interfaces.

  7. Characterization of novel sulfonium photoacid generators and their microwave-assisted synthesis.

    PubMed

    Yanez, Ciceron O; Andrade, Carolina D; Belfield, Kevin D

    2009-02-21

    Microwave-assisted synthesis of triarylsulfonium salt photoacid generators (PAGs) afforded reaction times 90 to 420 times faster than conventional thermal conditions, with photoacid quantum yields of new sulfonium PAGs ranging from 0.01 to 0.4.

  8. Effects of feedstock characteristics on microwave-assisted pyrolysis - A review.

    PubMed

    Zhang, Yaning; Chen, Paul; Liu, Shiyu; Peng, Peng; Min, Min; Cheng, Yanling; Anderson, Erik; Zhou, Nan; Fan, Liangliang; Liu, Chenghui; Chen, Guo; Liu, Yuhuan; Lei, Hanwu; Li, Bingxi; Ruan, Roger

    2017-04-01

    Microwave-assisted pyrolysis is an important approach to obtain bio-oil from biomass. Similar to conventional electrical heating pyrolysis, microwave-assisted pyrolysis is significantly affected by feedstock characteristics. However, microwave heating has its unique features which strongly depend on the physical and chemical properties of biomass feedstock. In this review, the relationships among heating, bio-oil yield, and feedstock particle size, moisture content, inorganics, and organics in microwave-assisted pyrolysis are discussed and compared with those in conventional electrical heating pyrolysis. The quantitative analysis of data reported in the literature showed a strong contrast between the conventional processes and microwave based processes. Microwave-assisted pyrolysis is a relatively new process with limited research compared with conventional electrical heating pyrolysis. The lack of understanding of some observed results warrant more and in-depth fundamental research. Copyright © 2017 Elsevier Ltd. All rights reserved.

  9. Microwave-assisted extraction of cyclotides from Viola ignobilis.

    PubMed

    Farhadpour, Mohsen; Hashempour, Hossein; Talebpour, Zahra; A-Bagheri, Nazanin; Shushtarian, Mozhgan Sadat; Gruber, Christian W; Ghassempour, Alireza

    2016-03-15

    Cyclotides are an interesting family of circular plant peptides. Their unique three-dimensional structure, comprising a head-to-tail circular backbone chain and three disulfide bonds, confers them stability against thermal, chemical, and enzymatic degradation. Their unique stability under extreme conditions creates an idea about the possibility of using harsh extraction methods such as microwave-assisted extraction (MAE) without affecting their structures. MAE has been introduced as a potent extraction method for extraction of natural compounds, but it is seldom used for peptide and protein extraction. In this work, microwave irradiation was applied to the extraction of cyclotides. The procedure was performed in various steps using a microwave instrument under different conditions. High-performance liquid chromatography (HPLC) and matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) results show stability of cyclotide structures on microwave radiation. The influential parameters, including time, temperature, and the ratio of solvents that are affecting the MAE potency, were optimized. Optimal conditions were obtained at 20 min of irradiation time, 1200 W of system power in 60 °C, and methanol/water at the ratio of 90:10 (v/v) as solvent. The comparison of MAE results with maceration extraction shows that there are similarities between cyclotide sequences and extraction yields.

  10. Microwave-assisted extraction of phenolic antioxidants from potato peels.

    PubMed

    Singh, Ashutosh; Sabally, Kebba; Kubow, Stan; Donnelly, Danielle J; Gariepy, Yvan; Orsat, Valérie; Raghavan, G S V

    2011-03-07

    A response surface method was used to optimize the microwave-assisted extraction parameters such as extraction time (t) (min), solvent (methanol) concentration (S) (v/v) and microwave power level (MP) for extraction of antioxidants from potato peels. Max. total phenolics content of 3.94 mg g⁻¹ dry weight (dw) was obtained at S of 67.33%, t of 15 min and a MP of 14.67%. For ascorbic acid (1.44 mg g⁻¹ dw), caffeic acid (1.33 mg g⁻¹ dw), ferulic acid (0.50 mg g⁻¹ dw) max contents were obtained at S of 100%, t of 15 min, and MP of 10%, while the max chlorogenic acid content (1.35 mg g⁻¹ dw) was obtained at S of 100%, t of 5 min, and MP of 10%. The radical scavenging activity of the extract was evaluated by using the DPPH assay and optimum antioxidant activity was obtained at S of 100%, t of 5 min, and MP of 10%.

  11. Spectrophotometric determination of paracetamol with microwave assisted alkaline hydrolysis

    NASA Astrophysics Data System (ADS)

    Xu, Chunli; Li, Baoxin

    2004-07-01

    A novel and rapid spectrophotometric method for the determination of paracetamol is proposed in this paper. The proposed method is based on the microwave assisted alkaline hydrolysis of paracetamol to p-aminophenol that reacts with S 2- in the presence of Fe 3+ as oxidant to produce a methylene blue-like dye having an absorptivity maximum at 540 nm. The experiment showed that paracetamol could be hydrolysed quantitatively to p-aminophenol in only 1.5 min under radiation power 640 W using a microwave in NaOH medium. The system obeys Beer's law in the range of 0-3.0×10 -4 mol l -1 paracetamol. The molar absorptivity and Sandell's sensitivity were found to be 3.2×10 3 l mol -1 cm -1 and 0.047 μg cm -2, respectively. The relative standard deviation ( n=11) was 1.7% for 8.0×10 -5 mol l -1 paracetamol. The method has been applied successfully to analysis of paracetamol in pharmaceutical preparation.

  12. Fast microwave assisted pyrolysis of biomass using microwave absorbent.

    PubMed

    Borges, Fernanda Cabral; Du, Zhenyi; Xie, Qinglong; Trierweiler, Jorge Otávio; Cheng, Yanling; Wan, Yiqin; Liu, Yuhuan; Zhu, Rongbi; Lin, Xiangyang; Chen, Paul; Ruan, Roger

    2014-03-01

    A novel concept of fast microwave assisted pyrolysis (fMAP) in the presence of microwave absorbents was presented and examined. Wood sawdust and corn stover were pyrolyzed by means of microwave heating and silicon carbide (SiC) as microwave absorbent. The bio-oil was characterized, and the effects of temperature, feedstock loading, particle sizes, and vacuum degree were analyzed. For wood sawdust, a temperature of 480°C, 50 grit SiC, with 2g/min of biomass feeding, were the optimal conditions, with a maximum bio-oil yield of 65 wt.%. For corn stover, temperatures ranging from 490°C to 560°C, biomass particle sizes from 0.9mm to 1.9mm, and vacuum degree lower than 100mmHg obtained a maximum bio-oil yield of 64 wt.%. This study shows that the use of microwave absorbents for fMAP is feasible and a promising technology to improve the practical values and commercial application outlook of microwave based pyrolysis.

  13. Microwave-Assisted Synthesis of Cinnamyl Long Chain Aroma Esters.

    PubMed

    Worzakowska, Marta

    2015-06-08

    Cinnamyl long chain aroma esters were prepared by using the conventional and microwave-assisted methods. The esterification reaction of naturally occurring 3-phenyl-prop-2-en-1-ol and different chain lengths acidic and diol reagents was carried out at the temperature of 140 °C under solvent free conditions. As acidic reagents, oxolane-2,5-dione, oxane-2,6-dione, hexanedioic acid and decanedioic acid were applied. Ethane-1,2-diol and 2,2'-[oxybis(2,1-ethandiyloxy)]diethanol were used as diol reagents. The synthesis of high molecular mass cinnamyl esters under conventional method conditions requires a long time to obtain high yields. The studies confirm that by using microwave irradiation, it is possible to reduce the reaction times to only 10-20 min. The structures of prepared esters were confirmed on the basis of FTIR, 1H-NMR and 13C-NMR. In addition, the newly obtained cinnamyl long chain esters were tested for their thermal properties. The TG studies proved the high thermal resistance of the obtained esters under inert and oxidative conditions.

  14. Novel microwave assisted synthesis of ZnS nanomaterials.

    PubMed

    Synnott, Damian W; Seery, Michael K; Hinder, Steven J; Colreavy, John; Pillai, Suresh C

    2013-02-01

    A novel ambient pressure microwave assisted technique is developed in which silver and indium-modified ZnS is synthesized. The as-prepared ZnS is characterized by x-ray diffraction, UV-vis spectroscopy, x-ray photoelectron spectroscopy and luminescence spectroscopy. This procedure produced crystalline materials with particle sizes below 10 nm. The synthesis technique leads to defects in the crystal which induce mid-energy levels in the band gap and lead to indoor light photocatalytic activity. Increasing the amount of silver causes a phase transition from cubic blende to hexagonal phase ZnS. In a comparative study, when the ZnS cubic blende is heated in a conventional chamber furnace, it is completely converted to ZnO at 600 °C. Both cubic blende and hexagonal ZnS show excellent photocatalytic activity under irradiation from a 60 W light bulb. These ZnS samples also show significantly higher photocatalytic activity than the commercially available TiO(2) (Evonik-Degussa P-25).

  15. Novel microwave assisted synthesis of ZnS nanomaterials

    NASA Astrophysics Data System (ADS)

    Synnott, Damian W.; Seery, Michael K.; Hinder, Steven J.; Colreavy, John; Pillai, Suresh C.

    2013-02-01

    A novel ambient pressure microwave assisted technique is developed in which silver and indium-modified ZnS is synthesized. The as-prepared ZnS is characterized by x-ray diffraction, UV-vis spectroscopy, x-ray photoelectron spectroscopy and luminescence spectroscopy. This procedure produced crystalline materials with particle sizes below 10 nm. The synthesis technique leads to defects in the crystal which induce mid-energy levels in the band gap and lead to indoor light photocatalytic activity. Increasing the amount of silver causes a phase transition from cubic blende to hexagonal phase ZnS. In a comparative study, when the ZnS cubic blende is heated in a conventional chamber furnace, it is completely converted to ZnO at 600 °C. Both cubic blende and hexagonal ZnS show excellent photocatalytic activity under irradiation from a 60 W light bulb. These ZnS samples also show significantly higher photocatalytic activity than the commercially available TiO2 (Evonik-Degussa P-25).

  16. Microwave-assisted hydrodistillation of essential oil from rosemary.

    PubMed

    Karakaya, Sibel; El, Sedef Nehir; Karagozlu, Nural; Sahin, Serpil; Sumnu, Gulum; Bayramoglu, Beste

    2014-06-01

    Effects of microwave assisted hydrodistillation (MAHD) and conventional hydrodistillation (HD) methods on yield, composition, specific gravity, refractive index, and antioxidant and antimicrobial activities of essential oil of Rosmarinus officinalis L were studied. The main aroma compounds of rosemary essential oil were found as 1,8-cineole and camphor. Trolox equivalent antioxidant capacity (TEAC) values for essential oils extracted by MAHD and HD were 1.52 mM/ml oil and 1.95 mM/ml oil, respectively. DPPH radical scavenging activity of the oils obtained by MAHD and HD were found as 60.55% and 51.04% respectively. Inhibitory effects of essential oils obtained by two methods on linoleic acid peroxidation were almost the same. Essential oils obtained by two methods inhibited growth of Esherichia coli O157:H7, Salmonella typhimurium NRRLE 4463 and Listeria monocytogenes Scott A with the same degree. However, inhibitory activity of essential oil obtained by MAHD on Staphylococcus aureus 6538P was stronger than that of obtained by HD (p < 0.05).

  17. Microwave-assisted extraction of lipid from fish waste

    NASA Astrophysics Data System (ADS)

    Rahimi, M. A.; Omar, R.; Ethaib, S.; Siti Mazlina, M. K.; Awang Biak, D. R.; Nor Aisyah, R.

    2017-06-01

    Processing fish waste for extraction of value added products such as protein, lipid, gelatin, amino acids, collagen and oil has become one of the most intriguing researches due to its valuable properties. In this study the extraction of lipid from sardine fish waste was carried out using microwave-assisted extraction (MAE) and compared with Soxhlets and Hara and Radin methods. A mixture of two organic solvents isopropanol/hexane and distilled water were used for MAE and Hara and Radin methods. Meanwhile, Soxhlet method utilized only hexane as solvent. The results show that the higher yield of lipid 80.5 mg/g was achieved using distilled water in MAE method at 10 min extraction time. Soxhlet extraction method only produced 46.6 mg/g of lipid after 4 hours of extraction time. Lowest yield of lipid was found at 15.8 mg/g using Hara and Radin method. Based on aforementioned results, it can be concluded MAE method is superior compared to the Soxhlet and Hara and Radin methods which make it an attractive route to extract lipid from fish waste.

  18. Microwave-assisted extraction of glycyrrhizic acid from licorice root.

    PubMed

    Pan; Liu; Jia; Shu

    2000-07-01

    In the present study, a microwave-assisted extraction (MAE) technique has been developed for the extraction of glycyrrhizic acid (GA) from licorice root. Various experimental conditions, such as extraction time, different ethanol and ammonia concentration, liquid/solid ratios, pre-leaching time before MAE and material size for the MAE procedure were investigated to optimize the efficiency of the extraction. Under appropriate MAE conditions, such as extraction times of 4-5min, ethanol concentrations of 50-60% (v/v), ammonia concentrations of 1-2% (v/v) and liquid/solid ratios of 10:1(ml/g), the recovery of GA from licorice root with MAE was equivalent with conventional extraction methods. Those methods include extraction at room temperature (ERT), the traditional Soxhlet extraction, heat reflux extraction and ultrasonic extraction. Due to the considerable savings in time and solvent, MAE was more effective than the conventional methods. This novel method is suitable for fast extraction of GA from licorice root.

  19. Microwave assisted magnetization switching in Co/Pt multilayer

    SciTech Connect

    Okamoto, S.; Kikuchi, N.; Kitakami, O.; Shimatsu, T.; Aoi, H.

    2011-04-01

    In this study, we have experimentally investigated the microwave assisted magnetization by switching (MAS) on the microstructured Co/Pt multilayer. The sample exhibits the typical magnetization curve peculiar to perpendicular anisotropy films, that is, a steep reversal initiated by nucleation of a reversed domain followed by its subsequent gradual expansion by the domain wall displacement. By applying microwaves with the frequency of GHz order, the nucleation field H{sub n} is significantly reduced at three frequencies. Taking into account the effective anisotropy field of our sample, the first dip of H{sub n} at the lowest frequency probably corresponds to the Kittel mode excitation, and the other two dips at higher frequencies correspond to unidentified excitation modes other than the Kittel mode. Among them, the last dip of H{sub n} at the highest frequency reaches about 1/3 of that without microwave application. These results suggest the existence of more effective excitation modes for MAS than the Kittel mode.

  20. Microwave-assisted polyol synthesis of Cu nanoparticles

    NASA Astrophysics Data System (ADS)

    Blosi, M.; Albonetti, S.; Dondi, M.; Martelli, C.; Baldi, G.

    2011-01-01

    Microwave heating was applied to synthesize copper colloidal nanoparticles by a polyol method that exploits the chelating and reducing power of a polidentate alcohol (diethylenglycol). The synthesis was carried out in the presence of eco-friendly additives such as ascorbic acid (reducing agent) and polyvinylpirrolidone (chelating polymer) to improve the reduction kinetics and sols stability. Prepared suspensions, obtained with very high reaction yield, were stable for months in spite of the high metal concentration. In order to optimize suspensions, synthesis parameters were modified and the effects on particle size, optical properties, and reaction yield were investigated. XRD analysis, scanning transmission electron microscopy (STEM), and DLS measurements confirmed that prepared sols consist of crystalline metallic copper with a diameter ranging from 45 to 130 nm. Surface plasmon resonance (SPR) of Cu nanoparticles was monitored by UV-Vis spectroscopy and showed both a red shift and a band weakening due to nanoparticle diameter increase. Microwave use provides rapid, uniform heating of reagents and solvent, while accelerating the reduction of metal precursors and the nucleation of metal clusters, resulting in monodispersed nanostructures. The proposed microwave-assisted synthesis, also usable in large-scale continuous production, makes process intensification possible.

  1. Microwave-assisted pyrolysis of microalgae for biofuel production.

    PubMed

    Du, Zhenyi; Li, Yecong; Wang, Xiaoquan; Wan, Yiqin; Chen, Qin; Wang, Chenguang; Lin, Xiangyang; Liu, Yuhuan; Chen, Paul; Ruan, Roger

    2011-04-01

    The pyrolysis of Chlorella sp. was carried out in a microwave oven with char as microwave reception enhancer. The results indicated that the maximum bio-oil yield of 28.6% was achieved under the microwave power of 750 W. The bio-oil properties were characterized with elemental, GC-MS, GPC, FTIR, and thermogravimetric analysis. The algal bio-oil had a density of 0.98 kg/L, a viscosity of 61.2 cSt, and a higher heating value (HHV) of 30.7 MJ/kg. The GC-MS results showed that the bio-oils were mainly composed of aliphatic hydrocarbons, aromatic hydrocarbons, phenols, long chain fatty acids and nitrogenated compounds, among which aliphatic and aromatic hydrocarbons (account for 22.18% of the total GC-MS spectrum area) are highly desirable compounds as those in crude oil, gasoline and diesel. The results in this study indicate that fast growing algae are a promising source of feedstock for advanced renewable fuel production via microwave-assisted pyrolysis (MAP).

  2. Saponins: a renewable and biodegradable surfactant from its microwave-assisted extraction to the synthesis of monodisperse lattices.

    PubMed

    Schmitt, C; Grassl, B; Lespes, G; Desbrières, J; Pellerin, V; Reynaud, S; Gigault, J; Hackley, V A

    2014-03-10

    Synthetic surfactants are widely used in emulsion polymerization, but it is increasingly desirable to replace them with naturally derived molecules with a reduced environmental burden. This study demonstrates the use of saponins as biodegradable and renewable surfactants for emulsion polymerization. This chemical has been extracted from soapnuts by microwave assisted extraction and characterized in terms of surfactant properties prior to emulsion polymerization. The results in terms of particle size distribution and morphology control have been compared to those obtained with classical nonionic (NP40) or anionic (SDS) industrial surfactants. Microwave-extracted saponins were able to lead to latexes as stable as standard PS latex, as shown by the CMC and CCC measurements. The saponin-stabilized PS particles have been characterized in terms of particle size and distribution by Dynamic Light Scattering and Asymmetrical Flow Field Flow Fractionation. Monomodal and monodispersed particles ranging from 250 to 480 nm in terms of diameter with a particle size distribution below 1.03 have been synthesized.

  3. Synthesis of sterically hindered ortho-substituted tetraphenylethenes. Electronic effects in the McMurry olefination reaction.

    PubMed

    Chung, Mee-Kyung; Qi, Guizhong; Stryker, Jeffrey M

    2006-03-30

    [reaction: see text] Contrary to literature consensus, the McMurry olefination reaction can be extended to the direct synthesis of sterically encumbered tetrakis(2-substituted) tetraphenylethenes from the corresponding 2,2'-disubstituted benzophenones. The reaction exploits previously unrecognized substrate-based electronic effects that dominate over otherwise controlling steric considerations and provides highly efficient access to derivatives of tetrakis(2-hydroxyphenyl)ethene, a novel preorganized ligand system for polymetallic coordination chemistry and catalysis.

  4. Central composite rotatable design for investigation of microwave-assisted extraction of ginger (Zingiber officinale)

    NASA Astrophysics Data System (ADS)

    Fadzilah, R. Hanum; Sobhana, B. Arianto; Mahfud, M.

    2015-12-01

    Microwave-assisted extraction technique was employed to extract essential oil from ginger. The optimal condition for microwave assisted extraction of ginger were determined by resposnse surface methodology. A central composite rotatable design was applied to evaluate the effects of three independent variables. The variables is were microwave power 400 - 800W as X1, feed solvent ratio of 0.33 -0.467 as X2 and feed size 1 cm, 0.25 cm and less than 0.2 cm as X3. The correlation analysis of mathematical modelling indicated that quadratic polynomial could be employed to optimize microwave assisted extraction of ginger. The optimal conditions to obtain highest yield of essential oil were : microwave power 597,163 W : feed solvent ratio and size of feed less than 0.2 cm.

  5. Novel poly(ethylene oxide)-b-poly(propylene oxide) copolymer-glucose conjugate by the microwave-assisted ring opening of a sugar lactone.

    PubMed

    Glisoni, Romina J; Sosnik, Alejandro

    2014-11-01

    In this work, we investigated for the first time the conjugation of gluconolactone to a poly(ethylene oxide)-poly(propylene oxide) block copolymer by a microwave-assisted ring opening reaction. The glucosylated copolymer was obtained with high yield (90%). A conjugation extent of approximately 100% was achieved within 15 min. The modification reduced the critical micellar concentration and increased the size of the micelles. The agglutination of the modified polymeric micelles by a soluble lectin that binds glucose confirmed the recognizability of the modified nanocarrier. Finally, the solubilization of darunavir, an anti-HIV protease inhibitor, showed a sharp increase of the aqueous solubility from 91 microgram/mL to 14.2 and 18.9 mg/mL for 10% w/v pristine and glucosylated polymeric micelles, respectively. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Microwave-assisted extraction of quercetin and acid degradation of its glycosides in Psidium guajava leaves.

    PubMed

    Huang, Jianlin; Zhang, Zhanxia

    2004-02-01

    Microwave-assisted extraction (MAE) and microwave-assisted hydrolysis (MAAH) were developed for the sample preparation of guava leaves prior to GC determination of quercetin and its glycosides. Ethanol was selected as the solvent. The optimum MAE temperature, particle size, solvent volume and MAE time are 120 degrees C, 40 - 60 mesh, 20 mL and 5 min, respectively; the optimum MAAH temperature and time, HCl concentration, solvent are 100 degrees C, 5 min, 1.2 mol L(-1) HCl and ethanol, respectively.

  7. Comparative Studies between Conventional and Microwave Assisted Extraction for Rice Bran Oil.

    PubMed

    Shukla, Himanshu S; Pratap, Amit

    2017-09-01

    The present work deals with comparison of microwave assisted extraction to that of conventional solvent extraction for the extraction of rice bran oil (RBO); focusing on extraction yield and oil composition. Microwave assisted extraction act as a green process over other method and proved that it is effective method for extraction of oil. The investigation also focuses on the study of functional group and component present in oil. Natural antioxidant component; its activity was confirmed by DPPH assay. The oryzanol content was also determined by measuring the optical density of the sample at 315 nm in n-heptane using UV visible spectrophotometer.

  8. Extraction of Vanadium from Stone Coal by Microwave Assisted Sulfation Roasting

    NASA Astrophysics Data System (ADS)

    Wang, Mingyu; Xian, Pengfei; Wang, Xuewen; Li, Bowen

    2015-02-01

    The extraction of vanadium from stone coal was investigated by microwave-assisted sulfation roasting followed by water leaching. The results showed that this process is an effective method for the extraction of vanadium from stone coal. Microwave-assisted sulfation roasting promotes the reaction of sulfuric acid with vanadium oxides and decreases roasting time. Under optimized conditions (roasting temperature 200°C, heating rate of 10°C/min, 25% sulfuric acid addition, water leaching at 75°C for 1 h, and liquid/solid ratio of 1.5 ml/g), the leaching rate of vanadium reached 92.6%.

  9. Microwave-assisted magnetization reversal in a Co/Pd multilayer with perpendicular magnetic anisotropy

    NASA Astrophysics Data System (ADS)

    Nozaki, Yukio; Narita, Naoyuki; Tanaka, Terumitsu; Matsuyama, Kimihide

    2009-08-01

    Microwave-assisted magnetization reversal in a rectangle of a Co/Pd multilayer with a perpendicular magnetic anisotropy is examined using vector network analyzer ferromagnetic resonance (FMR) spectroscopy. A microwave field is applied along the in-plane direction of the rectangle together with a negative dc easy-axis field smaller than the coercive field. Broadening or splitting of the peak profile in the FMR spectrum suggesting the formation of multidomain structure appears after the microwave field is applied. The dominance of microwave-assisted nucleation of magnetization is supported by the frequency dependence of the probability with which the multidomain structure appears.

  10. Phase Dependence of Microwave-Assisted Switching of a Single Magnetic Nanoparticle

    NASA Astrophysics Data System (ADS)

    Piquerel, R.; Gaier, O.; Bonet, E.; Thirion, C.; Wernsdorfer, W.

    2014-03-01

    Microwave-assisted switching of the magnetization is an efficient way to reduce the magnetic field required to reverse the magnetization of nanostructures. Here, the phase sensitivity of microwave-assisted switching of an individual cobalt nanoparticle is studied using a pump-probe technique. The pump microwave pulse prepares an initial state of the magnetization, and the probe pulse tests its stability against switching. Precession states are established, which are stable against switching. Their basin of attraction is measured and is in qualitative agreement with numerical macrospin calculations. The damping parameter is evaluated using the variable delay pump-probe technique.

  11. The Microwave Assisted Composite Manufacturing and Repair (MACMAR) Project

    NASA Technical Reports Server (NTRS)

    Falker, John; Terrier, Douglas; Clayton, Ronald G.; Worthy, Erica; Sosa, Edward

    2015-01-01

    The inherent microwave property of carbon nanotubes (CNTs) generates the thermal energy required to induce reversible polymerization of the matrix in these self-healing composites. Microwaves will be used to demonstrate advanced composite manufacturing and repair using self-healing composites.

  12. Complex-mediated microwave-assisted synthesis of polyacrylonitrile nanoparticles

    PubMed Central

    Biswal, Trinath; Samal, Ramakanta; Sahoo, Prafulla K

    2010-01-01

    The polymerization of acrylonitrile (AN) is efficiently, easily, and quickly achieved in the presence of trans-[Co(III)en2Cl2]Cl complex in a domestic microwave (MW) oven. MW irradiation notably promoted the polymerization reaction; this phenomenon is ascribed to the acceleration of the initiator, ammonium persulfate (APS), decomposition by microwave irradiation in the presence of [Co(III)en2Cl2]Cl. The conversion of monomer to the polymer was mostly excellent in gram scale. Irradiation at low power and time produced more homogeneous polymers with high molecular weight and low polydispersity when compared with the polymer formed by a conventional heating method. The interaction of reacting components was monitored by UV-visible spectrometer. The average molecular weight was derived by gel permeation chromatography (GPC), viscosity methods, and sound velocity by ultrasonic interferometer. The uniform and reduced molecular size was characterized by transmission electron microscopy, the diameter of polyacrylonitrile nanoparticles (PAN) being in the range 50–115 nm and 40–230 nm in microwave and conventional heating methods respectively. The surface morphology of PAN prepared by MW irradiation was characterized by scanning electron microscope (SEM). From the kinetic results, the rate of polymerization (Rp) was expressed as Rp = [AN]0.63 [APS]0.57 [complex (I)].0.88 PMID:24198473

  13. Complex-mediated microwave-assisted synthesis of polyacrylonitrile nanoparticles.

    PubMed

    Biswal, Trinath; Samal, Ramakanta; Sahoo, Prafulla K

    2010-01-01

    The polymerization of acrylonitrile (AN) is efficiently, easily, and quickly achieved in the presence of trans-[Co(III)en2Cl2]Cl complex in a domestic microwave (MW) oven. MW irradiation notably promoted the polymerization reaction; this phenomenon is ascribed to the acceleration of the initiator, ammonium persulfate (APS), decomposition by microwave irradiation in the presence of [Co(III)en2Cl2]Cl. The conversion of monomer to the polymer was mostly excellent in gram scale. Irradiation at low power and time produced more homogeneous polymers with high molecular weight and low polydispersity when compared with the polymer formed by a conventional heating method. The interaction of reacting components was monitored by UV-visible spectrometer. The average molecular weight was derived by gel permeation chromatography (GPC), viscosity methods, and sound velocity by ultrasonic interferometer. The uniform and reduced molecular size was characterized by transmission electron microscopy, the diameter of polyacrylonitrile nanoparticles (PAN) being in the range 50-115 nm and 40-230 nm in microwave and conventional heating methods respectively. The surface morphology of PAN prepared by MW irradiation was characterized by scanning electron microscope (SEM). From the kinetic results, the rate of polymerization (Rp) was expressed as Rp = [AN](0.63) [APS](0.57) [complex (I)].(0.88.)

  14. 2-Carbaborane-3-phenyl-1H-indoles--synthesis via McMurry reaction and cyclooxygenase (COX) inhibition activity.

    PubMed

    Laube, Markus; Neumann, Wilma; Scholz, Matthias; Lönnecke, Peter; Crews, Brenda; Marnett, Lawrence J; Pietzsch, Jens; Kniess, Torsten; Hey-Hawkins, Evamarie

    2013-02-01

    Cyclooxygenase-2 (COX-2) inhibitors have been the focus of medicinal chemistry efforts for years, and many compounds that exhibit high selectivity and affinity have been developed. As carbaboranes represent interesting pharmacophores as phenyl mimetics in drug development, this paper presents the synthesis of carbaboranyl derivatives of COX-2-selective 2,3-disubstituted indoles. Despite the lability of carbaboranes under reducing conditions, 2-carbaborane-3-phenyl-1H-indoles could be synthesized by McMurry cyclization of the corresponding amides. Whereas the meta-carbaboranyl-substituted derivatives lacked COX inhibitory activity, an ortho-carbaboranyl analogue was active, but showed a selectivity shift toward COX-1.

  15. Microwave assisted total synthesis of a benzothiophene-based new chemical entity (NCE)

    EPA Science Inventory

    Pharmaceutical scientists are required to generate diverse arrays of complex targets in short span of time, which can now be achieved by microwave-assisted organic synthesis. New chemical entities (NCE) can be built in a fraction of the time using this technique. However, there a...

  16. Microwave assisted apatite coating deposition on Ti6Al4V implants.

    PubMed

    Zhou, Huan; Nabiyouni, Maryam; Bhaduri, Sarit B

    2013-10-01

    In this work we report a novel microwave assisted technology to deposit a uniform, ultra-thin apatite coating without any cracks on titanium implants in minutes. This method comprises of conventional biomimetic coating in synergism with microwave irradiation to result in alkaline earth phosphate nucleation. The microwave assisted coating process mainly follows the initial stages of biomimetic coating until the step of the Ca-P nuclei formation. After that, due to microwave irradiation more Ca-P nuclei are formed to cover the whole surface of the implant instead of the growth of deposited Ca-P nuclei to Ca-P globules and coatings. It is interesting to note the doping of Mg(2+) to Ca-P apatite coating can significantly change the properties and performances of as-deposited coatings. The hydrophilicity, physical properties, bioactivity, cell adhesion, and growth capability of as-deposited microwave assisted coatings were investigated. The study shows that this coating technology has great potential in biomedical applications. Additionally, since biomimetic coating can be applied to series of implant materials such as polymer, metals and glass, it is expected this microwave assisted coating technology can also be applied to these materials if they can remains stable at 100 °C, the boiling point of water.

  17. Microwave-assisted maleation of tung oil for bio-based products with versatile applications

    USDA-ARS?s Scientific Manuscript database

    In this work, a simple, “green” and convenient chemical modification of tung oil for maleinized tung oil (TOMA) was developed via microwave-assisted one-step maleation. This modifying process did not involve any solvent, catalyst, or initiator, but demonstrated the most efficiency of functionalizing...

  18. 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...

  19. Microwave-Assisted Synthesis of Mesoporous Nano-Hydroxyapatite Using Surfactant Templates

    EPA Science Inventory

    Mesoporous nano-hydroxyapatite (n-HAP) was expeditiously synthesized using the pseudo sol-gel microwave-assisted protocol (30 min) in the presence of two novel templates, namely sodium lauryl ether sulfate (SLES) and linear alkylbenzenesulfonate (LABS). The cooperative self-assem...

  20. Cd–cysteine precursor nanowire templated microwave-assisted transformation route to CdS nanotubes

    SciTech Connect

    Liu, Xiao-Lin; Zhu, Ying-Jie; Zhang, Qian; Li, Zhi-Feng; Yang, Bin

    2012-12-15

    Graphical abstract: Cadmium sulfide polycrystalline nanotubes have been successfully synthesized by microwave-assisted transformation method using Cd–cysteine precursor nanowires as the source material and template in ethylene glycol at 160 °C or ethanol at 60 °C. Display Omitted Highlights: ► Cd–cysteine precursor nanowires were successfully synthesized in alkaline solution. ► CdS nanotubes were prepared by templated microwave-assisted transformation method. ► CdS nanotubes can well duplicate the size and morphology of precursor nanowires. ► This method has the advantages of the simplicity and low cost. -- Abstract: We report the Cd–cysteine precursor nanowire templated microwave-assisted transformation route to CdS nanotubes. In this method, the Cd–cysteine precursor nanowires are synthesized using CdCl{sub 2}·2.5H{sub 2}O, L-cysteine and ethanolamine in water at room temperature. The Cd–cysteine precursor nanowires are used as the source material and template for the subsequent preparation of CdS nanotubes by a microwave-assisted transformation method using ethylene glycol or ethanol as the solvent. This method has the advantages of the simplicity and low cost, and may be extended to the synthesis of nanotubes of other compounds. The products are characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM).

  1. Microwave-Assisted Organic Synthesis in the Organic Teaching Lab: A Simple, Greener Wittig Reaction

    ERIC Educational Resources Information Center

    Martin, Eric; Kellen-Yuen, Cynthia

    2007-01-01

    A greener, microwave-assisted Wittig reaction has been developed for the second-semester organic teaching laboratory. Utilizing this microwave technique, a variety of styrene derivatives have been successfully synthesized from aromatic aldehydes in good yields (41-68%). The reaction not only occurs under neat reaction conditions, but also employs…

  2. Microwave-Assisted Organic Synthesis in the Organic Teaching Lab: A Simple, Greener Wittig Reaction

    ERIC Educational Resources Information Center

    Martin, Eric; Kellen-Yuen, Cynthia

    2007-01-01

    A greener, microwave-assisted Wittig reaction has been developed for the second-semester organic teaching laboratory. Utilizing this microwave technique, a variety of styrene derivatives have been successfully synthesized from aromatic aldehydes in good yields (41-68%). The reaction not only occurs under neat reaction conditions, but also employs…

  3. MICROWAVE-ASSISTED SYNTHESIS OF NOBLE NANOSTRUCTURES USING BIODEGRADABLE POLYMER CARBOXYMETHYL CELLULOSE

    EPA Science Inventory

    Microwave-assisted synthesis of noble nanostructures (Au, Pt, and Pd) using biodegradable polymer carboxymethyl cellulose (CMC) under microwave irradiation (MW) at 100 0C is reported. The reaction occurs within a few minutes, whereas at room temperature the reaction does not pro...

  4. Microwave-assisted maleation of tung oil for bio-based products

    USDA-ARS?s Scientific Manuscript database

    In this work, a simple, “green” and convenient chemical modification of tung oil for maleinized tung oil (TOMA) was developed via microwave-assisted one-step maleation. This modifying process did not involve any solvent, catalyst, or initiator, but demonstrated the most efficiency of functionalizing...

  5. MICROWAVE-ASSISTED SYNTHESIS OF NOBLE NANOSTRUCTURES USING BIODEGRADABLE POLYMER CARBOXYMETHYL CELLULOSE

    EPA Science Inventory

    Microwave-assisted (MW) synthesis of noble metals such as Au, Pt and Pd is reported using biodegradable polymer carboxymethyl cellulose (CMC) at 100°C within few seconds. The possible reduction entails the coupling of polar hydroxyl units in beta-glucopyranose units with micr...

  6. MICROWAVE ASSISTED PREPARATION OF CYCLIC UREAS FROM DIAMINES IN THE PRESENCE OF ZNO

    EPA Science Inventory

    A microwave-assisted facile method for the preparation of various ureas, cyclic ureas, and urethanes has been developed that affords nearly quantitative yield of products at 120 degrees C (150 W), 71 kPa within 10 min using ZnO as a catalyst. The enhanced selectivity in this rea...

  7. Microwave-assisted liquefaction of rape straw for the production of bio-oils

    Treesearch

    Xing-Yan Huang; Feng Li; Jiu-Long Xie; Cornelis F. De Hoop; Chung-Yun Hse; Jin-Qiu Qi; Hui. Xiao

    2017-01-01

    The acid-catalyzed liquefaction of rape straw in methanol using microwave energy was examined. Conversion yield and energy consumption were evaluated to profile the microwave-assisted liquefaction process. Chemical components of the bio-oils from various liquefaction conditions were identified. A higher reaction temperature was found to be beneficial to obtain higher...

  8. Effect of anatomical characteristics and chemical components on microwave-assisted liquefaction of bamboo wastes

    Treesearch

    JiuLong Xie; XingYan Huang; JinQiu Qi; Chung Hse; Todd Shupe

    2014-01-01

    The epidermis layer waste (ELW) and the inner layer waste (ILW) were removed from Phyllostachys pubescens bamboo, and the anatomical characteristics and chemical components of these wastes were comparatively investigated. Both the ELW and the ILW were subjected to a microwave-assisted liquefaction process to evaluate the relationship between bamboo...

  9. 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...

  10. MICROWAVE-ASSISTED SHAPE-CONTROLLED BULK SYNTHESIS OF NOBLE NANOCRYSTALS AND THEIR CATALYTIC PROPERTIES

    EPA Science Inventory

    Bulk and shape-controlled synthesis of gold (Au) nanostructures with various shapes such as prisms, cubes and hexagons is described that occurs via microwave-assisted spontaneous reduction of noble metal salts using an aqueous solution of α-D-glucose, sucrose and maltose. The exp...

  11. MICROWAVE-ASSISTED SYNTHESIS OF NOBLE NANOSTRUCTURES USING BIODEGRADABLE POLYMER CARBOXYMETHYL CELLULOSE

    EPA Science Inventory

    Microwave-assisted synthesis of noble nanostructures (Au, Pt, and Pd) using biodegradable polymer carboxymethyl cellulose (CMC) under microwave irradiation (MW) at 100 0C is reported. The reaction occurs within a few minutes, whereas at room temperature the reaction does not pro...

  12. Microwave-Assisted Synthesis of Mesoporous Nano-Hydroxyapatite Using Surfactant Templates

    EPA Science Inventory

    Mesoporous nano-hydroxyapatite (n-HAP) was expeditiously synthesized using the pseudo sol-gel microwave-assisted protocol (30 min) in the presence of two novel templates, namely sodium lauryl ether sulfate (SLES) and linear alkylbenzenesulfonate (LABS). The cooperative self-assem...

  13. Global structure of microwave-assisted flash extracted sugar beet pectin

    USDA-ARS?s Scientific Manuscript database

    We have studied the global structure of microwave assisted, flash extracted pectins isolated from fresh sugar beet pulp. The objective was to minimize the disassembly and possibly the degradation of pectin molecules during extraction. We have characterized these pectins by HPSEC with light scatter...

  14. Mathematical Modeling of Microwave-Assisted Convective Heating and Drying of Grapes

    USDA-ARS?s Scientific Manuscript database

    This research studied the processing performance and product quality of Thompson seedless grapes dried using microwave-assisted convective hot air drying as well as the effect of blanching and dipping pretreatments. Two pretreatment methods were compared, dipping into 2% ethyl oleate (V/V) and 5% p...

  15. Influence of solvent type on microwave-assisted liquefaction of bamboo

    Treesearch

    Jiulong Xie; Chung Hse; Todd F. Shupe; Tingxing Hu

    2016-01-01

    Microwave-assisted liquefaction of bamboo in glycerol, polyethylene glycerol (PEG), methanol, ethanol, and water were comparatively investigated by evaluating the temperature-dependence for conversion and liquefied residue characteristics. The conversion for the liquefaction in methanol, ethanol, and water increased with an increase in reaction temperature, while that...

  16. Acceleration of microwave-assisted enzymatic digestion reactions by magnetite beads.

    PubMed

    Chen, Wei-Yu; Chen, Yu-Chie

    2007-03-15

    In this study, we demonstrated that microwave-assisted enzymatic digestion could be greatly accelerated by multifunctional magnetite beads. The acceleration of microwave-assisted enzymatic digestion by the presence of the magnetite beads was attributable to several features of the beads. Their capacity to absorb microwave radiation leads to rapid heating of the beads. Furthermore, their negatively charged functionalities cause adsorption of proteins with opposite charges onto their surfaces by electrostatic interactions, leading to a concentration on the surfaces of the beads of proteins present in trace amounts in the solution. The adsorbed proteins are denatured and hence rendered vulnerable to enzymatic digestion and are digested on the beads. For microwave heating, 30 s was sufficient for carrying out the tryptic digestion of cytochrome c, in the presence of magnetite beads, while 1 min was adequate for tryptic digestion of myoglobin. The digestion products were characterized by MALDI-MS. This rapid enzymatic digestion allowed the entire time for identification of proteins to be greatly reduced. Furthermore, specific proteins present in trace quantities were enriched from the sample on the magnetite beads and could be rapidly isolated from the sample by employing an external magnetic field. These multiple roles of magnetite beads, as the absorber for microwave irradiation, the concentrating probe, and the agent for unfolding proteins, contributed to their capability of accelerating microwave-assisted enzymatic digestion. We also demonstrated that trypsin immobilized magnetite beads were suitable for use in microwave-assisted enzymatic digestion.

  17. MICROWAVE-ASSISTED EXTRACTION OF ORGANIC COMPOUNDS FROM STANDARD REFERENCE SOILS AND SEDIMENTS

    EPA Science Inventory

    As part of an ongoing evaluation of new sample preparation techniques by the U.S. Environmental Protection Agency (EPA), especially those that minimize waste solvents, microwave-assisted extraction (MAE) of organic compounds from solid materials (or "matrices") was evaluated. Six...

  18. MICROWAVE-ASSISTED SHAPE-CONTROLLED BULK SYNTHESIS OF NOBLE NANOCRYSTALS AND THEIR CATALYTIC PROPERTIES

    EPA Science Inventory

    Bulk and shape-controlled synthesis of gold (Au) nanostructures with various shapes such as prisms, cubes and hexagons is described that occurs via microwave-assisted spontaneous reduction of noble metal salts using an aqueous solution of α-D-glucose, sucrose and maltose. The exp...

  19. Microwave-assisted functionalization of carbon nanohorns via [2+1] nitrenes cycloaddition.

    PubMed

    Karousis, Nikolaos; Ichihashi, Toshinari; Yudasaka, Masako; Iijima, Sumio; Tagmatarchis, Nikos

    2011-02-07

    The microwave-assisted functionalization of carbon nanohorns (CNHs) via [2+1] nitrenes cycloaddition, providing well dispersible hybrid materials possessing aziridino-rings covalently grafted onto the graphitic network of CNHs, was accomplished, while condensation of hydroxy-functionalized CNHs with thioctic acid, furnishing an endocyclic disulfide bond extended from the aziridino-rings, allowed the stabilization of Au nanoparticles.

  20. Microwave-assisted synthesis of biofunctional and fluorescent silicon nanoparticles using proteins as hydrophilic ligands.

    PubMed

    Zhong, Yiling; Peng, Fei; Wei, Xinpan; Zhou, Yanfeng; Wang, Jie; Jiang, Xiangxu; Su, Yuanyuan; Su, Shao; Lee, Shuit-Tong; He, Yao

    2012-08-20

    Protective shell: A microwave-assisted method allows rapid production of biofunctional and fluorescent silicon nanoparticles (SiNPs), which can be used for cell labeling. Such SiNPs feature excellent aqueous dispersibility, are strongly fluorescent, storable, photostable, stable at different pH values, and biocompatible. The method opens new avenues for designing multifunctional SiNPs and related silicon nanostructures.

  1. Microwave assisted total synthesis of a benzothiophene-based new chemical entity (NCE)

    EPA Science Inventory

    Pharmaceutical scientists are required to generate diverse arrays of complex targets in short span of time, which can now be achieved by microwave-assisted organic synthesis. New chemical entities (NCE) can be built in a fraction of the time using this technique. However, there a...

  2. Microwave-assisted digestion and NaOH treatment of waste-activated sludge to recover phosphorus by crystallizing struvite.

    PubMed

    Wang, Yingcai; Zhang, Tao; Westerhoff, Paul; Jiang, Rongfeng; Ren, Hongqiang; Yang, Yu; Li, Zhen

    2017-05-01

    A number of studies of waste-activated sludge (WAS) pretreatments, aimed at releasing phosphorus (P) from WAS and increasing the amount of P that can be recovered, have been performed. Here, a microwave-assisted digestion and NaOH treatment (MWs & NaOH) coupled crystallizing struvite, to promote the solubilization, transformation, and recovery of P from WAS, is proposed. Microwaves (MWs) can cause cavities to form in WAS, weakening the bonds between extracellular polymeric substances and the solid phase. Irradiating with MWs significantly increased the efficiency at which P was dissolved (i.e. transferred from the solid to the liquid phase) and the efficiency at which organic P was hydrolyzed and transformed into inorganic P when the NaOH treatment was performed. The P solubilization and transformation characteristic achieved in different treatments was examined by scanning electron microscopy and three-dimensional excitation emission matrix analysis. The MWs & NaOH method released 34.20-43.73% of total P from WAS, and 23.48-32.07% of the total P was recovered by crystallizing struvite at pH 9.5 and Mg:P ratio of 1.5:1. It would cost about USD 85-103 per ton of dry WAS to treat WAS using the MWs & NaOH method.

  3. Microwave-Assisted Extraction Followed by Solid-Phase Extraction for the Chromatographic Analysis of Alkaloids in Stephania cepharantha.

    PubMed

    Liu, Ying; Xie, Daotao; Kang, Yun; Wang, Yaqin; Yang, Ping; Guo, Jixian; Huang, Jianming

    2016-04-01

    A procedure involving microwave-assisted extraction (MAE) followed by solid-phase extraction (SPE) was established for the extraction and purification of three bisbenzylisoquinoline alkaloids from Stephania cepharantha, and a reversed-phase high-performance liquid chromatography (HPLC) method was developed for the quantification of the target alkaloids. Chromatographic separation was achieved on a Phenomenex Luna Phenyl-Hexyl column. Prior to the HPLC analysis, the alkaloids were rapidly extracted by an optimized MAE process using 0.01 mol/L hydrochloric acid as the solvent. The MAE extract was subsequently purified by SPE using a cation-exchange polymeric cartridge. The MAE-SPE procedure extracted the three alkaloids with satisfactory recoveries ranging from 100.44 to 102.12%. In comparison with the MAE, Soxhlet and ultrasonic-assisted extractions, the proposed MAE-SPE method showed satisfactory cleanup efficiency. Thus, the validated MAE-SPE-HPLC method is specific, accurate and applicable to the determination of alkaloids in S. cepharantha.

  4. Microwave-Assisted Extraction Followed by Solid-Phase Extraction for the Chromatographic Analysis of Alkaloids in Stephania cepharantha

    PubMed Central

    Liu, Ying; Xie, Daotao; Kang, Yun; Wang, Yaqin; Yang, Ping; Guo, Jixian; Huang, Jianming

    2016-01-01

    A procedure involving microwave-assisted extraction (MAE) followed by solid-phase extraction (SPE) was established for the extraction and purification of three bisbenzylisoquinoline alkaloids from Stephania cepharantha, and a reversed-phase high-performance liquid chromatography (HPLC) method was developed for the quantification of the target alkaloids. Chromatographic separation was achieved on a Phenomenex Luna Phenyl-Hexyl column. Prior to the HPLC analysis, the alkaloids were rapidly extracted by an optimized MAE process using 0.01 mol/L hydrochloric acid as the solvent. The MAE extract was subsequently purified by SPE using a cation-exchange polymeric cartridge. The MAE–SPE procedure extracted the three alkaloids with satisfactory recoveries ranging from 100.44 to 102.12%. In comparison with the MAE, Soxhlet and ultrasonic-assisted extractions, the proposed MAE–SPE method showed satisfactory cleanup efficiency. Thus, the validated MAE–SPE–HPLC method is specific, accurate and applicable to the determination of alkaloids in S. cepharantha. PMID:26759486

  5. Rapid microwave-assisted synthesis of molecularly imprinted polymers on carbon quantum dots for fluorescent sensing of tetracycline in milk.

    PubMed

    Hou, Juan; Li, Huiyu; Wang, Long; Zhang, Ping; Zhou, Tianyu; Ding, Hong; Ding, Lan

    2016-01-01

    In this paper, a novel, selective and eco-friendly sensor for the detection of tetracycline was developed by grafting imprinted polymers onto the surface of carbon quantum dots. A simple microwave-assisted approach was utilized to fabricate the fluorescent imprinted composites rapidly for the first time, which could shorten the polymerization time and simplify the experimental procedure dramatically. The novel composites not only demonstrated excellent fluorescence stability and special binding sites, but also could selectively accumulate target analytes. Under optimal conditions, the relative fluorescence intensity of the composites decreased linearly with increasing the concentration of tetracycline from 20 nM to 14 µM. The detection limit of tetracycline was 5.48 nM. The precision and reproducibility of the proposed sensor were also acceptable. Significantly, the practicality of this ultrasensitive sensor for tetracycline detection in milk was further validated, revealing the advantages of simplicity, sensitivity, selectivity and low cost. This approach combines the high selective adsorption property of molecular imprinted polymers and the sensitivity of fluorescence detection. It is envisioned that the development of fluorescent molecularly imprinted composites will offer a new way of thinking for rapid analysis in complex samples.

  6. An evaluation of microwave-assisted fusion and microwave-assisted acid digestion methods for determining elemental impurities in carbon nanostructures using inductively coupled plasma optical emission spectrometry.

    PubMed

    Patole, Shashikant P; Simões, Filipa; Yapici, Tahir F; Warsama, Bashir H; Anjum, Dalaver H; Costa, Pedro M F J

    2016-02-01

    It is common for as-prepared carbon nanotube (CNT) and graphene samples to contain remnants of the transition metals used to catalyze their growth; contamination may also leave other trace elemental impurities in the samples. Although a full quantification of impurities in as-prepared samples of carbon nanostructures is difficult, particularly when trace elements are intercalated or encapsulated within a protective layer of graphitic carbon, reliable information is essential for reasons such as quantifying the adulteration of physico-chemical properties of the materials and for evaluating environmental issues. Here, we introduce a microwave-based fusion method to degrade single- and double-walled CNTs and graphene nanoplatelets into a fusion flux thereby thoroughly leaching all metallic impurities. Subsequent dissolution of the fusion product in diluted hydrochloric and nitric acid allowed us to identify their trace elemental impurities using inductively coupled plasma optical emission spectrometry. Comparisons of the results from the proposed microwave-assisted fusion method against those of a more classical microwave-assisted acid digestion approach suggest complementarity between the two that ultimately could lead to a more reliable and less costly determination of trace elemental impurities in carbon nanostructured materials. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Microwave-assisted Facile and Ultrafast Growth of ZnO Nanostructures and Proposition of Alternative Microwave-assisted Methods to Address Growth Stoppage.

    PubMed

    Rana, Abu Ul Hassan Sarwar; Kang, Mingi; Kim, Hyun-Seok

    2016-04-22

    The time constraint in the growth of ZnO nanostructures when using a hydrothermal method is of paramount importance in contemporary research, where a long fabrication time rots the very essence of the research on ZnO nanostructures. In this study, we present the facile and ultrafast growth of ZnO nanostructures in a domestic microwave oven within a pressurized environment in just a few minutes. This method is preferred for the conventional solution-based method because of the ultrafast supersaturation of zinc salts and the fabrication of high-quality nanostructures. The study of the effect of seed layer density, growth time, and the solution's molar concentration on the morphology, alignment, density, and aspect ratio of ZnO nanorods (ZNRs) is explored. It is found in a microwave-assisted direct growth method that ~5 mins is the optimum time beyond which homogeneous nucleation supersedes heterogeneous nucleation, which results in the growth stoppage of ZNRs. To deal with this issue, we propound different methods such as microwave-assisted solution-replacement, preheating, and PEI-based growth methods, where growth stoppage is addressed and ZNRs with a high aspect ratio can be grown. Furthermore, high-quality ZnO nanoflowers and ZnO nanowalls are fabricated via ammonium hydroxide treatment in a very short time.

  8. Microwave-assisted Facile and Ultrafast Growth of ZnO Nanostructures and Proposition of Alternative Microwave-assisted Methods to Address Growth Stoppage

    PubMed Central

    Rana, Abu ul Hassan Sarwar; Kang, Mingi; Kim, Hyun-Seok

    2016-01-01

    The time constraint in the growth of ZnO nanostructures when using a hydrothermal method is of paramount importance in contemporary research, where a long fabrication time rots the very essence of the research on ZnO nanostructures. In this study, we present the facile and ultrafast growth of ZnO nanostructures in a domestic microwave oven within a pressurized environment in just a few minutes. This method is preferred for the conventional solution-based method because of the ultrafast supersaturation of zinc salts and the fabrication of high-quality nanostructures. The study of the effect of seed layer density, growth time, and the solution’s molar concentration on the morphology, alignment, density, and aspect ratio of ZnO nanorods (ZNRs) is explored. It is found in a microwave-assisted direct growth method that ~5 mins is the optimum time beyond which homogeneous nucleation supersedes heterogeneous nucleation, which results in the growth stoppage of ZNRs. To deal with this issue, we propound different methods such as microwave-assisted solution-replacement, preheating, and PEI-based growth methods, where growth stoppage is addressed and ZNRs with a high aspect ratio can be grown. Furthermore, high-quality ZnO nanoflowers and ZnO nanowalls are fabricated via ammonium hydroxide treatment in a very short time. PMID:27103612

  9. Microwave-assisted Facile and Ultrafast Growth of ZnO Nanostructures and Proposition of Alternative Microwave-assisted Methods to Address Growth Stoppage

    NASA Astrophysics Data System (ADS)

    Rana, Abu Ul Hassan Sarwar; Kang, Mingi; Kim, Hyun-Seok

    2016-04-01

    The time constraint in the growth of ZnO nanostructures when using a hydrothermal method is of paramount importance in contemporary research, where a long fabrication time rots the very essence of the research on ZnO nanostructures. In this study, we present the facile and ultrafast growth of ZnO nanostructures in a domestic microwave oven within a pressurized environment in just a few minutes. This method is preferred for the conventional solution-based method because of the ultrafast supersaturation of zinc salts and the fabrication of high-quality nanostructures. The study of the effect of seed layer density, growth time, and the solution’s molar concentration on the morphology, alignment, density, and aspect ratio of ZnO nanorods (ZNRs) is explored. It is found in a microwave-assisted direct growth method that ~5 mins is the optimum time beyond which homogeneous nucleation supersedes heterogeneous nucleation, which results in the growth stoppage of ZNRs. To deal with this issue, we propound different methods such as microwave-assisted solution-replacement, preheating, and PEI-based growth methods, where growth stoppage is addressed and ZNRs with a high aspect ratio can be grown. Furthermore, high-quality ZnO nanoflowers and ZnO nanowalls are fabricated via ammonium hydroxide treatment in a very short time.

  10. Comparison of microwave-assisted and conventional extraction of mangiferin from mango (Mangifera indica L.) leaves.

    PubMed

    Zou, Tangbin; Wu, Hongfu; Li, Huawen; Jia, Qing; Song, Gang

    2013-10-01

    Mangiferin is the main bioactive component in mango leaves, which possesses anti-inflammatory, antioxidative, antidiabetic, immunomodulatory, and antitumor activities. In the present study, a microwave-assisted extraction method was developed for the extraction of mangiferin from mango leaves. Some parameters such as ethanol concentration, liquid-to-solid ratio, microwave power, and extraction time were optimized by single-factor experiments and response surface methodology. The optimal extraction conditions were 45% ethanol, liquid-to-solid ratio of 30:1 (mL/g), and extraction time of 123 s under microwave irradiation of 474 W. Under optimal conditions, the yield of mangiferin was 36.10 ± 0.72 mg/g, significantly higher than that of conventional extraction. The results obtained are beneficial for the full utilization of mango leaves and also indicate that microwave-assisted extraction is a very useful method for extracting mangiferin from plant materials.

  11. Application of Ionic Liquids in the Microwave-Assisted Extraction of Pectin from Lemon Peels

    PubMed Central

    Guolin, Huang; Jeffrey, Shi; Kai, Zhang; Xiaolan, Huang

    2012-01-01

    Microwave-assisted extraction of pectin from lemon peels by using ionic liquid as alternative solvent was investigated. The extracted pectin was detected by Fourier transform infrared spectra. The extraction conditions were optimized through the different experiments in conjunction with the response surface methodology. A pectin yield of 24.68 % was obtained under the optimal parameters: the extraction temperature of 88°C, the extraction time of 9.6 min, and a liquid-solid ratio of 22.7 ml · g−1. The structure of the pretreated lemon peel samples and the samples after microwave-assisted extraction were characterized by a field emission scanning electron microscope. PMID:22567554

  12. Efficient rapid microwave-assisted route to synthesize InP micrometer hollow spheres

    SciTech Connect

    Zheng Xiuwen Hu Qitu; Sun Chuansheng

    2009-01-08

    The efficiencies of two methods of synthesizing InP micro-scale hollow spheres are compared via the analogous solution-liquid-solid (ASLS) growth mechanism, either through a traditional solvothermal procedure, or via a microwave-assisted method. Scanning electronic microscopy (SEM) images show that most of the as-grown samples are micrometer hollow spheres, which indicates the efficiency of both methods. For traditional solvothermal route, long time (10 h) is necessary to obtain the desired samples, however, for the microwave-assisted route, 30 min is enough for hollow spherical products. An optimal choice of microwave irradiating time allows reducing the reaction time from hours to minutes. The proposed ASLS growth mechanism has also been discussed in detail.

  13. Optimization of microwave-assisted extraction of polysaccharide from Psidium guajava L. fruits.

    PubMed

    Amutha Gnana Arasi, Michael Antony Samy; Gopal Rao, Manchineela; Bagyalakshmi, Janardanan

    2016-10-01

    This study deals with the optimization of microwave assisted extraction of polysaccharide from Psidium guajava L. fruit using Response surface methodology. To evaluate the effect of three independent variables, Water to plant material ratio, microwave power used for extraction and Irradiation time, central composite design has been employed. The yield is considered as dependent variable. The design model estimated the optimum yield of 6.81677% at 200W microwave power level, 3:1 water to plant material ratio and 20min of irradiation time. Three factors three levels Central composite design coupled with RSM was used to model the extraction process. ANOVA was performed to find the significance of the model. The polysaccharide extracted using microwave assisted extraction process was analyzed using FTIR Spectroscopy.

  14. Microwave-assisted synthesis and antioxidant properties of hydrazinyl thiazolyl coumarin derivatives

    PubMed Central

    2012-01-01

    Background Coumarin derivatives exhibit a wide range of biological properties including promising antioxidant activity. Furthermore, microwave-assisted organic synthesis has delivered rapid routes to N- and O-containing heterocycles, including coumarins and thiazoles. Combining these features, the use of microwave-assisted processes will provide rapid access to a targeted coumarin library bearing a hydrazino pharmacophore for evaluation of antioxidant properties Results Microwave irradiation promoted 3 of the 4 steps in a rapid, convergent synthesis of a small library of hydrazinyl thiazolyl coumarin derivatives, all of which exhibited significant antioxidant activity comparable to that of the natural antioxidant quercetin, as established by DPPH and ABTS radical assays Conclusions Microwave dielectric heating provides a rapid and expedient route to a series of hydrazinyl thiazolyl coumarins to investigate their radical scavenging properties. Given their favourable properties, in comparison with known antioxidants, these coumarin derivatives are promising leads for further development and optimization. PMID:22510146

  15. Microwave-assisted fast vapor-phase transport synthesis of MnAPO-5 molecular sieves

    SciTech Connect

    Shao Hui; Yao Jianfeng; Ke Xuebin; Zhang Lixiong Xu Nanping

    2009-04-02

    MnAPO-5 was prepared by a microwave-assisted vapor-phase transport method at 180 deg. C in short times. The products were characterized by X-ray diffraction, scanning electron microscopy, Fourier transform infrared spectra, UV-vis spectroscopic measurement, NH{sub 3}-temperature-programmed desorption and esterification reaction. It was found that dry gels prepared with aluminum isopropoxide, phosphoric acid and manganese acetate could be transferred to MnAPO-5 in the vapors of triethylamine and water by the microwave-assisted vapor-phase transport method at 180 deg. C for less than 30 min. The crystallization time was greatly reduced by the microwave heating compared with the conventional heating. The resulting MnAPO-5 exhibited much smaller particle sizes, higher surface areas and slightly higher catalytic activity in the esterification of acetic acid and butyl alcohol than those prepared by the conventional vapor-phase transport method and hydrothermal synthesis.

  16. Microwave-assisted extraction of green coffee oil and quantification of diterpenes by HPLC.

    PubMed

    Tsukui, A; Santos Júnior, H M; Oigman, S S; de Souza, R O M A; Bizzo, H R; Rezende, C M

    2014-12-01

    The microwave-assisted extraction (MAE) of 13 different green coffee beans (Coffea arabica L.) was compared to Soxhlet extraction for oil obtention. The full factorial design applied to the microwave-assisted extraction (MAE), related to time and temperature parameters, allowed to develop a powerful fast and smooth methodology (10 min at 45°C) compared to a 4h Soxhlet extraction. The quantification of cafestol and kahweol diterpenes present in the coffee oil was monitored by HPLC/UV and showed satisfactory linearity (R(2)=0.9979), precision (CV 3.7%), recovery (<93%), limit of detection (0.0130 mg/mL), and limit of quantification (0.0406 mg/mL). The space-time yield calculated on the diterpenes content for sample AT1 (Arabica green coffee) showed a six times higher value compared to the traditional Soxhlet method. Copyright © 2014 Elsevier Ltd. All rights reserved.

  17. Building conjugated organic structures on Si(111) surfaces via microwave-assisted Sonogashira coupling.

    PubMed

    Lin, Jui-Ching; Kim, Jun-Hyun; Kellar, Joshua A; Hersam, Mark C; Nguyen, SonBinh T; Bedzyk, Michael J

    2010-03-16

    A novel step-by-step method employing microwave-assisted Sonogashira coupling is developed to grow fully conjugated organosilicon structures. As the first case study, p-(4-bromophenyl)acetylene is covalently conjugated to a p-(4-iodophenyl)acetylene-derived monolayer on a Si(111) surface. By bridging the two aromatic rings with C[triple bond]C, the pregrown monolayer is structurally extended outward from the Si surface, forming a fully conjugated (p-(4-bromophenylethynyl)phenyl)vinylene film. The film growth process, which reaches 90% yield after 2 h, is characterized thoroughly at each step by using X-ray reflectivity (XRR), X-ray standing waves (XSW), and X-ray fluorescence (XRF). The high yield and short reaction time offered by microwave-assisted surface Sonogashira coupling chemistry make it a promising strategy for functionalizing Si surfaces.

  18. Building Conjugated Organic Structures on Si(111) Surfaces via Microwave-Assisted Sonogashira Coupling

    SciTech Connect

    Lin, Jui-Ching; Kim, Jun-Hyun; Kellar, Joshua A.; Hersam, Mark C.; Nguyen, SonBinh T.; Bedzyk, Michael J.

    2010-08-27

    A novel step-by-step method employing microwave-assisted Sonogashira coupling is developed to grow fully conjugated organosilicon structures. As the first case study, p-(4-bromophenyl)acetylene is covalently conjugated to a p-(4-iodophenyl)acetylene-derived monolayer on a Si(111) surface. By bridging the two aromatic rings with C {triple_bond} C, the pregrown monolayer is structurally extended outward from the Si surface, forming a fully conjugated (p-(4-bromophenylethynyl)phenyl)vinylene film. The film growth process, which reaches 90% yield after 2 h, is characterized thoroughly at each step by using X-ray reflectivity (XRR), X-ray standing waves (XSW), and X-ray fluorescence (XRF). The high yield and short reaction time offered by microwave-assisted surface Sonogashira coupling chemistry make it a promising strategy for functionalizing Si surfaces.

  19. Microwave-Assisted Tissue Preparation for Rapid Fixation, Decalcification, Antigen Retrieval, Cryosectioning, and Immunostaining

    PubMed Central

    2016-01-01

    Microwave irradiation of tissue during fixation and subsequent histochemical staining procedures significantly reduces the time required for incubation in fixation and staining solutions. Minimizing the incubation time in fixative reduces disruption of tissue morphology, and reducing the incubation time in staining solution or antibody solution decreases nonspecific labeling. Reduction of incubation time in staining solution also decreases the level of background noise. Microwave-assisted tissue preparation is applicable for tissue fixation, decalcification of bone tissues, treatment of adipose tissues, antigen retrieval, and other special staining of tissues. Microwave-assisted tissue fixation and staining are useful tools for histological analyses. This review describes the protocols using microwave irradiation for several essential procedures in histochemical studies, and these techniques are applicable to other protocols for tissue fixation and immunostaining in the field of cell biology. PMID:27840640

  20. Microwave-assisted step reduced extraction of seaweed (Gelidiella aceroso) cellulose nanocrystals.

    PubMed

    Singh, Suman; Gaikwad, Kirtiraj K; Park, Su-Il; Lee, Youn Suk

    2017-06-01

    In the present work, cellulose nanocrystals were isolated from seaweed by microwave-assisted alkali treatment, bleaching, and an acid hydrolysis process. Microwave-assisted alkali treatment reduces the heating time and eliminates the traditional dewaxing process. This is different from the commonly adopted procedure for cellulose nanocrystal (CNC) synthesis, in which CNC synthesis generally follows the dewaxing process. Further, samples obtained after each stage of treatment were characterized and final samples were freeze-dried for further characterization. TEM results revealed that isolated CNCs had a 32nm average diameter and an average length of 408nm. FTIR and XRD data showed that after each stage of chemical treatment, no cellulosic components were removed. The adopted method is faster than the previous traditional method used for isolation of CNCs from seaweed fibers. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Microwave-assisted fabrication of strontium doped apatite coating on Ti6Al4V.

    PubMed

    Zhou, Huan; Kong, Shiqin; Pan, Yan; Zhang, Zhiguo; Deng, Linhong

    2015-11-01

    Strontium has been shown to be a beneficial dopant to calcium phosphates when incorporated at nontoxic level. In the present work we studied the possibility of solution derived doping strontium into calcium phosphate coatings on titanium alloy Ti6Al4V based implants by a recently reported microwave-assisted method. By using this method strontium doped calcium phosphate nuclei were deposited to pretreated titanium alloy surface dot by dot to compose a crack-free coating layer. The presence of strontium in solution led to reduced roughness of the coating and finer nucleus size formed. In vitro study found that proliferation and differentiation of osteoblast cells seeded on the coating were influenced by strontium content in coatings, showing an increasing followed by a decreasing behavior with increasing substitution of calcium by strontium. It is suggested that this new microwave-assisted strontium doped calcium phosphate coatings may have great potential in implant modification.

  2. Microwave-assisted pyrolysis of methyl ricinoleate for continuous production of undecylenic acid methyl ester (UAME).

    PubMed

    Nie, Yong; Duan, Ying; Gong, Ruchao; Yu, Shangzhi; Lu, Meizhen; Yu, Fengwen; Ji, Jianbing

    2015-06-01

    Undecylenic acid methyl ester (UAME) was continuously produced from methyl ricinoleate using a microwave-assisted pyrolysis system with atomization feeding. The UAME yield of 77 wt.% was obtained at 500°C using SiC as the microwave absorbent and heating medium. The methyl ricinoleate conversion and UAME yield from microwave-assisted pyrolysis process were higher than those from conventional pyrolysis. The effect of temperature on the pyrolysis process was also investigated. The methyl ricinoleate conversion increased but the cracking liquid yield decreased when the temperature increased from 460°C to 560°C. The maximum UAME yield was obtained at the temperature of 500°C.

  3. Focused microwave-assisted digestion of vegetal materials for the determination of essential mineral nutrients.

    PubMed

    Mingorance, M D

    2002-06-01

    An open focused microwave-assisted digestion procedure has been developed to decompose and dissolve vegetal matrices for subsequent macro- and micronutrients analysis. The parameters of the microwave oven were evaluated using an experimental design. Sulfuric acid (5 mL) and hydrogen peroxide (3 mL) were found to be suitable for quantitative determination of Ca, Cu, Fe, K, Mg, Mn, N, P, and Zn in 0.100-0.500 g of vegetal sample. The precision was better than 6% for all elements at different concentrations. Results for reference and laboratory control materials are in agreement with certified and indicative values. In addition, the sample digest could be used for ICP-OES of all the elements mentioned. The proposed microwave-assisted digestion procedure offers the ability to determine the most important essential plant nutrients in one unique solution by means of analytical techniques usually found in most laboratories.

  4. Digestion completeness of microwave-assisted and conventional trypsin-catalyzed reactions.

    PubMed

    Reddy, P Muralidhar; Hsu, Wan-Yu; Hu, Jun-Fu; Ho, Yen-Peng

    2010-03-01

    Microwave-assisted proteolytic digestion often yields misscleaved peptides, attributed to incomplete hydrolysis reactions between enzymes and substrates. The number of missed cleavages is an important parameter in proteome database searching. This study investigates how various factors affect digestion processes. Optimum conditions for microwave-assisted digestion (50 mM Tris buffer, 30 min at 60 degrees C, and enzyme to protein molar ratio of 1:5) were determined. The digestion products obtained from eight standard proteins were characterized based on matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). Experimental results indicate that the digestion temperature, reaction time, enzyme to substrate ratio, and digestion buffer affect the number of misscleaved peptides and incomplete digestion percentages. Although all protein molecules in a sample could be digested into peptides within a few minutes under microwave irradiation, longer reaction times or methods to maximize the enzyme activity should be considered if digestion completeness is a major concern.

  5. Microwave-assisted oxidative digestion of lignin with hydrogen peroxide for TOC and color removal.

    PubMed

    Ouyang, Xinping; Huang, Xiangzhen; Ruan, Tao; Qiu, Xueqing

    2015-01-01

    Dilute lignin solution was successfully digested into colorless and clarified liquor under microwave-assisted oxidative digestion with hydrogen peroxide. High dosage of hydrogen peroxide is needed to effectively digest lignin, but excessive hydrogen peroxide may lead to recondensation of formed fragments in digested lignin. Microwave irradiation greatly facilitates the oxidative digestion of lignin. Compared with conventional heating technique, microwave-assisted digestion achieves the same or higher digestion rate within a shorter time and/or at lower temperature. After digestion, total organic carbon content of lignin solution decreases by 93.9%, and a small amount of aliphatic alkane, alcohol, acid and ester are formed via the cleavage of aromatic rings as well as the deprivation of side chains in original lignin. This work provides an alternative way to efficiently treat spent pulping liquor.

  6. Microwave-assisted protein staining, destaining, and in-gel/in-solution digestion of proteins.

    PubMed

    Lill, Jennie R; Nesatyy, Victor J

    2012-01-01

    Rapid evolution of state-of-the-art proteomic analyses has encompassed development of high-throughput analytical instrumentation and bioinformatic tools. However, recently, there has been a particular emphasis on increasing the throughput of sample preparation, which has become one of the rate-limiting steps in protein characterization workflows. Researchers have been investigating alternative methods to conventional convection oven incubations to try and reduce sample preparation time for protein characterization. Several protocols have appeared in the literature, which employ microwave irradiation as a tool for the preparation of biological samples for subsequent characterization by a variety of analytical techniques. In this chapter, techniques for microwave-assisted protein staining, destaining, and digestion are described. In general, the application of microwave-assisted technologies resulted in the drastic reduction of overall sample preparation time, though discrepancies in the reproducibility of several published digestion protocols still remain to be clarified.

  7. Time-resolved imaging of pulse-induced magnetization reversal with a microwave assist field

    PubMed Central

    Rao, Siddharth; Rhensius, Jan; Bisig, Andre; Mawass, Mohamad-Assaad; Weigand, Markus; Kläui, Mathias; Bhatia, Charanjit S.; Yang, Hyunsoo

    2015-01-01

    The reversal of the magnetization under the influence of a field pulse has been previously predicted to be an incoherent process with several competing phenomena such as domain wall relaxation, spin wave-mediated instability regions, and vortex-core mediated reversal dynamics. However, there has been no study on the direct observation of the switching process with the aid of a microwave signal input. We report a time-resolved imaging study of magnetization reversal in patterned magnetic structures under the influence of a field pulse with microwave assistance. The microwave frequency is varied to demonstrate the effect of resonant microwave-assisted switching. We observe that the switching process is dominated by spin wave dynamics generated as a result of magnetic instabilities in the structures, and identify the frequencies that are most dominant in magnetization reversal. PMID:26023723

  8. Microwave-assisted extraction versus Soxhlet extraction to determine triterpene acids in olive skins.

    PubMed

    Fernandez-Pastor, Ignacio; Fernandez-Hernandez, Antonia; Perez-Criado, Sergio; Rivas, Francisco; Martinez, Antonio; Garcia-Granados, Andres; Parra, Andres

    2017-03-01

    Microwave-assisted extraction is compared with a more classical technique, Soxhlet extraction, to determine the content of triterpene acids in olive skins. The samples used in their original unmilled state and milled were extracted with ethyl acetate or methanol as solvents. The optimized operating conditions (e.g., amount and type of solvent, and time and temperature of extractions) to attain the better extraction yields have been established. For the identification and quantitation of the target compounds, an ultra high performance liquid chromatography with tandem mass spectrometry method was employed. The best results were achieved using the microwave-assisted extraction technique, which was much faster than the Soxhlet extraction method, and showed higher efficiency in the extraction of the triterpenic acids (oleanolic and maslinic).

  9. Application of Ionic Liquids in the Microwave-Assisted Extraction of Proanthocyanidins from Larix gmelini Bark

    PubMed Central

    Yang, Lei; Sun, Xiaowei; Yang, Fengjian; Zhao, Chunjian; Zhang, Lin; Zu, Yuangang

    2012-01-01

    Ionic liquid based, microwave-assisted extraction (ILMAE) was successfully applied to the extraction of proanthocyanidins from Larix gmelini bark. In this work, in order to evaluate the performance of ionic liquids in the microwave-assisted extraction process, a series of 1-alkyl-3-methylimidazolium ionic liquids with different cations and anions were evaluated for extraction yield, and 1-butyl-3-methylimidazolium bromide was selected as the optimal solvent. In addition, the ILMAE procedure for the proanthocyanidins was optimized and compared with other conventional extraction techniques. Under the optimized conditions, satisfactory extraction yield of the proanthocyanidins was obtained. Relative to other methods, the proposed approach provided higher extraction yield and lower energy consumption. The Larix gmelini bark samples before and after extraction were analyzed by Thermal gravimetric analysis, Fourier-transform infrared spectroscopy and characterized by scanning electron microscopy. The results showed that the ILMAE method is a simple and efficient technique for sample preparation. PMID:22606036

  10. Microwave-assisted Extraction of Alantolactone and Isoalantolactone from Inula helenium

    PubMed Central

    Zhao, Y. M.; Wang, J.; Liu, H. B.; Guo, C. Y.; Zhang, W. M.

    2015-01-01

    Microwave-assisted extraction was used for the extraction of alantolactone and isoalantolactone from Inula helenium. Effects of various experimental factors including ethanol concentration, particle size, microwave radiation time, the ratio of material to liquid and extraction temperature on yield of alantolactone and isoalantolactone were evaluated. The optimal extracting process of the alantolactone and isoalantolactone from the root of the Inula helenium was 1 g plant sample (sifted through 140 mesh) mixed with 15 ml of 80% ethanol solution, microwave radiation 120 s at 50°. Under these optimal conditions, the yield of alantolactone and isoalantolactone was 31.83±2.08 mg/g and 21.25±1.37 mg/g, respectively. Compared with heat reflux extraction, ultrasound-assisted extraction, microwave-assisted extraction was more efficient and timesaving for the extraction of alantolactone and isoalantolactone from Inula helenium. PMID:25767328

  11. Microwave-assisted solid-phase peptide synthesis based on the Fmoc protecting group strategy (CEM).

    PubMed

    Vanier, Grace S

    2013-01-01

    Microwave-assisted peptide synthesis has become one of the most widely used tools by peptide chemists for the synthesis of both routine and difficult peptide sequences. Microwave technology significantly reduces the synthesis time while also improving the quality of the peptides produced. Microwave energy allows most amino acid couplings to be completed in just 5 min. The Fmoc removal can also be accelerated in the microwave decreasing the reaction time from at least 15 min to only 3 min in most cases. Common side reactions such as racemization and aspartimide formation are easily controllable with optimized methods that can be applied routinely. This protocol outlines the detailed procedure for performing both manual and automated microwave-assisted peptide synthesis of two difficult peptide sequences, ACP (65-74) and β-amyloid, in high purity and yield.

  12. MICROWAVE-ASSISTED PREPARATION OF 1-BUTYL-3-METHYLIMIDAZOLIUM TETRACHLOROGALLATE AND ITS CATALYTIC USE IN ACETAL FORMATION UNDER MILD CONDITIONS

    EPA Science Inventory

    1-Butyl-3-methylimidazolium tetrachlorogallate, [bmim][GaCl4], prepared via microwave-assisted protocol, is found to be an active catalyst for the efficient acetalization of aldehydes under mild conditions.

  13. Microwave-assisted Kochetkov amination followed by permanent charge derivatization: a facile strategy for glycomics.

    PubMed

    Liu, Xin; Zhang, Guisen; Chan, Kenneth; Li, Jianjun

    2010-10-21

    We report a simple and rapid microwave-assisted method for the preparation of oligosaccharide-glycosylamines, followed by labelling with tris(2,4,6-trimethoxyphenyl)phosphonium acetic acid N-hydroxysuccinimide ester. The facile strategy introduced a permanent charge at the reducing end of the oligosaccharide. In combination of MALDI-MS, the detection limit for maltoheptaose was as low as 2 fmol μL(-1).

  14. Saffron Samples of Different Origin: An NMR Study of Microwave-Assisted Extracts

    PubMed Central

    Sobolev, Anatoly P.; Carradori, Simone; Capitani, Donatella; Vista, Silvia; Trella, Agata; Marini, Federico; Mannina, Luisa

    2014-01-01

    An NMR analytical protocol is proposed to characterize saffron samples of different geographical origin (Greece, Spain, Hungary, Turkey and Italy). A microwave-assisted extraction procedure was developed to obtain a comparable recovery of metabolites with respect to the ISO specifications, reducing the solvent volume and the extraction time needed. Metabolite profiles of geographically different saffron extracts were compared showing significant differences in the content of some metabolites. PMID:28234327

  15. Synthesis of Amino-Benzothiaoxazepine-1,1-dioxides Utilizing a Microwave-Assisted, SNAr Protocol

    PubMed Central

    Rolfe, Alan; Ullah, Farman; Samarakoon, Thiwanka B.; Kurtz, Ryan D.; Porubsky, Patrick; Neuenswander, Benjamin; Lushington, Gerald H.; Santini, Conrad; Organ, Michael G.; Hanson, Paul R.

    2011-01-01

    The development of a microwave-assisted, intermolecular SNAr protocol for the synthesis of a 126-member benzothiaoxazepine-1,1-dioxide library is reported. Diversification of 12 benzothiaoxazepine-1,1-dioxides was achieved in rapid fashion utilizing a variety of 2° amines and amino alcohols to generate an 80-member library. A second 48-member library was subsequently generated via a two-step alkylation, intermolecular SNAr diversification protocol. PMID:21902243

  16. MCRs reshaped into a switchable microwave-assisted protocol toward 5-aminoimidazoles and dihydrotriazines

    PubMed Central

    Bell, Christan E.; Shaw, Arthur Y.; De Moliner, Fabio; Hulme, Christopher

    2014-01-01

    A tunable microwave-assisted protocol for the synthesis of two biologically relevant families of heterocycles has been designed. Via a simple switch of reaction conditions, the same starting materials can be engaged in either an improved synthesis of the dihydrotriazine scaffold or a novel, first-in-class MCR to render the challenging 5-aminoimidazole nucleus in a single step. An additional first in class MCR is also reported utilizing guanidines to afford 2,5-aminoimidazoles. PMID:24535889

  17. Non-Aqueous Microwave-Assisted Syntheses of Deca- and Hexa-Molybdovanadates.

    PubMed

    Spillane, Samuel; Sharma, Rupali; Zavras, Athanasios; Mulder, Roger; Ohlin, C André; Goerigk, Lars; O'Hair, Richard A J; Ritchie, Chris

    2017-01-16

    We report a new approach for the synthesis of heterohexa- and heterodecametalates via the use of non-aqueous, microwave-assisted reaction conditions. The two novel molybdovanadates have been isolated and characterized in the solid and solution states using single-crystal X-ray diffraction, FT-IR, UV/Vis, multinuclear NMR spectroscopy, and ESI-MS. The relative stabilities of the possible structural isomers were probed using dispersion-corrected DFT calculations for both polyoxometalate systems.

  18. Renewable platform chemicals from directional microwave-assisted liquefaction coupling stepwise extraction of waste biomass

    Treesearch

    Junfeng Feng; Chungyun Hse; Zhongzhi Yang; Kui Wang; Jianchun Jiang; Junming Xu

    2017-01-01

    Directional microwave-assisted liquefaction and stepwise extraction are introduced for producing platform chemicals: aromatics and monosaccharides. When sulfuric acid was used as a catalyst, a 45% monosaccharides yield and a 29% aromatics yield were obtained from bamboo with 0.3 g catalyst per 18 g methanol and 2 g bamboo at 160 °C with 10 min. Approximately 78–86 wt%...

  19. Extraction and characterization of holocellulose fibers by microwave-assisted selective liquefaction of bamboo

    Treesearch

    Jiulong Xie; Chung Hse; Todd F. Shupe; Hui Pan; Tingxing Hu

    2016-01-01

    Microwave-assisted selective liquefaction was proposed and used as a novel method for the isolation of holocellulose fibers. The results showed that the bamboo lignin component and extractives were almost completely removed by using a liquefaction process at 120 8C for 9 min, and the residual lignin and extractives in the solid residue were as low as 0.65% and 0.49%,...

  20. An Efficient, Microwave-Assisted, One-Pot Synthesis of Indoles Under Sonogashira Conditions

    PubMed Central

    Chen, Yu; Markina, Nataliya A.; Larock, Richard C.

    2009-01-01

    A microwave-assisted, one-pot, three-component coupling reaction for the synthesis of indoles has been developed. The reaction is carried out in two steps under standard Sonogashira coupling conditions from an N-substituted/N,N-disubstituted 2-iodoaniline and a terminal alkyne, followed by the addition of acetonitrile and an aryl iodide. A variety of polysubstituted indoles have been prepared in moderate to excellent yields using the present method. PMID:20160894

  1. Literature study of microwave-assisted digestion using electrothermal atomic absorption spectrometry.

    PubMed

    Chakraborty, R; Das, A K; Cervera, M L; De La Guardia, M

    1996-05-01

    The literature on the use of microwave-assisted digestion procedures for subsequent sample analysis by means of electrothermal atomic absorption spectrometry (ETAAS) is reviewed. The literature survey reveals that this digestion technique has been applied mainly for biological materials. The elements most extensively determined by this method are cadmium and lead followed by copper, chromium, nickel and iron. The microwave digestion conditions, ETAAS furnace programmes and analytical details of the developed methodologies have been carefully revised.

  2. Efficient ytterbium triflate catalyzed microwave-assisted synthesis of 3-acylacrylic acid building blocks.

    PubMed

    Tolstoluzhsky, Nikita V; Gorobets, Nikolay Yu; Kolos, Nadezhda N; Desenko, Sergey M

    2008-01-01

    The derivatives of 4-(hetero)aryl-4-oxobut-2-enoic acid are useful as building blocks in the synthesis of biologically active compounds. An efficient general protocol for the synthesis of these building blocks was developed. This method combines microwave assistance and ytterbium triflate catalyst and allows the fast preparation of the target acids starting from different (hetero)aromatic ketones and glyoxylic acid monohydrate giving pure products in 52-75% isolated yields.

  3. Microwave-assisted separation of ionic liquids from aqueous solution of ionic liquids.

    PubMed

    Ha, Sung Ho; Mai, Ngoc Lan; Koo, Yoon-Mo

    2010-12-03

    Microwave-assisted separation has been applied to recover ionic liquid (IL) from its aqueous solution as an efficient method with respect to time and energy compared to the conventional vacuum distillation. Hydrophilic ILs such as 1-butyl-3-methylimidazolium tetrafluoroborate ([Bmim][BF(4)]), 1-butyl-3-methylimidazolium trifluoromethanesulfonate ([Bmim][TfO]) and 1-ethyl-3-methylimidazolium methylsulfate ([Emim][MS]) could be recovered in 6 min from the mixture of ILs and water (1:1, w/w) under microwave irradiation at constant power of 10 W while it took at least 240 min to obtain ILs containing same water content (less than 0.5 wt%) by conventional vacuum oven at 363.15 K with 90 kPa of vacuum pressure. Energy consumptions per gram of evaporated water from the homogeneous mixture of hydrophilic ILs and water (1:1, w/w) by microwave-assisted separation were at least 52 times more efficient than those in conventional vacuum oven. It demonstrated that microwave-assisted separation could be used for complete recovery of ILs in sense of time and energy as well as relevant purity.

  4. Preparation of Silica Nanoparticles Through Microwave-assisted Acid-catalysis

    PubMed Central

    Lovingood, Derek D.; Owens, Jeffrey R.; Seeber, Michael; Kornev, Konstantin G.; Luzinov, Igor

    2013-01-01

    Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle diameters ranging from 30-250 nm by varying the reaction conditions. Through the selection of a microwave compatible solvent, silicic acid precursor, catalyst, and microwave irradiation time, these microwave-assisted methods were capable of overcoming the previously reported shortcomings associated with synthesis of silica nanoparticles using microwave reactors. The siloxane precursor was hydrolyzed using the acid catalyst, HCl. Acetone, a low-tan δ solvent, mediates the condensation reactions and has minimal interaction with the electromagnetic field. Condensation reactions begin when the silicic acid precursor couples with the microwave radiation, leading to silica nanoparticle sol formation. The silica nanoparticles were characterized by dynamic light scattering data and scanning electron microscopy, which show the materials' morphology and size to be dependent on the reaction conditions. Microwave-assisted reactions produce silica nanoparticles with roughened textured surfaces that are atypical for silica sols produced by Stöber's methods, which have smooth surfaces. PMID:24379052

  5. A study of thermal properties of sodium titanate nanotubes synthesized by microwave-assisted hydrothermal method

    SciTech Connect

    Preda, Silviu; Rutar, Melita; Umek, Polona; Zaharescu, Maria

    2015-11-15

    Highlights: • The microwave-assisted hydrothermal route was used for titanate nanotubes synthesis. • Conversion to single-phase nanotube morphology completes after 8 h reaction time. • The nanotube morphology is stable up to 600 °C, as determined by in-situ XRD and SEM. • Sodium ions migrate to the surface due to thermal motion and structure condensation. - Abstract: Sodium titanate nanotubes (NaTiNTs) were synthesized by microwave-assisted hydrothermal treatment of commercial TiO{sub 2}, at constant temperature (135 °C) and different irradiation times (15 min, 1, 4, 8 and 16 h). The products were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, differential scanning calorimetry and specific surface area measurements. The irradiation time turned out to be the key parameter for morphological control of the material. Nanotubes were observed already after 15 min of microwave irradiation. The analyses of the products irradiated for 8 and 16 h confirm the complete transformation of the starting TiO{sub 2} powder to NaTiNTs. The nanotubes are open ended with multi-wall structures, with the average outer diameter of 8 nm and specific surface area up to 210 m{sup 2}/g. The morphology, surface area and crystal structure of the sodium titanate nanotubes synthesized by microwave-assisted hydrothermal method were similar to those obtained by conventional hydrothermal method.

  6. Optimization of microwave-assisted extraction of flavonoids from young barley leaves

    NASA Astrophysics Data System (ADS)

    Gao, Tian; Zhang, Min; Fang, Zhongxiang; Zhong, Qifeng

    2017-01-01

    A central composite design combined with response surface methodology was utilized to optimise microwave-assisted extraction of flavonoids from young barley leaves. The results showed that using water as solvent, the optimum conditions of microwave-assisted extraction were extracted twice at 1.27 W g-1 microwave power and liquid-solid ratio 34.02 ml g-1 for 11.12 min. The maximum extraction yield of flavonoids (rutin equivalents) was 80.78±0.52%. Compared with conventional extraction method, the microwave-assisted extraction was more efficient as the extraction time was only 6.18% of conventional extraction, but the extraction yield of flavonoids was increased by 5.47%. The main flavonoid components from the young barley leaf extract were probably 33.36% of isoorientin-7-O-glueoside and 54.17% of isovitexin-7-O-glucoside, based on the HPLC-MS analysis. The barley leaf extract exhibited strong reducing power as well as the DPPH radical scavenging capacity.

  7. Microwave assisted rapid and complete degradation of atrazine using TiO(2) nanotube photocatalyst suspensions.

    PubMed

    Zhanqi, Gao; Shaogui, Yang; Na, Ta; Cheng, Sun

    2007-07-16

    A technology, microwave-assisted photocatalysis on TiO(2) nanotubes, which can be applied to degrade atrazine rapidly and completely, was investigated. TiO(2) nanotubes were prepared, and confirmed by XRD, TEM and ESR. Microwave-assisted photocatalytic degradation of atrazine in aqueous solution was investigated. The result indicates that atrazine is completely degraded in 5min and the mineralization efficiency is 98.5% in 20min, which is obviously more efficient than that by the traditional photocatalytic degradation methods. It may be attributed to the intense UV radiation generated by electrodeless discharge lamps under microwave irradiation, the increased number of OH, additional defect sites on TiO(2) under the irradiation of microwave and larger specific surface area of TiO(2) nanotubes which could adsorb more organic substances to degrade than TiO(2) nanoparticles. Along with the degradation of atrazine, the concentrations of Cl(-) and NO(3)(-) increase gradually. In 20min [Cl(-)] and [NO(3)(-)] are 3, 27.8mg/L, respectively, which are close to their stoichiometric values. The major intermediates of atrazine were identified by HPLC/MS and possible degradation pathways of atrazine in microwave-assisted photocatalysis on TiO(2) nanotubes were proposed.

  8. Evaluating the potential nonthermal microwave effects of microwave-assisted proteolytic reactions.

    PubMed

    Reddy, P Muralidhar; Huang, Yu-Shan; Chen, Cheng-Tung; Chang, Po-Chi; Ho, Yen-Peng

    2013-03-27

    Microwave-assisted proteolytic digestion methods have evolved into a highly effective approach and serve as an alternative to conventional overnight digestion. This approach typically exploits the unique microwave properties to facilitate the digestion of proteins into their peptides within minutes. Conventional digestion is carried out at 37°C while microwave-assisted digestion requires much higher and sometimes inconsistent temperatures. Thus, this study aims to investigate whether the faster reaction rate is due to the microwave quantum effect or the thermal effect. Quantitative mass spectrometry was used to conduct kinetic analysis of tryptic digestion for several proteins by microwave and conventional heating. The percentages of digestion products relative to internal standards showed no significant difference between microwave and conventional heating conditions at the same digestion temperature. The optimum temperature for tryptic digestion was determined to be 50°C. Furthermore, this study compares the digestion completeness indicators of several proteins under microwave and conventional heating. Again, the values obtained from microwave and conventional heating were similar given identical temperatures. The overall results prove that a nonthermal effect does not exist in microwave-assisted tryptic digestion. Therefore, conventional heating at high temperatures (50°C) can be also used to accelerate digestion reactions.

  9. Processed Meat Protein and Heat-Stable Peptide Marker Identification Using Microwave-Assisted Tryptic Digestion.

    PubMed

    Montowska, Magdalena; Pospiech, Edward

    2016-12-01

    New approaches to rapid examination of proteins and peptides in complex food matrices are of great interest to the community of food scientists. The aim of the study is to examine the influence of microwave irradiation on the acceleration of enzymatic cleavage and enzymatic digestion of denatured proteins in cooked meat of five species (cattle, horse, pig, chicken and turkey) and processed meat products (coarsely minced, smoked, cooked and semi-dried sausages). Severe protein aggregation occurred not only in heated meat under harsh treatment at 190 °C but also in processed meat products. All the protein aggregates were thoroughly hydrolyzed after 1 h of trypsin treatment with short exposure times of 40 and 20 s to microwave irradiation at 138 and 303 W. There were much more missed cleavage sites observed in all microwave-assisted digestions. Despite the incompleteness of microwave-assisted digestion, six unique peptide markers were detected, which allowed unambiguous identification of processed meat derived from the examined species. Although the microwave-assisted tryptic digestion can serve as a tool for rapid and high-throughput protein identification, great caution and pre-evaluation of individual samples is recommended in protein quantitation.

  10. Determination of antioxidant components in rice bran oil extracted by microwave-assisted method.

    PubMed

    Zigoneanu, I G; Williams, L; Xu, Z; Sabliov, C M

    2008-07-01

    Rice bran oil was extracted by microwave-assisted extraction with isopropanol and hexane using a solvent-to-rice bran ratio of 3:1 (w/w). The experiments were done in triplicate at 40, 60, 80, 100, and 120 degrees C with a total extraction time of 15 min/sample. The oil components were separated by normal-phase HPLC and quantified with a fluorescence detector. The radical scavenging capability of the oil was tested with DPPH and was expressed as mumol Trolox Equivalent Antioxidant Activity. The increase in total vitamin E with temperature from 40 to 120 degrees C was 59.63% for isopropanol and 342.01% for hexane. Isopropanol was the best solvent for the extraction of gamma-tocopherol and gamma-tocotrienol as compared with hexane for both microwave-assisted and conventional solvent extraction. Isopropanol was better for oil yield extraction at high temperatures. Samples extracted with isopropanol at 120 degrees C had higher antioxidant activity. No differences in oil yield, total vitamin E, and antioxidant activity of oil was noticed between the two methods (microwave-assisted and solvent extractions), at 40 degrees C. No degradation of alpha-tocopherol was noticed during the process.

  11. Processed Meat Protein and Heat-Stable Peptide Marker Identification Using Microwave-Assisted Tryptic Digestion

    PubMed Central

    Pospiech, Edward

    2016-01-01

    Summary New approaches to rapid examination of proteins and peptides in complex food matrices are of great interest to the community of food scientists. The aim of the study is to examine the influence of microwave irradiation on the acceleration of enzymatic cleavage and enzymatic digestion of denatured proteins in cooked meat of five species (cattle, horse, pig, chicken and turkey) and processed meat products (coarsely minced, smoked, cooked and semi-dried sausages). Severe protein aggregation occurred not only in heated meat under harsh treatment at 190 °C but also in processed meat products. All the protein aggregates were thoroughly hydrolyzed after 1 h of trypsin treatment with short exposure times of 40 and 20 s to microwave irradiation at 138 and 303 W. There were much more missed cleavage sites observed in all microwave-assisted digestions. Despite the incompleteness of microwave-assisted digestion, six unique peptide markers were detected, which allowed unambiguous identification of processed meat derived from the examined species. Although the microwave-assisted tryptic digestion can serve as a tool for rapid and high-throughput protein identification, great caution and pre-evaluation of individual samples is recommended in protein quantitation. PMID:28115907

  12. Preliminary study: kinetics of oil extraction from sandalwood by microwave-assisted hydrodistillation

    NASA Astrophysics Data System (ADS)

    Kusuma, H. S.; Mahfud, M.

    2016-04-01

    Sandalwood and its oil, is one of the oldest known perfume materials and has a long history (more than 4000 years) of use as mentioned in Sanskrit manuscripts. Sandalwood oil plays an important role as an export commodity in many countries and its widely used in the food, perfumery and pharmaceuticals industries. The aim of this study is to know and verify the kinetics and mechanism of microwave-assisted hydrodistillation of sandalwood based on a second-order model. In this study, microwave-assisted hydrodistillation is used to extract essential oils from sandalwood. The extraction was carried out in ten extraction cycles of 15 min to 2.5 hours. The initial extraction rate, the extraction capacity and the second-order extraction rate constant were calculated using the model. Kinetics of oil extraction from sandalwood by microwave-assisted hydrodistillation proved that the extraction process was based on the second-order extraction model as the experimentally done in three different steps. The initial extraction rate, h, was 0.0232 g L-1 min-1, the extraction capacity, C S, was 0.6015 g L-1, the second-order extraction rate constant, k, was 0.0642 L g-1 min-1 and coefficient of determination, R 2, was 0.9597.

  13. The microwave-assisted ionic-liquid method: a promising methodology in nanomaterials.

    PubMed

    Ma, Ming-Guo; Zhu, Jie-Fang; Zhu, Ying-Jie; Sun, Run-Cang

    2014-09-01

    In recent years, the microwave-assisted ionic-liquid method has been accepted as a promising methodology for the preparation of nanomaterials and cellulose-based nanocomposites. Applications of this method in the preparation of cellulose-based nanocomposites comply with the major principles of green chemistry, that is, they use an environmentally friendly method in environmentally preferable solvents to make use of renewable materials. This minireview focuses on the recent development of the synthesis of nanomaterials and cellulose-based nanocomposites by means of the microwave-assisted ionic-liquid method. We first discuss the preparation of nanomaterials including noble metals, metal oxides, complex metal oxides, metal sulfides, and other nanomaterials by means of this method. Then we provide an overview of the synthesis of cellulose-based nanocomposites by using this method. The emphasis is on the synthesis, microstructure, and properties of nanostructured materials obtained through this methodology. Our recent research on nanomaterials and cellulose-based nanocomposites by this rapid method is summarized. In addition, the formation mechanisms involved in the microwave-assisted ionic-liquid synthesis of nanostructured materials are discussed briefly. Finally, the future perspectives of this methodology in the synthesis of nanostructured materials are proposed.

  14. Microwave-assisted organic acid extraction of lignin from bamboo: structure and antioxidant activity investigation.

    PubMed

    Li, Ming-Fei; Sun, Shao-Ni; Xu, Feng; Sun, Run-Cang

    2012-10-01

    Microwave-assisted extraction in organic acid aqueous solution (formic acid/acetic acid/water, 3/5/2, v/v/v) was applied to isolate lignin from bamboo. Additionally, the structural features of the extracted lignins were thoroughly investigated in terms of C₉ formula, molecular weight distribution, FT-IR, (1)H NMR and HSQC spectroscopy. It was found that with an increase in the severity of microwave-assisted extraction, there was an increase of phenolic hydroxyl content in the lignin. In addition, an increase of the severity resulted in a decrease of the bound carbohydrate content as well as molecular weight of the lignin. Antioxidant activity investigation indicated that the radical scavenging index of the extracted lignins (0.35-1.15) was higher than that of BHT (0.29) but lower than that of BHA (3.85). The results suggested that microwave-assisted organic acid extraction provides a promising way to prepare lignin from bamboo with good antioxidant activity for potential application in the food industry. Copyright © 2012 Elsevier Ltd. All rights reserved.

  15. New para-para stilbenophanes: synthesis by McMurry coupling, conformational analysis and inhibition of tubulin polymerisation.

    PubMed

    Álvarez, Raquel; López, Vilmarí; Mateo, Carmen; Medarde, Manuel; Peláez, Rafael

    2011-03-14

    The synthesis of a new family of methoxy-substituted [2.7]- and [2.8]paracyclophanes linked by 3-oxapentamethylene-1,5-dioxy and hexamethylene-1,6-dioxy bridges has been carried out by using the McMurry methodology. Related indole compounds were also synthesised. Olefin-to-diol ratios depended on the bridge length, the structure of the aromatic ring and the reaction conditions. Macrocyclisation, the methoxy substituents and the presence of a rigid indole moiety restricted the conformational equilibria, as observed by NMR spectroscopy and according to theoretical calculations. The synthesised compounds display micromolar tubulin polymerisation inhibitory activity. The conformational implications on the tubulin polymerisation inhibitory activity derived from the macrocyclisation when compared with combretastatins, closely related stilbenes, are also discussed.

  16. 2-Carbaborane-3-phenyl-1H-indoles – Synthesis via McMurry Reaction and COX Inhibition Activity

    PubMed Central

    Neumann, Wilma; Scholz, Matthias; Lönnecke, Peter; Crews, Brenda; Marnett, Lawrence J.; Pietzsch, Jens; Kniess, Torsten

    2013-01-01

    Cyclooxygenase-2 (COX-2) inhibitors have been in the focus of medicinal chemistry for years and many compounds exhibiting high selectivity and affinity were developed. As carbaboranes represent interesting pharmacophores as phenyl mimetics in drug development, this paper presents the synthesis of carbaboranyl derivatives of COX-2-selective 2,3-disubstituted indoles. Despite the lability of carbaboranes under reducing conditions, 2-carbaborane-3-phenyl-1H-indoles could be synthesized by McMurry cyclization of the corresponding amides. While the meta-carbaboranyl-substituted derivatives (3a-c) lacked COX inhibition activity, the ortho-carbaboranyl analog (3d) was active but showed a selectivity shift towards COX-1. PMID:23303738

  17. Temperature-programmed microwave-assisted synthesis of SBA-15 ordered mesoporous silica.

    PubMed

    Celer, Ewa B; Jaroniec, Mietek

    2006-11-08

    The currently available microwave technology permits the development and implementation of a temperature-programmed microwave-assisted synthesis (TPMS) of ordered mesoporous silicas (OMSs). Unlike in previously reported syntheses of OMSs, in which only the final hydrothermal treatment was carried out under microwave irradiation, this work takes advantage of the existing capabilities of modern microwave systems to program the temperature and time for the entire synthesis of these materials. To demonstrate the flexibility of the proposed microwave-assisted synthesis, besides programming two consecutive steps involving initial stirring of the gel at a lower temperature and static hydrothermal treatment at a higher temperature, we explored the possibility of temperature programming of the latter step. A major advantage of microwave technology is the feasibility of temperature and time programming, which has been demonstrated by the synthesis of one of the most popular OMSs, SBA-15, over an unprecedented range of temperatures from 40 to 200 degrees C. Since the synthesis of OMSs has not yet been explored and reported at temperatures exceeding 150 degrees C, this work is focused on the SBA-15 samples prepared at higher temperatures (such as 160, 180, and even 200 degrees C). These SBA-15 samples show better thermal stability than those synthesized at commonly used temperatures either under conventional or microwave conditions. Moreover, a partial decomposition of the template during high-temperature microwave-assisted syntheses does not compromise the formation of well-ordered SBA-15 materials. This study shows that the simplicity and capability of temperature and time programming in TPMS allows one not only to tune the adsorption and structural properties of OMSs but also to easily screen a wide range of conditions in order to optimize and scale-up their preparation as well as to significantly reduce the time of synthesis from days to hours.

  18. Novel microwave-assisted digestion by trypsin-immobilized magnetic nanoparticles for proteomic analysis.

    PubMed

    Lin, Shuang; Yun, Dong; Qi, Dawei; Deng, Chunhui; Li, Yan; Zhang, Xiangmin

    2008-03-01

    In this study, a novel microwave-assisted protein digestion method was developed using trypsin-immobilized magnetic nanoparticles (TIMNs). The magnetic nanoparticles worked as not only substrate for enzyme immobilization, but also excellent microwave irradiation absorber and, thus, improved the efficiency of microwave-assisted digestion greatly. Three standard proteins, bovine serum albumin (BSA), myoglobin, and cytochrome c, were used to optimize the conditions of this novel digestion method. With the optimized conditions, peptide fragments produced in very short time (only 15 s) could be identified successfully by MALDI-TOF-MS. When it was compared to the conventional in-solution digestion (12 h), equivalent or better digestion efficiency was observed. Even when protein quantity was as low as micrograms, this novel digestion method still could digest proteins successfully, while the same samples by conventional in-solution digestion failed. Moreover, with an external magnetic field, the enzyme could be removed easily and reused. It was verified that, after 4 replicate runs, the TIMNs still kept high activity. To further confirm the efficiency of this rapid digestion method for proteome analysis, it was applied to the protein extract of rat liver. Without any preparation and prefractionation processing, the entire proteome digested by TIMNs in 15 s went through LC-ESI-MS/MS direct analysis. The whole shotgun proteomic experiment was finished in only 1 h with the identification of 313 proteins ( p < 0.01). This new application of TIMNs in microwave-assisted protein digestion really opens a route for large-scale proteomic analysis.

  19. Biodiesel Production from Chlorella protothecoides Oil by Microwave-Assisted Transesterification

    PubMed Central

    Gülyurt, Mustafa Ömer; Özçimen, Didem; İnan, Benan

    2016-01-01

    In this study, biodiesel production from microalgal oil by microwave-assisted transesterification was carried out to investigate its efficiency. Transesterification reactions were performed by using Chlorella protothecoides oil as feedstock, methanol, and potassium hydroxide as the catalyst. Methanol:oil ratio, reaction time and catalyst:oil ratio were investigated as process parameters affected methyl ester yield. 9:1 methanol/oil molar ratio, 1.5% KOH catalyst/oil ratio and 10 min were optimum values for the highest fatty acid methyl ester yield. PMID:27110772

  20. Microwave-assisted synthesis and electrochemical evaluation of VO2 (B) nanostructures

    DOE PAGES

    Ashton, Thomas E.; Borras, David Hevia; Iadecola, Antonella; ...

    2015-12-01

    Understanding how intercalation materials change during electrochemical operation is paramount to optimising their behaviour and function and in situ characterisation methods allow us to observe these changes without sample destruction. Here, we first report the improved intercalation properties of bronze phase vanadium dioxide VO2 (B) prepared by a microwave assisted route which exhibits a larger electrochemical capacity (232 mAh g-1) compared to VO2 (B) prepared by a solvothermal route (197 mAh g-1). These electrochemical differences have also been followed using in situ X-ray absorption spectroscopy allowing us to follow oxidation state changes as they occur during battery operation.

  1. Simultaneous phase and morphology controllable synthesis of copper selenide films by microwave-assisted nonaqueous approach

    NASA Astrophysics Data System (ADS)

    Li, Jing; Fa, Wenjun; Li, Yasi; Zhao, Hongxiao; Gao, Yuanhao; Zheng, Zhi

    2013-02-01

    Copper selenide films with different phase and morphology were synthesized on copper substrate through controlling reaction solvent by microwave-assisted nonaqueous approach. The films were characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM). The result showed that the pure films could be obtained using cyclohexyl alcohol or benzyl alcohol as solvent. The cubic Cu2-xSe dendrites were synthesized in cyclohexyl alcohol reaction system and hexagonal CuSe flaky crystals were obtained with benzyl alcohol as solvent.

  2. Microwave-assisted polyol synthesis of carbon nitride dots from folic acid for cell imaging.

    PubMed

    Guan, Weiwei; Gu, Wei; Ye, Ling; Guo, Chenyang; Su, Su; Xu, Pinxiang; Xue, Ming

    2014-01-01

    A green, one-step microwave-assisted polyol synthesis was employed to prepare blue luminescent carbon nitride dots (CNDs) using folic acid molecules as both carbon and nitrogen sources. The as-prepared CNDs had an average size of around 4.51 nm and could be well dispersed in water. Under excitation at 360 nm, the CNDs exhibited a strong blue luminescence and the quantum yield was estimated to be 18.9%, which is greater than that of other reported CNDs. Moreover, the CNDs showed low cytotoxicity and could efficiently label C6 glioma cells, demonstrating their potential in cell imaging.

  3. Microwave assisted organic synthesis (MAOS) of small molecules as potential HIV-1 integrase inhibitors.

    PubMed

    Ferro, Stefania; Grazia, Sara De; De Luca, Laura; Gitto, Rosaria; Faliti, Caterina Elisa; Debyzer, Zeger; Chimirri, Alba

    2011-08-11

    Integrase (IN) represents a clinically validated target for the development of antivirals against human immunodeficiency virus (HIV). In recent years our research group has been engaged in the stucture-function study of this enzyme and in the development of some three-dimensional pharmacophore models which have led to the identification of a large series of potent HIV-1 integrase strand-transfer inhibitors (INSTIs) bearing an indole core. To gain a better understanding of the structure-activity relationships (SARs), herein we report the design and microwave-assisted synthesis of a novel series of 1-H-benzylindole derivatives.

  4. Biodiesel Production from Chlorella protothecoides Oil by Microwave-Assisted Transesterification.

    PubMed

    Gülyurt, Mustafa Ömer; Özçimen, Didem; İnan, Benan

    2016-04-22

    In this study, biodiesel production from microalgal oil by microwave-assisted transesterification was carried out to investigate its efficiency. Transesterification reactions were performed by using Chlorella protothecoides oil as feedstock, methanol, and potassium hydroxide as the catalyst. Methanol:oil ratio, reaction time and catalyst:oil ratio were investigated as process parameters affected methyl ester yield. 9:1 methanol/oil molar ratio, 1.5% KOH catalyst/oil ratio and 10 min were optimum values for the highest fatty acid methyl ester yield.

  5. Microwave-assisted solid-state synthesis of oxide ion conducting stabilized bismuth vanadate phases

    SciTech Connect

    Vaidhyanathan, B.; Balaji, K.; Rao, K.J.

    1998-11-01

    A microwave-assisted method for the preparation of substituted bismuth vanadates has been described. The method consists of starting with the respective oxides mixed in stoichiometric proportions and exposing the mixture to microwaves. Substitution takes place at the vanadium sites and it has been possible to prepare Ag{sup +}-, Mn{sup 4+}-, Ga{sup 3+}-, Y{sup 3+}-, and Ce{sup 4+}-substituted compounds with up to 10% substitution. Mn{sup 4+}- and Ag{sup +}-substituted compounds are found to exhibit better oxygen ion conductivities than any reported so far in the literature.

  6. Microwave-assisted synthesis of II-VI semiconductor micro-and nanoparticles towards sensor applications

    NASA Astrophysics Data System (ADS)

    Majithia, Ravish Yogesh

    Engineering particles at the nanoscale demands a high degree of control over process parameters during synthesis. For nanocrystal synthesis, solution-based techniques typically include application of external convective heat. This process often leads to slow heating and allows decomposition of reagents or products over time. Microwave-assisted heating provides faster, localized heating at the molecular level with near instantaneous control over reaction parameters. In this work, microwave-assisted heating has been applied for the synthesis of II-VI semiconductor nanocrystals namely, ZnO nanopods and CdX (X = Se, Te) quantum dots (QDs). Based on factors such as size, surface functionality and charge, optical properties of such nanomaterials can be tuned for application as sensors. ZnO is a direct bandgap semiconductor (3.37 eV) with a large exciton binding energy (60 meV) leading to photoluminescence (PL) at room temperature. A microwave-assisted hydrothermal approach allows the use of sub-5 nm ZnO zero-dimensional nanoparticles as seeds for generation of multi-legged quasi one-dimensional nanopods via heterogeneous nucleation. ZnO nanopods, having individual leg diameters of 13-15 nm and growing along the [0001] direction, can be synthesized in as little as 20 minutes. ZnO nanopods exhibit a broad defect-related PL spanning the visible range with a peak at ~615 nm. Optical sensing based on changes in intensity of the defect PL in response to external environment (e.g., humidity) is demonstrated in this work. Microwave-assisted synthesis was also used for organometallic synthesis of CdX(ZnS) (X = Se, Te) core(shell) QDs. Optical emission of these QDs can be altered based on their size and can be tailored to specific wavelengths. Further, QDs were incorporated in Enhanced Green-Fluorescent Protein -- Ultrabithorax (EGFP-Ubx) fusion protein for the generation of macroscale composite protein fibers via hierarchal self-assembly. Variations in EGFP- Ubx˙QD composite

  7. Catalyst-free microwave-assisted amination of 2-chloro-5-nitrobenzoic acid.

    PubMed

    Baqi, Younis; Müller, Christa E

    2007-07-20

    The synthesis of N-substituted 5-nitroanthranilic acid derivatives 3a-w was achieved by a new, mild, microwave-assisted, regioselective amination reaction of 5-nitro-2-chlorobenzoic acid (1a) with a diverse range of aliphatic and aromatic amines 2a-w without added solvent or catalyst. Up to >99% isolated yield was obtained within 5-30 min at 80-120 degrees C. The reaction, which is suitable for upscaling, yielded new compounds that are of considerable interest as useful building blocks and as potential drugs.

  8. Portable microwave assisted extraction: An original concept for green analytical chemistry.

    PubMed

    Perino, Sandrine; Petitcolas, Emmanuel; de la Guardia, Miguel; Chemat, Farid

    2013-11-08

    This paper describes a portable microwave assisted extraction apparatus (PMAE) for extraction of bioactive compounds especially essential oils and aromas directly in a crop or in a forest. The developed procedure, based on the concept of green analytical chemistry, is appropriate to obtain direct in-field information about the level of essential oils in natural samples and to illustrate green chemical lesson and research. The efficiency of this experiment was validated for the extraction of essential oil of rosemary directly in a crop and allows obtaining a quantitative information on the content of essential oil, which was similar to that obtained by conventional methods in the laboratory.

  9. Advances in microwave-assisted combinatorial chemistry without polymer-supported reagents.

    PubMed

    Martínez-Palou, Rafael

    2006-08-01

    Combinatorial methodologies have dramatically changed the chemical research and discovery process, offering an unlimited source of new molecule entities to be screened for activity. The application of microwave irradiation in Combinatorial Chemistry and high-throughput synthesis has become increasingly popular. By taking advantage of this energy source, compound libraries for lead generation can be assembled in a fraction of time required by conventional thermal heating. This review focuses on the advances in developing synthetic methodologies in microwave without polymer-supported reagents suitable for combinatorial chemistry, including the advances in microwave-assisted fluorous synthesis technology.

  10. A general microwave-assisted two-phase strategy for nanocrystals synthesis.

    PubMed

    Li, Yizhao; Yang, Chao; Ge, Jianhua; Sun, Chao; Wang, Jide; Su, Xintai

    2013-10-01

    A general microwave-assisted two-phase strategy (MTS) has been developed for the synthesis of monodisperse inorganic nanocrystals (NCs). A series of metal oxides, ferrite, hydroxides, and metal sulfide NCs were synthesized by using water-soluble metal salts. The obtained NCs were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The composition, size, and shape of the NCs can be tuned by the types of precursors, the concentrations of metal ions, and the species of ligands. This protocol creates a new synthetic route, which may also be further extended to synthesize other nanomaterials, including alloy, noble metal, rare-earth fluorescent, etc.

  11. TiO2 synthesized by microwave assisted solvothermal method: Experimental and theoretical evaluation

    NASA Astrophysics Data System (ADS)

    Moura, K. F.; Maul, J.; Albuquerque, A. R.; Casali, G. P.; Longo, E.; Keyson, D.; Souza, A. G.; Sambrano, J. R.; Santos, I. M. G.

    2014-02-01

    In this study, a microwave assisted solvothermal method was used to synthesize TiO2 with anatase structure. The synthesis was done using Ti (IV) isopropoxide and ethanol without templates or alkalinizing agents. Changes in structural features were observed with increasing time of synthesis and evaluated using periodic quantum chemical calculations. The anatase phase was obtained after only 1 min of reaction besides a small amount of brookite phase. Experimental Raman spectra are in accordance with the theoretical one. Micrometric spheres constituted by nanometric particles were obtained for synthesis from 1 to 30 min, while spheres and sticks were observed after 60 min.

  12. Carbohydrate Conjugation through Microwave-Assisted Functionalization of Single-Walled Carbon Nanotubes Using Perfluorophenyl Azides

    PubMed Central

    Kong, Na; Shimpi, Manishkumar R.; Park, Jae Hyeung

    2015-01-01

    Carbohydrate-functionalized single-walled carbon nanotubes (SWNTs) were synthesized using microwave-assisted reaction of perfluorophenyl azide with the nanotubes. The results showed that microwave radiation provides a rapid and effective means to covalently attach carbohydrates to SWNTs, producing carbohydrate-SWNT conjugates for biorecognition. The carbohydrate-functionalized SWNTs were furthermore shown to interact specifically with cognate carbohydrate-specific proteins (lectins), resulting in predicted recognition patterns. The carbohydrate-presenting SWNTs constitute a new platform for sensitive protein- or cell recognition, which pave the way for glycoconjugated carbon nanomaterials in biorecognition applications. PMID:25746392

  13. From lignocellulosic biomass to lactic- and glycolic-acid oligomers: a gram-scale microwave-assisted protocol.

    PubMed

    Carnaroglio, Diego; Tabasso, Silvia; Kwasek, Beata; Bogdal, Dariusz; Gaudino, Emanuela Calcio; Cravotto, Giancarlo

    2015-04-24

    The conversion of lignocellulosic biomass into platform chemicals is the key step in the valorization of agricultural waste. Of the biomass-derived platform chemicals currently produced, lactic acid plays a particularly pivotal role in modern biorefineries as it is a versatile commodity chemical and building block for the synthesis of biodegradable polymers. Microwave-assisted processes that furnish lactic acid avoid harsh depolymerization conditions while cutting down reaction time and energy consumption. We herein report a flash catalytic conversion (2 min) of lignocellulosic biomass into lactic and glycolic acids under microwave irradiation. The batch procedure was successfully adapted to a microwave-assisted flow process (35 mL min(-1) ), with the aim of designing a scalable process with higher productivity. The C2 and C4 units recovered from the depolymerization were directly used as the starting material for a solvent and catalyst-free microwave-assisted polycondensation that afforded oligomers in good yields.

  14. Green microwave-assisted synthesis of cellulose/calcium silicate nanocomposites in ionic liquids and recycled ionic liquids.

    PubMed

    Jia, Ning; Li, Shu-Ming; Ma, Ming-Guo; Sun, Run-Cang; Zhu, Lei

    2011-12-27

    Fabrication of biomass materials by a microwave-assisted method in ionic liquids allows the high value-added applications of biomass by combining three major green chemistry principles: using environmentally preferable solvents, using an environmentally friendly method, and making use of renewable biomass materials. Herein, we report a rapid and green microwave-assisted method for the synthesis of the cellulose/calcium silicate nanocomposites in ionic liquids and recycled ionic liquids. These calcium silicate nanoparticles or nanosheets as prepared were homogeneously dispersed in the cellulose matrix. The experimental results confirm that the ionic liquids can be used repeatedly. Of course, the slight differences were also observed using ionic liquids and recycled ionic liquids. Compared with other conventional methods, the rapid, green, and environmentally friendly microwave-assisted method in ionic liquids opens a new window to the high value-added applications of biomass.

  15. Mono-amine functionalized phthalocyanines: microwave-assisted solid-phase synthesis and bioconjugation strategies.

    PubMed

    Erdem, S Sibel; Nesterova, Irina V; Soper, Steven A; Hammer, Robert P

    2009-12-18

    Phthalocyanines (Pcs) are excellent candidates for use as fluors for near-infrared (near-IR) fluorescent tagging of biomolecules for a wide variety of bioanalytical applications. Monofunctionalized Pcs, having two different types of peripheral substitutents, one for covalent conjugation of the Pc to biomolecules and others to improve the solubility of the macrocycle, are ideally suited for the desired applications. To date, difficulties faced during the purification of monofunctionalized Pcs limited their usage in various types of applications. Herein are reported a new synthetic method for rapid synthesis of the target Pcs and bioconjugation techniques for labeling of the oligonucleotides with the near-IR fluors. A novel synthetic route was developed utilizing a hydrophilic, poly(ethylene glycol) (PEG)-based support with an acid-labile Rink Amide linker. The Pcs were functionalized with an amine group for covalent conjugation purposes and were decorated with short PEG chains, serving as solubilizing groups. Microwave-assisted solid-phase synthetic method was successfully applied to obtain pure asymmetrically substituted monoamine functionalized Pcs in a short period of time. Three different bioconjugation techniques, reductive amination, amidation, and Huisgen cycloaddition, were employed for covalent conjugation of Pcs to oligonucleotides. The described microwave-assisted bioconjugation methods give an opportunity to synthesize and isolate the Pc-oligonucleotide conjugate in a few hours.

  16. TiO{sub 2} synthesized by microwave assisted solvothermal method: Experimental and theoretical evaluation

    SciTech Connect

    Moura, K.F.; Maul, J.; Albuquerque, A.R.; Casali, G.P.

    2014-02-15

    In this study, a microwave assisted solvothermal method was used to synthesize TiO{sub 2} with anatase structure. The synthesis was done using Ti (IV) isopropoxide and ethanol without templates or alkalinizing agents. Changes in structural features were observed with increasing time of synthesis and evaluated using periodic quantum chemical calculations. The anatase phase was obtained after only 1 min of reaction besides a small amount of brookite phase. Experimental Raman spectra are in accordance with the theoretical one. Micrometric spheres constituted by nanometric particles were obtained for synthesis from 1 to 30 min, while spheres and sticks were observed after 60 min. - Graphical abstract: FE-SEM images of anatase obtained with different periods of synthesis associated with the order–disorder degree. Display Omitted - Highlights: • Anatase microspheres were obtained by the microwave assisted hydrothermal method. • Only ethanol and titanium isopropoxide were used as precursors during the synthesis. • Raman spectra and XRD patterns were compared with quantum chemical calculations. • Time of synthesis increased the short-range disorder in one direction and decreased in another.

  17. Microwave-assisted low temperature synthesis of wurtzite ZnS quantum dots

    SciTech Connect

    Shahid, Robina; Toprak, Muhammet S.; Muhammed, Mamoun

    2012-03-15

    In this work we report, for the first time, on microwave assisted synthesis of wurtzite ZnS quantum dots (QDs) in controlled reaction at temperature as low as 150 Degree-Sign C. The synthesis can be done in different microwave absorbing solvents with multisource or single source precursors. The QDs are less than 3 nm in size as characterized by transmission electron microscopy (TEM) using selected area electron diffraction (SAED) patterns to confirm the wurtzite phase of ZnS QDs. The optical properties were investigated by UV-Vis absorption which shows blue shift in absorption compared to bulk wurtzite ZnS due to quantum confinement effects. The photoluminescence (PL) spectra of QDs reveal point defects related emission of ZnS QDs. - Graphical abstract: Microwave assisted synthesis of wurtzite ZnS quantum dots (QDs) have been achieved in controlled reaction at temperature as low as 150 Degree-Sign C. The synthesis was performed in different microwave absorbing solvents with multisource or single source precursors for very short reaction periods due to effective heating with microwaves. Highlights: Black-Right-Pointing-Pointer Wurtzite a high temperature phase of ZnS was synthesized at low temperature. Black-Right-Pointing-Pointer Low temperature synthesis was possible because of the use of microwave absorbing solvents. Black-Right-Pointing-Pointer Capping agent was used to control the size of Quantum Dots. Black-Right-Pointing-Pointer Two different systems were developed using single molecular precursor and multisource precursors.

  18. Extraction of dihydroquercetin from Larix gmelinii with ultrasound-assisted and microwave-assisted alternant digestion.

    PubMed

    Ma, Chunhui; Yang, Lei; Wang, Wenjie; Yang, Fengjian; Zhao, Chunjian; Zu, Yuangang

    2012-01-01

    An ultrasound and microwave assisted alternant extraction method (UMAE) was applied for extracting dihydroquercetin (DHQ) from Larix gmelinii wood. This investigation was conducted using 60% ethanol as solvent, 1:12 solid to liquid ratio, and 3 h soaking time. The optimum treatment time was ultrasound 40 min, microwave 20 min, respectively, and the extraction was performed once. Under the optimized conditions, satisfactory extraction yield of the target analyte was obtained. Relative to ultrasound-assisted or microwave-assisted method, the proposed approach provides higher extraction yield. The effect of DHQ of different concentrations and synthetic antioxidants on oxidative stability in soy bean oil stored for 20 days at different temperatures (25 °C and 60 °C) was compared. DHQ was more effective in restraining soy bean oil oxidation, and a dose-response relationship was observed. The antioxidant activity of DHQ was a little stronger than that of BHA and BHT. Soy bean oil supplemented with 0.08 mg/g DHQ exhibited favorable antioxidant effects and is preferable for effectively avoiding oxidation. The L. gmelinii wood samples before and after extraction were characterized by scanning electron microscopy. The results showed that the UMAE method is a simple and efficient technique for sample preparation.

  19. Microwave-assisted extraction of polysaccharides from Yupingfeng powder and their antioxidant activity

    PubMed Central

    Wang, Dan; Zhang, Bi-Bo; Qu, Xiao-Xia; Gao, Feng; Yuan, Min-Yong

    2015-01-01

    Background: Microwave-assisted reflux extraction of polysaccharides YPF-P from the famous Chinese traditional drug, Yupingfeng powder, optimization of extracting conditions and evaluation of their antioxidant activity were conducted in this study. Results: Single factor effect trends were achieved through yields and contends of YPF-P obtained from different extracting conditions. Then through a three-level, four-variable Box-Behnken design of response surface methodology adopting yield as response, the optimal conditions were determined as follows: Material/solvent ratio 1:23.37, microwave power 560 W, Extraction temperature 64°C, and extraction time 9.62 min. Under the optimal conditions, the YPF-P extraction yield was 3.23%, and its content was detected as 38.52%. In antioxidant assays, the YPF-P was tested to possess 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging activities with an IC50 value of 0.262 mg/ml. In addition, YPF-P was also proved to have relatively low ferric reducing antioxidant power (FRAP), compared to Vc, through FRAP assay. Conclusion: In the microwave assisted reflux extraction research, good YPF-P yield was achieved from materials with relatively low YPF-P content. And for the first time, both DPPH and FRAP assays were conducted on YPF-P, which proved that the antioxidant activity of YPF-P contributed to the functions of this medicine. PMID:26246730

  20. Microwave-assisted steam distillation for the determination of organochlorine pesticides and pyrethroids in Chinese teas.

    PubMed

    Ji, Jie; Deng, Chunhui; Zhang, Huiqin; Wu, Yunyun; Zhang, Xiangmin

    2007-02-28

    In this work, microwave-assisted steam distillation (MASD) extraction method followed by gas chromatography/electron capture detection (GC/ECD) was developed for the determination of organochlorine pesticides (OCPs) and pyrethroids in the Chinese teas. MASD is a combination of microwave-assisted extraction (MAE) and steam distillation techniques. Water vapor generated by microwave irradiation is used to accelerate desorption of the analytes from the sample, and the nonpolar organic solvent used for trapping the analytes is kept from direct contact with the sample by the water. Therefore, relatively clean extracts were obtained compared to the method directly using organic solvent as extraction solvent, such as ultrasonic extraction (USE). Microwave power of 200W and irradiation time of 2min was found to be the optimum conditions for the MASD process, and n-heptane was chosen as the analyte-trapping solvent in the study. Five OCPs (alpha-HCH, gamma-HCH, dicofol, p,p'-DDE, p,p'-DDT) and two pyrethroids (bifenthrin, fenvalate) were determined using this extraction method in the tea samples. The relative standard deviation (R.S.D.) of the analytes varied from 2.2 to 8.4%, and the method detection limits (MDLs) found were lower than 0.23mug/kg. The recoveries of the seven compounds in the Jasmine tea sample were between 84.04 and 110.1%. Comparative results obtained by MASD and USE were also discussed in the study.

  1. Producing Lignin-Based Polyols through Microwave-Assisted Liquefaction for Rigid Polyurethane Foam Production

    PubMed Central

    Xue, Bai-Liang; Wen, Jia-Long; Sun, Run-Cang

    2015-01-01

    Lignin-based polyols were synthesized through microwave-assisted liquefaction under different microwave heating times (5–30 min). The liquefaction reactions were carried out using polyethylene glycol (PEG-400)/glycerol as liquefying solvents and 97 wt% sulfur acid as a catalyst at 140 °C. The polyols obtained were analyzed for their yield, composition and structural characteristics using gel permeation chromatography (GPC), Fourier transform infrared (FT-IR) and nuclear magnetic resonance (NMR) spectra. FT-IR and NMR spectra showed that the liquefying solvents reacted with the phenol hydroxyl groups of the lignin in the liquefied product. With increasing microwave heating time, the viscosity of polyols was slightly increased and their corresponding molecular weight (MW) was gradually reduced. The optimal condition at the microwave heating time (5 min) ensured a high liquefaction yield (97.47%) and polyol with a suitable hydroxyl number (8.628 mmol/g). Polyurethane (PU) foams were prepared by polyols and methylene diphenylene diisocyanate (MDI) using the one-shot method. With the isocyanate/hydroxyl group ([NCO]/[OH]) ratio increasing from 0.6 to 1.0, their mechanical properties were gradually increased. This study provided some insight into the microwave-assisted liquefied lignin polyols for the production of rigid PU foam. PMID:28787959

  2. Microwave-assisted acid hydrolysis of konjac products for determining the konjac powder content.

    PubMed

    Tanaka, Yuuki; Okamoto, Ken; Matsushima, Ayako; Ota, Tomoki; Matsumoto, Yoshitsugu; Akasaki, Tetsuya

    2013-01-01

    The complete hydrolysis of konjac glucomannan (KGM) with an acid or enzyme generally takes a long time. To accelerate KGM hydrolysis without diminishing the conventional quality, a diluted acid hydrolysis of KGM with sulfuric acid was conducted using a microwave digestion system. The optimum conditions of microwave-assisted acid hydrolysis for KGM were: 10 mL of 0.25 M sulfuric acid, hydrolysis temperature of 135°C (microwave power of 600 W), and total microwave-irradiation time of 45 min. The yields of the component sugars, mannose and glucose, from two konjac powders were similar to those by conventional acid hydrolysis with 1 M sulfuric acid in a boiling water bath for 5 h. Furthermore, a pretest for microwave-assisted acid hydrolysis using mixtures of konjac powder and starch at different ratios proved that their konjac content can be calculated by determining the mannose generated by the new rapid hydrolysis method, if the raw materials are provided.

  3. Mechanism on microwave-assisted acidic solvolysis of black-liquor lignin.

    PubMed

    Dong, Chengjian; Feng, Chunguang; Liu, Qian; Shen, Dekui; Xiao, Rui

    2014-06-01

    Microwave-assisted degradation of black-liquor lignin with formic acid was studied, concerning the product yield and distribution of phenolic compounds against reaction temperature (110-180°C) and reaction time (5-90 min). The liquid product consisting of bio-oil 1 and bio-oil 2, achieved the maxima yield of 64.08% at 160°C and 30 min (bio-oil 1: 9.69% and bio-oil 2: 54.39%). The chemical information of bio-oil 1 and bio-oil 2 were respectively identified by means of Gas Chromatography-Mass Spectrometer (GC-MS) and Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS), while the solid residue was analyzed by Gel Permeation Chromatography (GPC) and Fourier Transform Infrared Spectroscopy (FTIR). A possible mechanism was proposed for the microwave-assisted acidic solvolysis of lignin, specifying the kinetic relationship among the primary cracking of lignin, repolymerization of the oligomers and formation of solid residue.

  4. Microwave-assisted synthesis of porous carbon-titania and highly crystalline titania nanostructures.

    PubMed

    Parker, Alison; Marszewski, Michal; Jaroniec, Mietek

    2013-03-01

    Porous carbon-titania and highly crystalline titania nanostructured materials were obtained through a microwave-assisted one-pot synthesis. Resorcinol and formaldehyde were used as carbon precursors, triblock copolymer Pluronic F127 as a stabilizing agent, and titanium isopropoxide as a titania precursor. This microwave-assisted one-pot synthesis involved formation of carbon spheres according to the recently modified Stöber method followed by hydrolysis and condensation of titania precursor. This method afforded carbon-titania composite materials containing anatase phase with specific surface areas as high as 390 m(2) g(-1). The pure nanostructured titania, obtained after removal of carbon through calcination of the composite material in air, was shown to be the anatase phase with considerably higher degree of crystallinity and the specific surface area as high as 130 m(2) g(-1). The resulting titania, because of its high surface area, well-developed porosity, and high crystallinity, is of great interest for catalysis, water treatment, lithium batteries, and other energy-related applications.

  5. Fast microwave-assisted catalytic gasification of biomass for syngas production and tar removal.

    PubMed

    Xie, Qinglong; Borges, Fernanda Cabral; Cheng, Yanling; Wan, Yiqin; Li, Yun; Lin, Xiangyang; Liu, Yuhuan; Hussain, Fida; Chen, Paul; Ruan, Roger

    2014-03-01

    In the present study, a microwave-assisted biomass gasification system was developed for syngas production. Three catalysts including Fe, Co and Ni with Al2O3 support were examined and compared for their effects on syngas production and tar removal. Experimental results showed that microwave is an effective heating method for biomass gasification. Ni/Al2O3 was found to be the most effective catalyst for syngas production and tar removal. The gas yield reached above 80% and the composition of tar was the simplest when Ni/Al2O3 catalyst was used. The optimal ratio of catalyst to biomass was determined to be 1:5-1:3. The addition of steam was found to be able to improve the gas production and syngas quality. Results of XRD analyses demonstrated that Ni/Al2O3 catalyst has good stability during gasification process. Finally, a new concept of microwave-assisted dual fluidized bed gasifier was put forward for the first time in this study.

  6. Nitrogen-protected microwave-assisted extraction of ascorbic acid from fruit and vegetables.

    PubMed

    Yu, Yingjia; Chen, Bin; Chen, Yile; Xie, Meifen; Duan, Haotian; Li, Yan; Duan, Gengli

    2009-12-01

    In this study, nitrogen-protected microwave-assisted extraction (NPMAE), in which microwave-assisted extraction was performed under nitrogen protection, was initially developed and combined with HPLC separation for the determination of ascorbic acid (AA), an oxidizable component, from fruit and vegetables. The extraction conditions of NPMAE were investigated by extraction of AA from guava, and the chosen conditions were as follows: extraction solvent of 0.25% metaphosphoric acid solution, solid/liquid ratio of 1:10 g/mL, microwave power of 400 W and irradiation time of 10 min. Subsequently, this novel NPMAE method was evaluated by extraction of AA from different fruit and vegetables, such as guava, yellow pepper, green pepper and cayenne pepper. Compared with conventional MAE and solvent extraction methods, the oxidation of AA was significantly reduced or prevented in the process of NPMAE, providing higher extraction yield of AA. These results suggested the potential of NPMAE method for the extraction of oxidizable compounds from different spices of matrices.

  7. Central composite rotatable design for investigation of microwave-assisted extraction of okra pod hydrocolloid.

    PubMed

    Samavati, Vahid

    2013-10-01

    Microwave-assisted extraction (MAE) technique was employed to extract the hydrocolloid from okra pods (OPH). The optimal conditions for microwave-assisted extraction of OPH were determined by response surface methodology. A central composite rotatable design (CCRD) was applied to evaluate the effects of three independent variables (microwave power (X1: 100-500 W), extraction time (X2: 30-90 min), and extraction temperature (X3: 40-90 °C)) on the extraction yield of OPH. The correlation analysis of the mathematical-regression model indicated that quadratic polynomial model could be employed to optimize the microwave extraction of OPH. The optimal conditions to obtain the highest recovery of OPH (14.911±0.27%) were as follows: microwave power, 395.56 W; extraction time, 67.11 min and extraction temperature, 73.33 °C. Under these optimal conditions, the experimental values agreed with the predicted ones by analysis of variance. It indicated high fitness of the model used and the success of response surface methodology for optimizing OPH extraction. After method development, the DPPH radical scavenging activity of the OPH was evaluated. MAE showed obvious advantages in terms of high extraction efficiency and radical scavenging activity of extract within the shorter extraction time.

  8. Fast microwave-assisted catalytic pyrolysis of sewage sludge for bio-oil production.

    PubMed

    Xie, Qinglong; Peng, Peng; Liu, Shiyu; Min, Min; Cheng, Yanling; Wan, Yiqin; Li, Yun; Lin, Xiangyang; Liu, Yuhuan; Chen, Paul; Ruan, Roger

    2014-11-01

    In this study, fast microwave-assisted catalytic pyrolysis of sewage sludge was investigated for bio-oil production, with HZSM-5 as the catalyst. Pyrolysis temperature and catalyst to feed ratio were examined for their effects on bio-oil yield and composition. Experimental results showed that microwave is an effective heating method for sewage sludge pyrolysis. Temperature has great influence on the pyrolysis process. The maximum bio-oil yield and the lowest proportions of oxygen- and nitrogen-containing compounds in the bio-oil were obtained at 550°C. The oil yield decreased when catalyst was used, but the proportions of oxygen- and nitrogen-containing compounds were significantly reduced when the catalyst to feed ratio increased from 1:1 to 2:1. Essential mineral elements were concentrated in the bio-char after pyrolysis, which could be used as a soil amendment in place of fertilizer. Results of XRD analyses demonstrated that HZSM-5 catalyst exhibited good stability during the microwave-assisted pyrolysis of sewage sludge. Copyright © 2014 Elsevier Ltd. All rights reserved.

  9. Sequential ultrasound-microwave assisted acid extraction (UMAE) of pectin from pomelo peels.

    PubMed

    Liew, Shan Qin; Ngoh, Gek Cheng; Yusoff, Rozita; Teoh, Wen Hui

    2016-12-01

    This study aims to optimize sequential ultrasound-microwave assisted extraction (UMAE) on pomelo peel using citric acid. The effects of pH, sonication time, microwave power and irradiation time on the yield and the degree of esterification (DE) of pectin were investigated. Under optimized conditions of pH 1.80, 27.52min sonication followed by 6.40min microwave irradiation at 643.44W, the yield and the DE value of pectin obtained was respectively at 38.00% and 56.88%. Based upon optimized UMAE condition, the pectin from microwave-ultrasound assisted extraction (MUAE), ultrasound assisted extraction (UAE) and microwave assisted extraction (MAE) were studied. The yield of pectin adopting the UMAE was higher than all other techniques in the order of UMAE>MUAE>MAE>UAE. The pectin's galacturonic acid content obtained from combined extraction technique is higher than that obtained from sole extraction technique and the pectin gel produced from various techniques exhibited a pseudoplastic behaviour. The morphological structures of pectin extracted from MUAE and MAE closely resemble each other. The extracted pectin from UMAE with smaller and more regular surface differs greatly from that of UAE. This has substantiated the highest pectin yield of 36.33% from UMAE and further signified their compatibility and potentiality in pectin extraction. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Rapid microwave-assisted growth of silver nanoparticles on 3D graphene networks for supercapacitor application.

    PubMed

    Khamlich, S; Khamliche, T; Dhlamini, M S; Khenfouch, M; Mothudi, B M; Maaza, M

    2017-05-01

    Silver nanoparticles (AgNPs) grown on a three dimensional (3d) graphene networks (GNs) has been successfully prepared by an efficient and rapid microwave-assisted growth process to form GNs/AgNPs nanocomposite electrode materials for supercapacitor application. The 3d nature of the used GNs offers a unique architecture, which creates an efficient conduction networks and maximum utilization of space and interface, and acts as a conductive layer for the deposited AgNPs. The electrochemical performances of the fabricated electrode were evaluated by cyclic voltammetry (CV), galvanostatic charge/discharge and electrochemical impedance spectroscopy (EIS) tests. Specifically, the optimal GNs/AgNPs nanocomposite exhibits remarkable performances with a high specific capacitance of 528Fg(-1) at a current density of 1Ag(-1) and excellent capacitance retention of ∼93% after 3000cycles. Moreover, this microwave-assisted growth strategy of AgNPs is simple and effective, which could be extended to the construction of other three dimensional graphene based metallic composites for energy storage and conversion applications.

  11. Microwave-Assisted Extraction of Oleanolic Acid and Ursolic Acid from Ligustrum lucidum Ait

    PubMed Central

    Xia, En-Qin; Wang, Bo-Wei; Xu, Xiang-Rong; Zhu, Li; Song, Yang; Li, Hua-Bin

    2011-01-01

    Oleanolic acid and ursolic acid are the main active components in fruit of Ligustrum lucidum Ait, and possess anticancer, antimutagenic, anti-inflammatory, antioxidative and antiprotozoal activities. In this study, microwave-assisted extraction of oleanolic acid and ursolic acid from Ligustrum lucidum was investigated with HPLC-photodiode array detection. Effects of several experimental parameters, such as type and concentration of extraction solvent, ratio of liquid to material, microwave power, extraction temperature and microwave time, on the extraction efficiencies of oleanolic acid and ursolic acid from Ligustrum lucidum were evaluated. The influence of experimental parameters on the extraction efficiency of ursolic acid was more significant than that of oleanolic acid (p < 0.05). The optimal extraction conditions were 80% ethanol aqueous solution, the ratio of material to liquid was 1:15, and extraction for 30 min at 70 °C under microwave irradiation of 500 W. Under optimal conditions, the yields of oleanolic acid and ursolic acid were 4.4 ± 0.20 mg/g and 5.8 ± 0.15 mg/g, respectively. The results obtained are helpful for the full utilization of Ligustrum lucidum, which also indicated that microwave-assisted extraction is a very useful method for extraction of oleanolic acid and ursolic acid from plant materials. PMID:21954361

  12. Self-assembly of silica nanoparticles into hollow spheres via a microwave-assisted aerosol process

    SciTech Connect

    Li, Shan; Wang, Fei; Dai, Hongqi; Jiang, Xingmao; Ye, Chunhong; Min, Jianzhong

    2016-02-15

    Highlights: • The silica hollow spheres were fabricated via a microwave-assisted aerosol process. • The formation of the hollow spheres was obtained through a one-step process. • The spheres indicated the remarkable sustained release of potassium persulfate. - Abstract: In this work, a simple and efficient strategy for fabrication of silica hollow spheres (SHSs) has been successfully introduced with a one-step microwave-assisted aerosol process using silica nanoparticles (SiO{sub 2}, 12–50 nm) and NH{sub 4}HCO{sub 3} as precursor materials. This approach combines the merits of microwave radiation and the aerosol technique. And the formation of SHSs is ascribed to solvent evaporation and the as-generated gas from NH{sub 4}HCO{sub 3} decomposition in the microwave reactor. The morphology of the SHSs can be easily tuned by varying the residence time, amount of NH{sub 4}HCO{sub 3} and silica sources. The formation mechanism of SHSs was also investigated by structure analysis. In addition, the hollow spheres exhibited remarkable sustained release of potassium persulfate, by loading it into the porous structures. The results provide new sights into the fabrication of inorganic hollow spheres via a one-step process.

  13. Microwave Assisted Organic Synthesis of Heterocycles in Aqueous Media: Recent Advances in Medicinal Chemistry.

    PubMed

    Frecentese, Francesco; Saccone, Irene; Caliendo, Giuseppe; Corvino, Angela; Fiorino, Ferdinando; Magli, Elisa; Perissutti, Elisa; Severino, Beatrice; Santagada, Vincenzo

    2016-01-01

    Green chemistry is a discipline of great interest in medicinal chemistry. It involves all fields of chemistry and it is based on the principle to conduct chemical reactions protecting the environment at the same time, through the use of chemical procedures able to avoid pollution. In this context, water as solvent is a good choice because it is abundant, nontoxic, non-caustic, and non-combustible. Even if microwave assisted organic reactions in conventional solvents have quickly progressed, in the recent years medicinal chemists have focused their attention to processes deemed not dangerous for the environment, using nanotechnology and greener solvents as water. Several reports of reaction optimizations and selectivities, demonstrating the capability of microwave to allow the obtaining of increased yields have been recently published using water as solvent. In this review, we selected the available knowledge related to microwave assisted organic synthesis in aqueous medium, furnishing examples of the newest strategies to obtain useful scaffolds and novel derivatives for medicinal chemistry purposes. The intention of this review is to demonstrate the exclusive ability of MAOS in water as solvent or as co-solvent. For this purpose we report here the most representative applications of MAOS using water as solvent, focusing on medicinal chemistry processes leading to interesting nitrogen containing heterocycles with potential pharmaceutical applications.

  14. Microwave-assisted rapid synthesis, characterization and application of poly (D,L-lactide)-graft-pullulan.

    PubMed

    Tang, Xiao-Jiao; Huang, Jun; Xu, Liang-Yu; Li, Yang; Song, Juan; Ma, Yue; Yang, Li; Yuan, Dan; Wu, Hai-Yang

    2014-07-17

    A novel microwave-assisted method was developed to synthetize amphiphilic copolymer poly (d,l-lactide)-graft-pullulan (PL) in a monomode microwave reactor. The effects of microwave power, ratio of catalyst/lactide, ratio of lactide/hydroxyl group of pullulan (lactide/OH-P) and solvent on the synthesis were further investigated. Three samples (designated as PL 8, 9, and 6), characterized by FT-IR and NMR, were applied to form nanoparticles and microparticles investigated by dynamic light scattering, fluorescence spectroscopy and transmission electron microscopy. PL9 and PL6 were used for loading model drug curcumin. The results indicated that microwave-assisted synthesis shortened the copolymerization of PL, with higher yield and lactide conversion, from 24h to 5 min and showed some specific microwave effects compared with conventional oil heating. PL with a relative higher substitution degree gave nanoparticles with smaller sizes and critical aggregation concentrations. The solubility of curcumin was increased to 1.97 mg mL(-1) as the forms of nanoparticles. Copyright © 2014 Elsevier Ltd. All rights reserved.

  15. Box-Behnken design for investigation of microwave-assisted extraction of patchouli oil

    NASA Astrophysics Data System (ADS)

    Kusuma, Heri Septya; Mahfud, Mahfud

    2015-12-01

    Microwave-assisted extraction (MAE) technique was employed to extract the essential oil from patchouli (Pogostemon cablin). The optimal conditions for microwave-assisted extraction of patchouli oil were determined by response surface methodology. A Box-Behnken design (BBD) was applied to evaluate the effects of three independent variables (microwave power (A: 400-800 W), plant material to solvent ratio (B: 0.10-0.20 g mL-1) and extraction time (C: 20-60 min)) on the extraction yield of patchouli oil. The correlation analysis of the mathematical-regression model indicated that quadratic polynomial model could be employed to optimize the microwave extraction of patchouli oil. The optimal extraction conditions of patchouli oil was microwave power 634.024 W, plant material to solvent ratio 0.147648 g ml-1 and extraction time 51.6174 min. The maximum patchouli oil yield was 2.80516% under these optimal conditions. Under the extraction condition, the experimental values agreed with the predicted results by analysis of variance. It indicated high fitness of the model used and the success of response surface methodology for optimizing and reflect the expected extraction condition.

  16. Novel microwave assisted chemical synthesis of Nd₂Fe₁₄B hard magnetic nanoparticles.

    PubMed

    Swaminathan, Viswanathan; Deheri, Pratap Kumar; Bhame, Shekhar Dnyaneswar; Ramanujan, Raju Vijayaraghavan

    2013-04-07

    The high coercivity and excellent energy product of Nd2Fe14B hard magnets have led to a large number of high value added industrial applications. Chemical synthesis of Nd2Fe14B nanoparticles is challenging due to the large reduction potential of Nd(3+) and the high tendency for Nd2Fe14B oxidation. We report the novel synthesis of Nd2Fe14B nanoparticles by a microwave assisted combustion process. The process consisted of Nd-Fe-B mixed oxide preparation by microwave assisted combustion, followed by the reduction of the mixed oxide by CaH2. This combustion process is fast, energy efficient and offers facile elemental substitution. The coercivity of the resulting powders was ∼8.0 kOe and the saturation magnetization was ∼40 emu g(-1). After removal of CaO by washing, saturation magnetization increased and an energy product of 3.57 MGOe was obtained. A range of magnetic properties was obtained by varying the microwave power, reduction temperature and Nd to Fe ratio. A transition from soft to exchange coupled to hard magnetic properties was obtained by varying the composition of NdxFe1-xB8 (x varies from 7% to 40%). This synthesis procedure offers an inexpensive and facile platform to produce exchange coupled hard magnets.

  17. Microwave-Assisted Surface Modification of Metallocene Polyethylene for Improving Blood Compatibility

    PubMed Central

    Sivakumar, Gunalan; Kasi, Palaniappan; Jaganathan, Saravana Kumar; Supriyanto, Eko

    2013-01-01

    A wide number of polymers are being used for various medical applications. In this work, microwave-assisted surface modification of metallocene polyethylene (mPE) was studied. FTIR analysis showed no significant changes in the chemical groups after treatment. Contact angle analysis revealed a decrease in contact angle of the treated samples insinuating increasing hydrophilicity and better biocompatibility. Qualitative analysis of treated samples using scanning electron microscope (SEM) depicted increasing surface roughness and holes formation further corroborating the results. Coagulation assays performed for estimating prothrombin time (PT) and activated partial thromboplastin time (APTT) showed an increase in the clotting time which further confirmed the improved blood compatibility of the microwave-treated surfaces. Further, the extent of hemolysis in the treated sample was lower than the untreated one. Hence, microwave-assisted surface modification of mPE resulted in enhanced blood compatibility. Improved blood compatibility of mPE may be exploited for fabrication of artificial vascular prostheses, implants, and various blood contacting devices. PMID:23841059

  18. MICROWAVE-ASSISTED EXTRACTION OF PHENOLIC COMPOUNDS FROM POLYGONUM MULTIFLORUM THUNB. ROOTS.

    PubMed

    Quoc, Le Pham Tan; Muoi, Nguyen Van

    2016-01-01

    The aim of this study was to determine the best extraction conditions for total phenolic content (TPC) and antioxidant capacity (AC) of Polygonum multiflorum Thunb. root using microwave-assisted extraction (MAE). The raw material used was Polygonum multiflorum Thunb. root powder. Five factors such as solvent type, solvent concentrations, solvent/material ratio, extraction time and microwave power were studied; TPC and AC values were determined by the Folin-Ciocalteu method and DPPH free radical scavenging activity measurement, respectively. In addition, studies involved assaying the HPLC test of extracts and SEM of samples. Optimal results pointed to acetone as the solvent, acetone concentration of 60%, solvent/material ratio of 40/1 (v/w), extraction time of 5 mins and microwave power of 127 W. TPC and AC obtained were approximates 44.3 ±0.13 mg GAE/g DW and 341.26 ±1.54 μmol TE/g DW, respectively. The effect of microwaving on the cell destruction of Polygonum multiflorum Thunb. root was observed by scanning electron microscopy (SEM). Some phenolic compounds were determined by the HPLC method, for instance, gallic acid, catechin and resveratrol. These factors significantly affected TPC and AC. We can use acetone as a solvent with microwave-assisted extraction to achieve the best result.

  19. Effect of acid concentration on closed-vessel microwave-assisted digestion of plant materials

    NASA Astrophysics Data System (ADS)

    Araújo, Geórgia C. L.; Gonzalez, Mário H.; Ferreira, Antônio G.; Nogueira, Ana Rita A.; Nóbrega, Joaquim A.

    2002-12-01

    The efficiency of microwave-assisted acid digestion of plants using different concentrations of nitric acid (2.0, 3.0, 5.0, 7.0 and 14 mol l -1) with hydrogen peroxide (30% v/v) was evaluated by measuring the residual carbon content (RCC) using inductively coupled plasma optical emission spectrometry (ICP-OES) with axial viewing. Certified reference materials were used for evaluating the accuracy attained when 2 mol l -1 HNO 3 was employed for digestion. Under all experimental conditions RCC values were always lower than 13% w/v, and even the highest concentration did not cause any interference with element recovery. It seems that the high pressure reached for closed-vessel operation improved the oxidative action of nitric acid due to consequent temperature increase, even when this reagent was not used at high concentrations. According to acid-base titration data, residual acid in the digestates varied from 1.2 to 4.0 mol l -1, depending on the acid concentration initially added. It can be concluded that for plant materials, microwave-assisted acid digestion can be carried out under mild conditions, which implies that digestates do not need extensive dilution before introduction by pneumatic nebulization to ICP-OES. An additional advantage is the lower amount of residue generated when working with less concentrated acid solutions.

  20. Producing Lignin-Based Polyols through Microwave-Assisted Liquefaction for Rigid Polyurethane Foam Production.

    PubMed

    Xue, Bai-Liang; Wen, Jia-Long; Sun, Run-Cang

    2015-02-10

    Lignin-based polyols were synthesized through microwave-assisted liquefaction under different microwave heating times (5-30 min). The liquefaction reactions were carried out using polyethylene glycol (PEG-400)/glycerol as liquefying solvents and 97 wt% sulfur acid as a catalyst at 140 °C. The polyols obtained were analyzed for their yield, composition and structural characteristics using gel permeation chromatography (GPC), Fourier transform infrared (FT-IR) and nuclear magnetic resonance (NMR) spectra. FT-IR and NMR spectra showed that the liquefying solvents reacted with the phenol hydroxyl groups of the lignin in the liquefied product. With increasing microwave heating time, the viscosity of polyols was slightly increased and their corresponding molecular weight (MW) was gradually reduced. The optimal condition at the microwave heating time (5 min) ensured a high liquefaction yield (97.47%) and polyol with a suitable hydroxyl number (8.628 mmol/g). Polyurethane (PU) foams were prepared by polyols and methylene diphenylene diisocyanate (MDI) using the one-shot method. With the isocyanate/hydroxyl group ([NCO]/[OH]) ratio increasing from 0.6 to 1.0, their mechanical properties were gradually increased. This study provided some insight into the microwave-assisted liquefied lignin polyols for the production of rigid PU foam.

  1. Microwave-assisted derivatization: application to steroid profiling by gas chromatography/mass spectrometry.

    PubMed

    Casals, Gregori; Marcos, Josep; Pozo, Oscar J; Alcaraz, José; Martínez de Osaba, María Jesús; Jiménez, Wladimiro

    2014-06-01

    Gas chromatography-mass spectrometry (GC-MS) remains as the gold-standard technique for the study of the steroid metabolome. A main limitation is the need of performing a derivatization step since incubation with strong silylations agents for long periods of time (usually 16 h) is required for the derivatization of hindered hydroxyls present in some steroids of interest. In the present work, a rapid, simple and reproducible microwave-assisted derivatization method was developed. In the method, 36 steroids already treated with methoxyamine (2% in pyridine) were silylated with 50 μl of N-trimethylsilylimidazole by using microwave irradiation, and the formed methyloxime-trimethylsilyl derivatives were analyzed by GC-MS. Microwave power and derivatization time silylation conditions were optimized being the optimum conditions 600 W and 3 min respectively. In order to evaluate the usefulness of this technique, the urine steroid profiles for 20 healthy individuals were analyzed. The results of a comparison of microwave irradiation with the classical heating protocol showed similar derivatization yields, thus suggesting that microwave-assisted silylation is a valid tool for the rapid steroid metabolome study.

  2. A Rapid Microwave-Assisted Thermolysis Route to Highly Crystalline Carbon Nitrides for Efficient Hydrogen Generation.

    PubMed

    Guo, Yufei; Li, Jing; Yuan, Yupeng; Li, Lu; Zhang, Mingyi; Zhou, Chenyan; Lin, Zhiqun

    2016-11-14

    Highly crystalline graphitic carbon nitride (g-C3 N4 ) with decreased structural imperfections benefits from the suppression of electron-hole recombination, which enhances its hydrogen generation activity. However, producing such g-C3 N4 materials by conventional heating in an electric furnace has proven challenging. Herein, we report on the synthesis of high-quality g-C3 N4 with reduced structural defects by judiciously combining the implementation of melamine-cyanuric acid (MCA) supramolecular aggregates and microwave-assisted thermolysis. The g-C3 N4 material produced after optimizing the microwave reaction time can effectively generate H2 under visible-light irradiation. The highest H2 evolution rate achieved was 40.5 μmol h(-1) , which is two times higher than that of a g-C3 N4 sample prepared by thermal polycondensation of the same supramolecular aggregates in an electric furnace. The microwave-assisted thermolysis strategy is simple, rapid, and robust, thereby providing a promising route for the synthesis of high-efficiency g-C3 N4 photocatalysts. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Rapid characterization of protein chips using microwave-assisted protein tryptic digestion and MALDI mass spectrometry.

    PubMed

    Ha, Na Young; Kim, Shin Hye; Lee, Tae Geol; Han, Sang Yun

    2011-08-16

    We demonstrate that the microwave-assisted protein enzymatic digestion (MAPED) method can be successfully applied to the mass spectrometric characterization of proteins captured on the affinity surfaces of protein chips. The microwave-assisted on-chip tryptic digestion method was developed using a domestic microwave, completing the on-chip proteolysis reaction in minutes, whereas the previous on-chip digestion methods by incubation took hours of incubation time. For the model protein chips, antibody-presenting surfaces were prepared, where anti-α-tubulin1 and antibovine serum albumin (BSA) were immobilized on self-assembled monolayers. The resulting digestion efficiency, displaying sequence coverages of 30 and 14% for α-tubulin1 and BSA, respectively, was comparable to the previous time-consuming incubation studies. It allowed the characterization of immunosensed proteins by MASCOT search using peptide mass fingerprinting. In an example of this method for protein chip applications, BSA naturally involved in fetal bovine serum was unambiguously identified on a model protein chip by imaging mass spectrometry. This work shows that biomass spectrometry techniques can be implemented for surface mass spectrometry and biochip applications. Along with recent advances in imaging mass spectrometry, this technique will provide a new opportunity for high-speed, and thus high-throughput in the future, label-free mass spectrometric assays using protein arrays.

  4. Rapid and efficient glycoprotein identification through microwave-assisted enzymatic digestion.

    PubMed

    Segu, Zaneer M; Hammad, Loubna A; Mechref, Yehia

    2010-12-15

    Identification of protein glycosylation sites is analytically challenging due to the diverse glycan structures associated with a glycoprotein. Mass spectrometry (MS)-based identification and characterization of glycoproteins has been achieved predominantly with the bottom-up approach, which typically involves the enzymatic cleavage of proteins to peptides prior to LC/MS or LC/MS/MS analysis. However, the process can be challenging due to the structural variations and steric hindrance imposed by the attached glycans. Alternatives to conventional heating protocols, that increase the rate of enzymatic cleavage of glycoproteins, may aid in addressing these challenges. An enzymatic digestion of a glycoprotein can be accelerated and made more efficient through microwave-assisted digestion. In this paper, a systematic study was conducted to explore the efficiency of microwave-assisted enzymatic (trypsin) digestion (MAED) of glycoproteins as compared with the conventional method. In addition, the optimum experimental parameters for the digestion such as temperature, reaction time, and microwave radiation power were investigated. It was determined that efficient tryptic digestion of glycoproteins was attained in 15 min, allowing comparable if not better sequence coverage through LC/MS/MS analysis. Optimum tryptic cleavage was achieved at 45°C irrespective of the size and complexity of the glycoprotein. Moreover, MAED allowed the detection and identification of more peptides and subsequently higher sequence coverage for all model glycoprotein. MAED also did not appear to prompt a loss or partial cleavage of the glycan moieties attached to the peptide backbones.

  5. Extraction of hydrocarbons from seaweed samples using sonication and microwave-assisted extraction: a comparative study.

    PubMed

    Punín Crespo, M O; Cam, D; Gagni, S; Lombardi, N; Lage Yusty, M A

    2006-01-01

    A sonication method is compared with a microwave-assisted extraction method for recovering polycyclic aromatic hydrocarbons and aliphatic hydrocarbons from seaweed and acid humic samples. Different extracting solvents and adsorbents for the purification step are tested. For the sonication extraction, 10 g of the sample are extracted in an ultrasonic bath (60 degrees C for 15 min with 20 mL of hexane). For the microwave-assisted extraction two steps are carried out, each step at 90 degrees C under pressure in closed vessels with 20 mL of hexane for 10 min at 950 W. A clean-up step is performed for both extraction techniques. The results indicate that the recovery of hydrocarbons is dependent on both the extraction technique and the type of matrix. The most suitable technique appears to be sonication employing hexane as the extraction solvent. The recoveries obtained for aliphatic hydrocarbons are higher than those achieved for the polycyclic aromatic hydrocarbons, with values ranging within 81-109% and 40-76%, respectively.

  6. Optimization of microwave assisted extraction (MAE) and soxhlet extraction of phenolic compound from licorice root.

    PubMed

    Karami, Zohreh; Emam-Djomeh, Zahra; Mirzaee, Habib Allah; Khomeiri, Morteza; Mahoonak, Alireza Sadeghi; Aydani, Emad

    2015-06-01

    In present study, response surface methodology was used to optimize extraction condition of phenolic compounds from licorice root by microwave application. Investigated factors were solvent (ethanol 80 %, methanol 80 % and water), liquid/solid ratio (10:1-25:1) and time (2-6 min). Experiments were designed according to the central composite rotatable design. The results showed that extraction conditions had significant effect on the extraction yield of phenolic compounds and antioxidant capacities. Optimal condition in microwave assisted method were ethanol 80 % as solvent, extraction time of 5-6 min and liquid/solid ratio of 12.7/1. Results were compared with those obtained by soxhlet extraction. In soxhlet extraction, Optimum conditions were extraction time of 6 h for ethanol 80 % as solvent. Value of phenolic compounds and extraction yield of licorice root in microwave assisted (MAE), and soxhlet were 47.47 mg/g and 16.38 %, 41.709 mg/g and 14.49 %, respectively. These results implied that MAE was more efficient extracting method than soxhlet.

  7. Microwave-assisted synthesis of carbon nanodots through an eggshell membrane and their fluorescent application.

    PubMed

    Wang, Qi; Liu, Xing; Zhang, Lichun; Lv, Yi

    2012-11-21

    Carbon nanodots (C-Dots) as a new form of carbonaceous nanomaterials have aroused much interest and intensive research due to their inspiring properties. Compared to traditional semiconductor quantum dots, these newly emergent nanodots possess a number of advantageous characteristics, among which low-toxicity is particularly fascinating. More and more research into C-Dots have focused on synthesis methods and biology-related applications. Microwave-assisted approaches have attracted attention because microwave treatment can provide intensive and efficient energy, and as a consequence shorten the reaction time. In this article, we designed a "green", rapid, eco-friendly and waste-reused approach to synthesize fluorescent and water-soluble C-Dots from eggshell membrane (ESM) ashes according to a microwave-assisted process. ESM selected as the carbon source was a common protein-rich waste in daily life and can be obtained easily and cheaply. The C-Dots from our method showed the maximal fluorescence emission peak at 450 nm and the fluorescence quantum yield was about 14%. We further designed a sensitive probe for glutathione based on the fluorescence turn off and on of the C-Dots-Cu(2+) system, which showed a linear range of 0.5-80 μmol L(-1) and detection limit of 0.48 μmol L(-1). In general, the C-Dots prepared briefly and inexpensively from ESM revealed excellent fluorescent property with promising potential for applications such as sample detection and biotechnology.

  8. Microwave-assisted extraction of pectic polysaccharide from waste mango peel.

    PubMed

    Maran, J Prakash; Swathi, K; Jeevitha, P; Jayalakshmi, J; Ashvini, G

    2015-06-05

    This present study investigates the extraction characteristics and optimal parameters of the microwave-assisted extraction of pectin from waste mango peel (WMP). Microwave power, pH, time and solid-liquid ratio were selected as the extraction parameters and was studied by using Box-Behnken response surface design. The experimental data was analyzed by least square regression analysis method and a second order polynomial model was constructed for response from the experimental data. The constructed model was adequate to explain the relationships between independent variables and response. All studied factors had great influence on the yield of pectin by individually and interactively. The optimum microwave assisted extraction conditions for the highest pectin yield (28.86%) from WMP was found to be: microwave power of 413W, pH of 2.7, time of 134s and solid-liquid ratio of 1:18g/ml. The experimental value was well correlated with predicted value at the optimal condition.

  9. Synthesis and characterization of biodegradable peptide-based polymers prepared by microwave-assisted click chemistry.

    PubMed

    van Dijk, Maarten; Nollet, Maria L; Weijers, Pascal; Dechesne, Annemarie C; van Nostrum, Cornelus F; Hennink, Wim E; Rijkers, Dirk T S; Liskamp, Rob M J

    2008-10-01

    In this study, the microwave-assisted copper(I)-catalyzed 1,3-dipolar cycloaddition reaction was used to synthesize peptide triazole-based polymers from two novel peptide-based monomers: azido-phenylalanyl-alanyl-lysyl-propargyl amide (1) and azido-phenylalanyl-alanyl-glycolyl-lysyl-propargyl amide (2). The selected monomers have sites for enzymatic degradation as well as for chemical hydrolysis to render the resulting polymer biodegradable. Depending on the monomer concentration in DMF, the molecular mass of the polymers could be tailored between 4.5 and 13.9 kDa (corresponding with 33-100 amino acid residues per polymer chain). As anticipated, both polymers can be enzymatically degraded by trypsin and chymotrypsin, whereas the ester bond in the polymer of 2 undergoes chemical hydrolysis under physiological conditions, as was shown by a ninhydrin-based colorimetric assay and MALDI-TOF analysis. In conclusion, the microwave-assisted copper(I)-catalyzed 1,3-dipolar cycloaddition reaction is an effective tool for synthesizing biodegradable peptide polymers, and it opens up new approaches toward the synthesis of (novel) designed biomedical materials.

  10. Extraction of Dihydroquercetin from Larix gmelinii with Ultrasound-Assisted and Microwave-Assisted Alternant Digestion

    PubMed Central

    Ma, Chunhui; Yang, Lei; Wang, Wenjie; Yang, Fengjian; Zhao, Chunjian; Zu, Yuangang

    2012-01-01

    An ultrasound and microwave assisted alternant extraction method (UMAE) was applied for extracting dihydroquercetin (DHQ) from Larix gmelinii wood. This investigation was conducted using 60% ethanol as solvent, 1:12 solid to liquid ratio, and 3 h soaking time. The optimum treatment time was ultrasound 40 min, microwave 20 min, respectively, and the extraction was performed once. Under the optimized conditions, satisfactory extraction yield of the target analyte was obtained. Relative to ultrasound-assisted or microwave-assisted method, the proposed approach provides higher extraction yield. The effect of DHQ of different concentrations and synthetic antioxidants on oxidative stability in soy bean oil stored for 20 days at different temperatures (25 °C and 60 °C) was compared. DHQ was more effective in restraining soy bean oil oxidation, and a dose-response relationship was observed. The antioxidant activity of DHQ was a little stronger than that of BHA and BHT. Soy bean oil supplemented with 0.08 mg/g DHQ exhibited favorable antioxidant effects and is preferable for effectively avoiding oxidation. The L. gmelinii wood samples before and after extraction were characterized by scanning electron microscopy. The results showed that the UMAE method is a simple and efficient technique for sample preparation. PMID:22942735

  11. Microwave-assisted Bi2Se3 nanoparticles using various organic solvents

    NASA Astrophysics Data System (ADS)

    Vijila, J. Joy Jeba; Mohanraj, K.; Henry, J.; Sivakumar, G.

    2016-01-01

    Microwave assisted Bi2Se3 nanoparticles were synthesized from five different solvents DMF, EG, EG + H2O, EDA + dil.HNO3 and N2H4 + H2O + Ethanol. The influence of solvents on purity of the compound was analysed by using X-ray diffraction patterns. The result indicates pure rhombohedral Bi2Se3 nanoparticles formed for N2H4 + H2O + Ethanol. The presence of vibrational bands in the range of 400-800 cm- 1 is confirmed the formation of Bi2Se3. The maximum optical absorption observed around 450 nm and the band gap values are found in the range of 1.5 eV-2.17 eV for all the solvents. The nanostructure of the Bi2Se3 particles change with solvents. From the experimental results, the solvent N2H4 + H2O + Ethanol produces pure nanosize Bi2Se3 particles under the microwave assisted method.

  12. [Determination of benzo(alpha)pyrene in food with microwave-assisted extraction].

    PubMed

    Zhou, Na; Luo, He-Dong; Li, Na; Li, Yao-Qun

    2014-03-01

    Coupling derivative technique and constant-energy synchronous fluorescence scanning technique, a method of determining benzo[alpha] pyrene in foods by second derivative constant-energy synchronous spectrofluorimetry after microwave-assisted treatment of samples was established using domestic microwave oven. The main factors of influencing the efficiency of microwave extraction were discussed, including the extraction solvent types and amounts, the microwave extraction time, microwave radiation power and cooling time. And the comparison with ultrasonic extraction was made. Low-fat food samples, which were just microwave-extracted with mixed-solvents, could be analyzed immediately by the spectrofluorimetric technique. For high-fat food samples, microwave-assisted saponification and extraction were made at the same time, thus simplifying operation steps and reducing sample analysis time. So the whole sample analysis process could be completed within one hour. This method was simple, rapid and inexpensive. In consequence, it was applied to determine benzo(a)pyrene in food with good reproducibility and the recoveries of benzo(alpha) pyrene ranged from 90.0% to 105.0% for the low fat samples and 83.3% to 94.6% for high-fat samples.

  13. Microwave assisted solvent-free synthesis and biological activities of novel imines (Schiff bases).

    PubMed

    Kundu, Aditi; Shakil, Najam Akhtar; Saxena, Dinesh B; Kumar, Jitendra; Walia, Suresh

    2009-06-01

    Twelve new ortho-Hydroxyketimines were synthesized by conventional as well as microwave method and evaluated for their antinemic activity against Meloidogyne incognita [(Kofoid and White) Chitwood]. Conventional methods for synthesis of Schiff bases require refluxing at 140 degrees C of the reactants in different solvents for at least 24 h or more, where as the microwave-assisted synthesis has brought down the reaction time from 24 h to 1 minute. The procedure reported is simple as it does not require any organic solvents and the time has been reduced to only 1 minute. Comparative yields of all compounds by different methods revealed that the yield was low in conventional method (79-87%) as compared to microwave assisted synthesis (94-97%). The bioassay revealed that all the test compounds exhibited promising nematicidal activity; N-propyl-2-hydroxypropiophenonimine being the most effective with LC(50) value of 74.46 mgL(-1) followed by N-hexyl-2-hydroxyacetophenonimine with LC(50) value of 99.60 mgL(-1) after 72 h of exposure. The results obtained from bioassay indicated that this class of compounds has not only given a lead with regard to potential of Schiff bases in pest control, but has suggested that a carbon chain length of 6 atoms in the side chain is optimum on the basis of structure activity relationship (SAR).

  14. Rapid synthesis of 3-amino-imidazopyridines by a microwave-assisted four-component coupling in one pot.

    PubMed

    Dimauro, Erin F; Kennedy, Joseph M

    2007-02-02

    The rapid and efficient synthesis of various 2,6-disubstituted-3-amino-imidazopyridines using a microwave-assisted one-pot cyclization/Suzuki coupling approach is described. The utility of a 2-aminopyridine-5-boronic acid pinacol ester as a robust and versatile building block for the synthesis of diverse compound libraries is emphasized. The boronate functional group is remarkably tolerant to the Lewis acid catalyzed cyclizations, and the subsequent Pd(0)-catalyzed Suzuki coupling reactions proceed cleanly in the presence of magnesium salts. This work highlights the vast potential of microwave-assisted, metal-catalyzed, multicomponent reactions.

  15. Microwave-assisted synthesis and characterization of hierarchically structured calcium fluoride

    SciTech Connect

    Yang, Zhenxing; Wang, Guangjian; Guo, Yajie; Kang, Fangfang; Huang, Yanhong; Bo, Dongsheng

    2012-12-15

    Graphical abstract: CaF{sub 2} with different morphologies and hierarchical structure such as dendrites, spherical and cube was prepared under microwave-assisted condition by a simple solvothermal synthesis route using CaCl{sub 2} and [BMIM]BF{sub 4} as initial reagents, respectively. It was found that the species of precursor was of vital importance for the formation of CaF{sub 2} crystals. That is, precursors itself also acted as structure directing agent. The outstanding features of the approach to obtain hierarchical structure CaF{sub 2} were its simplicity, effectiveness and ease of assembly. On the basis of the experimental results, a possible growth mechanism of the CaF{sub 2} crystals was proposed. Display Omitted Highlights: ► CaF{sub 2} with hierarchical structure was synthesized under microwave-assisted conditions. ► Characteristic morphologies with cube, dendrite, hierarchical sphere, etc. were observed. ► Thin cubes assembled into a spherical structure. ► Ionic liquid of [BMIM]BF{sub 4} was fluorine source. ► Possible growth mechanisms of CaF{sub 2} crystals were discussed. -- Abstract: CaF{sub 2} with different morphologies and hierarchical structures was prepared under microwave-assisted condition by a simple hydrothermal route using CaCl{sub 2} and ionic liquid [BMIM]BF{sub 4} as initial reagents, respectively. It was found that both the precursor and pH values played an important role in the formation of CaF{sub 2} crystals with different morphologies. The results suggested that the CaF{sub 2} with cube and spherical structures was obtained at different pH values (4, 8, 11), while the CaF{sub 2} with dendrite shape was formed through an oriented self-assembly growth using (NH{sub 4}){sub 2}HPO{sub 4} as a structure directing agent. Scanning electron microscope observation showed that the as-prepared CaF{sub 2} was of three-dimensional eight-horn-shaped dendritic structure. The influence of the pH values for the reaction solution and

  16. Design of guanidinium ionic liquid based microwave-assisted extraction for the efficient extraction of Praeruptorin A from Radix peucedani.

    PubMed

    Ding, Xueqin; Li, Li; Wang, Yuzhi; Chen, Jing; Huang, Yanhua; Xu, Kaijia

    2014-12-01

    A series of novel tetramethylguanidinium ionic liquids and hexaalkylguanidinium ionic liquids have been synthesized based on 1,1,3,3-tetramethylguanidine. The structures of the ionic liquids were confirmed by (1)H NMR spectroscopy and mass spectrometry. A green guanidinium ionic liquid based microwave-assisted extraction method has been developed with these guanidinium ionic liquids for the effective extraction of Praeruptorin A from Radix peucedani. After extraction, reversed-phase high-performance liquid chromatography with UV detection was employed for the analysis of Praeruptorin A. Several significant operating parameters were systematically optimized by single-factor and L9 (3(4)) orthogonal array experiments. The amount of Praeruptorin A extracted by [1,1,3,3-tetramethylguanidine]CH2CH(OH)COOH is the highest, reaching 11.05 ± 0.13 mg/g. Guanidinium ionic liquid based microwave-assisted extraction presents unique advantages in Praeruptorin A extraction compared with guanidinium ionic liquid based maceration extraction, guanidinium ionic liquid based heat reflux extraction and guanidinium ionic liquid based ultrasound-assisted extraction. The precision, stability, and repeatability of the process were investigated. The mechanisms of guanidinium ionic liquid based microwave-assisted extraction were researched by scanning electron microscopy and IR spectroscopy. All the results show that guanidinium ionic liquid based microwave-assisted extraction has a huge potential in the extraction of bioactive compounds from complex samples.

  17. A Student-Centered First-Semester Introductory Organic Laboratory Curriculum Facilitated by Microwave-Assisted Synthesis (MAOS)

    ERIC Educational Resources Information Center

    Russell, Cianán B.; Mason, Jeremy D.; Bean, Theodore G.; Murphree, S. Shaun

    2014-01-01

    An instructional laboratory curriculum for a first-semester introductory organic chemistry course has been developed using microwave-assisted organic synthesis (MAOS). Taking advantage of short reaction times, materials were developed to facilitate collaborative experimental design, analysis, and debriefing of results during the normal laboratory…

  18. A Student-Centered First-Semester Introductory Organic Laboratory Curriculum Facilitated by Microwave-Assisted Synthesis (MAOS)

    ERIC Educational Resources Information Center

    Russell, Cianán B.; Mason, Jeremy D.; Bean, Theodore G.; Murphree, S. Shaun

    2014-01-01

    An instructional laboratory curriculum for a first-semester introductory organic chemistry course has been developed using microwave-assisted organic synthesis (MAOS). Taking advantage of short reaction times, materials were developed to facilitate collaborative experimental design, analysis, and debriefing of results during the normal laboratory…

  19. Application of response surface methodology to optimize microwave-assisted extraction of silymarin from milk thistle seeds

    USDA-ARS?s Scientific Manuscript database

    Several parameters of Microwave-assisted extraction (MAE) including extraction time, extraction temperature, ethanol concentration and solid-liquid ratio were selected to describe the MAE processing. The silybin content, measured by an UV-Vis spectrophotometry, was considered as the silymarin yield....

  20. Microwave-assisted synthesis of triple-helical, collagen-mimetic lipopeptides.

    PubMed

    Banerjee, Jayati; Hanson, Andrea J; Muhonen, Wallace W; Shabb, John B; Mallik, Sanku

    2010-01-01

    Collagen-mimetic peptides and lipopeptides are widely used as substrates for matrix degrading enzymes, as new biomaterials for tissue engineering, as drug delivery systems and so on. However, the preparation and subsequent purification of these peptides and their fatty-acid conjugates are really challenging. Herein, we report a rapid microwave-assisted, solid-phase synthetic protocol to prepare the fatty-acid conjugated, triple-helical peptides containing the cleavage site for the enzyme matrix metalloproteinase-9 (MMP-9). We employed a PEG-based resin as the solid support and the amino acids were protected with Fmoc- and tert-butyl groups. The amino acids were coupled at 50 degrees C (25 W of microwave power) for 5 min. The deprotection reactions were carried out at 75 degrees C (35 W of microwave power) for 3 min. Using this protocol, a peptide containing 23 amino acids was synthesized and then conjugated to stearic acid in 14 h.

  1. Microwave-assisted synthesis and electrochemical evaluation of VO2 (B) nanostructures

    SciTech Connect

    Ashton, Thomas E.; Borras, David Hevia; Iadecola, Antonella; Wiaderek, Kamila Magdalena; Chapman, Karena W.; Corr, Serena A.

    2015-12-01

    Understanding how intercalation materials change during electrochemical operation is paramount to optimising their behaviour and function and in situ characterisation methods allow us to observe these changes without sample destruction. Here, we first report the improved intercalation properties of bronze phase vanadium dioxide VO2 (B) prepared by a microwave assisted route which exhibits a larger electrochemical capacity (232 mAh g-1) compared to VO2 (B) prepared by a solvothermal route (197 mAh g-1). These electrochemical differences have also been followed using in situ X-ray absorption spectroscopy allowing us to follow oxidation state changes as they occur during battery operation.

  2. Microwave assisted conversion of microcrystalline cellulose into value added chemicals using dilute acid catalyst.

    PubMed

    Ching, Teck Wei; Haritos, Victoria; Tanksale, Akshat

    2017-02-10

    One of the grand challenges of this century is to transition fuels and chemicals production derived from fossil feedstocks to renewable feedstocks such as cellulosic biomass. Here we describe fast microwave conversion of microcrystalline cellulose (MCC) in water, with dilute acid catalyst to produce valuable platform chemicals. Single 10min microwave assisted treatment was able to convert >60% of MCC, with >50mol% yield of desirable products such as glucose, HMF, furfural and levulinic acid. Recycling of residual MCC with make-up fresh MCC resulted in an overall conversion of >93% after 5 cycles while maintaining >60% conversion in each cycle. Addition of isopropanol (70%v/v) as a co-solvent increased the yields of HMF and levulinic acid. This work shows for the first time proof of concept for complete conversion of recalcitrant microcrystalline cellulose in mild conditions of low temperature, dilute acid and short residence time using energy efficient microwave technology.

  3. Microwave-assisted rapid determination of vitamins a and e in beverages.

    PubMed

    Höller, Ulrich; Wolter, Didier; Hofmann, Peter; Spitzer, Volker

    2003-03-12

    A new rapid procedure for the determination of vitamins A and E in beverages has been developed and validated. Key steps include a microwave-assisted saponification of the sample and a single-step extraction of the vitamins prior to HPLC analysis. All sample preparation steps are carried out consecutively in the same vial. The vitamins are determined using normal-phase (Si-60) HPLC with fluorescence detection. The method is applicable to beverages with a content of all-trans-retinol >0.14 mg/L and/or a content of alpha-tocopherol >1 mg/L. Recoveries determined by spiking experiments ranged from 91.3 to 106.3%. The precision of the method is characterized by relative standard deviations of <2% for alpha-tocopherol and <5% for all-trans-retinol.

  4. Microwave assisted reconstruction of optical interferograms for distributed fiber optic sensing.

    PubMed

    Huang, Jie; Hua, Lei; Lan, Xinwei; Wei, Tao; Xiao, Hai

    2013-07-29

    This paper reports a distributed fiber optic sensing technique through microwave assisted separation and reconstruction of optical interferograms in spectrum domain. The approach involves sending a microwave-modulated optical signal through cascaded fiber optic interferometers. The microwave signal was used to resolve the position and reflectivity of each sensor along the optical fiber. By sweeping the optical wavelength and detecting the modulation signal, the optical spectrum of each sensor can be reconstructed. Three cascaded fiber optic extrinsic Fabry-Perot interferometric sensors were used to prove the concept. Their microwave-reconstructed interferogram matched well with those recorded individually using an optical spectrum analyzer. The application in distributed strain measurement has also been demonstrated.

  5. Microwave-assisted synthesis of carbon-supported carbides catalysts for hydrous hydrazine decomposition

    NASA Astrophysics Data System (ADS)

    Mnatsakanyan, Raman; Zhurnachyan, Alina R.; Matyshak, Valery A.; Manukyan, Khachatur V.; Mukasyan, Alexander S.

    2016-09-01

    Microwave-assisted synthesis of carbon-supported Mo2C and WC nanomaterials was studied. Two different routes were utilized to prepare MoO3 (WO3) - C precursors that were then subjected to microwave irradiation in an inert atmosphere. The effect of synthesis conditions, such as irradiation time and gas environment, was investigated. The structure and formation mechanism of the carbide phases were explored. As-synthesized nanomaterials exhibited catalytic activity for hydrous hydrazine (N2H4·H2O) decomposition at 30-70 °C. It was shown that the catalyst activity significantly increases if microwave irradiation is applied during the decomposition process. Such conditions permit complete conversion of hydrazine to ammonia and nitrogen within minutes. This effect can be attributed to the unique nanostructure of the catalysts that includes microwave absorbing carbon and active carbide constituents.

  6. Microwave-Assisted Synthesis, Microstructure, and Magnetic Properties of Rare-Earth Cobaltites.

    PubMed

    Gutiérrez Seijas, Julia; Prado-Gonjal, Jesús; Ávila Brande, David; Terry, Ian; Morán, Emilio; Schmidt, Rainer

    2017-01-03

    The series of perovskite rare-earth (RE) doped cobaltites (RE)CoO3 (RE = La-Dy) was prepared by microwave-assisted synthesis. The crystal structure undergoes a change of symmetry depending on the size of the RE cation. LaCoO3 is rhombohedral, S.G. R3̅c (No. 167), while, for the rest of the RE series (Pr-Dy), the symmetry is orthorhombic, S.G. Pnma (No. 62). The crystal structure obtained by X-ray diffraction was confirmed by high-resolution transmission electron microscopy, which yielded a good match between experimental and simulated images. It is further shown that the well-known magnetism in LaCoO3, which involves a thermally induced Co(3+) (d(6)) low spin to intermediate or high spin state transition, is strongly modified by the RE cation, and a rich variety of magnetic order has been detected across the series.

  7. Antioxidant activity and phenolic content of microwave-assisted Solanum melongena extracts.

    PubMed

    Salerno, Loredana; Modica, Maria N; Pittalà, Valeria; Romeo, Giuseppe; Siracusa, Maria A; Di Giacomo, Claudia; Sorrenti, Valeria; Acquaviva, Rosaria

    2014-01-01

    Eggplant fruit is a very rich source of polyphenol compounds endowed with antioxidant properties. The aim of this study was to extract polyphenols from eggplant entire fruit, pulp, or skin, both fresh and dry, and compare results between conventional extraction and microwave-assisted extraction (MAE). The effects of time exposure (15, 30, 60, and 90 min) and solvent (water 100% or ethanol/water 50%) were also evaluated. The highest amount of polyphenols was found in the extract obtained from dry peeled skin treated with 50% aqueous ethanol, irradiated with microwave; this extract contained also high quantity of flavonoids and showed good antioxidant activity expressed by its capacity to scavenge superoxide anion and to inhibit lipid peroxidation.

  8. Preliminary Study on Synthesis of Composite rGO/Ni by Microwave Assisted Method

    NASA Astrophysics Data System (ADS)

    Fakhri, Hafizh A.; Husnah, Miftahul; Hasdi Aimon, Akfiny; Ferry, Iskandar

    2017-07-01

    Composite reduced graphene oxide-nickel (rGO/Ni) was successfully synthesized by wet chemical process via microwave assisted method. The nickel fraction was varied 0%, 5% and 20%. Crystallinity, morphology, chemical composition, chemical bonding, and conductivity were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), elemental dispersive X-ray spectroscopy (EDS), Fourier transform infrared spectroscopy (FTIR), 4 point probes and electrochemical impedance spectroscopy (EIS). Based on the XRD patterns, the crystal sizes were 1.62 nm for 5% rGO/Ni and 1.64 nm for 20% rGO/Ni respectively. Furthermore, vibration of C=C aromatic stretching was detected in the FTIR spectra, which corresponds to rGO fingerprint. These results give a new perspective on synthesis of composite rGO/Ni.

  9. Preliminary Study of Heat Supply during Carbon Nanodots Synthesis by Microwave-assisted Method

    NASA Astrophysics Data System (ADS)

    Nakul, F.; Aimon, A. H.; Nuryadin, B. W.; Iskandar, F.

    2016-08-01

    Carbon nanodots (CNDs) are known to be good phosphor materials with wide range emission band, low cytotoxicity and excellent biocompatibility. In this work, CNDs were synthesized from a precursor consisting of citric acid [C6H8O7] as carbon source and urea [(NH2)2CO] as nitrogen source through a microwave-assisted method. The heat energy supplied during the microwave process was controlled. Further, we studied the effect of citric acid mass on the photoluminescence (PL) properties of the CNDs by varying its percentage in the precursors. The optimum luminescence intensity was obtained from the sample that was produced from 1.2 wt% citric acid mass. It had a single emission band with bright yellow luminescence.

  10. Antioxidant Activity and Phenolic Content of Microwave-Assisted Solanum melongena Extracts

    PubMed Central

    Modica, Maria N.; Pittalà, Valeria; Siracusa, Maria A.; Sorrenti, Valeria; Acquaviva, Rosaria

    2014-01-01

    Eggplant fruit is a very rich source of polyphenol compounds endowed with antioxidant properties. The aim of this study was to extract polyphenols from eggplant entire fruit, pulp, or skin, both fresh and dry, and compare results between conventional extraction and microwave-assisted extraction (MAE). The effects of time exposure (15, 30, 60, and 90 min) and solvent (water 100% or ethanol/water 50%) were also evaluated. The highest amount of polyphenols was found in the extract obtained from dry peeled skin treated with 50% aqueous ethanol, irradiated with microwave; this extract contained also high quantity of flavonoids and showed good antioxidant activity expressed by its capacity to scavenge superoxide anion and to inhibit lipid peroxidation. PMID:24683354

  11. Biodiesel from wet microalgae: extraction with hexane after the microwave-assisted transesterification of lipids.

    PubMed

    Cheng, Jun; Huang, Rui; Li, Tao; Zhou, Junhu; Cen, Kefa

    2014-10-01

    A chloroform-free novel process for the efficient production of biodiesel from wet microalgae is proposed. Crude biodiesel is produced through extraction with hexane after microwave-assisted transesterification (EHMT) of lipids in wet microalgae. Effects of different parameters, including reaction temperature, reaction time, methanol dosage, and catalyst dosage, on fatty acids methyl esters (FAMEs) yield are investigated. The yield of FAME extracted into the hexane from the wet microalgae is increased 6-fold after the transesterification of lipids. The yield of FAME obtained through EHMT of lipids in wet microalgae is comparable to that obtained through direct transesterification of dried microalgae biomass with chloroform; however, FAME content in crude biodiesel obtained through EHMT is 86.74%, while that in crude biodiesel obtained through the chloroform-based process is 75.93%. EHMT ensures that polar pigments present in microalgae are not extracted into crude biodiesel, which leads to a 50% reduction in nitrogen content in crude biodiesel.

  12. Microwave-assisted nile red method for in vivo quantification of neutral lipids in microalgae.

    PubMed

    Chen, Wei; Sommerfeld, Milton; Hu, Qiang

    2011-01-01

    In vivo determination of neutral lipids with Nile red fluorescence has been used as a rapid screening method for certain types of microalgae, but has been unsuccessful in others, particularly those with thick, rigid cell walls that prevent penetration of the fluorescence dye into the cell. To solve the problem, a microwave-assisted Nile red staining method for microalgal lipid determination was developed. In a two-step staining protocol, 50 and 60s were selected as the optimal microwave times for the pretreatment and staining process, respectively. Moreover, several calibration methods for quantitative analysis of neutral lipids in microalgae were investigated and compared with conventional gravimetric methods. Factors that affected the in vivo quantification of cellular neutral lipids were also investigated. Application of the new method for detection and quantification of neutral lipids in a number of green microalgae was demonstrated.

  13. Microwave-assisted synthesis of nanocrystalline TiO2 for dye-sensitized solar cells

    NASA Astrophysics Data System (ADS)

    Kuo, Ta-Chuan; Guo, Tzung-Fang; Chen, Peter

    2012-09-01

    The main purposes of this study are replacing conventional hydro-thermal method by microwave heating using water as reaction medium to rapidly synthesize TiO2.Titanium tetraisopropoxide (TTIP) was hydrolyzed in water. The solution is subsequently processed with microwave heating for crystal growth. The reaction time could be shortened into few minutes. Then we chose different acids as dispersion agents to prepare TiO2 paste for investigating the effects of dispersion on the power conversion efficiency of dye-sensitized solar cells (DSCs). The photovoltaic performance of the microwave-assisted synthesized TiO2 achieved power conversion efficiency of 6.31% under AM 1.5 G condition (100 mW/cm2). This PCE value is compatible with that of the devices made from commercial TiO2.

  14. Microwave assisted synthesis of bithiophene based donor-acceptor-donor oligomers and their optoelectronic performances

    NASA Astrophysics Data System (ADS)

    Bathula, Chinna; Buruga, Kezia; Lee, Sang Kyu; Khazi, Imtiyaz Ahmed M.; Kang, Youngjong

    2017-07-01

    In this article we present the synthesis of two novel bithiophene based symmetrical π conjugated oligomers with donor-acceptor-donor (D-A-D) structures by microwave assisted PdCl2(dppf) catalyzed Suzuki coupling reaction. These molecules contain electron rich bithiophene as a donor, dithienothiadiazole[3,4-c]pyridine and phthalic anhydride units as acceptors. The shorter reaction time, excellent yields and easy product isolation are the advantages of this method. The photophysical prerequisites for electronic application such as strong and broad optical absorption, thermal stability, and compatible energy levels were determined for synthesized oligomers. Optical band gap for the oligomers is found to be 1.72-1.90 eV. The results demonstrated the novel oligomers to be promising candidates in organic optoelectronic applications.

  15. Microwave-Assisted γ-Valerolactone Production for Biomass Lignin Extraction: A Cascade Protocol.

    PubMed

    Tabasso, Silvia; Grillo, Giorgio; Carnaroglio, Diego; Calcio Gaudino, Emanuela; Cravotto, Giancarlo

    2016-03-26

    The general need to slow the depletion of fossil resources and reduce carbon footprints has led to tremendous effort being invested in creating "greener" industrial processes and developing alternative means to produce fuels and synthesize platform chemicals. This work aims to design a microwave-assisted cascade process for a full biomass valorisation cycle. GVL (γ-valerolactone), a renewable green solvent, has been used in aqueous acidic solution to achieve complete biomass lignin extraction. After lignin precipitation, the levulinic acid (LA)-rich organic fraction was hydrogenated, which regenerated the starting solvent for further biomass delignification. This process does not requires a purification step because GVL plays the dual role of solvent and product, while the reagent (LA) is a product of biomass delignification. In summary, this bio-refinery approach to lignin extraction is a cascade protocol in which the solvent loss is integrated into the conversion cycle, leading to simplified methods for biomass valorisation.

  16. Multivariate optimisation of the microwave-assisted extraction of oleuropein and related biophenols from olive leaves.

    PubMed

    Japón-Luján, R; Luque-Rodríguez, J M; Luque de Castro, M D

    2006-06-01

    Microwave assistance is proposed for the first time in order to accelerate the extraction of biophenols from olive leaves. Under optimal working conditions, obtained using a multivariate methodology, complete extraction of the target analytes was achieved in 8 min. The extracts required no clean-up nor concentration prior to injection into a chromatograph-photodiode array detector assembly for individual separation-quantification. The optimal extractant (an 80:20 ethanol-water mixture) was also used in the development of a stirring-based extraction method which required around 24 h for complete extraction of the target compounds. These mixtures can be used as replacements for toxic extractants, with a view to exploiting olive leaves in order to obtain biophenols for human use.

  17. Influence of polarity on the scalability and reproducibility of solvent-free microwave-assisted reactions.

    PubMed

    Díaz-Ortiz, Angel; de la Hoz, Antonio; Alcázar, Jesús; Carrillo, José R; Herrero, María A; Fontana, Alberto; Muñoz, Juan de M; Prieto, Pilar; de Cózar, Abel

    2011-02-01

    Organic reactions performed in the absence of solvent in domestic ovens without appropriate temperature control are generally considered as not reproducible, particularly when different instruments are used. For this reason, reproducibility has historically been one of the major issues associated with Microwave-Assisted Organic Synthesis (MAOS) especially when domestic ovens are involved. The lack of reproducibility limits the general applicability and the scale up of these reactions. In this work several solvent-free reactions previously carried out in domestic ovens have been translated into a single-mode microwave reactor and then scaled up in a multimode oven. The results show that most of these reactions, although not considered as reproducible, can be easily updated and applied in microwave reactors using temperature-controlled conditions. Furthermore, computational calculations can assist to explain and/or predict whether a reaction will be reproducible or not.

  18. 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

  19. Rapid ZnO nanopillar array growth by microwave assisted heating

    NASA Astrophysics Data System (ADS)

    Yao, Jimmy; Chang, Yun-Ching; Mei, Hao; Cheng, Jiping; Yin, Stuart (Shizhuo); Luo, Claire

    2010-08-01

    Zinc oxide (ZnO) nano-wires have draw people's attention in recent studies. The unique structural and physical properties offer fascinating potential for future technological applications. The state-of-the-art fabrication process of ZnO nano-wires is based on vapor-liquid-solid (VLS) method. In this paper, the microwave assisted heating technique is introduced for the growth of ZnO nanopillar arrays. The microwave grown ZnO nanowires were characterized by fieldemission scanning electron microscopy, X-ray diffraction, transmission electron microscopy, and photoluminescence spectroscopy. It was demonstrated that (001) oriented single crystal ZnO nanowires can be grown vertically and uniformly on a-plane sapphire wafers.

  20. Microwave assisted extraction of sulfated polysaccharides (fucoidan) from Ascophyllum nodosum and its antioxidant activity.

    PubMed

    Yuan, Yuan; Macquarrie, Duncan

    2015-09-20

    Sulfated polysaccharides (fucoidan) from brown seaweed Ascophyllum nodosum were extracted by microwave assisted extraction (MAE) technology. Different conditions of temperature (90-150°C), extraction time (5-30 min) were evaluated and optimal fucoidan yield was 16.08%, obtained from 120°C for 15 min's extraction. Compositional analysis, GPC, HPAEC and IR analysis were employed for characterization of extracted sulfated polysaccharides. Fucose was the main monosaccharide of fucoidan extracted at 90°C while glucuronic acid was the main monosaccharide of fucoidan extracted at 150°C. Both the molecular weight and sulfate content of extracted fucoidan increased with decreasing extraction temperature. All fucoidans exhibited antioxidant activities as measured by DPPH scavenging and reducing power, among which fucoidan extracted at 90°C was highest. This study shows that MAE is an efficient technology to extract sulfated polysaccharides from seaweed and Ascophyllum nodosum could potentially be a resource for natural antioxidants.

  1. Microwave-assisted formation of organic monolayers from 1-alkenes on silicon carbide.

    PubMed

    van den Berg, Sebastiaan A; Alonso, Jose Maria; Wadhwa, Kuldeep; Franssen, Maurice C R; Wennekes, Tom; Zuilhof, Han

    2014-09-09

    The rate of formation of covalently linked organic monolayers on HF-etched silicon carbide (SiC) is greatly increased by microwave irradiation. Upon microwave treatment for 60 min at 100 °C (60 W), 1-alkenes yield densely packed, covalently attached monolayers on flat SiC surfaces, a process that typically takes 16 h at 130 °C under thermal conditions. This approach was extended to SiC microparticles. The monolayers were characterized by X-ray photoelectron spectroscopy and static water contact angle measurements. The microwave-assisted reaction is compatible with terminal functionalities such as alkenes that enable subsequent versatile "click" chemistry reactions, further broadening the range and applicability of chemically modified SiC surfaces.

  2. Timesaving microwave assisted synthesis of insulin amyloid fibrils with enhanced nanofiber aspect ratio.

    PubMed

    Carvalho, Tiago; Pinto, Ricardo J B; Martins, Manuel A; Silvestre, Armando J D; Freire, Carmen S R

    2016-11-01

    Insulin amyloid fibrils with enhanced aspect ratio, were prepared using a timesaving microwave assisted (MW) methodology, reducing the incubation time from 13 to 2h. The fibrillation process was followed indirectly by Thioflavin T Fluorescence and UV-vis analysis, by measuring the amount of β-sheets formed and the insulin present in solution, respectively. TEM and AFM analysis revealed that the insulin fibrils obtained through the MW method, have very similar lengths but are much thinner than the ones obtained using the conventional method (CM). Additionally, it was verified that the nature of the peptides present in the final insulin fibrils was not affected by microwave irradiation. These morphological differences might reflect on noticeably enhanced mechanical and optical properties that can exploited on the development of advanced bionanomaterials.

  3. Microwave-assisted 18O-labeling of proteins catalyzed by formic acid.

    PubMed

    Liu, Ning; Wu, Hanzhi; Liu, Hongxia; Chen, Guonan; Cai, Zongwei

    2010-11-01

    Oxygen exchange may occur at carboxyl groups catalyzed by acid. The reaction, however, takes at least several days at room temperature. The long-time exchanging reaction often prevents its application from protein analysis. In this study, an (18)O-labeling method utilizing microwave-assisted acid hydrolysis was developed. After being dissolved in (16)O/(18)O (1:1) water containing 2.5% formic acid, protein samples were exposed to microwave irradiation. LC-MS/MS analysis of the resulted peptide mixtures indicated that oxygen in the carboxyl groups from glutamic acid, aspartic acid, and the C-terminal residues could be efficiently exchanged with (18)O within less than 15 min. The rate of back exchange was so slow that no detectable back exchange could be found during the HPLC run.

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

    PubMed

    Solis-Pomar, F; Meléndrez, Mf; Esparza, R; Pérez-Tijerina, E

    2011-10-10

    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.

  5. Subnanosecond microwave-assisted magnetization switching in a circularly polarized microwave magnetic field

    NASA Astrophysics Data System (ADS)

    Suto, Hirofumi; Kanao, Taro; Nagasawa, Tazumi; Kudo, Kiwamu; Mizushima, Koichi; Sato, Rie

    2017-06-01

    We study microwave-assisted magnetization switching (MAS) of a perpendicularly magnetized nanomagnet with a diameter of 50 nm in a circularly polarized microwave magnetic field. The MAS effect appears when the rotation direction of the microwave field matches that of the ferromagnetic resonance excitation, and a large switching field decrease from 7.1 kOe to 1.5 kOe is demonstrated. In comparison with a linearly polarized microwave magnetic field, the circularly polarized microwave field induces the same MAS effect at half the microwave field amplitude, thereby showing its efficiency. We also examine MAS in the subnanosecond region and show that the magnetization switching can be induced by a microwave field with the duration of 0.2 ns.

  6. Microwave-assisted synthesis of Pt/CNT nanocomposite electrocatalysts for PEM fuel cells.

    PubMed

    Zhang, Weimin; Chen, Jun; Swiegers, Gerhard F; Ma, Zi-Feng; Wallace, Gordon G

    2010-02-01

    Microwave-assisted heating of functionalized, single-wall carbon nanotubes (FCNTs) in ethylene glycol solution containing H(2)PtCl(6), led to the reductive deposition of Pt nanoparticles (2.5-4 nm) over the FCNTs, yielding an active catalyst for proton-exchange membrane fuel cells (PEMFCs). In single-cell testing, the Pt/FCNT composites displayed a catalytic performance that was superior to Pt nanoparticles supported by raw (unfunctionalized) CNTs (RCNTs) or by carbon black (C), prepared under identical conditions. The supporting single-wall carbon nanotubes (SWNTs), functionalized with carboxyl groups, were studied by thermogravimetric analysis (TGA), cyclic voltammetry (CV), and Raman spectroscopy. The loading level, morphology, and crystallinity of the Pt/SWNT catalysts were determined using TGA, SEM, and XRD. The electrochemically active catalytic surface area of the Pt/FCNT catalysts was 72.9 m(2)/g-Pt.

  7. Microwave Assisted Synthesis, Characterisation and Fluorescence Studies of some Transition Metal Complexes with a Luminol Derivative.

    PubMed

    Aswathy, R; Mohanan, K

    2017-03-07

    A novel heterocyclic luminol derivative was synthesized by coupling diazotized 5-aminophthalhydrazide with 2-naphthol. This compound viz., Phthalhydrazide-5-azo-2-naphthol is versatile in forming stable metal complexes with cobalt(II), nickel(II), copper(II) and zinc(II) ions under microwave assisted solvent free conditions. The ligand and the metal complexes were characterized on the basis of elemental analyses, molar conductance, magnetic susceptibility measurements, UV-Visible, IR, (1)H NMR, and ESR spectral studies wherever possible and applicable. The fluorescence spectra of the ligand and its metal complexes were also recorded. The fluorescence life time measurements were conducted and it was observed that binding of the ligand to the metal ion decreases the average life time of the metal complexes.

  8. Microwave-assisted extraction versus Soxhlet extraction in the analysis of 21 organochlorine pesticides in plants.

    PubMed

    Barriada-Pereira, M; Concha-Graña, E; González-Castro, M J; Muniategui-Lorenzo, S; López-Mahía, P; Prada-Rodríguez, D; Fernández-Fernández, E

    2003-08-01

    A method to determine 21 organochlorine pesticides in vegetation samples using microwave-assisted extraction (MAE) is described and compared with Soxhlet extraction. Samples were extracted with hexane-acetone (1:1, v/v) and the extracts were cleaned using solid-phase extraction with Florisil and alumine as adsorbents. Pesticides were eluted with hexane-ethyl acetate (80:20, v/v) and determined by gas chromatography and electron-capture detection. Recoveries obtained (75.5-132.7% for Soxhlet extraction and 81.5-108.4% for MAE) show that both methods are suitable for the determination of chlorinated pesticides in vegetation samples. The method using microwave energy was applied to grass samples from parks of A Coruña (N.W. Spain) and to vegetation from the contaminated industrial area of Torneiros (Pontevedra, N.W. Spain).

  9. Development of microwave assisted spectrophotometric method for the determination of glucose

    NASA Astrophysics Data System (ADS)

    Ali, Asif; Hussain, Zahid; Arain, Muhammad Balal; Shah, Nasrullah; Khan, Khalid Mohammad; Gulab, Hussain; Zada, Amir

    2016-01-01

    A spectrophotometric method was developed based on the microwave assisted synthesis of Maillard product. Various conditions of the reaction were optimized by varying the relative concentration of the reagents, operating temperature and volume of solutions used in the reaction in the microwave synthesizer. The absorbance of the microwave synthesized Maillard product was measured in the range of 360-740 nm using UV-Visible spectrophotometer. Based on the maximum absorbance, 370 nm was selected as the optimum wave length for further studies. The LOD and LOQ of glucose was found 3.08 μg mL- 1 and 9.33 μg mL- 1 with standard deviation of ± 0.05. The developed method was also applicable to urine sample.

  10. Microwave-assisted one-step patterning of aqueous colloidal silver.

    PubMed

    Yang, G; Zhou, Y W; Guo, Z R; Wan, Y; Ding, Q; Bai, T T; Wang, C L; Gu, N

    2012-07-05

    A new approach of utilizing microwave to pattern gradient concentric silver nanoparticle ring structures has been presented. The width and height of a single ring and the space between adjacent rings can be adjusted by changing the silver colloidal concentration and the microwave output power. By simply enhancing the ambient vapour pressure to the saturated value during microwave-assisted evaporation, sub-100 nm rings can be deposited in between adjacent micro-rings over a distance of millimetres. Combined with microwave sintering, this approach can also create conductive silver tracks in a single step, showing huge potential in fabricating micro- and nano-electronic devices in an ultra-fast and cost-effective fashion.

  11. Modified microwave-assisted extraction of ergosterol for measuring fungal biomass in grain cultures.

    PubMed

    Zhang, Huimin; Wolf-Hall, Charlene; Hall, Clifford

    2008-12-10

    Ergosterol is a measure for fungal biomass. The recovery rates using a previously described microwave-assisted-extraction (MAE) method for ergosterol analysis tended to be low for grain cultures (pure culture in sterilized 40% moisture content grain) inoculated with Fusarium graminearum . An improved MAE method for measuring ergosterol in grain cultures was developed and compared. Modification to the original MAE included alterations in duration of microwave exposure and extraction solvents. Four autoclaved grains (wheat, rice, barley, and corn) were inoculated with F. graminearum or spiked with ergosterol at concentrations from 0.88 to 100 microg/g and extracted with both methods. The ergosterol recovery rates were significantly different (p < 0.05) for the two methods in assaying both the spiked and grain culture samples. The modified method provided greater recovery rates than the previously reported MAE method for the spiked samples and F. graminearum grain cultures.

  12. Microwave assisted alkali-catalyzed transesterification of Pongamia pinnata seed oil for biodiesel production.

    PubMed

    Kumar, Ritesh; Kumar, G Ravi; Chandrashekar, N

    2011-06-01

    In this study, microwave assisted transesterification of Pongamia pinnata seed oil was carried out for the production of biodiesel. The experiments were carried out using methanol and two alkali catalysts i.e., sodium hydroxide (NaOH) and potassium hydroxide (KOH). The experiments were carried out at 6:1 alcohol/oil molar ratio and 60°C reaction temperature. The effect of catalyst concentration and reaction time on the yield and quality of biodiesel was studied. The result of the study suggested that 0.5% sodium hydroxide and 1.0% potassium hydroxide catalyst concentration were optimum for biodiesel production from P. pinnata oil under microwave heating. There was a significant reduction in reaction time for microwave induced transesterification as compared to conventional heating.

  13. Microwave-assisted extraction of the main phenolic compounds in flaxseed.

    PubMed

    Beejmohun, Vickram; Fliniaux, Ophélie; Grand, Eric; Lamblin, Frédéric; Bensaddek, Lamine; Christen, Philippe; Kovensky, José; Fliniaux, Marc-André; Mesnard, François

    2007-01-01

    A microwave-assisted extraction (MAE) method has been applied for the first time to the extraction of the main lignan, secoisolariciresinol diglucoside (SDG), and the two most concentrated hydroxycinnamic acid glucosides in flaxseed. The effects of microwave power, extraction time and alkaline treatment were investigated. It was shown that a 3 min MAE resulted in an SDG content of 16.1+/-0.4 mg/g, a p-coumaric acid glucoside content of 3.7+/-0.2 mg/g and a ferulic acid glucoside content of 4.1+/-0.2 mg/g. These values were compared with those obtained using conventional extraction methods and the results demonstrated that MAE was more effective in terms of both yield and time consumption.

  14. Microwave-assisted hydrothermal extraction of sulfated polysaccharides from Ulva spp. and Monostroma latissimum.

    PubMed

    Tsubaki, Shuntaro; Oono, Kiriyo; Hiraoka, Masanori; Onda, Ayumu; Mitani, Tomohiko

    2016-11-01

    Microwave-assisted hydrothermal extraction was applied for production of sulfated polysaccharides from Ulva spp. and Monostroma latissimum. The maximum ulvan yields attained 40.4±3.2% (Ulva meridionalis) and 36.5±3.1% (Ulva ohnoi) within 4min of come-up time and 10min of extraction time at 160°C, respectively. The rhamnan sulfate yield from M. latissimum further attained 53.1±7.2% at 140°C. The sulfated polysaccharides were easily recovered from the extract by simple ethanol precipitation. In addition, molecular weights and viscosity of the extracted polysaccharides could be controlled by varying the extraction temperature. Dielectric measurement revealed that ionic conduction was the important parameter that affect the microwave susceptibility of algae-water mixture. The sulfated polysaccharides extracts are expected as potential feedstock for medical and food applications. Copyright © 2016 Elsevier Ltd. All rights reserved.

  15. Microwave assisted synthesis and characterization of barium titanate nanoparticles for multi layered ceramic capacitor applications.

    PubMed

    Thirumalai, Sundararajan; Shanmugavel, Balasivanandha Prabu

    2011-01-01

    Barium titanate is a common ferroelectric electro-ceramic material having high dielectric constant, with photorefractive effect and piezoelectric properties. In this research work, nano-scale barium titanate powders were synthesized by microwave assisted mechano-chemical route. Suitable precursors were ball milled for 20 hours. TGA studies were performed to study the thermal stability of the powders. The powders were characterized by XRD, SEM and EDX Analysis. Microwave and Conventional heating were performed at 1000 degrees C. The overall heating schedule was reduced by 8 hours in microwave heating thereby reducing the energy and time requirement. The nano-scale, impurity-free and defect-free microstructure was clearly evident from the SEM micrograph and EDX patterns. LCR meter was used to measure the dielectric constant and dielectric loss values at various frequencies. Microwave heated powders showed superior dielectric constant value with low dielectric loss which is highly essential for the fabrication of Multi Layered Ceramic Capacitors.

  16. Process optimization and analysis of microwave assisted extraction of pectin from dragon fruit peel.

    PubMed

    Thirugnanasambandham, K; Sivakumar, V; Prakash Maran, J

    2014-11-04

    Microwave assisted extraction (MAE) technique was employed for the extraction of pectin from dragon fruit peel. The extracting parameters were optimized by using four-variable-three-level Box-Behnken design (BBD) coupled with response surface methodology (RSM). RSM analysis indicated good correspondence between experimental and predicted values. 3D response surface plots were used to study the interactive effects of process variables on extraction of pectin. The optimum extraction conditions for the maximum yield of pectin were power of 400 W, temperature of 45 °C, extracting time of 20 min and solid-liquid ratio of 24 g/mL. Under these conditions, 7.5% of pectin was extracted.

  17. One step microwaved-assisted hydrothermal synthesis of nitrogen doped graphene for high performance of supercapacitor

    NASA Astrophysics Data System (ADS)

    Sari, Fitri Nur Indah; Ting, Jyh-Ming

    2015-11-01

    Nitrogen doped graphene (NDG) has been synthesized using a microwave-assisted hydrothermal (MHT) method within only several minute. In the method, homemade graphene oxide was reduced using ethylene glycol (EG) to obtain the graphene while ammonia liquid was used as the nitrogen source. However, it was found that the reduction and doping simultaneously occurred and the addition of ammonia further enhanced the reduction. The reduction and doping were examined through various analysis and the mechanisms were proposed. The effects of the hydrothermal temperature and time on the reduction and doping were discussed. It was also shown that the doping leads to enhanced specific capacitance by as much as 54%, a high specific energy density of 42.8 W h kg-1 at a power density of 4330 W kg-1, and excellent long term stability up to 98% retention after 1000 cycles at wide working voltage of 1.6 V in 2 M H2SO4.

  18. Microwave-assisted techniques (MATs); a quick way to extract a fragrance: a review.

    PubMed

    Kokolakis, Antonios K; Golfinopoulos, Spyridon K

    2013-10-01

    In recent years microwave-assisted techniques (MATs) have been introduced as a new process design and operation for essential oils extraction, representing a viable alternative to conventional old-type methods of distillation which are routinely used for the isolation of essential oils from herbs, flowers and spices prior to gas chromatographic analysis. The novelty of the technique lies in a microwave heating source generating a mixture of boiling solvent with the raw plant material settled above (or drenched inside). Several variations of distillation techniques are evaluated in terms of substantial energy saving, rapidity, product yield, cleanliness and product quality. Results confirm the effectiveness of MATs, which allow extraction of essential oils in shorter extraction time (up-to 9 times faster), using "greener" procedures and provide a higher quality essential oil with better sensory and antioxidant properties.

  19. Microwave-assisted hydrolysis of lutein and zeaxanthin esters in marigold (Tagetes erecta L.).

    PubMed

    Liu, Hongcheng; Zhang, Ying; Zheng, Bin; Li, Qiwan; Zou, Yanhong

    2011-12-01

    Saponification of lutein and zeaxanthin was performed by microwave-assisted hydrolysis (MAH) and analysed by ultra performance liquid chromatography. The optimal condition of MAH was studied, and the degradation or isomerization of lutein and zeaxanthin were estimated under MAH. The concentrations of lutein and zeaxanthin in 20 marigold samples were assessed by saponification using traditional heater and MAH, the regression coefficient of lutein obtained by two methods was 0.9688 and that of zeaxanthin was 0.9527. The limit of detection for lutein and zeaxanthin was 0.05 and 0.1 μg/ml, respectively, and the limit of quantification for lutein and zeaxanthin was 0.05 mg/100 g and 0.1 mg/100 g, respectively.

  20. Microwave-assisted synthesis of gold nanoparticles self-assembled into self-supported superstructures

    PubMed Central

    Esparza, R.; Vargas-Hernández, C.; Fernández García, M. E.; José-Yacamán, M.

    2014-01-01

    Passivated gold nanoparticles were synthesized through a microwave-assisted process in a two-phase system, in the presence of 1-dodecanethiol. An average particle size of 1.8 nm of the gold nanoparticles obtained and 0.35 S.D. was determined through HRTEM and STEM analysis. It was observed that these nanoparticles spontaneously self-assemble into self-supported superstructures of 1 μm in diameter avg and 400 nm thickness, yielding an off-white powder which can be handled as a simple powder. XRD analysis indicates that n-alkanethiol molecules used as a passivating compound, besides protecting against crystal growth, interact to form cubic ordered arrays between the nanoparticles. This interaction leads to the superstructure formation, with an average distance between nanoparticles in the array, of 3.56 nm. Theoretical calculations and molecular dynamics simulations were performed to analyze the resulting structure. PMID:22398420

  1. Preparation Of KF-Modified Kaolinite As Green And Reusable Catalyst For Microwave Assisted Biodiesel Conversion

    NASA Astrophysics Data System (ADS)

    Fatimah, I.; Andiena, R. Z.; Yudha, S. P.

    2017-02-01

    Preparation of KF-modified kaolinite catalyst for microwave-assisted biodiesel conversion has been investigated. Kaolinite modification was conducted by solid-solid reaction between naturally occurring kaolinite mineral and KF salt followed by heating at 200oC for 2h. Prepared catalyst was characterized by using XRD, BET surface area analyzer, and SEM-EDX analysis and for catalytic activity tests, biodiesel conversion of jatropha oil was simulated. The comparison between microwave utilization and conventional method of biodiesel conversion were studied, moreover study on the catalyst reusability was performed. The results show that prepared catalyst gives the better physicochemical character of kaolinite as heterogeneous catalysts application as shown by the higher conversion and also reusability. Furthermore, the use of microwave irradiation exhibits the more time effectiveness. In general, the greener biodiesel conversion using presented methods is promising technique to be developed.

  2. The microwave assisted-synthesis of carboxymethyl cellulose from nata de-coco bacterial cellulose

    NASA Astrophysics Data System (ADS)

    Ramadhan, L. O. A. N.; Nur Rahmat, M.; Susilowati, P. E.; Ahmad, L. O.; Edy Rusbandi, U.

    2017-07-01

    Bacterial cellulose (BC) is one of natural biopolymers which can be derivatized to make functionalized materials. Carboxymethyl cellulose (CMC) is a candidate derivative for such a direction. The aim of the present study is to investigate the usability of microwave energy to transform BC into CMC. The results showed that CMC was produced in a yellowish white powder by a short irradiation for 30 s at 650 W. The best combination of monochloroacetic acid and BC as anhydrogucose unit was found at the molar ratio of 1:5. The obtained CMC is soluble in distilled water, and aqueous NaOH solution. The highest degree of substitution, viscosity, and molecular weight of the CMC are 0.263, 15.61 Pa·s and 197,187, respectively. This study showed the usefulness of the microwave-assisted reaction to transform BC rapidly into water-soluble ionized derivative.

  3. Fabrication of silica nanostructures with a microwave assisted direct patterning process

    NASA Astrophysics Data System (ADS)

    Shin, Ju-Hyeon; Go, Bit-Na; Choi, Je-Hong; Kim, Jin-Seoung; Jung, Gun-Young; Kim, Heetae; Lee, Heon

    2014-06-01

    Silica nanostructures were fabricated on glass substrate using a microwave assisted direct patterning (MADP) process, which is a variety of soft lithography. During the MADP process using polydimethylsiloxane (PDMS), mold and microwave heating are performed simultaneously. Blanket thin film and micro- to nano-sized structures, including moth-eye patterns of SiO2, which consisted of coalesced silica nanoparticles, were formed on glass substrates from SiO2 nano-particle dispersed solutions with varied microwave heating time. Optical properties and surface morphologies of micro-sized hemisphere, nano-sized pillar, moth-eye and 50 nm sized line/space silica patterns were measured using UV-vis and a scanning electron microscope. X-ray diffraction analysis of SiO2 thin films with and without microwave heating was also carried out.

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

    NASA Astrophysics Data System (ADS)

    Solis-Pomar, F.; Meléndrez, Mf; Esparza, R.; Pérez-Tijerina, E.

    2011-10-01

    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.

  5. Defect chemistry of phospho-olivine nanoparticles synthesized by a microwave-assisted solvothermal process

    SciTech Connect

    Bridges, Craig A.; Harrison, Katharine L.; Unocic, Raymond R.; Idrobo, Juan-Carlos; Parans Paranthaman, M.; Manthiram, Arumugam

    2013-09-15

    Nanocrystalline LiFePO{sub 4} powders synthesized by a microwave-assisted solvothermal (MW-ST) process have been structurally characterized with a combination of high resolution powder neutron diffraction, synchrotron X-ray diffraction, and aberration-corrected HAADF STEM imaging. A significant level of defects has been found in the samples prepared at 255 and 275 °C. These temperatures are significantly higher than what has previously been suggested to be the maximum temperature for defect formation in LiFePO{sub 4}, so the presence of defects is likely related to the rapid MW-ST synthesis involving a short reaction time (∼5 min). A defect model has been tentatively proposed, though it has been shown that powder diffraction data alone cannot conclusively determine the precise defect distribution in LiFePO{sub 4} samples. The model is consistent with other literature reports on nanopowders synthesized at low temperatures, in which the unit cell volume is significantly reduced relative to defect-free, micron-sized LiFePO{sub 4} powders. - Graphical abstract: Temperature-dependent antisite defect formation has been observed in nanocrystalline LiFePO{sub 4} powders synthesized by a microwave solvothermal process, using high resolution diffraction and STEM imaging. Display Omitted - Highlights: • LiFePO{sub 4} nanopowders synthesized by a microwave-assisted solvothermal process. • Defects directly observed by aberration-corrected HAADF STEM imaging. • Antisite defects present from synthesis at 255 and 275 °C. • Defects present from higher temperature synthesis than previously reported. • Powder diffraction data have been analyzed in detail for various defect models.

  6. Microwave-assisted synthesis and optical properties of cuprous oxide micro/nanocrystals

    SciTech Connect

    Sun, Dandan; Du, Yi; Tian, Xiuying; Li, Zhongfu; Chen, Zhongtao; Zhu, Chaofeng

    2014-12-15

    Graphical abstract: Cuprous oxide micro/nanocrystals were fabricated by a facile and green microwave-assisted method using soluble starch as reductant and dispersant. Spheres with the diameter of about 100 and 600 nm, octahedron and truncated octahedron with the edge length of about 0.8–3 μm cuprous oxide micro/nanocrystals were successfully obtained. Microwave heating was proved to be a efficient method and was advantageous to the homogeneous nucleation. Growth mechanism of the prepared Cu{sub 2}O microcrystals were investigated carefully. Furthermore, the optical properties of the prepared cuprous oxide microcrystals were investigated by UV–vis diffuse reflectance spectroscopy, demonstrating that their band gaps of obtained samples were 1.96–2.07 eV, assigned to their different sizes and morphologies. - Abstract: Cuprous oxide micro/nanocrystals were fabricated by a facile and green microwave-assisted method using soluble starch as reductant and dispersant. It was observed that the addition amounts of NaOH had a prominent effect on the morphologies and size of cuprous oxide products, and microwave heating was proved to be a efficient method and was advantageous to the homogeneous nucleation. The as-obtained samples were characterized by X-ray diffraction (XRD), and field-emission scanning electron microscopy (FESEM). The results indicated that the samples were pure cuprous oxide. Spheres with the diameter of about 100 and 600 nm, octahedron and truncated octahedron with the edge length of about 0.8–3 μm cuprous oxide micro/nanocrystals were successfully obtained. Furthermore, the UV–vis diffuse reflectance spectroscopy was used to investigate the optical properties of the prepared cuprous oxide microcrystals, demonstrating that their band gaps of obtained samples were 1.96–2.07 eV, assigned to their different sizes and morphologies.

  7. Kinetics and Quality of Microwave-Assisted Drying of Mango (Mangifera indica)

    PubMed Central

    Abano, Ernest Ekow

    2016-01-01

    The effect of microwave-assisted convective air-drying on the drying kinetics and quality of mango was evaluated. Both microwave power and pretreatment time were significant factors but the effect of power was more profound. Increase in microwave power and pretreatment time had a positive effect on drying time. The nonenzymatic browning index of the fresh samples increased from 0.29 to 0.60 while the ascorbic acid content decreased with increase in microwave power and time from 3.84 mg/100g to 1.67 mg/100g. The effective moisture diffusivity varied from 1.45 × 10−9 to 2.13 × 10−9 m2/s for microwave power range of 300-600 W for 2 to 4 minutes of pretreatment. The Arrhenius type power-dependent activation energy was found to be in the range of 8.58–17.48 W/mm. The fitting of commonly used drying models to the drying data showed the Midilli et al. model as the best. Microwave power of 300 W and pretreatment time of 4 minutes emerged as the optimum conditions prior to air-drying at 7°C. At this ideal condition, the energy savings as a result of microwave application was approximately 30%. Therefore, microwave-assisted drying should be considered for improved heat and mass transfer processes during drying to produce dried mangoes with better quality. PMID:26904667

  8. Ethanol production from cashew apple bagasse: improvement of enzymatic hydrolysis by microwave-assisted alkali pretreatment.

    PubMed

    Rodrigues, Tigressa Helena Soares; Rocha, Maria Valderez Ponte; de Macedo, Gorete Ribeiro; Gonçalves, Luciana R B

    2011-07-01

    In this work, the potential of microwave-assisted alkali pretreatment in order to improve the rupture of the recalcitrant structures of the cashew able bagasse (CAB), lignocellulosic by-product in Brazil with no commercial value, is obtained from cashew apple process to juice production, was studied. First, biomass composition of CAB was determined, and the percentage of glucan and lignin was 20.54 ± 0.70% and 33.80 ± 1.30%, respectively. CAB content in terms of cellulose, hemicelluloses, and lignin, 19.21 ± 0.35%, 12.05 ± 0.37%, and 38.11 ± 0.08%, respectively, was also determined. Results showed that, after enzymatic hydrolysis, alkali concentration exerted influence on glucose formation, after pretreatment with 0.2 and 1.0 mo L(-1) of NaOH (372 ± 12 and 355 ± 37 mg g(glucan)(-1) ) when 2% (w/v) of cashew apple bagasse pretreated by microwave-assisted alkali pretreatment (CAB-M) was used. On the other hand, pretreatment time (15-30 min) and microwave power (600-900 W) exerted no significant effect on hydrolysis. On enzymatic hydrolysis step, improvement on solid percentage (16% w/v) and enzyme load (30 FPU g (CAB-M) (-1) ) increased glucose concentration to 15 g L(-1). The fermentation of the hydrolyzate by Saccharomyces cerevesiae resulted in ethanol concentration and productivity of 5.6 g L(-1) and 1.41 g L(-1) h(-1), respectively.

  9. Final Technical Report Microwave Assisted Electrolyte Cell for Primary Aluminum Production

    SciTech Connect

    Xiaodi Huang; J.Y. Hwang

    2007-04-18

    This research addresses the high priority research need for developing inert anode and wetted cathode technology, as defined in the Aluminum Industry Technology Roadmap and Inert Anode Roadmap, with the performance targets: a) significantly reducing the energy intensity of aluminum production, b) ultimately eliminating anode-related CO2 emissions, and c) reducing aluminum production costs. This research intended to develop a new electrometallurgical extraction technology by introducing microwave irradiation into the current electrolytic cells for primary aluminum production. This technology aimed at accelerating the alumina electrolysis reduction rate and lowering the aluminum production temperature, coupled with the uses of nickel based superalloy inert anode, nickel based superalloy wetted cathode, and modified salt electrolyte. Michigan Technological University, collaborating with Cober Electronic and Century Aluminum, conducted bench-scale research for evaluation of this technology. This research included three sub-topics: a) fluoride microwave absorption; b) microwave assisted electrolytic cell design and fabrication; and c) aluminum electrowinning tests using the microwave assisted electrolytic cell. This research concludes that the typically used fluoride compound for aluminum electrowinning is not a good microwave absorbing material at room temperature. However, it becomes an excellent microwave absorbing material above 550°C. The electrowinning tests did not show benefit to introduce microwave irradiation into the electrolytic cell. The experiments revealed that the nickel-based superalloy is not suitable for use as a cathode material; although it wets with molten aluminum, it causes severe reaction with molten aluminum. In the anode experiments, the chosen superalloy did not meet corrosion resistance requirements. A nicked based alloy without iron content could be further investigated.

  10. Beneficial effects of microwave-assisted heating versus conventional heating in noble metal nanoparticle synthesis.

    PubMed

    Dahal, Naween; García, Stephany; Zhou, Jiping; Humphrey, Simon M

    2012-11-27

    An extensive comparative study of the effects of microwave versus conventional heating on the nucleation and growth of near-monodisperse Rh, Pd, and Pt nanoparticles has revealed distinct and preferential effects of the microwave heating method. A one-pot synthetic method has been investigated, which combines nucleation and growth in a single reaction via precise control over the precursor addition rate. Using this method, microwave-assisted heating enables the convenient preparation of polymer-capped nanoparticles with improved monodispersity, morphological control, and higher crystallinity, compared with samples heated conventionally under otherwise identical conditions. Extensive studies of Rh nanoparticle formation reveal fundamental differences during the nucleation phase that is directly dependent on the heating method; microwave irradiation was found to provide more uniform seeds for the subsequent growth of larger nanostructures of desired size and surface structure. Nanoparticle growth kinetics are also markedly different under microwave heating. While conventional heating generally yields particles with mixed morphologies, microwave synthesis consistently provides a majority of tetrahedral particles at intermediate sizes (5-7 nm) or larger cubes (8+ nm) upon further growth. High-resolution transmission electron microscopy indicates that Rh seeds and larger nanoparticles obtained from microwave-assisted synthesis are more highly crystalline and faceted versus their conventionally prepared counterparts. Microwave-prepared Rh nanoparticles also show approximately twice the catalytic activity of similar-sized conventionally prepared particles, as demonstrated in the vapor-phase hydrogenation of cyclohexene. Ligand exchange reactions to replace polymer capping agents with molecular stabilizing agents are also easily facilitated under microwave heating, due to the excitation of polar organic moieties; the ligand exchange proceeds with excellent retention of

  11. Room temperature ferromagnetism in undoped and Fe doped ZnO nanorods: Microwave-assisted synthesis

    SciTech Connect

    Limaye, Mukta V.; Singh, Shashi B.; Das, Raja; Poddar, Pankaj; Kulkarni, Sulabha K.

    2011-02-15

    One-dimensional (1D) undoped and Fe doped ZnO nanorods of average length {approx}1 {mu}m and diameter {approx}50 nm have been obtained using a microwave-assisted synthesis. The magnetization (M) and coercivity (H{sub c}) value obtained for undoped ZnO nanorods at room temperature is {approx}5x10{sup -3} emu/g and {approx}150 Oe, respectively. The Fe doped ZnO samples show significant changes in M -H loop with increasing doping concentration. Both undoped and Fe doped ZnO nanorods exhibit a Curie transition temperature (T{sub c}) above 390 K. Electron spin resonance and Moessbauer spectra indicate the presence of ferric ions. The origin of ferromagnetism in undoped ZnO nanorods is attributed to localized electron spin moments resulting from surface defects/vacancies, where as in Fe doped samples is explained by F center exchange mechanism. -- Graphical abstract: Room temperature ferromagnetism has been reported in undoped and Fe doped ZnO nanorods of average length {approx}1 {mu}m and diameter {approx}50 nm. Display Omitted Research Highlights: {yields} Microwave-assisted synthesis of undoped and Fe doped ZnO nanorods. {yields} Observation of room temperature ferromagnetism in undoped and Fe doped ZnO nanorods. {yields} Transition temperature (T{sub c}) obtained in undoped and doped samples is above 390 K. {yields} In undoped ZnO origin of ferromagnetism is explained in terms of defects/vacancies. {yields} Ferromagnetism in Fe doped ZnO is explained by F-center exchange mechanism.

  12. Microwave-assisted hydrothermal synthesis of zinc oxide particles starting from chloride precursor

    SciTech Connect

    Tseng, Chun-Chieh; Chou, Yu-Hsien; Liu, Chung-Ming; Liu, Yih-Ming; Ger, Ming-Der; Shu, Youn-Yuen

    2012-01-15

    Graphical abstract: Schematic of the mechanism for ZnO nanoparticles obtained by the calcination. Highlights: Black-Right-Pointing-Pointer Nanocrystalline ZnO particles were successfully prepared by a microwave-assisted method. Black-Right-Pointing-Pointer Sponge-like morphology of ZnO change to a net-like structure after thermal treatment. Black-Right-Pointing-Pointer The PL spectra exhibited a nearband-edge emission at 393 nm. -- Abstract: Zinc oxide (ZnO) was synthesized using a microwave assisted hydrothermal (MAH) process based on chloride/urea/water solution and under 800 W irradiation for 5 min. In the bath, Zn{sup 2+} ions reacted with the complex carbonate and hydroxide ions to form zinc carbonate hydroxide hydrate (Zn{sub 4}CO{sub 3}(OH){sub 6}{center_dot}H{sub 2}O), and the conversion from Zn{sub 4}CO{sub 3}(OH){sub 6}{center_dot}H{sub 2}O to ZnO was synchronously achieved by a MAH process. The as-prepared ZnO has a sponge-like morphology. However, the initial sponge-like morphology of ZnO could change to a net-like structure after thermal treatment, and compact nano-scale ZnO particles were finally obtained when the period of thermal treatment increased to 30 min. Pure ZnO nanoparticles was obtained from calcination of loose sponge-like ZnO particles at 500 Degree-Sign C. The analysis of optical properties of these ZnO nanoparticles showed that the intensity of 393 nm emission increased with the calcination temperature because the defects were reduced and the crystallinity was improved.

  13. Microwave-Assisted Alkali Pre-Treatment, Densification and Enzymatic Saccharification of Canola Straw and Oat Hull

    PubMed Central

    Agu, Obiora S.; Tabil, Lope G.; Dumonceaux, Tim

    2017-01-01

    The effects of microwave-assisted alkali pre-treatment on pellets’ characteristics and enzymatic saccharification for bioethanol production using lignocellulosic biomass of canola straw and oat hull were investigated. The ground canola straw and oat hull were immersed in distilled water, sodium hydroxide and potassium hydroxide solutions at two concentrations (0.75% and 1.5% w/v) and exposed to microwave radiation at power level 713 W and three residence times (6, 12 and 18 min). Bulk and particle densities of ground biomass samples were determined. Alkaline-microwave pre-treated and untreated samples were subjected to single pelleting test in an Instron universal machine, pre-set to a load of 4000 N. The measured parameters, pellet density, tensile strength and dimensional stability were evaluated and the results showed that the microwave-assisted alkali pre-treated pellets had a significantly higher density and tensile strength compared to samples that were untreated or pre-treated by microwave alone. The chemical composition analysis showed that microwave-assisted alkali pre-treatment was able to disrupt and break down the lignocellulosic structure of the samples, creating an area of cellulose accessible to cellulase reactivity. The best enzymatic saccharification results gave a high glucose yield of 110.05 mg/g dry sample for canola straw ground in a 1.6 mm screen hammer mill and pre-treated with 1.5% NaOH for 18 min, and a 99.10 mg/g dry sample for oat hull ground in a 1.6 mm screen hammer mill and pre-treated with 0.75% NaOH for 18 min microwave-assisted alkali pre-treatments. The effects of pre-treatment results were supported by SEM analysis. Overall, it was found that microwave-assisted alkali pre-treatment of canola straw and oat hull at a short residence time enhanced glucose yield. PMID:28952504

  14. Microwave-Assisted Alkali Pre-Treatment, Densification and Enzymatic Saccharification of Canola Straw and Oat Hull.

    PubMed

    Agu, Obiora S; Tabil, Lope G; Dumonceaux, Tim

    2017-03-26

    The effects of microwave-assisted alkali pre-treatment on pellets' characteristics and enzymatic saccharification for bioethanol production using lignocellulosic biomass of canola straw and oat hull were investigated. The ground canola straw and oat hull were immersed in distilled water, sodium hydroxide and potassium hydroxide solutions at two concentrations (0.75% and 1.5% w/v) and exposed to microwave radiation at power level 713 W and three residence times (6, 12 and 18 min). Bulk and particle densities of ground biomass samples were determined. Alkaline-microwave pre-treated and untreated samples were subjected to single pelleting test in an Instron universal machine, pre-set to a load of 4000 N. The measured parameters, pellet density, tensile strength and dimensional stability were evaluated and the results showed that the microwave-assisted alkali pre-treated pellets had a significantly higher density and tensile strength compared to samples that were untreated or pre-treated by microwave alone. The chemical composition analysis showed that microwave-assisted alkali pre-treatment was able to disrupt and break down the lignocellulosic structure of the samples, creating an area of cellulose accessible to cellulase reactivity. The best enzymatic saccharification results gave a high glucose yield of 110.05 mg/g dry sample for canola straw ground in a 1.6 mm screen hammer mill and pre-treated with 1.5% NaOH for 18 min, and a 99.10 mg/g dry sample for oat hull ground in a 1.6 mm screen hammer mill and pre-treated with 0.75% NaOH for 18 min microwave-assisted alkali pre-treatments. The effects of pre-treatment results were supported by SEM analysis. Overall, it was found that microwave-assisted alkali pre-treatment of canola straw and oat hull at a short residence time enhanced glucose yield.

  15. Closed vessel miniaturized microwave assisted chelating extraction for determination of trace metals in plant materials

    NASA Astrophysics Data System (ADS)

    Czarnecki, Sezin; Duering, Rolf-Alexander

    2013-04-01

    In recent years, the use of closed vessel microwave assisted extraction (MAE) for plant samples has shown increasing research interest which will probably substitute conventional procedures in the future due to their general disadvantages including consumption of time and solvents. The objective of this study was to demonstrate an innovative miniaturized closed vessel microwave assisted extraction (µMAE) method under the use of EDTA (µMAE-EDTA) to determine metal contents (Cd, Co, Cu, Mn, Ni, Pb, Zn) in plant samples (Lolio-Cynosuretum) by inductively coupled plasma-optical emission spectrometry (ICP-OES). Validation of the method was done by comparison of the results with another miniaturized closed vessel microwave HNO3 method (µMAE-H) and with two other macro scale MAE procedures (MAE-H and MAE-EDTA) which were applied by using a mixture of nitric acid (HNO3) and hydrogen peroxide (H2O2) (MAE-H) and EDTA (MAE-EDTA), respectively. The already established MAE-H method is taken into consideration as a reference validation MAE method for plant material. A conventional plant extraction (CE) method, based on dry ashing and dissolving of the plant material in HNO3, was used as a confidence comparative method. Certified plant reference materials (CRMs) were used for comparison of recovery rates from different extraction protocols. This allowed the validation of the applicability of the µMAE-EDTA procedure. For 36 real plant samples with triplicates each, µMAE-EDTA showed the same extraction yields as the MAE-H in the determination of Cd, Co, Cu, Mn, Ni, Pb, and Zn contents in plant samples. Analytical parameters in µMAE-EDTA should be further investigated and adapted for other metals of interest. By the reduction and elimination of the use of hazardous chemicals in environmental analysis and thus allowing a better understanding of metal distribution and accumulation process in plants and also the metal transfer from soil to plants and into the food chain, µ

  16. Atypical McMurry cross-coupling reactions leading to a new series of potent antiproliferative compounds bearing the key [ferrocenyl-ene-phenol] motif.

    PubMed

    Pigeon, Pascal; Görmen, Meral; Kowalski, Konrad; Müller-Bunz, Helge; McGlinchey, Michael J; Top, Siden; Jaouen, Gérard

    2014-07-17

    In the course of the preparation of a series of ferrocenyl derivatives of diethylstilbestrol (DES), in which one of the 4-hydroxyphenyl moieties was replaced by a ferrocenyl group, the McMurry reaction of chloropropionylferrocene with a number of mono-aryl ketones unexpectedly yielded the hydroxylated ferrocenyl DES derivatives, 5a-c, in poor yields (10%-16%). These compounds showed high activity on the hormone-independent breast cancer cell line MDA-MB-231 with IC50 values ranging from 0.14 to 0.36 µM. Surprisingly, non-hydroxylated ferrocenyl DES, 4, showed only an IC50 value of 1.14 µM, illustrating the importance of the hydroxyethyl function in this promising new series. For comparison, McMurry reactions of the shorter chain analogue chloroacetylferrocene were carried out to see the difference in behaviour with mono-aryl ketones versus a diaryl ketone. The effect of changing the length of the alkyl chain adjacent to the phenolic substituent of the hydroxylated ferrocenyl DES was studied, a mechanistic rationale to account for the unexpected products is proposed, and the antiproliferative activities of all of these compounds on MDA-MB-231 cells lines were measured and compared. X-ray crystal structures of cross-coupled products and of pinacol-pinacolone rearrangements are reported.

  17. Ultra fast microwave-assisted leaching for the recovery of copper and tellurium from copper anode slime

    NASA Astrophysics Data System (ADS)

    Ma, Zhi-yuan; Yang, Hong-ying; Huang, Song-tao; Lü, Yang; Xiong, Liu

    2015-06-01

    The decomposition of copper anode slime heated by microwave energy in a sulfuric acid medium was investigated. Leaching experiments were carried out in a multi-mode cavity with microwave assistance. The leaching process parameters were optimized using response surface methodology (RSM). Under the optimized conditions, the leaching efficiencies of copper and tellurium were 99.56% ± 0.16% and 98.68% ± 0.12%, respectively. Meanwhile, a conventional leaching experiment was performed in order to evaluate the influence of microwave radiation. The mechanism of microwave-assisted leaching of copper anode slime was also investigated. In the results, the microwave technology is demonstrated to have a great potential to improve the leaching efficiency and reduce the leaching time. The enhanced recoveries of copper and tellurium are believed to result from the presence of a temperature gradient due to the shallow microwave penetration depth and the superheating at the solid-liquid interface.

  18. Photocatalytic Decomposition of Methylene Blue Over MIL-53(Fe) Prepared Using Microwave-Assisted Process Under Visible Light Irradiation.

    PubMed

    Trinh, Nguyen Duy; Hong, Seong-Soo

    2015-07-01

    Iron-based MIL-53 crystals with uniform size were successfully synthesized using a microwave-assisted solvothermal method and characterized by XRD, FE-SEM and DRS. We also investigated the photocatalytic activity of MIL-53(Fe) for the decomposition of methylene blue using H2O2 as an electron acceptor. From XRD and SEM results, the fully crystallized MIL-53(Fe) materials were obtained regardless of preparation method. From DRS results, MIL-53(Fe) samples prepared using microwave-assisted process displayed the absorption spectrum up to the visible region and then they showed the high photocatalytic activity under visible light irradiation. The MIL-53(Fe) catalyst prepared by two times microwave irradiation showed the highest activity.

  19. Optimisation of pulsed ultrasonic and microwave-assisted extraction for curcuminoids by response surface methodology and kinetic study.

    PubMed

    Li, Ming; Ngadi, Michael O; Ma, Ying

    2014-12-15

    A response surface methodology and a kinetic study were used to optimise the pulsed ultrasonic and microwave techniques in the extraction of curcuminoids. Microwave-assisted extraction had the same efficiency as pulsed ultrasonic-assisted extraction, and both methods were better than continuous ultrasonic extraction of curcuminoids. For the pulsed ultrasonic-assisted extraction, the optimal conditions were 60% amplitude (AMP), 83% ethanol (v/v), 3/1 (s/s) pulsed duration/interval time and 10 min irradiation time. For the microwave-assisted extraction, the optimal conditions were 82% ethanol, 10% power level and 7 min of extraction time. Both methods used a 1:200 mass to solvent ratio.

  20. Solution-based formation of high-quality gate dielectrics on epitaxial graphene by microwave-assisted annealing

    NASA Astrophysics Data System (ADS)

    Kim, Kwan-Soo; Park, Goon-Ho; Fukidome, Hirokazu; Suemitsu, Tetsuya; Otsuji, Taiichi; Cho, Won-Ju; Suemitsu, Maki

    2017-06-01

    We propose a damage-free formation method for high-quality gate dielectrics on epitaxial graphene (EG), which involves solution-based Al2O3 coating combined with microwave-assisted annealing (MW-sol-Al2O3). This method substantially preserves the pristine properties of EG with minimized hole doping and strain induction. The MW-sol-Al2O3 showed a surface roughness of ˜0.237 nm and a dielectric constant of 7.5. A leakage current of 8.7 × 10-6 A/cm2, which is 3 orders of magnitude smaller than that of natural Al2O3 at the same electric field, was obtained. These excellent MW-sol-Al2O3 properties are ascribed to the effective elimination of hydroxyl- and carboxyl-related components from the film by microwave-assisted annealing.

  1. Microwave assisted esterification of acidified oil from waste cooking oil by CERP/PES catalytic membrane for biodiesel production.

    PubMed

    Zhang, Honglei; Ding, Jincheng; Zhao, Zengdian

    2012-11-01

    The traditional heating and microwave assisted method for biodiesel production using cation ion-exchange resin particles (CERP)/PES catalytic membrane were comparatively studied to achieve economic and effective method for utilization of free fatty acids (FFAs) from waste cooking oil (WCO). The optimal esterification conditions of the two methods were investigated and the experimental results showed that microwave irradiation exhibited a remarkable enhanced effect for esterification compared with that of traditional heating method. The FFAs conversion of microwave assisted esterification reached 97.4% under the optimal conditions of reaction temperature 60°C, methanol/acidified oil mass ratio 2.0:1, catalytic membrane (annealed at 120°C) loading 3g, microwave power 360W and reaction time 90min. The study results showed that it is a fast, easy and green way to produce biodiesel applying microwave irradiation. Copyright © 2012 Elsevier Ltd. All rights reserved.

  2. Microwave-assisted digestion using nitric acid for heavy metals and sulfated ash testing in active pharmaceutical ingredients.

    PubMed

    Pluhácek, T; Hanzal, J; Hendrych, J; Milde, D

    2016-04-01

    The monitoring of inorganic impurities in active pharmaceutical ingredients plays a crucial role in the quality control of the pharmaceutical production. The heavy metals and residue on ignition/sulfated ash methods employing microwave-assisted digestion with concentrated nitric acid have been demonstrated as alternatives to inappropriate compendial methods recommended in United States Pharmacopoeia (USP) and European Pharmacopoeia (Ph. Eur.). The recoveries using the heavy metals method ranged between 89% and 122% for nearly all USP and Ph. Eur. restricted elements as well as the recoveries of sodium sulfate spikes were around 100% in all tested matrices. The proposed microwave-assisted digestion method allowed simultaneous decomposition of 15 different active pharmaceutical ingredients with sample weigh up to 1 g. The heavy metals and sulfated ash procedures were successfully applied to the determination of heavy metals and residue on ignition/sulfated ash content in mycophenolate mofetil, nicergoline and silymarin.

  3. Kinetic study on microwave-assisted esterification of free fatty acids derived from Ceiba pentandra Seed Oil.

    PubMed

    Lieu, Thanh; Yusup, Suzana; Moniruzzaman, Muhammad

    2016-07-01

    Recently, a great attention has been paid to advanced microwave technology that can be used to markedly enhance the biodiesel production process. Ceiba pentandra Seed Oil containing high free fatty acids (FFA) was utilized as a non-edible feedstock for biodiesel production. Microwave-assisted esterification pretreatment was conducted to reduce the FFA content for promoting a high-quality product in the next step. At optimum condition, the conversion was achieved 94.43% using 2wt% of sulfuric acid as catalyst where as 20.83% conversion was attained without catalyst. The kinetics of this esterification reaction was also studied to determine the influence of factors on the rate of reaction and reaction mechanisms. The results indicated that microwave-assisted esterification was of endothermic second-order reaction with the activation energy of 53.717kJ/mol.

  4. Microwave-assisted rapid extracellular synthesis of stable bio-functionalized silver nanoparticles from guava ( Psidium guajava) leaf extract

    NASA Astrophysics Data System (ADS)

    Raghunandan, Deshpande; Mahesh, Bedre D.; Basavaraja, S.; Balaji, S. D.; Manjunath, S. Y.; Venkataraman, A.

    2011-05-01

    Our research interest centers on microwave-assisted rapid extracellular synthesis of bio-functionalized silver nanoparticles of 26 ± 5 nm from guava ( Psidium guajava) leaf extract with control over dimension and composition. The reaction occurs very rapidly as the formation of spherical nanoparticles almost completed within 90 s. The probable pathway of the biosynthesis is suggested. Appearance, crystalline nature, size and shape of nanoparticles are understood by UV-vis (UV-vis spectroscopy), FTIR (fourier transform infrared spectroscopy), XRD (X-ray diffraction), FESEM (field emission scanning electron microscopy) and TEM (transmission electron microscopy) techniques. Microwave-assisted route is selected for the synthesis of silver nanoparticles to carry out the reaction fast, suppress the enzymatic action and to keep the process environmentally clean and green.

  5. Efficient microwave-assisted one-pot preparation of angular 2,2-dimethyl-2H-chromone containing compounds

    PubMed Central

    Zhou, Ting; Shi, Qian; Lee, Kuo Hsing

    2010-01-01

    A novel and efficient microwave-assisted one-pot reaction was developed to synthesize angular 2,2-dimethyl-2H-chromone containing compounds, which is the first and key step in the synthesis of potent DCK and DCP anti-HIV agents. The newly developed microwave synthesis conditions dramatically shortened the reaction time from 2 days to 4 hours with improved yields. PMID:20936082

  6. Efficient microwave-assisted one-pot preparation of angular 2,2-dimethyl-2H-chromone containing compounds.

    PubMed

    Zhou, Ting; Shi, Qian; Lee, Kuo Hsing

    2010-08-18

    A novel and efficient microwave-assisted one-pot reaction was developed to synthesize angular 2,2-dimethyl-2H-chromone containing compounds, which is the first and key step in the synthesis of potent DCK and DCP anti-HIV agents. The newly developed microwave synthesis conditions dramatically shortened the reaction time from 2 days to 4 hours with improved yields.

  7. Rare-earth-doped bifunctional alkaline-earth metal fluoride nanocrystals via a facile microwave-assisted process.

    PubMed

    Pang, Min; Liu, Dapeng; Lei, Yongqian; Song, Shuyan; Feng, Jing; Fan, Weiqiang; Zhang, Hongjie

    2011-06-20

    Rare-earth-doped magnetic-optic bifunctional alkaline-earth metal fluoride nanocrystals have been successfully synthesized via a facile microwave-assisted process. The as-prepared nanocrystals were monodisperse and could form stable colloidal solutions in polar solvents, such as water and ethanol. They show bright-green fluorescence emisson. Furthermore, Gd(3+)-doped ones exhibit paramagnetic behavior at room temperature and superparamagnetic behavior at 2 K.

  8. Synthesis of amino-benzothiaoxazepine-1,1-dioxides utilizing a microwave-assisted, S(N)Ar protocol.

    PubMed

    Rolfe, Alan; Ullah, Farman; Samarakoon, Thiwanka B; Kurtz, Ryan D; Porubsky, Patrick; Neuenswander, Benjamin; Lushington, Gerald H; Santini, Conrad; Organ, Michael G; Hanson, Paul R

    2011-11-14

    The development of a microwave-assisted, intermolecular S(N)Ar protocol for the synthesis of a 126-member benzothiaoxazepine-1,1-dioxide library is reported. Diversification of 12 benzothiaoxazepine-1,1-dioxides was achieved in rapid fashion utilizing a variety of 2° amines and amino alcohols to generate an 80-member library. A second 48-member library was subsequently generated via a two-step alkylation, intermolecular S(N)Ar diversification protocol.

  9. The microwave adsorption behavior and microwave-assisted heteroatoms doping of graphene-based nano-carbon materials.

    PubMed

    Tang, Pei; Hu, Gang; Gao, Yongjun; Li, Wenjing; Yao, Siyu; Liu, Zongyuan; Ma, Ding

    2014-08-11

    Microwave-assisted heating method is used to treat graphite oxide (GO), pyrolytic graphene oxide (PGO) and hydrogen-reduced pyrolytic graphene oxide (HPGO). Pure or doped graphene are prepared in the time of minutes and a thermal deoxygenization reduction mechanism is proposed to understand their microwave adsorption behaviors. These carbon materials are excellent catalysts in the reduction of nitrobenzene. The defects are believed to play an important role in the catalytic performance.

  10. The microwave-assisted solvothermal synthesis of a crystalline two-dimensional covalent organic framework with high CO2 capacity.

    PubMed

    Wei, Hao; Chai, Shuangzhi; Hu, Nantao; Yang, Zhi; Wei, Liangming; Wang, Lin

    2015-08-07

    We report the synthesis of a two-dimensional enamine-linked covalent organic framework (COF) using a rapid microwave-assisted solvothermal method in significantly less time and high yield under a relatively low temperature. This COF was found to have a high crystallinity, high stability, high BET surface area, and a high CO2 capacity and adsorption selectivity of CO2/N2.

  11. Fast and efficient proteolysis by microwave-assisted protein digestion using trypsin-immobilized magnetic silica microspheres.

    PubMed

    Lin, Shuang; Yao, Guoping; Qi, Dawei; Li, Yan; Deng, Chunhui; Yang, Pengyuan; Zhang, Xiangmin

    2008-05-15

    A fast and efficient proteolysis approach of microwave-assisted protein digestion was developed by using trypsin-immobilized magnetic silica (MS) microspheres. In the work, immobilization of the enzyme onto MS microspheres was very simple and only through a one-step reaction with 3-glycidoxypropyltrimethoxysilane (GLYMO) which provides the epoxy group as a reactive spacer. Considering that the magnetic particles are excellent microwave absorbers, we developed a novel microwave-assisted digestion method based on the easily prepared trypsin-immobilized MS microspheres. This novel digestion method combined the advantages of immobilized trypsin and the rapid-fashion of microwave-assisted digestion, which resulted in high digestion efficiency. BSA and myoglobin were used as model proteins to optimize the conditions of this method. Peptide fragments produced in 15 s could be confidently identified by matrix-assisted laser desorption ionization-time-of-flight mass spectrometry (MALDI-TOF MS) analysis. Equivalent or better digestion efficiency was observed comparing to current in-solution digestion. Besides, because of the unique magnetic responsivity, the immobilized trypsin can be isolated easily with the help of an external magnet and thus used repeatedly. High activity was obtained even after seven runs of the trypsin-immobilized MS microspheres. To further verify its efficiency in proteome analysis, one reversed-phase liquid chromatography (RPLC) fraction of rat liver extract was applied. After 15 s incubation, 16 totally unique peptides corresponding to two proteins were identified. Finally, the rat liver sample was used to evaluate its worth for the application. With analysis by liquid chromatography-electrospray-tandem mass spectrometry (LC-ESI-MS/MS), comparable digestion efficiency was observed with typical in-solution digestion but the incubation time was largely shortened. This new microwave-assisted digestion method will hasten the application of the proteome

  12. The microwave adsorption behavior and microwave-assisted heteroatoms doping of graphene-based nano-carbon materials

    NASA Astrophysics Data System (ADS)

    Tang, Pei; Hu, Gang; Gao, Yongjun; Li, Wenjing; Yao, Siyu; Liu, Zongyuan; Ma, Ding

    2014-08-01

    Microwave-assisted heating method is used to treat graphite oxide (GO), pyrolytic graphene oxide (PGO) and hydrogen-reduced pyrolytic graphene oxide (HPGO). Pure or doped graphene are prepared in the time of minutes and a thermal deoxygenization reduction mechanism is proposed to understand their microwave adsorption behaviors. These carbon materials are excellent catalysts in the reduction of nitrobenzene. The defects are believed to play an important role in the catalytic performance.

  13. Microwave-Assisted Protein Digestion in a Plate Well for Facile Sampling and Rapid Digestion.

    PubMed

    Kim, Hyeonil; Kim, Han Sol; Lee, Dabin; Shin, Dongwon; Shin, Daeho; Kim, Jeongkwon; Kim, Jungbae

    2017-09-25

    Protein digestion is one of the most important processes in proteomic analysis. Here, we report microwave-assisted protein digestion in a plate well, which allows for facile sampling as well as rapid protein digestion based on the combination of highly stable enzyme immobilization and 3D printing technologies. Trypsin (TR) was immobilized on polystyrene-based nanofibers via an enzyme coating (EC) approach. The EC with stabilized TR activity was assembled with the 3D-printed structure in the plate well (EC/3D), which provides two separated compartments for the solution sampling and the TR-catalyzed protein digestion, respectively. EC/3D can effectively prevent the interference of sampling by accommodating EC in the separated compartment from the sampling hole in the middle. EC/3D in the plate well maintained its protein digestion performance under shaking over 160 days. Microwave irradiation enabled the digestion of bovine serum albumin within 10 min, generating the MALDI-TOF MS results of 75.0% sequence coverage and 61 identified peptides. EC/3D maintained its protein digestion performance under microwave irradiation after 30 times of recycled uses. EC/3D in the plate well has demonstrated its potential as a robust and facile tool for the development of an automated protein digestion platform. The combination of stable immobilized enzymes and 3D-printed structures can be potentially utilized not only for the protein digestion, but also for many other enzyme applications, including bioconversion and biosensors.

  14. Experimental and modeling studies on microwave-assisted extraction of mangiferin from Curcuma amada.

    PubMed

    Kullu, Jeke; Dutta, Abhishek; Constales, Denis; Chaudhuri, Surabhi; Dutta, Debjani

    2014-04-01

    Mangiferin, a bioactive compound having potent nutraceutical, strong antioxidant and pharmacological significance has been extracted using microwave-assisted extraction (MAE) technique from Curcuma amada, commonly known as mango ginger. The extraction solvent ethanol is eco-friendly, nontoxic and reduces the risk of environmental hazards. The influence of several independent variables such as microwave power, ethanol concentration, extraction (irradiation) time and pre-leaching time has been studied under varying conditions using one-factor-at-a-time analysis to obtain an optimal extraction ratio. The maximum mangiferin content of 1.1156 mg/g is obtained at microwave power of 550 W and extraction time of 50 s with 80 % ethanol as a solvent and pre-leaching time of 20 min. The results indicate that microwave power and ethanol concentration have the most significant effect on the yield of mangiferin content. The presence of mangiferin in final Curcuma amada extract is confirmed through high-performance liquid chromatography and the functional groups are identified through Fourier transform infrared spectroscopy analyses using standard mangiferin. The experimental profiles are fitted into a two-parameter modified first-order kinetic model and a three-parameter modified logistic model and checked using the goodness-of-fit criterion. The Curcuma amada retained its antioxidant activity after MAE treatment and the antioxidant activity of mangiferin obtained after extraction using DPPH free radical scavenging assay is studied.

  15. Response surface methodology applied to the study of the microwave-assisted synthesis of quaternized chitosan.

    PubMed

    dos Santos, Danilo Martins; Bukzem, Andrea de Lacerda; Campana-Filho, Sérgio Paulo

    2016-03-15

    A quaternized derivative of chitosan, namely N-(2-hydroxy)-propyl-3-trimethylammonium chitosan chloride (QCh), was synthesized by reacting glycidyltrimethylammonium chloride (GTMAC) and chitosan (Ch) in acid medium under microwave irradiation. Full-factorial 2(3) central composite design and response surface methodology (RSM) were applied to evaluate the effects of molar ratio GTMAC/Ch, reaction time and temperature on the reaction yield, average degree of quaternization (DQ) and intrinsic viscosity ([η]) of QCh. The molar ratio GTMAC/Ch was the most important factor affecting the response variables and RSM results showed that highly substituted QCh (DQ = 71.1%) was produced at high yield (164%) when the reaction was carried out for 30min. at 85°C by using molar ratio GTMAC/Ch 6/1. Results showed that microwave-assisted synthesis is much faster (≤30min.) as compared to conventional reaction procedures (>4h) carried out in similar conditions except for the use of microwave irradiation.

  16. Ionic liquids based simultaneous ultrasonic and microwave assisted extraction of phenolic compounds from burdock leaves.

    PubMed

    Lou, Zaixiang; Wang, Hongxin; Zhu, Song; Chen, Shangwei; Zhang, Ming; Wang, Zhouping

    2012-02-24

    The ionic liquids based simultaneous ultrasonic and microwave assisted extraction (IL-UMAE) technique was first proposed and applied to isolate compounds. The ionic liquids comprising a range of four anions, five 1-alkyl-3-methylimidazolium derivatives were designed and prepared. The results suggested that varying the anion and cation both had apparent effects on the extraction of phenolics. The results also showed that irradiation power, time and solid-liquid ratio significantly affected the yields. The yields of caffeic acid and quercetin obtained by IL-UMAE were higher than those by regular UMAE. Compared with conventional heat-reflux extraction (HRE), the proposed approach exhibited higher efficiency (8-17% enhanced) and shorter extraction time (from 5h to 30s). The results indicated ILUMAE to be a fast and efficient extraction technique. Moreover, the proposed method was validated by the reproducibility and recovery experiments. The ILUMAE method provided good recoveries (from 96.1% to 105.3%) with RSD lower than 5.2%, which indicated that the proposed method was credible. Based on the designable nature of ionic liquids, and the rapid and highly efficient performance of the proposed approach, ILUMAE provided a new alternative for preparation of various useful substances from solid samples. Copyright © 2011 Elsevier B.V. All rights reserved.

  17. Dynamic microwave assisted extraction coupled with dispersive micro-solid-phase extraction of herbicides in soybeans.

    PubMed

    Li, Na; Wu, Lijie; Nian, Li; Song, Ying; Lei, Lei; Yang, Xiao; Wang, Kun; Wang, Zhibing; Zhang, Liyuan; Zhang, Hanqi; Yu, Aimin; Zhang, Ziwei

    2015-09-01

    Non-polar solvent dynamic microwave assisted extraction was firstly applied to the treatment of high-fat soybean samples. In the dispersive micro-solid-phase extraction (D-µ-SPE), the herbicides in the high-fat extract were directly adsorbed on metal-organic frameworks MIL-101(Cr). The effects of several experimental parameters, including extraction solvent, microwave absorption medium, microwave power, volume and flow rate of extraction solvent, amount of MIL-101(Cr), and D-µ-SPE time, were investigated. At the optimal conditions, the limits of detection for the herbicides ranged from 1.56 to 2.00 μg kg(-1). The relative recoveries of the herbicides were in the range of 91.1-106.7%, and relative standard deviations were equal to or lower than 6.7%. The present method was simple, rapid and effective. A large amount of fat was also removed. This method was demonstrated to be suitable for treatment of high-fat samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  18. Ultrafast Preparation of Monodisperse Fe3 O4 Nanoparticles by Microwave-Assisted Thermal Decomposition.

    PubMed

    Liang, Yi-Jun; Zhang, Yu; Guo, Zhirui; Xie, Jun; Bai, Tingting; Zou, Jiemeng; Gu, Ning

    2016-08-08

    Thermal decomposition, as the main synthetic procedure for the synthesis of magnetic nanoparticles (NPs), is facing several problems, such as high reaction temperatures and time consumption. An improved a microwave-assisted thermal decomposition procedure has been developed by which monodisperse Fe3 O4 NPs could be rapidly produced at a low aging temperature with high yield (90.1 %). The as-synthesized NPs show excellent inductive heating and MRI properties in vitro. In contrast, Fe3 O4 NPs synthesized by classical thermal decomposition were obtained in very low yield (20.3 %) with an overall poor quality. It was found for the first time that, besides precursors and solvents, magnetic NPs themselves could be heated by microwave irradiation during the synthetic process. These findings were demonstrated by a series of microwave-heating experiments, Raman spectroscopy and vector-network analysis, indicating that the initially formed magnetic Fe3 O4 particles were able to transform microwave energy into heat directly and, thus, contribute to the nanoparticle growth.

  19. Histology-Directed Microwave Assisted Enzymatic Protein Digestion for MALDI MS Analysis of Mammalian Tissue

    PubMed Central

    2015-01-01

    This study presents on-tissue proteolytic digestion using a microwave irradiation and peptide extraction method for in situ analysis of proteins from spatially defined regions of a tissue section. The methodology utilizes hydrogel discs (1 mm diameter) embedded with trypsin solution. The enzyme-laced hydrogel discs are applied to a tissue section, directing enzymatic digestion to a spatially confined area of the tissue. By applying microwave radiation, protein digestion is performed in 2 min on-tissue, and the extracted peptides are then analyzed by matrix assisted laser desorption/ionization mass spectrometry (MALDI MS) and liquid chromatography tandem mass spectrometry (LC-MS/MS). The reliability and reproducibility of the microwave assisted hydrogel mediated on-tissue digestion is demonstrated by the comparison with other on-tissue digestion strategies, including comparisons with conventional heating and in-solution digestion. LC-MS/MS data were evaluated considering the number of identified proteins as well as the number of protein groups and distinct peptides. The results of this study demonstrate that rapid and reliable protein digestion can be performed on a single thin tissue section while preserving the relationship between the molecular information obtained and the tissue architecture, and the resulting peptides can be extracted in sufficient abundance to permit analysis using LC-MS/MS. This approach will be most useful for samples that have limited availability but are needed for multiple analyses, especially for the correlation of proteomics data with histology and immunohistochemistry. PMID:25427280

  20. Study on the PEG-based microwave-assisted extraction of flavonoid compounds from persimmon leaves.

    PubMed

    Liu, Lei; Liu, Rui-Lin; Zhang, Jing; Zhang, Zhi-Qi

    2012-12-01

    A method for PEG-based microwave-assisted extraction (MAE) of flavonoid compounds from persimmon leaves has been successfully developed. The extraction efficiency of total flavonoid content was evaluated by the chromatographic peak areas of quercetin and kaempferol, which are two bioactive components typically found in persimmon leaves. The best combination of extraction parameters was obtained with response surface methodology. A microwave power of 525 W, liquid to solid ratio of 17:1 mL/g, and PEG aqueous solution concentration of 60% w/w were identified as the optimum parameters. Extraction dynamics analysis indicated that the quercetin, kaempferol, and total flavonoid contents were rising with increasing extraction time up to 20-25 min, from which point onwards they all decreased. Under the optimum conditions, quercetin, kaempferol, and total flavonoid contents obtained from the sample were 1.20 ± 0.05, 0.64 ± 0.11, and 16.90 ± 0.06 mg/g, respectively. Compared with ethanol-based MAE, and ethanol-based and PEG-based ultrasonic-assisted extractions, PEG-based MAE had higher efficiency for the extraction of flavonoid compounds from persimmon leaves. Overall, PEG-based MAE represents an efficient choice for the extraction of bioactive substances from traditional Chinese medicines. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Facile microwave-assisted synthesis of Klockmannite CuSe nanosheets and their exceptional electrical properties.

    PubMed

    Liu, Yong-Qiang; Wang, Feng-Xia; Xiao, Yan; Peng, Hong-Dan; Zhong, Hai-Jian; Liu, Zheng-Hui; Pan, Ge-Bo

    2014-08-08

    Klockmannite copper selenide nanosheets (CuSe NSs) are synthesized by a facile microwave-assisted method and fully characterized. The nanosheets have smooth surface and hexagonal shape. The lateral size is 200-500 nm × 400-800 nm and the thickness is 55 ± 20 nm. The current-voltage characteristics of CuSe NS films show unique Ohmic and high-conducting behaviors, comparable to the thermally-deposited gold electrode. The high electrical conductivity of CuSe NSs implies their promising applications in printed electronics and nanodevices. Moreover, the local electrical variation is observed, for the first time, within an individual CuSe NS at low bias voltages (0.1 ~ 3 V) by conductive atomic force microscopy (C-AFM). This is ascribed to the quantum size effect of NS and the presence of Schottky barrier. In addition, the influence of the molar ratio of Cu(2+)/SeO2, reaction temperature, and reaction time on the growth of CuSe NSs is explored. The template effect of oleylamine and the intrinsic crystal nature of CuSe NS are proposed to account for the growth of hexagonal CuSe NSs.

  2. Microwave assisted extraction of pectin from waste Citrullus lanatus fruit rinds.

    PubMed

    Prakash Maran, J; Sivakumar, V; Thirugnanasambandham, K; Sridhar, R

    2014-01-30

    In this present study, microwave-assisted extraction (MAE) was applied to extraction of pectin from waste Citrullus Lanatus fruit rinds. Extraction parameters which are employed in this study are microwave power (160-480 W), irradiation time (60-180s), pH (1-2) and solid-liquid ratio (1:10-1: 30 g/ml) and they were optimized using a four factor three levels Box-Behnken response surface design (BBD) coupled with desirability function methodology. The results showed that, all the process variables have significant effect on the extraction yield of pectin. Optimum MAE conditions for the highest pectin yield from waste C. Lanatus fruit rinds (25.79%) were obtained with microwave power of 477 W, irradiation time of 128 s, pH of 1.52, solid-liquid ratio of 1:20.3g/ml respectively. Validation experiment results were well agreed with predicted value. Copyright © 2013 Elsevier Ltd. All rights reserved.

  3. Microwave-assisted extraction of polysaccharides from Cyphomandra betacea and its biological activities.

    PubMed

    C, Senthil Kumar; M, Sivakumar; K, Ruckmani

    2016-11-01

    Response Surface Methodology (RSM) was used to optimize the parameters for microwave-assisted extraction of polysaccharides from Cyphomandra betacea. The results showed a good fit with a second-order polynomial equation that was statistically acceptable at P<0.05. Optimal conditions for the extraction of polysaccharides were: extraction time, 2h; microwave power, 400W; extraction temperature, 60°C; and ratio of raw material to water 1:40 (g/mL). Under the optimized conditions, the yield of polysaccharides was found to be relatively high (about 36.52%). The in vitro biological activities of antioxidant and antitumor were evaluated. The IC50 value of polysaccharides was found to be 3mg/mL. The percentage of Cell viability was determined by MTT assay. Our results showed that polysaccharides inhibited proliferation of MCF-7 (Breast carcinoma), A549 (Human lung carcinoma) and HepG2 (Liver carcinoma) with an IC50 of 0.23mg/mL, 0.17mg/mL and 0.62mg/mL respectively after 48h incubation. Polysaccharides were shown to promote apoptosis as seen in the nuclear morphological examination study using acridine orange (AO) and ethidium bromide (EB) staining. This is the first report on the effects of polysaccharides extracted from Cyphomandra betacea which exhibited stronger antioxidant and antitumor activities.

  4. Microwave-assisted synthesis of bismuth oxybromochloride nanoflakes for visible light photodegradation of pollutants

    NASA Astrophysics Data System (ADS)

    Bijanzad, Keyvan; Tadjarodi, Azadeh; Moghaddasi Khiavi, Mohammad; Akhavan, Omid

    2015-10-01

    BiOBrxCl1-x (0microwave-assisted synthesis method. The X-ray diffraction (XRD) studies confirmed the formation of pure crystalline phase of BiOBrxCl1-x. The UV-visible diffuse reflectance and photoluminescence (PL) spectroscopies revealed the indirect band gap of ~2.82 eV for the bismuth oxybromochloride nanoflakes. Visible light-assisted photocatalytic studies showed that the degradation efficiency of the as-prepared BiOBrxCl1-x for (100 mL of 10 mg L-1) Rhodamine B (RhB), Natural Red 4 (N-Red) dye solutions was 98.14% and for the colorless organic pentachlorophenol (PCP) solution was 91.09% over 150 min. The possible mechanisms involved in the visible light photodegradation of the pollutants by BiOBrxCl1-x photocatalyst were also discussed.

  5. Microwave assisted synthesis of nanocrystalline Fe-phosphates electrode materials and their electrochemical properties.

    PubMed

    Kim, D H; Kang, J W; Jung, I O; Im, J S; Kim, E J; Song, S J; Lee, J S; Kim, J

    2008-10-01

    LiFePO4 nanocrystalline particles were synthesized using microwave assisted polyol process within a fast reaction time of 20 minutes without any further heating as a post step. The synthesized LiFePO4 nanocrystalline particles showed mono-dispersed rod and orthorhombic-like shapes with a size of 60 approximately 180 nm. The refined X-ray diffraction pattern of the sample was indexed well to the olivine crystal structure (space group: Pnma) without any impurity phases. The LiFePO4 nanocrystalline particles show a capacity of 161 mAh/g in a voltage range of 2.5-4.2 V with a current density of 0.1 mA/cm2 without any observable capacity fading in extended cycles of 100th. A cyclic voltammetry analysis exhibits distinctly sharp peaks corresponding to the typical LiFePO4/FePO4 redox couples and demonstrates a good reversibility of the sample.

  6. Microwave-assisted direct liquefaction of Ulva prolifera for bio-oil production by acid catalysis.

    PubMed

    Zhuang, Yingbin; Guo, Jingxue; Chen, Limei; Li, Demao; Liu, Junhai; Ye, Naihao

    2012-07-01

    Production of bio-oil by microwave-assisted direct liquefaction (MADL) of Ulva prolifera was investigated, and the bio-oil was analyzed by elementary analysis, Fourier transform infrared spectroscopic analysis (FT-IR), and gas chromatography-mass spectrometry (GC-MS). The results indicate that the liquefaction yield is influenced by the microwave power, liquefaction temperature, liquefaction time, catalyst content, solvent-to-feedstock ratio and moisture content. The maximum liquefaction yield of U. prolifera (moisture content of 8%) was 84.81%, which was obtained under microwave power of 600 W for 30 min at 180 °C with solvent-to-feedstock ratio of 16:1 and 6% H(2)SO(4). The bio-oil was composed of benzenecarboxylic acid, diethyl phthalate, long-chain fatty acids (C(13) to C(18)), fatty acid methyl esters and water. The results suggest that U. prolifera is a viable eco-friendly, green feedstock substitute for biofuels and chemicals production.

  7. Microwave-assisted synthesis of SnO₂ nanorods for oxygen gas sensing at room temperature.

    PubMed

    Azam, Ameer; Habib, Sami S; Salah, Numan A; Ahmed, Faheem

    2013-01-01

    High-quality single-crystalline SnO₂ nanorods were synthesized using a microwave-assisted solution method. The nanorods were characterized using X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), ultraviolet-visible and Raman spectroscopy, Brunauer-Emmett-Teller (BET), and electrical resistance measurements. The XRD pattern indicated the formation of single-phase SnO₂ nanorods with rutile structure. FE-SEM and TEM images revealed tetragonal nanorods of about 450-500 nm in length and 60-80 nm in diameter. The nanorods showed a higher BET surface area of 288 m²/g, much higher than that of previously reported work. The Raman scattering spectra indicated a typical rutile phase of the SnO₂. The absorption spectrum showed an absorption peak centered at 340 nm, and the band-gap value was found to be 3.64 eV. The gas-sensing properties of the SnO₂ nanorods for oxygen gas with different concentrations were measured at room temperature. It was found that the value of resistance increased with the increase in oxygen gas concentration in the test chamber. The SnO₂ nanorods exhibited high sensitivity and rapid response-recovery characteristics to oxygen gas, and could detect oxygen concentration as low as 1, 3, 5, and 10 ppm.

  8. Quality and high yield synthesis of Ag nanowires by microwave-assisted hydrothermal method.

    PubMed

    Meléndrez, Manuel F; Medina, Carlos; Solis-Pomar, Francisco; Flores, Paulo; Paulraj, Mani; Pérez-Tijerina, Eduardo

    2015-01-01

    Silver nanowires (Ag-NWs) were obtained using microwave-assisted hydrothermal method (MAH). The main advantage of the method is its high NWs production which is greater than 90%. It is also easy, fast, and highly reproducible process. One of the drawbacks presented so far in the synthesis of nanostructures by polyol path is the high temperature used in the process, which is superior than the boiling point of solvent (ethylene glycol), and also its excessive reaction time. Here, Ag-NWs with diameters of 70 to 110 nm were synthesized in 5 min in large quantities. Results showed that dimensions and shape of nanowires were very susceptible to changes with reaction parameters. The reactor power and reactor fill capacity were important for the synthesis. It was found that the reaction time needs to be decreased because of the NWs which start to deform and break up due to significant increase in the pressure's system. Energy-dispersive X-ray spectroscopy and electron diffraction analysis (SAED) did not show corresponding phases of AgO. Some aspects about synthesis parameters which are related to the percent yield and size of nanowires are also discussed.

  9. Microwave-assisted extraction followed by CE for determination of catechin and epicatechin in green tea.

    PubMed

    Li, Zhongbo; Huang, Danni; Tang, Zhuxin; Deng, Chunhui

    2010-04-01

    In this work, for the first time, microwave-assisted extraction (MAE) followed by CE was developed for the fast analysis of catechin and epicatechin in green tea. In the proposed method, catechin and epicatechin in green tea samples were rapidly extracted by MAE technique, and then analyzed by CE. The MAE conditions and the method's validation were studied. It is found that the extraction time of 1 min with 400 W microwave irradiation is enough to completely extract catechin and epicatechin in green tea sample, whereas the conventional ultrasonic extraction (USE) technique needs long extraction time of 60 min. The method validations were also studied in this work. The calibration curve shows good linearity in 0.01-3 mg/mL for catechin (R(2)=0.993), and 0.005-3 mg/mL for epicatechin (R(2)=0.996), respectively. The RSD values for catechin and epicatechin are 0.65 and 2.58%, respectively. This shows that the proposed method has good reproducibility. The proposed method has good recoveries, which are 118% for catechin and 120% for epicatechin. The proposed method was successfully applied to determination of the catechin and epicatechin in different green tea samples. The experiment results have demonstrated that the MAE following CE is a simple, fast and reliable method for the determination of catechin and epicatechin in green tea.

  10. Microwave assisted leaching and electrochemical recovery of copper from printed circuit boards of computer waste

    NASA Astrophysics Data System (ADS)

    Ivǎnuş, R. C.; ǎnuş, D., IV; Cǎlmuc, F.

    2010-06-01

    Due to the rapid technological progress, the replacement of electronic equipment is very often necessary, leading to huge amounts that end up as waste. In addition, waste electrical and electronic equipment (WEEE) contains metals of high commercial value and others that are supposed to be hazardous for the environment. Consequently, WEEE could be considered as a significant source for recovery of nonferrous metals. Among these wastes, computers appear to be distinctive, as far as further exploitation is concerned. The most ″useful″ parts of the computers are the printed circuit boards that contain many metals of interest. A study on microwave assisted electronic scrap (printed circuit boards of computer waste - PCBs) leaching was carried out with a microwave hydrothermal reactor. The leaching was conducted with thick slurries (50-100 g/L). The leaching media is a mixed solution of CuCl2 and NaCl. Preliminary electrolysis from leaching solution has investigated the feasibility of electrodeposition of copper. The results were discussed and compared with the conventional leaching method and demonstrated the potential for selective extraction of copper from PCBs.

  11. Facile Microwave-Assisted Synthesis of Klockmannite CuSe Nanosheets and Their Exceptional Electrical Properties

    NASA Astrophysics Data System (ADS)

    Liu, Yong-Qiang; Wang, Feng-Xia; Xiao, Yan; Peng, Hong-Dan; Zhong, Hai-Jian; Liu, Zheng-Hui; Pan, Ge-Bo

    2014-08-01

    Klockmannite copper selenide nanosheets (CuSe NSs) are synthesized by a facile microwave-assisted method and fully characterized. The nanosheets have smooth surface and hexagonal shape. The lateral size is 200-500 nm × 400-800 nm and the thickness is 55 +/- 20 nm. The current-voltage characteristics of CuSe NS films show unique Ohmic and high-conducting behaviors, comparable to the thermally-deposited gold electrode. The high electrical conductivity of CuSe NSs implies their promising applications in printed electronics and nanodevices. Moreover, the local electrical variation is observed, for the first time, within an individual CuSe NS at low bias voltages (0.1 ~ 3 V) by conductive atomic force microscopy (C-AFM). This is ascribed to the quantum size effect of NS and the presence of Schottky barrier. In addition, the influence of the molar ratio of Cu2+/SeO2, reaction temperature, and reaction time on the growth of CuSe NSs is explored. The template effect of oleylamine and the intrinsic crystal nature of CuSe NS are proposed to account for the growth of hexagonal CuSe NSs.

  12. Microwave assisted synthesis and optimization of Aegle marmelos-g-poly(acrylamide): release kinetics studies.

    PubMed

    Setia, A; Kumar, R

    2014-04-01

    Microwave assisted grafting of poly(acrylamide) on to Aegle marmelos gum was carried out employing 3-factor 3-level full factorial design. Microwave power, microwave exposure time and concentration of gum were selected as independent variable and grafting efficiency was taken as dependent variable. A. marmelos-g-poly(acrylamide) was characterized by FTIR, DSC, X-ray diffraction and scanning electron microscopy. Microwave power, microwave exposure time had synergistic effect on grafting efficiency where as concentration of the gum did not contributed much to grafting efficiency. Batch having microwave power - 80%, microwave exposure time -120 s and concentration of A. marmelos gum - 2% was selected as the optimized formulation. Comparative release behaviour of diclofenac sodium from the matrix tablets of A. marmelos gum and A. marmelos-g-polyacrylamide was evaluated. The results of kinetic studies revealed that the graft copolymer matrix, marketed tablets and polymer matrix tablets of A. marmelos gum released the drug by zero order kinetics and with n value greater than 1, indicating that the mechanism for release as super case II transport i.e. dominated by the erosion and swelling of the polymer.

  13. [Analysis of triterpenoids in Ganoderma lucidum by microwave-assisted continuous extraction].

    PubMed

    Lu, Yan-fang; An, Jing; Jiang, Ye

    2015-04-01

    For further improving the extraction efficiency of microwave extraction, a microwave-assisted contijuous extraction (MACE) device has been designed and utilized. By contrasting with the traditional methods, the characteristics and extraction efficiency of MACE has also been studied. The method was validated by the analysis of the triterpenoids in Ganoderma lucidum. The extraction conditions of MACE were: using 95% ethanol as solvent, microwave power 200 W and radiation time 14.5 min (5 cycles). The extraction results were subsequently compared with traditional heat reflux extraction ( HRE) , soxhlet extraction (SE), ultrasonic extraction ( UE) as well as the conventional microwave extraction (ME). For triterpenoids, the two methods based on the microwaves (ME and MACE) were in general capable of finishing the extraction in 10, 14.5 min, respectively, while other methods should consume 60 min and even more than 100 min. Additionally, ME can produce comparable extraction results as the classical HRE and higher extraction yield than both SE and UE, however, notably lower extraction yield than MASE. More importantly, the purity of the crud extract by MACE is far better than the other methods. MACE can effectively combine the advantages of microwave extraction and soxhlet extraction, thus enabling a more complete extraction of the analytes of TCMs in comparison with ME. And therefore makes the analytic result more accurate. It provides a novel, high efficient, rapid and reliable pretreatment technique for the analysis of TCMs, and it could potentially be extended to ingredient preparation or extracting techniques of TCMs.

  14. Microwave-Assisted Hydrothermal Rapid Synthesis of Calcium Phosphates: Structural Control and Application in Protein Adsorption

    PubMed Central

    Cai, Zhu-Yun; Peng, Fan; Zi, Yun-Peng; Chen, Feng; Qian, Qi-Rong

    2015-01-01

    Synthetic calcium phosphate (CaP)-based materials have attracted much attention in the biomedical field. In this study, we have investigated the effect of pH values on CaP nanostructures prepared using a microwave-assisted hydrothermal method. The hierarchical nanosheet-assembled hydroxyapatite (HAP) nanostructure was prepared under weak acidic conditions (pH 5), while the HAP nanorod was prepared under neutral (pH 7) and weak alkali (pH 9) condition. However, when the pH value increases to 11, a mixed product of HAP nanorod and tri-calcium phosphate nanoparticle was obtained. The results indicated that the pH value of the initial reaction solution played an important role in the phase and structure of the CaP. Furthermore, the protein adsorption and release performance of the as-prepared CaP nanostructures were investigated by using hemoglobin (Hb) as a model protein. The sample that was prepared at pH = 11 and consisted of mixed morphologies of nanorods and nanoprisms showed a higher Hb protein adsorption capacity than the sample prepared at pH 5, which could be explained by its smaller size and dispersed structure. The results revealed the relatively high protein adsorption capacity of the as-prepared CaP nanostructures, which show promise for applications in various biomedical fields such as drug delivery and protein adsorption.

  15. Microwave-assisted extraction and mild saponification for determination of organochlorine pesticides in oyster samples.

    PubMed

    Carro, N; García, I; Ignacio, M-C; Llompart, M; Yebra, M-C; Mouteira, A

    2002-10-01

    A sample-preparation procedure (extraction and saponification) using microwave energy is proposed for determination of organochlorine pesticides in oyster samples. A Plackett-Burman factorial design has been used to optimize the microwave-assisted extraction and mild saponification on a freeze dried sample spiked with a mixture of aldrin, endrin, dieldrin, heptachlor, heptachorepoxide, isodrin, transnonachlor, p, p'-DDE, and p, p'-DDD. Six variables: solvent volume, extraction time, extraction temperature, amount of acetone (%) in the extractant solvent, amount of sample, and volume of NaOH solution were considered in the optimization process. The results show that the amount of sample is statistically significant for dieldrin, aldrin, p, p'-DDE, heptachlor, and transnonachlor and solvent volume for dieldrin, aldrin, and p, p'-DDE. The volume of NaOH solution is statistically significant for aldrin and p, p'-DDE only. Extraction temperature and extraction time seem to be the main factors determining the efficiency of extraction process for isodrin and p, p'-DDE, respectively. The optimized procedure was compared with conventional Soxhlet extraction.

  16. Microwave assisted direct saponification for the simultaneous determination of cholesterol and cholesterol oxides in shrimp.

    PubMed

    Souza, Hugo A L; Mariutti, Lilian R B; Bragagnolo, Neura

    2016-03-22

    A novel microwave-assisted direct saponification method for the simultaneous determination of cholesterol and cholesterol oxides in shrimp was developed and validated. Optimal saponification conditions, determined by means of an experimental design, were achieved using 500mg of sample and 20mL of 1mol/L KOH ethanol solution for 16min at 45°C at maximum power at 200W and magnetic stirring at 120rpm. Higher extraction of cholesterol oxides in a reduced saponification time (∼75 times) was achieved in comparison with the direct cold saponification method. The new method showed low detection (≤0.57μg/mL) and quantification (≤1.73μg/mL) limits, good repeatability (≤10.50% intraday and ≤8.56% interday) and low artifact formation (evaluated by using a deuterated cholesterol-D6 standard). Raw, salted and dried-salted shrimps were successfully analyzed by the validated method. The content of cholesterol oxides increased after salting and decreased after drying.

  17. Photocatalytic perfermance of sandwich-like BiVO4 sheets by microwave assisted synthesis

    NASA Astrophysics Data System (ADS)

    Liu, Suqin; Tang, Huiling; Zhou, Huan; Dai, Gaopeng; Wang, Wanqiang

    2017-01-01

    Sandwich-like BiVO4 sheets were successfully synthesized in an aqueous solution containing bismuth nitrate, ammonium metavanadate and polyethylene glycol with a molecular weight of 10,000 (PEG-10000) using a facile microwave-assisted method. The as-prepared samples were characterized by scanning electron microscopy, N2 adsorption-desorption, X-ray diffraction, X-ray photoelectron spectroscopy (XPS), and UV-vis diffuse reflectance spectroscopy. The results show that the presence of PEG-10000 plays a critical role in the formation of BiVO4 sheets, and Ostwald ripening is the primary driving force for the formation of sandwich-like structures. The sandwich-like BiVO4 sheets exhibit a high activity for the degradation of methyl orange under visible light irradiation (λ ≥ 420 nm). The enhancement of photocatalytic activity of sandwich-like BiVO4 sheets can be attributed to its large surface area over the irregular BiVO4 particles.

  18. Microwave-assisted synthesis of novel purine nucleosides as selective cholinesterase inhibitors.

    PubMed

    Schwarz, S; Csuk, R; Rauter, A P

    2014-04-21

    Alzheimer's disease (AD), the most common form of senile dementia, is characterized by high butyrylcholinesterase (BChE) levels in the brain in later AD stages, for which no treatment is available. Pursuing our studies on selective BChE inhibitors, that may contribute to understand the role of this enzyme in disease progression, we present now microwave-assisted synthesis and anticholinesterase activity of a new nucleoside series embodying 6-chloropurine or 2-acetamido-6-chloropurine linked to D-glucosyl, D-galactosyl and D-mannosyl residues. It was designed to assess the contribution of sugar stereochemistry, purine structure and linkage to the sugar for cholinesterase inhibition efficiency and selectivity. Compounds were subjected to Ellman's assay and their inhibition constants determined. The α-anomers were the most active compounds, while selectivity for BChE or acetylcholinesterase (AChE) inhibition could be tuned by the purine base, by the glycosyl moiety and by N(7)-ligation. Some of the nucleosides were far more potent than the drug galantamine, and the most promising competitive and selective BChE inhibitor, the N(7)-linked 2-acetamido-α-D-mannosylpurine, showed a Ki of 50 nM and a selectivity factor of 340 fold for BChE over AChE.

  19. Microwave-assisted extraction of jujube polysaccharide: Optimization, purification and functional characterization.

    PubMed

    Rostami, Hosein; Gharibzahedi, Seyed Mohammad Taghi

    2016-06-05

    The operational parameters involved in microwave-assisted extraction (MAE) of jujube polysaccharide including microwave power, water to raw material ratio and extraction temperature and time were optimized by RSM. MAE at 400W, 75°C, 60 min, using 30 g water/g powdered jujube was the best condition for maximum yield (9.02%) of polysaccharide. Two novel water-soluble polysaccharides (JCP-1 and JCP-2) with average molecular weights of 9.1×10(4)-1.5×10(5)Da in term of the symmetrical narrow peaks were identified using the analytical purification procedures. The JCP-1 and JCP-2 mainly composed of glucose, arabinose, galactose and rhamnose in molar ratios of 1.4:2.1:4.2:0.9 and 1.2:1.8:4.1:1.1, respectively. The use of 1.5% JCP-1 led to a high emulsifying stability (95.5%) in a model oil-in-water type emulsion with a reduced surface tension (44.1 mN/m) and droplet size (1.32 μm), and an increased apparent viscosity (0.13 Pas) during 21-day cold storage. The antioxidant activities were increased in dose-dependent manners (25-200 μg/mL). Copyright © 2016 Elsevier Ltd. All rights reserved.

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

    SciTech Connect

    Xia Lixin; Wang Haibo; Wang Jian; Gong Ke; Jia Yi; Zhang Huili; Sun Mengtao

    2008-10-07

    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 a 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.

  1. Direct formation of LiFePO4/graphene composite via microwave-assisted polyol process

    NASA Astrophysics Data System (ADS)

    Lim, Jinsub; Gim, Jihyeon; Song, Jinju; Nguyen, Dang Thanh; Kim, Sungjin; Jo, Jeonggeun; Mathew, Vinod; Kim, Jaekook

    2016-02-01

    The present study reports on the direct synthesis of LiFePO4 nanoparticles and graphene nanosheets to form a composite cathode (LFP/GNs) in a one-step microwave-assisted polyol reaction. The polyol reaction induced by microwave irradiation for a few minutes produces nanocrystalline LFP and graphene nanosheets simultaneously from lithium, iron and phosphorus and carbon (5 wt% of graphite oxide) sources, respectively, used as starting precursors. Powder X-ray diffraction (XRD), electron microscopy, and atomic force microscopy (AFM) studies on microwave-reacted sample obtained using just graphite oxide confirms the formation of graphene nanosheets separately. Whereas, electron microscopy studies on the LFP/GNs composite reveals that olivine nanoparticles of average sizes ranging between 5 and 20 nm are well-dispersed on the graphene nanosheets. Electrochemical measurements reveal that the LiFePO4/GNs nanocomposite cathodes registered enhanced discharge capacities (79 and 108 mAh g-1 for the as-prepared and annealed composite cathodes, respectively) at 32 C rates with good capacity retention capabilities. The AC impedance measurements confirm that the enhanced cathode properties of the LFP/GNs nanocomposite are ascribed to the improved electronic conductivity of the graphene nanosheets and the nano-sized particles. The slightly better electrochemical properties of the annealed LFP/GNs are attributed to its higher crystallinity.

  2. ZnS nanosheets: Egg albumin and microwave-assisted synthesis and optical properties

    NASA Astrophysics Data System (ADS)

    Tian, Xiuying; Wen, Jin; Hu, Jilin; Chen, Zhanjun; Wang, Shumei; Peng, Hongxia; Li, Jing

    2016-09-01

    ZnS nanosheets were prepared via egg albumin and microwave-assisted method. The phases, crystalline lattice structures, morphologies, chemical and optical properties were characterized by X-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM), field-emission scanning electron microscope(FE-SEM), selected area electron diffraction (SAED), Fourier transform infrared (FTIR) spectroscopy, ultraviolet-visible (UV-Vis) spectroscopy and fluorescence(FL) spectrometer and growth mechanism of ZnS nanosheets was investigated. The results showed that all samples were pure cubic zinc blende with polycrystalline structure. The width of ZnS nanosheets with a rectangular nanostructure was in the range of 450-750 nm. The chemical interaction existed between egg albumin molecules and ZnS nanoparticles via the amide/carboxylate group. The band gap value calculated was 3.72 eV. The band at around 440 nm was attributed to the sulfur vacancies of the ZnS nanosheets. With increasing volumes of egg albumin, the photoluminescence (PL) intensity of ZnS samples firstly increased and then decreased, attributed to concentration quenching.

  3. Morphology and Properties of (Ba, Sr, Ca) Titanates Synthesized by Microwave-Assisted Hydrothermal Method

    NASA Astrophysics Data System (ADS)

    Souza, A. E.; Santos, G. T. A.; Silva, R. A.; Moreira, M. L.; Volante, D. P.; Teixeira, S. R.; Longo, E.

    2011-10-01

    Ba1-xCaxTiO3, Ba1-xSrxTiO3 and Sr1-xCaxTiO3 (x = 0, 0.25, 0.50, 0.75 and 1) nanoparticles were synthesized using the microwave-assisted hydrothermal method. Samples were prepared for 40 minutes at 140°C under a pressure of 3 MPa using an adapted domestic microwave oven. The samples were characterized by X-Ray diffraction (XRD), scanning electron microscopy (FE-SEM), and Raman, photoluminescence (PL) and ultraviolet-visible (UV-Vis) spectroscopies. XRD data show that ceramic powders have crystalline phases associated with a short-range structural disorder. This structural disorder is confirmed by Raman spectral bands indicating multi-phonon processes and the presence of defects or impurities. Such defects account for a broad band in the photoluminescence spectrum in the green light (460 nm) region for all samples. Gap energy variation, obtained from UV-Vis spectra, suggest a non-uniform band structure of these titanates in accordance with the PL results. The morphology of each sample is changed with doping and varies from a spherical to cubic appearance for energy minimization.

  4. Microwave-assisted extraction of active pharmaceutical ingredient from solid dosage forms.

    PubMed

    Hoang, T H; Sharma, R; Susanto, D; Di Maso, M; Kwong, E

    2007-07-13

    The microwave assisted extraction (MAE) technique has been evaluated for the extraction of active pharmaceutical ingredients (API) from various solid dosage forms. Using immediate release tablets of Compound A as a model, optimization of the extraction method with regards to extraction solvent composition, extraction time and temperature was briefly discussed. Complete recovery of Compound A was achieved when samples were extracted using acetonitrile as the extraction solvent under microwave heating at a constant cell temperature of 50 degrees C for 5 min. The optimized MAE method was applied for content uniformity (single tablet extraction) and potency (multiple tablets extraction) assays of release and stability samples of two products of Compound A (5 and 25mg dose strength) stored at various conditions. To further demonstrate the applicability of MAE, the instrumental extraction conditions (50 degrees C for 5 min) were adopted for the extraction of montelukast sodium (Singulair) from various solid dosage forms using methanol-water (75:25, v/v) as the extraction solvent. The MAE procedure demonstrated an extraction efficiency of 97.4-101.9% label claim with the greatest RSD at 1.4%. The results compare favorably with 97.6-102.3% label claim with the greatest RSD at 2.9% obtained with validated mechanical extraction procedures. The system is affordable, user-friendly and simple to operate and troubleshoot. Rapid extraction process (7 min/run) along with high throughput capacity (up to 23 samples simultaneously) would lead to reduced cycle time and thus increased productivity.

  5. Influence of Polarity and Activation Energy in Microwave-Assisted Organic Synthesis (MAOS).

    PubMed

    Rodríguez, Antonio M; Prieto, Pilar; de la Hoz, Antonio; Díaz-Ortiz, Ángel; Martín, D Raúl; García, José I

    2015-06-01

    The aim of this work was to determine the parameters that have decisive roles in microwave-assisted reactions and to develop a model, using computational chemistry, to predict a priori the type of reactions that can be improved under microwaves. For this purpose, a computational study was carried out on a variety of reactions, which have been reported to be improved under microwave irradiation. This comprises six types of reactions. The outcomes obtained in this study indicate that the most influential parameters are activation energy, enthalpy, and the polarity of all the species that participate. In addition to this, in most cases, slower reacting systems observe a much greater improvement under microwave irradiation. Furthermore, for these reactions, the presence of a polar component in the reaction (solvent, reagent, susceptor, etc.) is necessary for strong coupling with the electromagnetic radiation. We also quantified that an activation energy of 20-30 kcal mol(-1) and a polarity (μ) between 7-20 D of the species involved in the process is required to obtain significant improvements under microwave irradiation.

  6. Optimization of microwave assisted extraction of pectin from sour orange peel and its physicochemical properties.

    PubMed

    Hosseini, Seyed Saeid; Khodaiyan, Faramarz; Yarmand, Mohammad Saeid

    2016-04-20

    Microwave assisted extraction technique was used to extract pectin from sour orange peel. Box-Behnken design was used to study the effect of irradiation time, microwave power and pH on the yield and degree of esterification (DE) of pectin. The results showed that the optimum conditions for the highest yield of pectin (29.1%) were obtained at pH of 1.50, microwave power of 700W, and irradiation time of 3min. DE values of pectin ranged from 1.7% to 37.5%, indicating that the obtained pectin was low in methoxyl. Under optimal conditions, the galacturonic acid content and emulsifying activity were 71.0±0.8% and 40.7%, respectively. In addition, the emulsion stability value ranged from 72.1% to 83.4%. Viscosity measurement revealed that the solutions of pectin at low concentrations showed nearly Newtonian flow behavior, and as the concentration increased, pseudoplastic flow became dominant. Copyright © 2015 Elsevier Ltd. All rights reserved.

  7. BiOBr hierarchical microspheres: Microwave-assisted solvothermal synthesis, strong adsorption and excellent photocatalytic properties.

    PubMed

    Zhang, Lei; Cao, Xiao-Feng; Chen, Xue-Tai; Xue, Zi-Ling

    2011-02-15

    Two kinds of BiOBr nanosheets-assembled microspheres were successfully prepared via a facile, rapid and reliable microwave-assisted solvothermal route, employing Bi(NO(3))(3)·5H(2)O and cetyltrimethylammonium bromide (CTAB) as starting reagents in the absence or presence of oleic acid. The phase and morphology of the products were characterized by powder X-ray diffraction (XRD), energy dispersive spectrometry (EDS), selected area electron diffraction (SAED), high resolution transmission electron microscopy (HRTEM) and scanning electron microscopy (SEM). Experiments indicated that the formation of these building blocks of microspheres could be ascribed to the self-assembly of nanoparticles according to mesocrystal growth mode. Interestingly, both samples exhibited not only strong adsorption abilities, but also excellent photocatalytic activities for methyl orange (MO), rhodamine B (RhB) and phenol. The resulting BiOBr hierarchical microspheres are very promising adsorbents and photocatalysts for the treatment of organic pollutants. Copyright © 2010 Elsevier Inc. All rights reserved.

  8. Microwave-assisted one-pot synthesis of 1,6-anhydrosugars and orthogonally protected thioglycosides.

    PubMed

    Ko, Yen-Chun; Tsai, Cheng-Fang; Wang, Cheng-Chung; Dhurandhare, Vijay M; Hu, Pu-Ling; Su, Ting-Yang; Lico, Larry S; Zulueta, Medel Manuel L; Hung, Shang-Cheng

    2014-10-15

    Living organisms employ glycans as recognition elements because of their large structural information density. Well-defined sugar structures are needed to fully understand and take advantage of glycan functions, but sufficient quantities of these compounds cannot be readily obtained from natural sources and have to be synthesized. Among the bottlenecks in the chemical synthesis of complex glycans is the preparation of suitably protected monosaccharide building blocks. Thus, easy, rapid, and efficient methods for building-block acquisition are desirable. Herein, we describe routes directly starting from the free sugars toward notable monosaccharide derivatives through microwave-assisted one-pot synthesis. The procedure followed the in situ generation of per-O-trimethylsilylated monosaccharide intermediates, which provided 1,6-anhydrosugars or thioglycosides upon treatment with either trimethylsilyl trifluoromethanesulfonate or trimethyl(4-methylphenylthio)silane and ZnI2, respectively, under microwave irradiation. We successfully extended the methodology to regioselective protecting group installation and manipulation toward a number of thioglucosides and the glycosylation of persilylated derivatives, all of which were conducted in a single vessel. These developed approaches open the possibility for generating arrays of suitably protected building blocks for oligosaccharide assembly in a short period with minimal number of purification stages.

  9. The Microwave-Assisted Green Synthesis of TiC Powders.

    PubMed

    Wang, Hui; Zhu, Wencheng; Liu, Yanchun; Zeng, Lingke; Sun, Luyi

    2016-11-08

    Titanium carbide (TiC) is an important engineering material and has found widespread applications. Currently, TiC is typically synthesized through carbothermal reduction, requiring a high temperature (ca. 1700-2300 °C) and long reaction time (ca. 10-20 h), which is not eco-friendly. During a conventional reaction path, anatase TiO₂ (A-TiO₂) was first converted to rutile TiO₂ (R-TiO₂), which was subsequently reduced to TiC. Herein, we explored the synthesis of TiC powders with the assistance of microwave heating. In particular, we achieved the conversion of A-TiO₂, which was more reactive than R-TiO₂ for the carbothermal reduction, to TiC, which was directly due to quick microwave heating. As such, the carbothermal reduction started at a much lower temperature of ca. 1200 °C and finished within 30 min when reacting at 1400 °C, leading to significant energy saving. This study shows that microwave-assisted synthesis can be an effective and green process for preparing TiC powders, which is promising for future large-scale production. The influence of the reaction temperature, the reaction duration, and the carbon content on the synthesis of TiC powders was investigated.

  10. Fast Microwave-assisted Pretreatment for Bioconversion of Sawdust Lignocellulose to Glucose

    NASA Astrophysics Data System (ADS)

    Nyoman Sudiana, I.; Mitsudo, Seitaro; Endang Susilowati, Prima; Ketut Sutiari, Desak; Widana Arsana, Made; Zamrun Firihu, Muhammad; Ode Ngkoimani, La; Aba, La; Sahaluddin Hasan, Erzam; Cahyono, Edi; Sabchevski, Svilen; Aripin, Haji; Gde Suastika, Komang

    2017-05-01

    A preliminary study of application microwave energy for bioconversion of cellulosic sawdust to glucose was performed. The effects of the microwave were compared to those of the conventional method for each solvent. It was expected that a broader mechanism responsible for the microwave effects on the chemical processes, especially the pretreatment on the hydrolysis of cellulose can be explained. Reagents used were an acid (HCl), an alkali (NaOH), and distilled water (H2O). The experimental results showed that the microwave-assisted pretreatment on the lignocellulosic sawdust faster than by using conventional heating (hotplate). Moreover by using microwave a higher glucose content compared to the conventional method was found. With microwave during hydrolisis, high temperatures and high reagent concentrations were not required. Pretreatment with a microwave at 800 Watt and solvent NaOH 22,50 mg/mL at a temperature of 120°c appeared to be most efficient found in this experiment. These results indicate that microwave effective for bioconversion of cellulosic sawdust to glucose. The microstructure evaluation by using SEM and XRD should be performed to understand more detail the effect especially on their cellulosic structural evolution.

  11. Microwave-assisted extraction of polyphenols from Camellia oleifera fruit hull.

    PubMed

    Zhang, Liangliang; Wang, Yongmei; Wu, Dongmei; Xu, Man; Chen, Jiahong

    2011-05-27

    The abundant fruit hulls of tea-oil tree (Camellia oleifera) are still underutilized and wastefully discaded to pollute the environment. In order to solve this problem and better utilize the fruit hulls of C. oleifera, a microwave-assisted extraction system was used to extract their polyphenols using water as the extraction solvent. A central composite design (CCD) was used to monitor the effects of three extraction processing parameters--liquid:solid ratio (mL/g), extraction time (min) and extraction temperature (°C)--on the polyphenol yield (%). The results showed that the optimal conditions were liquid:solid ratio of 15.33:1 (mL/g), extraction time of 35 min and extraction temperature of 76 °C. Validation tests indicated that under the optimized conditions the actual yield of polyphenols was 15.05 ± 0.04% with RSD = 0.21% (n = 5), which was in good agreement with the predicted yield. Phenolic compounds in the extracts were analysed by HPLC, and gallic acid was found to be the predominant constituent. The total flavonoid content in the extracts was determined and high total flavonoid content was revealed (140.06 mg/g dry material).

  12. Effect of Microwave-Assisted Extraction on the Phenolic Compounds and Antioxidant Capacity of Blackthorn Flowers.

    PubMed

    Lovrić, Vanja; Putnik, Predrag; Kovačević, Danijela Bursać; Jukić, Marijana; Dragović-Uzelac, Verica

    2017-06-01

    This research was undertaken to investigate the influence of extraction parameters during microwave-assisted extraction on total phenolic content, total flavonoids, total hydroxycinnamic acids and total flavonols of blackthorn flowers as well as to evaluate the antioxidant capacity by two different methods (2,2-diphenyl-1-picrylhydrazyl free radical scavenging capacity and ferric reducing antioxidant power assays). The investigated extraction parameters were: solvent type and volume fraction of alcohol in solvent (50 and 70% aqueous solutions of ethanol and methanol), extraction time (5, 15 and 25 min) and extraction temperature (40, 50 and 60 °C) controlled by microwave power of 100, 200 and 300 W. Multivariate analysis of variance (MANOVA) was used to evaluate the differences at a 95% confidence level (p≤0.05). The obtained results show that aqueous solution of ethanol was more appropriate solvent for extraction of phenolic compounds (total flavonoids, total hydroxycinnamic acids and total flavonols) than aqueous solution of methanol. The amount of phenolic compounds was higher in 70% aqueous solution of ethanol or methanol, while higher antioxidant capacity was observed in 50% aqueous solution of methanol. Higher temperature of extraction improved the amount of phenolic compounds and also antioxidant capacity determined by 2,2-diphenyl-1-picrylhydrazyl free radical scavenging capacity assay. Extensive duration of extraction (15- to 25-minute interval) has a significant effect only on the increase of total phenolic content, while specific phenolic compound content and antioxidant capacity were the highest when microwave extraction time of 5 min was applied.

  13. Phytochemical analysis of Myrtus communis plant: Conventional versus microwave assisted-extraction procedures.

    PubMed

    Bouaoudia-Madi, Nadia; Boulekbache-Makhlouf, Lila; Kadri, Nabil; Dahmoune, Farid; Remini, Hocine; Dairi, Sofiane; Oukhmanou-Bensidhoum, Sonia; Madani, Khodir

    2017-06-10

    Background Myrtle (Myrtus communis L) may constitute an interesting dietary source of health protective compounds. Microwave-assisted extraction (MAE) of total phenolic compounds (TPC) from myrtle leaf, stems, pericarp, and seeds was studied and the results were compared with those of the conventional method extraction (CME) in terms of extraction time. Methods Extraction yield/efficiency and antioxidant activity were measured using radical scavenging assay (DPPH•) and reducing power. Results The results show that the MAE was higher in terms of saving energy, extraction time (62 s) and extraction efficiency of bioactive compound compared to CME (2 h). Leaf presented the optimum content of total phenols (250 mg GAE.g-1 DW) and flavonoids (13.65 mg GAE.g-1 DW). However, the anthocyanin content was most important in pericarp extract (176.50±2.17 mg Cyd-3-glu g-1 DW). The antioxidant activity was important in all parts, mainly in leaves. The results indicated that appropriate microwave treatment could be an efficient process to phenolic compounds recovery and thus, better the antioxidant activity of myrtle extract. Conclusions Principal component analysis (PCA) applied to the experimental data shows that the distribution of the myrtle phenolic compounds depended on their plant part localization as well as the extraction method.

  14. Microwave assisted synthesis of ZnO nanoparticles for lighting and dye removal application

    NASA Astrophysics Data System (ADS)

    Kumar, Vijay; Gohain, M.; Som, S.; Kumar, Vinod; Bezuindenhoudt, B. C. B.; Swart, Hendrik C.

    2016-01-01

    In this study, we report on the synthesis of ZnO nanoparticles (NPs) via the microwave-assisted technique. The as-synthesized ZnO nanoparticles were annealed at 500 °C for three hours. The ZnO NPs were characterized by X-ray diffraction (XRD) and scanning electron microscopic techniques. XRD results confirmed the formation of as-synthesized ZnO powder oriented along the (101) direction. The Kubelka-Munk function has been employed to determine the band gap of the ZnO powder. ZnO powder has been studied by photoluminescence (PL) before and after annealing to identify the emission of defects in the visible range. The intensity of the PL emission has decreased after annealing. The synthesized ZnO samples were also studied for methyl orange dye removal from waste water. It has been found that the as-synthesized ZnO shows better adsorption behaviour as compared to the annealed sample.

  15. Facile Microwave-Assisted Synthesis of Klockmannite CuSe Nanosheets and Their Exceptional Electrical Properties

    PubMed Central

    Liu, Yong-Qiang; Wang, Feng-Xia; Xiao, Yan; Peng, Hong-Dan; Zhong, Hai-Jian; Liu, Zheng-Hui; Pan, Ge-Bo

    2014-01-01

    Klockmannite copper selenide nanosheets (CuSe NSs) are synthesized by a facile microwave-assisted method and fully characterized. The nanosheets have smooth surface and hexagonal shape. The lateral size is 200–500 nm × 400–800 nm and the thickness is 55 ± 20 nm. The current-voltage characteristics of CuSe NS films show unique Ohmic and high-conducting behaviors, comparable to the thermally-deposited gold electrode. The high electrical conductivity of CuSe NSs implies their promising applications in printed electronics and nanodevices. Moreover, the local electrical variation is observed, for the first time, within an individual CuSe NS at low bias voltages (0.1 ~ 3 V) by conductive atomic force microscopy (C-AFM). This is ascribed to the quantum size effect of NS and the presence of Schottky barrier. In addition, the influence of the molar ratio of Cu2+/SeO2, reaction temperature, and reaction time on the growth of CuSe NSs is explored. The template effect of oleylamine and the intrinsic crystal nature of CuSe NS are proposed to account for the growth of hexagonal CuSe NSs. PMID:25104467

  16. Effect of microwave-assisted dry heating with xanthan on normal and waxy corn starches.

    PubMed

    Sun, Qingjie; Xu, Yicai; Xiong, Liu

    2014-07-01

    Normal corn starch (CS) and waxy corn starch (WCS) were impregnated with xanthan gum (1% based on starch) and heat-treated using a microwave in a dry state for 0, 4, or 6min (CS-X0, CS-X4, CS-X6, WCS-X0, WCS-X4, WCS-X6), respectively. Effects of the microwave-assisted dry heating (MADH) on pasting, morphological, and structural properties were evaluated. The results revealed that the viscosity of both the CS and WCS with xanthan increased compared with untreated samples after MADH, and the effect on WCS was more obvious. The syneresis values showed that the water-holding ability of CS-X6 and WCS-X6 increased, and that value of CS was lower than that of WCS after MADH with xanthan. The MADH with xanthan reduced the To, Tc, Tp, and ΔH values of both the CS and WCS. After MADH, the particle morphology of the starch-xanthan connected more densely, especially WCS, and the gelatinized samples exhibited a strong and smooth laminar structure. The Fourier transform Infrared Spectroscopy (FTIR) displayed that the absorption peak width of both CS-X6 and WCS-X6 became larger. X-ray diffraction showed that the crystallinity of CS-X6 and WCS-X6 decreased slightly as a result of MADH, and the crystalline pattern remained A-type. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Microwave assisted novel MoBi2S5 nanoflowers: Synthesis, characterization, photoelectrochemical performance

    NASA Astrophysics Data System (ADS)

    Pawar, Nita B.; Mali, Sawanta S.; Kharade, Suvarta D.; Kondalkar, Vijay V.; Ghanwat, Vishvanath B.; Khot, Kishorkumar V.; Patil, Pramod S.; Bhosale, Popatrao N.

    2016-11-01

    In the present article, we have studied the effect of post annealing treatment on microstructural, optical and photoelectrochemical (PEC) properties of MoBi2S5 thin films synthesized by microwave assisted technique. The synthesized thin films are vacuum annealed for 4 h at 473 K temperature. The X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM) and UV-Vis-NIR spectrophotometer techniques were used for characterization of the as deposited and annealed MoBi2S5 thin films. The XRD patterns confirm the synthesized and annealed thin films have nanocrystalline nature with rhombohedral-orthorhombic crystal structure. SEM micrographs indicate that, nanoflowers exhibit sharper end after annealing. The optical absorption study illustrates that the optical band gap energy has been decrease from 2.0 eV to 1.75 eV with annealing. Finally, applicability of synthesized thin films has been checked for PEC property. The J-V curves revealed that synthesized thin film photoanodes are suitable for PEC cell application. As well, used simple, economical method has great potential for synthesis of various thin film materials.

  18. Determination of dieldrin in wool products by gas chromatography with microwave-assisted extraction.

    PubMed

    Ohto, Mikiya; Kodama, Shuji; Saito, Yukio; Yamamoto, Atushi

    2006-12-01

    Dieldrin is a moth-proofing agent that was banned by the Stockholm Convention in 2001. The amount of dieldrin in wool products was measured by a microwave-assisted extraction (MAE) method. The optimal conditions were as follows: extraction solvent, acetone/n-hexane (1:1 v/v); extraction temperature, 110 degrees C; extraction time, 10 min; solvent volume, 25 mL. When six samples were used, dieldrin contents determined by GC with the proposed MAE agreed closely with those by the Japanese official method using GC with solvent extraction and cleanup by column chromatography. The proposed MAE has two merits. First, the pretreatment of the MAE needs only 4 h for 11 samples, while that using the Japanese official method needs 2 days for six samples. Second, the volume of organic solvents used for the proposed method was only about one-tenth of that used in the Japanese official method. Our proposed method seems to be easy and useful for daily (routine) tests. Dieldrin contents of 28 used wool products, which were obtained from local clothing shops and ordinary homes, were determined by GC with the proposed MAE, and six products contained dieldrin (0.310-175 ppm). The dry cleaning of the woolen yarn containing 175 ppm dieldrin did not remove a significant amount of dieldrin. Therefore, it seems likely that dieldrin is still distributed slightly but widely throughout the world.

  19. Fast microwave-assisted pyrolysis of microalgae using microwave absorbent and HZSM-5 catalyst.

    PubMed

    Borges, Fernanda Cabral; Xie, Qinglong; Min, Min; Muniz, Luis Antônio Rezende; Farenzena, Marcelo; Trierweiler, Jorge Otávio; Chen, Paul; Ruan, Roger

    2014-08-01

    Fast microwave-assisted pyrolysis (fMAP) in the presence of a microwave absorbent (SiC) and catalyst (HZSM-5) was tested on a Chlorella sp. strain and on a Nannochloropsis strain. The liquid products were characterized, and the effects of temperature and catalyst:biomass ratio were analyzed. For Chlorella sp., a temperature of 550 °C, with no catalyst were the optimal conditions, resulting in a maximum bio-oil yield of 57 wt.%. For Nannochloropsis, a temperature of 500 °C, with 0.5 of catalyst ratio were shown to be the optimal condition, resulting in a maximum bio-oil yield of 59 wt.%. These results show that the use of microwave absorbents in fMAP increased bio-oil yields and quality, and it is a promising technology to improve the commercial application and economic outlook of microwave pyrolysis technology. Additionally, the use of a different catalyst needs to be considered to improve the bio-oil characteristics. Copyright © 2014 Elsevier Ltd. All rights reserved.

  20. Parameters affecting microwave-assisted extraction of organophosphorus pesticides from agricultural soil.

    PubMed

    Fuentes, Edwar; Báez, María E; Labra, Ronnie

    2007-10-26

    This work describes an optimised method for the determination of six representative organophosphorus pesticides (OPPs) (diazinon, parathion, methyl pirimiphos, methyl parathion, ethoprophos, and fenitrothion) in agricultural soils. The method is based on microwave-assisted extraction using a water-methanol modified mixture for desorption and simultaneous partitioning on n-hexane (MAEP), together with gas chromatography-flame photometric detection (GC-FPD). To improve GC-FPD signals (peak intensity and shape) olive oil was used effectively as a "matrix mimic". The optimisation of the extraction method was achieved in two steps: an initial approach through experimental design and principal component analysis where recovery of compounds using a water-methanol mixture ranged from 54 to 77%, and the second one by studying the addition of KH2PO4 to the extracting solution where recoveries were significantly increased, molecular replacing of OPPs from adsorption sites by phosphate being the probable extraction mechanism. Under optimised conditions, recoveries of pesticides from different soils were higher than 73%, except for methyl parathion in some soils, with SD equal or lower than 11% and detection limits ranging from 0.004 to 0.012 microg g(-1). The proposed method was used to determine OPPs in soil samples from different agricultural zones of Chile.

  1. Rapid immunohistochemical diagnosis of tobacco mosaic virus disease by microwave-assisted plant sample preparation

    PubMed Central

    Zellnig, Günther; Möstl, Stefan; Zechmann, Bernd

    2013-01-01

    Immunoelectron microscopy is a powerful method to diagnose viral diseases and to study the distribution of the viral agent within plant cells and tissues. Nevertheless, current protocols for the immunological detection of viral diseases with transmission electron microscopy (TEM) in plants take between 3 and 6 days and are therefore not suited for rapid diagnosis of virus diseases in plants. In this study, we describe a method that allows rapid cytohistochemical detection of tobacco mosaic virus (TMV) in leaves of tobacco plants. With the help of microwave irradiation, sample preparation of the leaves was reduced to 90 min. After sample sectioning, virus particles were stained on the sections by immunogold labelling of the viral coat protein, which took 100 min. After investigation with the TEM, a clear visualization of TMV in tobacco cells was achieved altogether in about half a day. Comparison of gold particle density by image analysis revealed that samples prepared with the help of microwave irradiation yielded significantly higher gold particle density as samples prepared conventionally at room temperature. This study clearly demonstrates that microwave-assisted plant sample preparation in combination with cytohistochemical localization of viral coat protein is well suited for rapid diagnosis of plant virus diseases in altogether about half a day by TEM. PMID:23580761

  2. Optimization of microwave-assisted enzymatic extraction of polysaccharides from the fruit of Schisandra chinensis Baill.

    PubMed

    Cheng, Zhenyu; Song, Haiyan; Yang, Yingjie; Liu, Yan; Liu, Zhigang; Hu, Haobin; Zhang, Yang

    2015-05-01

    A microwave-assisted enzymatic extraction (MAEE) method had been developed, which was optimized by response surface methodology (RSM) and orthogonal test design, to enhance the extraction of crude polysaccharides (CPS) from the fruit of Schisandra chinensis Baill. The optimum conditions were as follows: microwave irradiation time of 10 min, extraction pH of 4.21, extraction temperature of 47.58°C, extraction time of 3h and enzyme concentration of 1.5% (wt% of S. chinensis powder) for cellulase, papain and pectinase, respectively. Under these conditions, the extraction yield of CPS was 7.38 ± 0.21%, which was well in close agreement with the value predicted by the model. The three methods including heat-refluxing extraction (HRE), ultrasonic-assisted extraction (UAE) and enzyme-assisted extraction (EAE) for extracting CPS by RSM were further compared. Results indicated MAEE method had the highest extraction yields of CPS at lower temperature. It was indicated that the proposed approach in this study was a simple and efficient technique for extraction of CPS in S. chinensis Baill.

  3. Numerical simulation of an industrial microwave assisted filter dryer: criticality assessment and optimization.

    PubMed

    Leonelli, Cristina; Veronesi, Paolo; Grisoni, Fabio

    2007-01-01

    Industrial-scale filter dryers, equipped with one or more microwave input ports, have been modelled with the aim of detecting existing criticalities, proposing possible solutions and optimizing the overall system efficiency and treatment homogeneity. Three different loading conditions have been simulated, namely the empty applicator, the applicator partially loaded by both a high-loss and low loss load whose dielectric properties correspond to the one measured on real products. Modeling results allowed for the implementation of improvements to the original design such as the insertion of a wave guide transition and a properly designed pressure window, modification of the microwave inlet's position and orientation, alteration of the nozzles' geometry and distribution, and changing of the cleaning metallic torus dimensions and position. Experimental testing on representative loads, as well as in production sites, allowed for the confirmation of the validity of the implemented improvements, thus showing how numerical simulation can assist the designer in removing critical features and improving equipment performances when moving from conventional heating to hybrid microwave-assisted processing.

  4. ICP-AES determination of minor- and major elements in apples after microwave assisted digestion.

    PubMed

    Juranović Cindrić, Iva; Krizman, Ivona; Zeiner, Michaela; Kampić, Štefica; Medunić, Gordana; Stingeder, Gerhard

    2012-12-15

    The aim of this paper was to determine the content of minor and major elements in apples by inductively coupled plasma atomic emission spectrometry (ICP-AES). Prior to ICP-AES measurement, dried apples were digested in a microwave assisted digestion system. The differences in the measured element concentrations after application of open and closed microwave system as sample preparation procedures are discussed. In whole apples, flesh and peel Ag, Al, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, Sr and Zn were analysed after optimisation and validating the analytical method using ICP-AES. The accuracy of the method determined by spiking experiments was very good (recoveries 88-115%) and the limits of detection of elements of interest were from 0.01 up to 14.7 μg g(-1). The reference ranges determined in all apple samples are 39-47 mg g(-1) for K, 9-14 mg g(-1) for Na, 3-7 mg g(-1) for Mg, 3-7 μg g(-1) for Zn, 0.7-2.8 μg g(-1) for Sr. The range of Mn in peel 4-6 μg g(-1) is higher compared to whole apple from 0.7 to 1.7 μg g(-1). Cd is found only in peel, in the concentration range of 0.4-1.1 μg g(-1).

  5. Analysis of deamidation artifacts induced by microwave-assisted tryptic digestion of a monoclonal antibody.

    PubMed

    Formolo, Trina; Heckert, Alan; Phinney, Karen W

    2014-10-01

    The thorough characterization of biopharmaceuticals is essential for ensuring their quality and safety since many potential variations can cause changes to the properties of a drug that may be detrimental to the patient such as decreased efficacy, shorter half-life or increased immunogenicity. Prior to approval and release, protein-based drugs are subject to a battery of analyses to assess the nature of those parameters that are considered critical quality attributes. In some cases the analytical method used may itself cause modifications that are impossible to distinguish from those induced by the intended test conditions (e.g. storage time/temperature, light exposure) which are used to assess drug stability. It is therefore important to develop and utilize analytical methods which impose as few artifactual modifications as possible. Asparagine deamidation is a common protein modification and it is known to be induced during tryptic digestion. Therefore we examined common tryptic digestion protocols and compared their propensities towards asparagine modification. Since microwave assisted hydrolysis techniques are often used to shorten digestion times and the effect on deamidation is unknown we sought to compare this method against alternate digestion protocols.

  6. Development of continuous microwave-assisted protein digestion with immobilized enzyme.

    PubMed

    Chen, Zhengyi; Li, Yongle; Lin, Shuhai; Wei, Meiping; Du, Fuyou; Ruan, Guihua

    2014-03-07

    In this study, an easy and efficiency protein digestion method called continuous microwave-assisted protein digestion (cMAED) with immobilized enzyme was developed and applied for proteome analysis by LC-MS(n). Continuous microwave power outputting was specially designed and applied. Trypsin and bromelain were immobilized onto magnetic micropheres. To evaluate the method of cMAED, bovine serum albumin (BSA) and protein extracted from ginkgo nuts were used as model and real protein sample to verify the digestion efficiency of cMAED. Several conditions including continuous microwave power, the ratio of immobilized trypsin/BSA were optimized according to the analysis of peptide fragments by Tricine SDS-PAGE and LC-MS(n). Subsequently, the ginkgo protein was digested with the protocols of cMAED, MAED and conventional heating enzymatic digestion (HED) respectively and the LC-MS(n) profiles of the hydrolysate was compared. Results showed that cMAED combined with immobilized enzyme was a fast and efficient digestion method for protein digestion and microwave power tentatively affected the peptide producing. The cMAED method will be expanded for large-scale preparation of bioactive peptides and peptide analysis in biological and clinical research.

  7. Histology-directed microwave assisted enzymatic protein digestion for MALDI MS analysis of mammalian tissue.

    PubMed

    Taverna, Domenico; Norris, Jeremy L; Caprioli, Richard M

    2015-01-06

    This study presents on-tissue proteolytic digestion using a microwave irradiation and peptide extraction method for in situ analysis of proteins from spatially defined regions of a tissue section. The methodology utilizes hydrogel discs (1 mm diameter) embedded with trypsin solution. The enzyme-laced hydrogel discs are applied to a tissue section, directing enzymatic digestion to a spatially confined area of the tissue. By applying microwave radiation, protein digestion is performed in 2 min on-tissue, and the extracted peptides are then analyzed by matrix assisted laser desorption/ionization mass spectrometry (MALDI MS) and liquid chromatography tandem mass spectrometry (LC-MS/MS). The reliability and reproducibility of the microwave assisted hydrogel mediated on-tissue digestion is demonstrated by the comparison with other on-tissue digestion strategies, including comparisons with conventional heating and in-solution digestion. LC-MS/MS data were evaluated considering the number of identified proteins as well as the number of protein groups and distinct peptides. The results of this study demonstrate that rapid and reliable protein digestion can be performed on a single thin tissue section while preserving the relationship between the molecular information obtained and the tissue architecture, and the resulting peptides can be extracted in sufficient abundance to permit analysis using LC-MS/MS. This approach will be most useful for samples that have limited availability but are needed for multiple analyses, especially for the correlation of proteomics data with histology and immunohistochemistry.

  8. Focused microwave-assisted Soxhlet extraction: a convincing alternative for total fat isolation from bakery products.

    PubMed

    Priego-Capote, F; Luque de Castro, M D

    2005-01-15

    An approach for automated fast extraction of the fat content in bakery products based on focused microwave-assisted Soxhlet extraction (FMASE) and gravimetric determination is proposed. The main factors affecting the extraction efficiency-namely, power of irradiation, number of cycles and irradiation time-were optimized using experimental design methodology. The proposed method was applied to six samples, which were classified in two groups-namely, snacks and cookies. The results obtained agree with those provided by the AOAC 920.39 reference extraction method. No significant differences in the extraction efficiency of the fat content in bakery samples using FMASE versus the official method were found. Moreover, a drastic reduction in both the extraction time (60 and 35min versus 16 and 8h, respectively, for the two above commented groups) and sample handling are achieved with similar precision (expressed as repeatability and within-laboratory reproducibility standard deviation) to that provided by the AOAC 920.39 method. In addition, the proposed method is cleaner than the reference method as 75-80% of the extractant is recycled.

  9. Extraction of polychlorinated biphenyls from soils by automated focused microwave-assisted Soxhlet extraction.

    PubMed

    Luque-García, J L; de Castro, Luque

    2003-05-23

    The application of a new focused microwave-assisted Soxhlet extractor for the extraction of polychlorinated biphenyls from differently aged soils is here presented. The new extractor overcomes the disadvantages of previous devices based on the same principle and enables a fully automated extraction of two samples simultaneously. The variables affecting the extraction step (namely, power of irradiation, irradiation time, extractant volume, extractant composition and number of extraction cycles) have been optimized using experimental design methodology. The optimized method has also been applied to a certified reference material (CRM910-050 "real" contaminated soil) for quality assurance validation. Quantification of the target compounds has been performed by GC with ion-trap MS. The mass spectrometer was operated in the electron-ionization mode, with selected-ion monitoring at m/z 152, 186, 292, 326 and 498. The results obtained have demonstrated that this approach is as efficient as conventional Soxhlet but with a drastic reduction of both extraction time (70 min vs. 24 h for the "real" contaminated soil) and organic solvent disposal, as 75-80% of the extractant is recycled.

  10. Focused microwave-assisted Soxhlet extraction: a convincing alternative for total fat isolation from bakery products.

    PubMed

    Priego-Capote, F; Luque de Castro, M D

    2005-01-15

    An approach for automated fast extraction of the fat content in bakery products based on focused microwave-assisted Soxhlet extraction (FMASE) and gravimetric determination is proposed. The main factors affecting the extraction efficiency namely; power of irradiation, number of cycles and irradiation time were optimized using experimental design methodology. The proposed method was applied to six samples, which were classified in two groups namely snacks and cookies. The results obtained agree with those provided by the AOAC 920.39 reference extraction method. No significant differences in the extraction efficiency of the fat content in bakery samples using FMASE versus the official method were found. Moreover, a drastic reduction in both the extraction time (60 and 35min versus 16 and 8h, respectively, for the two above commented groups) and sample handling are achieved with similar precision (expressed as repeatability and within laboratory reproducibility standard deviation) to that provided by the AOAC 920.39 method. In addition, the proposed method is cleaner than the reference method as 75-80% of the extractant is recycled.

  11. Renewable platform chemicals from directional microwave-assisted liquefaction coupling stepwise extraction of waste biomass.

    PubMed

    Feng, Junfeng; Hse, Chungyun; Yang, Zhongzhi; Wang, Kui; Jiang, Jianchun; Xu, Junming

    2017-11-01

    Directional microwave-assisted liquefaction and stepwise extraction are introduced for producing platform chemicals: aromatics and monosaccharides. When sulfuric acid was used as a catalyst, a 45% monosaccharides yield and a 29% aromatics yield were obtained from bamboo with 0.3g catalyst per 18g methanol and 2g bamboo at 160°C with 10min. Approximately 78-86wt% of the six biomass materials were converted into liquid products. After the stepwise extraction and precipitation process, the yields of monosaccharide derivatives and three phenolic compound fractions were 39-45% and 28-32%, respectively. Monosaccharides from holocellulose collected with a high purity of methyl glycosides were higher than 90%. Aromatic derivatives with different weight-molecular distributions were separated into three fractions with more than 80% phenolics. As their similar chemical properties within each fraction, platform chemicals have great commercial potential for producing high-quality chemicals and biofuels using mild upgrading conditions. Copyright © 2017. Published by Elsevier Ltd.

  12. Improving the efficiency of antioxidant extraction from mango peel by using microwave-assisted extraction.

    PubMed

    Dorta, Eva; Lobo, M Gloria; González, Mónica

    2013-06-01

    The purpose of this study was to analyze the extraction efficiency of antioxidants from mango peel by comparing two techniques: microwave-assisted (MAE) and traditional solvent (TE) extraction. The number of extraction steps, water content in the extractant, peel weight-to-solvent volume ratio in extractions and extraction time all had an influence on obtaining extracts with high antioxidant capacity, but the extraction technique and the water content in the extractant were the factors with the greatest effect. Using three steps, a water content of 50 % in the ethanol:water extractant, an extraction time of 60 min and a weight-to-volume ratio of 1:10 or 1:50 (w/v) led to the highest antioxidant activity and phytochemicals content in extracts. The extraction time needed to extract phytochemicals from mango peel was similar when MAE and TE were used. However, the antioxidant capacity and phytochemical content were around 1.5-6.0 times higher in the extracts obtained by MAE.

  13. Optimisation and validation of the microwave-assisted extraction of phenolic compounds from rice grains.

    PubMed

    Setyaningsih, W; Saputro, I E; Palma, M; Barroso, C G

    2015-02-15

    A new microwave-assisted extraction (MAE) method has been investigated for the extraction of phenolic compounds from rice grains. The experimental conditions studied included temperature (125-175°C), microwave power (500-1000W), time (5-15min), solvent (10-90% EtOAc in MeOH) and solvent-to-sample ratio (10:1 to 20:1). The extraction variables were optimised by the response surface methodology. Extraction temperature and solvent were found to have a highly significant effect on the response value (p<0.0005) and the extraction time also had a significant effect (p<0.05). The optimised MAE conditions were as follows: extraction temperature 185°C, microwave power 1000W, extraction time 20min, solvent 100% MeOH, and solvent-to-sample ratio 10:1. The developed method had a high precision (in terms of CV: 5.3% for repeatability and 5.5% for intermediate precision). Finally, the new method was applied to real samples in order to investigate the presence of phenolic compounds in a wide variety of rice grains.

  14. Microwave assisted extraction of biodiesel feedstock from the seeds of invasive chinese tallow tree.

    PubMed

    Boldor, Dorin; Kanitkar, Akanksha; Terigar, Beatrice G; Leonardi, Claudia; Lima, Marybeth; Breitenbeck, Gary A

    2010-05-15

    Chinese tallow tree (TT) seeds are a rich source of lipids and have the potential to be a biodiesel feedstock, but currently, its invasive nature does not favor large scale cultivation. Being a nonfood material, they have many advantages over conventional crops that are used for biodiesel production. The purpose of this study was to determine optimal oil extraction parameters in a batch-type and laboratory scale continuous-flow microwave system to obtain maximum oil recovery from whole TT seeds using ethanol as the extracting solvent. For the batch system, extractions were carried out for different time-temperature combinations ranging from 60 to 120 degrees C for up to 20 min. The batch system was modified for continuous extractions, which were carried out at 50, 60, and 73 degrees C and maintained for various residence times of up to 20 min. Control runs were performed under similar extraction conditions and the results compared well, especially when accounting for extremely short extraction times (minutes vs hours). Maximum yields of 35.32% and 32.51% (by weight of dry mass) were obtained for the continuous and batch process, respectively. The major advantage of microwave assisted solvent extraction is the reduced time of extraction required to obtain total recoverable lipids, with corresponding reduction in energy consumption costs per unit of lipid extracted. This study indicates that microwave extraction using ethanol as a solvent can be used as a viable alternative to conventional lipid extraction techniques for TT seeds.

  15. Microwave Assisted Synthesis of Ferrite Nanoparticles: Effect of Reaction Temperature on Particle Size and Magnetic Properties.

    PubMed

    Kalyani, S; Sangeetha, J; Philip, John

    2015-08-01

    The preparation of ferrite magnetic nanoparticles of different particle sizes by controlling the reaction temperature using microwave assisted synthesis is reported. The iron oxide nanoparticles synthesized at two different temperatures viz., 45 and 85 °C were characterized using techniques such as X-ray diffraction (XRD), small angle X-ray scattering (SAXS), vibrating sample magnetometry (VSM), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and Fourier transform infrared spectroscopy (FTIR). The average size of iron oxide nanoparticles synthesized at 45 and 85 °C is found to be 10 and 13.8 nm, respectively, and the nanoparticles exhibited superparamagantic behavior at room temperature. The saturation magnetization values of nanoparticles synthesized at 45 and 85 °C were found to be 67 and 72 emu/g, respectively. The increase in particle size and saturation magnetization values with increase in incubation temperature is attributed to a decrease in supersaturation at elevated temperature. The Curie temperature was found to be 561 and 566 0C for the iron oxide nanoparticles synthesized at 45 and 85 °C, respectively. The FTIR spectrum of the iron oxide nanoparticles synthesized at different temperatures exhibited the characteristic peaks that corresponded to the stretching of bonds between octahedral and tetrahedral metal ions to oxide ions. Our results showed that the ferrite nanoparticle size can be varied by controlling the reaction temperature inside a microwave reactor.

  16. Efficient Catalytic Activity BiFeO3 Nanoparticles Prepared by Novel Microwave-Assisted Synthesis.

    PubMed

    Zou, Jing; Gong, Wanyun; Ma, Jinai; Li, Lu; Jiang, Jizhou

    2015-02-01

    A novel microwave-assisted sol-gel method was applied to the synthesis of the single-phase perovskite bismuth ferrite nanoparticles (BFO NPs) with the mean diameter ca. 73.7 nm. The morphology was characterized by scanning electron microscope (SEM). The X-ray diffraction (XRD) revealed the rhombohedral phase with R3c space group. The weak ferromagnetic behavior at room temperature was affirmed by the vibrating sample magnetometer (VSM). According to the UV-vis diffuse reflectance spectrum (UV-DSR), the band gap energy of BFO NPs was determined to be 2.18 eV. The electrochemical activity was evaluated by BFO NPs-chitosan-glassy carbon electrode (BFO-CS-GCE) sensor for detection of p-nitrophenol contaminants. The material showed an efficient oxidation catalytic activity by degrading methylene blue (MB). It was found that the degradation efficiency of 10 mg L-1 MB at pH 6.0 was above 90.9% after ultrasound- and microwave-combined-assisted (US-MW) irradiation for 15 min with BFO NPs as catalyst and H202 as oxidant. A possible reaction mechanism of degradation of MB was also proposed.

  17. Microwave-assisted synthesis and antifungal activity of novel fused Osthole derivatives.

    PubMed

    Zhang, Ming-Zhi; Zhang, Rong-Rong; Wang, Jia-Qun; Yu, Xiang; Zhang, Ya-Ling; Wang, Qing-Qing; Zhang, Wei-Hua

    2016-11-29

    Based on the microwave-assisted synthetic protocol developed in our previous work, we have synthesized a series of novel furo[3,2-c]coumarins as fused Osthole derivatives, via the reaction of 4-hydroxycoumarins and β-ketoesters catalyzed by DMAP. All the target compounds were evaluated in vitro for their antifungal activity against six phytopathogenic fungi, some compounds exhibited potential activity in the primary assays. Especially compounds 6c, 7b, 8b and 8c (shown in Fig. 1) were the most active ones, EC50 values of these four compounds against Colletotrichum capsica, Botrytis cinerea and Rhizoctonia solani were further investigated. 6c was identified as the most promising candidate with the EC50 value at 0.110 μM against Botrytis cinerea and 0.040 μM against Colletotrichum capsica, respectively, representing better antifungal activity than that of the commonly used fungicide Azoxystrobin. Copyright © 2016 Elsevier Masson SAS. All rights reserved.

  18. Microwave-assisted carboxymethylation of cellulose extracted from brewer's spent grain.

    PubMed

    dos Santos, Danilo Martins; Bukzem, Andrea de Lacerda; Ascheri, Diego Palmiro Ramirez; Signini, Roberta; de Aquino, Gilberto Lucio Benedito

    2015-10-20

    Cellulose was extracted from brewer's spent grain (BSG) by alkaline and bleaching treatments. The extracted cellulose was used in the preparation of carboxymethyl cellulose (CMC) by reaction with monochloroacetic acid in alkaline medium with the use of a microwave reactor. A full-factorial 2(3) central composite design was applied in order to evaluate how parameters of carboxymethylation process such as reaction time, amount of monochloroacetic acid and reaction temperature affect the average degree of substitution (DS) of the cellulose derivative. An optimization strategy based on response surface methodology has been used for this process. The optimized conditions to yield CMC with the highest DS of 1.46 follow: 5g of monochloroacetic acid per gram of cellulose, reaction time of 7.5min and temperature of 70°C. This work demonstrated the feasibility of a fast and efficient microwave-assisted method to synthesize carboxymethyl cellulose from cellulose isolated of brewer's spent grain. Copyright © 2015 Elsevier Ltd. All rights reserved.

  19. Application of ionic liquid-based microwave-assisted extraction of flavonoids from Scutellaria baicalensis Georgi.

    PubMed

    Zhang, Qin; Zhao, San-Hu; Chen, Jue; Zhang, Li-Wei

    2015-10-01

    In the present work, a rapid ionic liquid-based microwave-assisted extraction (ILMAE) method was successfully applied to simultaneous extraction of baicalin, wogonoside, baicalein and wogonin from Scutellaria baicalensis Georgi. A series of 1-alkyl-3-methylirnidazolium ionic liquids with different anions and cations were assessed for extraction efficiency, and 1-octyl-3-methylimidazolium bromide was selected as the optimal solvent. In addition, the parameters of ILMAE procedure for the four flavonoids were optimized, and the optimal ILMAE method was validated in the linearity, stability, precision and recovery. Meanwhile, the microstructures of S. baicalensis powders were observed before and after extraction with the help of a scanning electron microscope (SEM) in order to explore the extraction mechanism, and the activity of the crude enzyme solution from S. baicalensis was determined through the hydrolysis of baicalin. Finally, the extraction yields and extraction time of WaterHRE, WaterMAE, ILHRE and Chp were 5.18% (30min), 8.77% (90s), 16.94% (30min) and 18.58% (3h), respectively. The results indicated that compared with the conventional extraction approaches, ILMAE possessed great advantages in extracting flavonoids, such as the highest extraction yield (22.28%), the shortest extraction time (90s), etc. Copyright © 2015 Elsevier B.V. All rights reserved.

  20. Microwave-assisted chemical process for treatment of hazardous waste: Annual report

    SciTech Connect

    Varma, R.; Nandi, S.P.; Cleaveland, D.C.

    1987-10-01

    Microwave energy provides rapid in situ uniform heating and can be used to initiate chemical processes at moderate temperatures. We investigate the technical feasibility of microwave-assisted chemical processes for detoxification of liquid hazardous waste. Trichloroethylene, a major constituent of waste streams, was selected for this detoxification study. Experiments were performed to investigate the oxidative degradation of trichloroethylene over active carbons (with and without catalysts) in air streams with microwave in situ heating, and to examine the feasibility of regenerating the used carbons. This study established that trichloroethylene in a vapor stream can be adsorbed at room temperature on active carbon beds that are loaded with Cu and Cr catalysts. When the bed is heated by a microwave radiation to moderate temperatures (<400/sup 0/C) while a moist air stream is passed through it, the trichloroethylene is readily converted into less-noxious products such as HCl, CO, CO/sub 2/ and C/sub 2/H/sub 2/Cl/sub 2/. Conversion higher than 80% was observed. Furthermore, the used carbon bed can be conveniently regenerated by microwave heating while a moist-N/sub 2/ or moist-air stream is passed through the bed. 4 refs., 5 figs., 10 tabs.

  1. Enhancement of biomass conversion in catalytic fast pyrolysis by microwave-assisted formic acid pretreatment.

    PubMed

    Feng, Yu; Li, Guangyu; Li, Xiangyu; Zhu, Ning; Xiao, Bo; Li, Jian; Wang, Yujue

    2016-08-01

    This study investigated microwave-assisted formic acid (MW-FA) pretreatment as a possible way to improve aromatic production from catalytic fast pyrolysis (CFP) of lignocellulosic biomass. Results showed that short duration of MW-FA pretreatment (5-10min) could effectively disrupt the recalcitrant structure of beech wood and selectively remove its hemicellulose and lignin components. This increased the accessibility of cellulose component of biomass to subsequent thermal conversion in CFP. Consequently, the MW-FA pretreated beech wood produced 14.0-28.3% higher yields (26.4-29.8C%) for valuable aromatic products in CFP than the untreated control (23.2C%). In addition, the yields of undesired solid residue (char/coke) decreased from 33.1C% for the untreated control to 28.6-29.8C% for the MW-FA pretreated samples. These results demonstrate that MW-FA pretreatment can provide an effective way to improve the product distribution from CFP of lignocellulose.

  2. Novel microwave assisted synthesis of highly doped phase pure Nd:YAG nanopowder

    NASA Astrophysics Data System (ADS)

    Kiranmala, L.; Rekha, M.; Neelam, M.

    2011-09-01

    For the first time, the studies on 2 to 10 at.% neodymium (Nd3+) ion doped Yttrium Aluminum Garnet (Nd:YAG) nanopowders obtained by microwave assisted citrate nitrate gel combustion synthesis is described in this work. This paper reports on high doping of Nd3+ ions with retaining the cubic garnet structure of YAG as evidenced from XRD, except the case of 8 at.% doped Nd:YAG. Phase pure YAG formation with 8 at.% Nd3+ doping was explored by using urea and alanine as alternative to citric acid complexing agents. Complete crystallization of YAG as a result of 2 hour thermal treatment at 900 °C under oxygen supply was studied by using Fourier Transform Infra-Red Spectroscopy (FTIR) and X-Ray Diffraction (XRD) techniques. With an increase in the dopant concentration a red shift in the FTIR peaks was observed. Using the XRD data, the cell parameter of Nd3+ (2 to 6 and 10 at.%) YAG was found to increase with an increase in the dopant concentration. The average primary particle size calculated using Scherrer's equation was ˜25 nm which was additionally supported by Transmission Electron Microscopy (TEM) results yielding particle sizes in the range of ˜25 to 30 nm for all the cases.

  3. Microwave-assisted extraction and pharmacological evaluation of polysaccharides from Posidonia oceanica.

    PubMed

    Ben Salem, Yosra; Abdelhamid, Amal; Mkadmini Hammi, Khaoula; Le Cerf, Didier; Bouraoui, Abderrahman; Majdoub, Hatem

    2017-08-09

    Microwave-assisted extraction was employed for the isolation of polysaccharides from Posidonia oceanica (PPO). The extracting parameters were optimized adopting response surface methodology. The highest polysaccharide yield (2.55 ± 0.09%), which is in concordance with the predicted value (2.76%), was obtained under the following conditions: extraction time 60 s, liquid-solid ratio of 50:1 (mL/g) and power of 800 W. This polysaccharide, with molecular weight of 524 KDa, characterized by gas chromatography-mass spectrometry showed that PPO was mainly composed of galactose, glucose, and arabinose with molar percentages 25.38, 24.37, and 21.64%, respectively. The pharmacological evaluation of PPO using animal models at the dose of 100 mg/kg indicated a significant anti-inflammatory activity with a percentage of inhibition of edema of 54.65% and a significant antinociceptive activity with 78.91% inhibition of writhing for peripheral analgesic activity and an increase in the hot plate reaction time for central analgesic activity.

  4. Pectin from Opuntia ficus indica: Optimization of microwave-assisted extraction and preliminary characterization.

    PubMed

    Lefsih, Khalef; Giacomazza, Daniela; Dahmoune, Farid; Mangione, Maria Rosalia; Bulone, Donatella; San Biagio, Pier Luigi; Passantino, Rosa; Costa, Maria Assunta; Guarrasi, Valeria; Madani, Khodir

    2017-04-15

    Optimization of microwave-assisted extraction (MAE) of water-soluble pectin (WSP) from Opuntia ficus indica cladodes was performed using Response Surface Methodology. The effect of extraction time (X1), microwave power (X2), pH (X3) and solid-to-liquid ratio (X4) on the extraction yield was examined. The optimum conditions of MAE were as follows: X1=2.15min; X2=517W; X3=2.26 and X4=2g/30.6mL. The maximum obtained yield of pectin extraction was 12.57%. Total carbohydrate content of WSP is about 95.5% including 34.4% of Galacturonic acid. Pectin-related proteins represent only the 0.66% of WSP mass. HPSEC and light scattering analyses reveal that WSP is mostly constituted of high molecular pectin and FTIR measurements show that the microwave treatment does not alter the chemical structure of WSP, in which Galacturonic acid content and yield are 34.4% and 4.33%, respectively. Overall, application of MAE can give rise to high quality pectin. Copyright © 2016 Elsevier Ltd. All rights reserved.

  5. Microwave-assisted extraction: Application to the determination of emerging pollutants in solid samples.

    PubMed

    Sanchez-Prado, Lucia; Garcia-Jares, Carmen; Llompart, Maria

    2010-04-16

    Flame retardants, surfactants, pharmaceutical and personal care products, among other compounds, have been the object of numerous environmental studies. In this chapter, the application of microwave-assisted extraction (MAE) in the development of analytical methods for several groups of organic compounds with growing concern as emerging pollutants has been considered. Compared to other extraction techniques, optimization of MAE experimental conditions is rather easy owing to the low number of influential parameters (i.e. matrix moisture, nature of the solvent, time, power, and temperature in closed vessels). The great reduction in the extraction time and solvent consumption, as well as the possibility of performing multiple extractions, increasing the sample throughput, can also be highlighted among MAE advantages. In summary, the study of several applications of MAE to environmental problems demonstrates that this technique constitutes a good alternative for the determination of organic compounds in environmental samples. It can be used as a rapid screening tool, and also to obtain detailed information on the sources, behaviour and fate of emerging pollutants in environmental matrices. Copyright 2009 Elsevier B.V. All rights reserved.

  6. Microwave-Assisted Radiosynthesis of [18F]Fluorinated Fatty Acid Analogs

    PubMed Central

    Belanger, Anthony P.; Pandey, Mukesh K.; DeGrado, Timothy R.

    2010-01-01

    Microwave reactors remain largely underutilized in the field of PET chemistry. This is particularly unfortunate since microwave synthesis elegantly addresses two of the most critical issues of PET radiochemistry with short-lived radionuclides: reaction rate and side-product formation. In this study we investigate the efficiency of synthesis of terminally [18F]fluorinated fatty acid analogs using a commercial microwave reactor in comparison with conventional heating. Methods The labeling precursors were methyl esters of terminally substituted alkyl bromides and iodides. Duration and temperatures of the [18F]fluorination reaction were varied. Chemical and radiochemical purities, and radiochemical yields were investigated for conventional (CH) and microwave-assisted (MW) radiosyntheses. Results The results demonstrate that microwave heating enhanced [18F]fluoride incorporation to >95% (up to 55% improvement), while reducing reaction times to 2 min (~10-fold reduction) or temperatures to 55–60°C (20°C reduction). Overall decay-corrected radiochemical yields of purified [18F]fluoro fatty acids were higher (MW=49.0 ± 4.5%, CH=23.6 ± 3.5%, p<0.05) with microwave heating and side-products were notably fewer. Conclusion For routine synthesis of [18F]fluoro fatty acid analogs, microwave heating is faster, milder, cleaner, less variable and higher yielding than conventional heating and therefore the preferred reaction method. PMID:21492792

  7. Microwave-assisted acid and base hydrolysis of intact proteins containing disulfide bonds for protein sequence analysis by mass spectrometry.

    PubMed

    Reiz, Bela; Li, Liang

    2010-09-01

    Controlled hydrolysis of proteins to generate peptide ladders combined with mass spectrometric analysis of the resultant peptides can be used for protein sequencing. In this paper, two methods of improving the microwave-assisted protein hydrolysis process are described to enable rapid sequencing of proteins containing disulfide bonds and increase sequence coverage, respectively. It was demonstrated that proteins containing disulfide bonds could be sequenced by MS analysis by first performing hydrolysis for less than 2 min, followed by 1 h of reduction to release the peptides originally linked by disulfide bonds. It was shown that a strong base could be used as a catalyst for microwave-assisted protein hydrolysis, producing complementary sequence information to that generated by microwave-assisted acid hydrolysis. However, using either acid or base hydrolysis, amide bond breakages in small regions of the polypeptide chains of the model proteins (e.g., cytochrome c and lysozyme) were not detected. Dynamic light scattering measurement of the proteins solubilized in an acid or base indicated that protein-protein interaction or aggregation was not the cause of the failure to hydrolyze certain amide bonds. It was speculated that there were some unknown local structures that might play a role in preventing an acid or base from reacting with the peptide bonds therein.

  8. Analysis of parameter and interaction between parameter of the microwave assisted transesterification process of coconut oil using response surface methodology

    NASA Astrophysics Data System (ADS)

    Hidayanti, Nur; Suryanto, A.; Qadariyah, L.; Prihatini, P.; Mahfud, Mahfud

    2015-12-01

    A simple batch process was designed for the transesterification of coconut oil to alkyl esters using microwave assisted method. The product with yield above 93.225% of alkyl ester is called the biodiesel fuel. Response surface methodology was used to design the experiment and obtain the maximum possible yield of biodiesel in the microwave-assisted reaction from coconut oil with KOH as the catalyst. The results showed that the time reaction and concentration of KOH catalyst have significant effects on yield of alkyl ester. Based on the response surface methodology using the selected operating conditions, the time of reaction and concentration of KOH catalyst in transesterification process were 150 second and 0.25%w/w, respectively. The largest predicted and experimental yield of alkyl esters (biodiesel) under the optimal conditions are 101.385% and 93.225%, respectively. Our findings confirmed the successful development of process for the transesterification reaction of coconut oil by microwave-assisted heating, which is effective and time-saving for alkyl ester production.

  9. Antioxidative Peptides Derived from Enzyme Hydrolysis of Bone Collagen after Microwave Assisted Acid Pre-Treatment and Nitrogen Protection

    PubMed Central

    Lin, Yun-Jian; Le, Guo-Wei; Wang, Jie-Yun; Li, Ya-Xin; Shi, Yong-Hui; Sun, Jin

    2010-01-01

    This study focused on the preparation method of antioxidant peptides by enzymatic hydrolysis of bone collagen after microwave assisted acid pre-treatment and nitrogen protection. Phosphoric acid showed the highest ability of hydrolysis among the four other acids tested (hydrochloric acid, sulfuric acid and/or citric acid). The highest degree of hydrolysis (DH) was 9.5% using 4 mol/L phosphoric acid with a ratio of 1:6 under a microwave intensity of 510 W for 240 s. Neutral proteinase gave higher DH among the four protease tested (Acid protease, neutral protease, Alcalase and papain), with an optimum condition of: (1) ratio of enzyme and substrate, 4760 U/g; (2) concentration of substrate, 4%; (3) reaction temperature, 55 °C and (4) pH 7.0. At 4 h, DH increased significantly (P < 0.01) under nitrogen protection compared with normal microwave assisted acid pre-treatment hydrolysis conditions. The antioxidant ability of the hydrolysate increased and reached its maximum value at 3 h; however DH decreased dramatically after 3 h. Microwave assisted acid pre-treatment and nitrogen protection could be a quick preparatory method for hydrolyzing bone collagen. PMID:21151439

  10. Antioxidative peptides derived from enzyme hydrolysis of bone collagen after microwave assisted acid pre-treatment and nitrogen protection.

    PubMed

    Lin, Yun-Jian; Le, Guo-Wei; Wang, Jie-Yun; Li, Ya-Xin; Shi, Yong-Hui; Sun, Jin

    2010-11-01

    This study focused on the preparation method of antioxidant peptides by enzymatic hydrolysis of bone collagen after microwave assisted acid pre-treatment and nitrogen protection. Phosphoric acid showed the highest ability of hydrolysis among the four other acids tested (hydrochloric acid, sulfuric acid and/or citric acid). The highest degree of hydrolysis (DH) was 9.5% using 4 mol/L phosphoric acid with a ratio of 1:6 under a microwave intensity of 510 W for 240 s. Neutral proteinase gave higher DH among the four protease tested (Acid protease, neutral protease, Alcalase and papain), with an optimum condition of: (1) ratio of enzyme and substrate, 4760 U/g; (2) concentration of substrate, 4%; (3) reaction temperature, 55 °C and (4) pH 7.0. At 4 h, DH increased significantly (P < 0.01) under nitrogen protection compared with normal microwave assisted acid pre-treatment hydrolysis conditions. The antioxidant ability of the hydrolysate increased and reached its maximum value at 3 h; however DH decreased dramatically after 3 h. Microwave assisted acid pre-treatment and nitrogen protection could be a quick preparatory method for hydrolyzing bone collagen.

  11. Analysis of glycyrrhizic acid and liquiritin in liquorice root with microwave-assisted micellar extraction and pre-concentration.

    PubMed

    Sun, Chen; Xie, Yuchun; Tian, Qinglai; Liu, Huizhou

    2008-01-01

    The feasibility of employing a non-ionic surfactant (Triton X-100) as an alternative and effective solvent for the microwave-assisted extraction of glycyrrhizic acid and liquiritin from liquorice root has been demonstrated. When compared with commonly used solvents, 5% Triton X-100 yielded higher extraction efficiency than aqueous solutions of ethanol or methanol. Under optimal conditions, i.e. 5% Triton X-100 (v/v) and microwave-assisted extraction for 3-5 min at 100 degrees C, the percentage extraction of active ingredients reached the highest value. The pre-concentration factor for the glycyrrhizic acid and liquiritin was about 13, and the cloud-point extraction recoveries for the two ingredients were 98.4 and 96.1%, respectively. The results showed that the coupling of microwave-assisted extraction and cloud-point extraction could be employed as a new and effective approach for the rapid extraction and pre-concentration of pharmacologically active ingredients from liquorice root without disturbing the subsequent chromatographic analysis. Copyright 2007 John Wiley & Sons, Ltd.

  12. Compare study CaCO3 crystals on the cellulose substrate by microwave-assisted method and ultrasound agitation method.

    PubMed

    Fu, Lian-Hua; Dong, Yan-Yan; Ma, Ming-Guo; Li, Shu-Ming; Sun, Run-Cang

    2013-05-01

    The purposes of this article were to investigate the influences of synthesis strategy on the CaCO(3) crystals on the cellulose substrate. In this study, CaCO(3) crystals were synthesized using cellulose as matrix by the microwave-assisted method and ultrasound agitation method, respectively. The CaCO(3) crystals on the cellulose substrate were characterized by means of X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). Experimental results demonstrated that the synthesis strategy had a dramatically influences on the phase, microstructure, morphology, thermal stability, and biological activity of the CaCO(3) crystals. The pure phase of vaterite spheres with the diameter of about 320-600nm were obtained by ultrasound agitation method, meanwhile, the mixed phases of calcite and vaterite with the diameter of about 0.82-1.24μm were observed by microwave-assisted method. In view of experimental results, one can conclude that the ultrasound agitation method do more favors to the synthesis of CaCO(3) crystals with uniform morphology and size, compared with microwave-assisted method. Furthermore, cytotoxicity experiments indicated that the CaCO(3) crystals on the cellulose substrate had good biocompatibility and could be a candidate for the biomedical applications. Copyright © 2012 Elsevier B.V. All rights reserved.

  13. Microwave-assisted synthesis of highly water-soluble graphene towards electrical DNA sensor

    NASA Astrophysics Data System (ADS)

    Choi, Bong Gill; Park, Hoseok; Yang, Min Ho; Jung, Young Mee; Lee, Sang Yup; Hong, Won Hi; Park, Tae Jung

    2010-12-01

    Graphene sheets have the potential for practical applications in electrochemical devices, but their development has been impeded by critical problems with aggregation of graphene sheets. Here, we demonstrated a facile and bottom-up approach for fabrication of DNA sensor device using water-soluble sulfonated reduced graphene oxide (SRGO) sheets via microwave-assisted sulfonation (MAS), showing enhanced sensitivity, reliability, and low detection limit. Key to achieving these performances is the fabrication of the SRGOs, where the MAS method enabled SRGOs to be highly dispersed in water (10 mg mL-1) due to the acidic sulfonated groups generated within 3 min of the functionalization reaction. The water-soluble SRGO-DNA (SRGOD) hybrids prepared by electrostatic interactions between a flat single layer of graphene sheets and DNAs are suitable for fabrication of electrical DNA sensor devices because of the unique electrical characteristics of SRGODs. The high sensing performance of SRGOD sensors was demonstrated with detection ofDNA hybridization using complementary DNAs, single base mismatched DNAs, and noncomplementary DNAs, with results showing higher sensitivity and lower detection limit than those of reduced graphene oxide-based DNA sensors. Simple and easy fabrication of DNA sensor devices using SRGODs is expected to provide an effective way for electrical detection ofDNA hybridization using miniature sensors without the labor-intensive labeling of the sensor and complex measurement equipment.Graphene sheets have the potential for practical applications in electrochemical devices, but their development has been impeded by critical problems with aggregation of graphene sheets. Here, we demonstrated a facile and bottom-up approach for fabrication of DNA sensor device using water-soluble sulfonated reduced graphene oxide (SRGO) sheets via microwave-assisted sulfonation (MAS), showing enhanced sensitivity, reliability, and low detection limit. Key to achieving these

  14. 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

  15. Microwave-assisted headspace solid-phase microextraction to quantify polycyclic aromatic hydrocarbons in pine trees.

    PubMed

    Ratola, Nuno; Herbert, Paulo; Alves, Arminda

    2012-06-01

    A methodology for the extraction and quantification of 16 polycyclic aromatic hydrocarbons (PAHs) based on microwave-assisted extraction coupled with headspace solid-phase microextraction followed by gas chromatography/mass spectroscopy was validated for needles and bark of two pine species (Pinus pinaster Ait. and Pinus pinea L.). The limits of detection were below 0.92 ng g(-1) (dry weight) for needles and below 0.43 ng g(-1) (dw) for bark. Recovery assays were performed with two sample masses spiked at three levels and the overall mean values were between 70 and 110 % for P. pinaster and 75 and 129 % for P. pinea. In the first species, the increase in sample mass lowered the recoveries slightly for most PAHs, whereas for the second, the recoveries were higher for the needles. Naturally contaminated samples from 4 sites were analysed, with higher levels for urban sites (1,320 and 942 ng g(-1) (dw) vs. 272 and 111 ng g(-1) (dw) for needles and 696 and 488 ng g(-1) (dw) vs. 270 and 103 ng g(-1) (dw) for bark) than for rural ones and also for P. pinaster samples over P. pinea. It is also shown that gas-phase PAHs are predominant in the needles (over 65 % of the total PAHs) and that the incidence for particulate material in bark, reaching 40 % as opposed to a maximum below 20 % for the needles. The method has proved to be fit and improved some of the existing approaches, on the assessment of particulate PAHs and bark levels.

  16. Microwave assisted transformation of N,N-diphenylamine as precursors of organic light emitting diodes (OLED)

    SciTech Connect

    Jefri,; Wahyuningrum, Deana

    2015-09-30

    In this research, study on the transformation of N,N-diphenylamine (DPA) using iodine (I2) utilizing solid state Microwave Assisted Organic Synthesis (MAOS) method has been carried out. The reaction was performed by variations of three parameters namely the mole of reagents, the amount and type of solid support (alumina/Al2O3), and the reaction conditions. Experimental results showed that neutral-alumina was a better solid support than basic-alumina. The optimum temperature for the reaction was approximately at 125-133 °C with reaction time of 15 minutes and microwave reactor power at 500-600 W. The separation of the yellowish green product solution with preparative Thin Layer Chromatography (TLC) method using n-hexane:ethyl acetate = 4:1 (v/v) as eluent yielded two fractions (I and II) and both fractions can undergo fluorescence under 365 nm UV light. Based on the LC chromatogram with methanol:water = 95:5 (v/v) as eluent and its corresponding mass spectra (ESI+), fraction I contained three compounds, which were tetracarbazole A, triphenylamine, and impurities in the form of plasticizer such as bis(2-ethylhexyl) phthalate. Fraction II also contained three compounds, which were tetracarbazole C, tetraphenylhydrazine, and plasticizer such as bis(2-ethylhexyl) phthalate. Both FT-IR (KBr disks) and NMR (500 MHz, CDCl{sub 3}) spectra of fraction I and II confirmed the aromatic amine groups in those compounds. The observed fluorescence colors of fraction I and II were violet and violet-blue, respectively. Based on their structures and fluorescence characters, the compounds in fraction I and II have the potential to be used as Organic Light Emitting Diode (OLED) compound precursors.

  17. Shape effect on the antibacterial activity of silver nanoparticles synthesized via a microwave-assisted method.

    PubMed

    Hong, Xuesen; Wen, Junjie; Xiong, Xuhua; Hu, Yongyou

    2016-03-01

    Silver nanoparticles (AgNPs) are used as sustained-release bactericidal agents for water treatment. Among the physicochemical characteristics of AgNPs, shape is an important parameter relevant to the antibacterial activity. Three typically shaped AgNPs, nanocubes, nanospheres, and nanowires, were prepared via a microwave-assisted method and characterized by TEM, UV-vis, and XRD. The antibacterial activity of AgNPs was determined by OD growth curves tests, MIC tests, and cell viability assay against Escherichia coli. The interaction between AgNPs and bacterial cells was observed by TEM. The results showed that the three differently shaped AgNPs were nanoscale, 55 ± 10 nm in edge length for nanocubes, 60 ± 15 nm in diameter for nanospheres, 60 ± 10 nm in diameter and 2-4 μm in length for nanowires. At the bacterial concentration of 10(4) CFU/mL, the MIC of nanocubes, nanospheres, and nanowires were 37.5, 75, and 100 μg/mL, respectively. Due to the worst contact with bacteria, silver nanowires exhibited the weakest antibacterial activity compared with silver nanocubes and silver nanospheres. Besides, silver nanocubes mainly covered by {100} facets showed stronger antibacterial activity than silver nanospheres covered by {111} facets. It suggests that the shape effect on the antibacterial activity of AgNPs is attributed to the specific surface areas and facets reactivity; AgNPs with larger effective contact areas and higher reactive facets exhibit stronger antibacterial activity.

  18. Microwave-assisted double insert vapour-phase digestion of organic samples.

    PubMed

    Eilola, Keijo; Perämäki, Paavo

    2009-02-23

    A microwave-assisted double insert multimode vapour-phase digestion method was developed for the digestion of organic samples. The experimental set-up was based on a third generation-type teflon microwave vessel, equipped with an automatic pressure regulating type vessel cover. A borosilicate glass holder insert, containing a smaller quartz sample insert, was fitted inside the vessel. Sulphuric acid was added to the holder insert as a microwave absorbing and temperature transferring liquid, which transferred heat to the sample insert (into which the sample was weighed) and charred the sample material. Oxidation of the sample material was carried out simultaneously with charring using nitric acid vapour, which was generated by the 1:1 (v/v) sulphuric acid-nitric acid mixture located in the bottom of the microwave vessel. This set-up generated high digestion efficiency, without any of the interferences normally associated with direct sulphuric acid usage. The method was used for determining the concentrations of Cd, Cr, Cu, Mn, Mo, Zn and Fe in certified organic reference materials using ICP-OES instrumentation. The certified organic reference materials were NRCC DOLT-2 dogfish liver, NIST-SRM 1577b bovine liver and IRMM VDA cadmium in polyethylene No. 001 and No. 004. The results were in good agreement with the certified values, forepart from Cd. For Cd the results were lower than the certified values due to volatilization losses. Sample materials that could not be digested by an earlier procedure were completely digested during a single-step, 30 min digestion. The tested sample materials included certified reference materials, 3-nitrobenzoic acid (3-NBA) and pike (Esox lucius) muscle. The residual carbon concentrations in the digestion solutions were below the detection limit of the TOC instrument. This type of digestion method is described here for the first time in the literature.

  19. Microwave assisted transformation of N,N-diphenylamine as precursors of organic light emitting diodes (OLED)

    NASA Astrophysics Data System (ADS)

    Jefri, Wahyuningrum, Deana

    2015-09-01

    In this research, study on the transformation of N,N-diphenylamine (DPA) using iodine (I2) utilizing solid state Microwave Assisted Organic Synthesis (MAOS) method has been carried out. The reaction was performed by variations of three parameters namely the mole of reagents, the amount and type of solid support (alumina/Al2O3), and the reaction conditions. Experimental results showed that neutral-alumina was a better solid support than basic-alumina. The optimum temperature for the reaction was approximately at 125-133 °C with reaction time of 15 minutes and microwave reactor power at 500-600 W. The separation of the yellowish green product solution with preparative Thin Layer Chromatography (TLC) method using n-hexane:ethyl acetate = 4:1 (v/v) as eluent yielded two fractions (I and II) and both fractions can undergo fluorescence under 365 nm UV light. Based on the LC chromatogram with methanol:water = 95:5 (v/v) as eluent and its corresponding mass spectra (ESI+), fraction I contained three compounds, which were tetracarbazole A, triphenylamine, and impurities in the form of plasticizer such as bis(2-ethylhexyl) phthalate. Fraction II also contained three compounds, which were tetracarbazole C, tetraphenylhydrazine, and plasticizer such as bis(2-ethylhexyl) phthalate. Both FT-IR (KBr disks) and NMR (500 MHz, CDCl3) spectra of fraction I and II confirmed the aromatic amine groups in those compounds. The observed fluorescence colors of fraction I and II were violet and violet-blue, respectively. Based on their structures and fluorescence characters, the compounds in fraction I and II have the potential to be used as Organic Light Emitting Diode (OLED) compound precursors.

  20. Rapid synthesis of tin oxide nanostructures by microwave-assisted thermal oxidation for sensor applications

    NASA Astrophysics Data System (ADS)

    Phadungdhitidhada, S.; Ruankham, P.; Gardchareon, A.; Wongratanaphisan, D.; Choopun, S.

    2017-09-01

    In the present work nanostructures of tin oxides were synthesized by a microwave-assisted thermal oxidation. Tin precursor powder was loaded into a cylindrical quartz tube and further radiated in a microwave oven. The as-synthesized products were characterized by scanning electron microscope, transmission electron microscope, and x-ray diffractometer. The results showed that two different morphologies of SnO2 microwires (MWs) and nanoparticles (NPs) were obtained in one minute of microwave radiation under atmospheric ambient. A few tens of the SnO2 MWs with the length of 10-50 µm were found. Some parts of the MWs were decorated with the SnO2 NPs. However, most of the products were SnO2 NPs with the diameter ranging from 30-200 nm. Preparation under loosely closed system lead to mixed phase SnO-SnO2 NPs with diameter of 30-200 nm. The single-phase of SnO2 could be obtained by mixing the Sn precursor powders with CuO2. The products were mostly found to be SnO2 nanowires (NWs) and MWs. The diameter of SnO2 NWs was less than 50 nm. The SnO2 NPs, MWs, and NWs were in the cassiterite rutile structure phase. The SnO NPs was in the tetragonal structure phase. The growth direction of the SnO2 NWs was observed in (1 1 0) and (2 2 1) direction. The ethanol sensor performance of these tin oxide nanostructures showed that the SnO-SnO2 NPs exhibited extremely high sensitivity. Invited talk at 5th Thailand International Nanotechnology Conference (Nano Thailand-2016), 27-29 November 2016, Nakhon Ratchasima, Thailand.

  1. Zinc-doped CdS nanoparticles synthesized by microwave-assisted deposition

    NASA Astrophysics Data System (ADS)

    Ibiyemi, Abideen A.; Awodugba, Ayodeji O.; Akinrinola, Olusola; Faremi, Abass A.

    2017-09-01

    Cd1‑x Zn x S nanoparticles were grown on pre-cleaned glass substrates using microwave-assisted chemical bath deposition technique. Nanoparticles obtained by this method were smooth, uniform, good adherent, brownish yellow in color where the brightness of the yellow color nature decreases with increasing Zn2+ content. The elemental composition analysis confirmed that the nanoparticles comprise of Cd2+, Zn2+ and S2‑. Scanning electron microscope images confirmed the surface uniformity of the Cd1‑x Zn x S nanoparticles devoid of any void, pinhole or cracks and covered the substrate well. The particle size also decreases with increasing Zn ion content. X-ray diffraction (XRD) indicates the hexagonal structure (002) without phase transition. The grain size decreases from 36.45 to 9.60 nm, dislocation density increases from 0.000745 to 0.01085 Line2/m2 and lattice parameter decreased from 6.868 to 6.155 nm with increasing Zn2+ content. The best transmittance of about 95% was achieved for x = 1.0. The nanoparticles showed reduction in the absorbance as Zn ion content increased. Four point probe revealed that the electrical resistivity increased from 1.51 × 1010 to 6.67× {10}10 {{Ω }}\\cdot {cm} while electrical conductivity decreases from 6.62 × 10‑11 to 1.49× {10}-11{({{Ω }}\\cdot {cm})}-1 with increasing Zn2+ content. The other electrical properties such as sheet resistance increased from 1.52 × 108 to 1.58× {10}8 {{Ω }}, charge carrier mobility decreased from 0.777 to 0.0105 cm2/(V \\cdot s) and charge carrier density increased from 1.06 × 1012 to 3.95 × 1012 cm‑3.

  2. Supercritical Carbon Dioxide and Microwave-Assisted Extraction of Functional Lipophilic Compounds from Arthrospira platensis

    PubMed Central

    Esquivel-Hernández, Diego A.; López, Víctor H.; Rodríguez-Rodríguez, José; Alemán-Nava, Gibrán S.; Cuéllar-Bermúdez, Sara P.; Rostro-Alanis, Magdalena; Parra-Saldívar, Roberto

    2016-01-01

    Arthrospira platensis biomass was used in order to obtain functional lipophilic compounds through green extraction technologies such as supercritical carbon dioxide fluid extraction (SFE) and microwave-assisted extraction (MAE). The temperature (T) factor was evaluated for MAE, while for SFE, pressure (P), temperature (T), and co-solvent (ethanol) (CS) were evaluated. The maximum extraction yield of the obtained oleoresin was (4.07% ± 0.14%) and (4.27% ± 0.10%) for SFE and MAE, respectively. Extracts were characterized by gas chromatography mass spectrometry (GC-MS) and gas chromatography flame ionization detector (GC-FID). The maximum contents of functional lipophilic compounds in the SFE and MAE extracts were: for carotenoids 283 ± 0.10 μg/g and 629 ± 0.13 μg/g, respectively; for tocopherols 5.01 ± 0.05 μg/g and 2.46 ± 0.09 μg/g, respectively; and for fatty acids 34.76 ± 0.08 mg/g and 15.88 ± 0.06 mg/g, respectively. In conclusion, the SFE process at P 450 bar, T 60 °C and CS 53.33% of CO2 produced the highest yield of tocopherols, carotenoids and fatty acids. The MAE process at 400 W and 50 °C gives the best extracts in terms of tocopherols and carotenoids. For yield and fatty acids, the MAE process at 400 W and 70 °C produced the highest values. Both SFE and MAE showed to be suitable green extraction technologies for obtaining functional lipophilic compounds from Arthrospira platensis. PMID:27164081

  3. Thrust Stand Measurements of the Microwave Assisted Discharge Inductive Plasma Accelerator

    NASA Technical Reports Server (NTRS)

    Hallock, Ashley K.; Polzin, Kurt A.; Emsellem, Gregory D.

    2011-01-01

    Pulsed inductive plasma thrusters [1-3] are spacecraft propulsion devices in which electrical energy is capacitively stored and then discharged through an inductive coil. This type of pulsed thruster is electrodeless, with a time-varying current in the coil interacting with a plasma covering the face of the coil to induce a plasma current. Propellant is accelerated and expelled at a high exhaust velocity (O(10-100 km/s)) by the Lorentz body force arising from the interaction of the magnetic field and the induced plasma current. While this class of thruster mitigates the life-limiting issues associated with electrode erosion, pulsed inductive plasma thrusters require high pulse energies to inductively ionize propellant. The Microwave Assisted Dis- charge Inductive Plasma Accelerator (MAD-IPA), shown in Fig. 1, is a pulsed inductive plasma thruster that addressees this issue by partially ionizing propellant inside a conical inductive coil before the main current pulse via an electron cyclotron resonance (ECR) discharge. The ECR plasma is produced using microwaves and a static magnetic field from a set of permanent magnets arranged to create a thin resonance region along the inner surface of the coil, restricting plasma formation, and in turn current sheet formation, to a region where the magnetic coupling between the plasma and the theta-pinch coil is high. The use of a conical theta-pinch coil also serves to provide neutral propellant containment and plasma plume focusing that is improved relative to the more common planar geometry of the Pulsed Inductive Thruster (PIT) [1, 2]. In this paper, we describe thrust stand measurements performed to characterize the performance (specific impulse, thrust efficiency) of the MAD-IPA thruster. Impulse data are obtained at various pulse energies, mass flow rates and inductive coil geometries. Dependencies on these experimental parameters are discussed in the context of the current sheet formation and electromagnetic plasma

  4. Optimization of microwave-assisted extraction of polyphenols from Myrtus communis L. leaves.

    PubMed

    Dahmoune, Farid; Nayak, Balunkeswar; Moussi, Kamal; Remini, Hocine; Madani, Khodir

    2015-01-01

    Phytochemicals, such as phenolic compounds, are of great interest due to their health-benefitting antioxidant properties and possible protection against inflammation, cardiovascular diseases and certain types of cancer. Maximum retention of these phytochemicals during extraction requires optimised process parameter conditions. A microwave-assisted extraction (MAE) method was investigated for extraction of total phenolics from Myrtus communis leaves. The total phenolic capacity (TPC) of leaf extracts at optimised MAE conditions was compared with ultrasound-assisted extraction (UAE) and conventional solvent extraction (CSE). The influence of extraction parameters including ethanol concentration, microwave power, irradiation time and solvent-to-solid ratio on the extraction of TPC was modeled by using a second-order regression equation. The optimal MAE conditions were 42% ethanol concentration, 500 W microwave power, 62 s irradiation time and 32 mL/g solvent to material ratio. Ethanol concentration and liquid-to-solid ratio were the significant parameters for the extraction process (p<0.01). Under the MAE optimised conditions, the recovery of TPC was 162.49 ± 16.95 mg gallic acidequivalent/gdry weight(DW), approximating the predicted content (166.13 mg GAE/g DW). When bioactive phytochemicals extracted from Myrtus leaves using MAE compared with UAE and CSE, it was also observed that tannins (32.65 ± 0.01 mg/g), total flavonoids (5.02 ± 0.05 mg QE/g) and antioxidant activities (38.20 ± 1.08 μg GAE/mL) in MAE extracts were higher than the other two extracts. These findings further illustrate that extraction of bioactive phytochemicals from plant materials using MAE method consumes less extraction solvent and saves time.

  5. Bit patterned media with composite structure for microwave assisted magnetic recording

    NASA Astrophysics Data System (ADS)

    Eibagi, Nasim

    Patterned magnetic nano-structures are under extensive research due to their interesting emergent physics and promising applications in high-density magnetic data storage, through magnetic logic to bio-magnetic functionality. Bit-patterned media is an example of such structures which is a leading candidate to reach magnetic densities which cannot be achieved by conventional magnetic media. Patterned arrays of complex heterostructures such as exchange-coupled composites are studied in this thesis as a potential for next generation of magnetic recording media. Exchange-coupled composites have shown new functionality and performance advantages in magnetic recording and bit patterned media provide unique capability to implement such architectures. Due to unique resonant properties of such structures, their possible application in spin transfer torque memory and microwave assisted switching is also studied. This dissertation is divided into seven chapters. The first chapter covers the history of magnetic recording, the need to increase magnetic storage density, and the challenges in the field. The second chapter introduces basic concepts of magnetism. The third chapter explains the fabrication methods for thin films and various lithographic techniques that were used to pattern the devices under study for this thesis. The fourth chapter introduces the exchanged coupled system with the structure of [Co/Pd] / Fe / [Co/Pd], where the thickness of Fe is varied, and presents the magnetic properties of such structures using conventional magnetometers. The fifth chapter goes beyond what is learned in the fourth chapter and utilizes polarized neutron reflectometry to study the vertical exchange coupling and reversal mechanism in patterned structures with such structure. The sixth chapter explores the dynamic properties of the patterned samples, and their reversal mechanism under microwave field. The final chapter summarizes the results and describes the prospects for future

  6. Evaluation of oxygen pressurized microwave-assisted digestion of botanical materials using diluted nitric acid.

    PubMed

    Bizzi, Cezar Augusto; Barin, Juliano Smanioto; Müller, Edson Irineu; Schmidt, Lucas; Nóbrega, Joaquim A; Flores, Erico Marlon Moraes

    2011-02-15

    The feasibility of diluted nitric acid solutions for microwave-assisted decomposition of botanical samples in closed vessels was evaluated. Oxygen pressurized atmosphere was used to improve the digestion efficiency and Al, Ca, K, Fe, Mg and Na were determined in digests by inductively coupled plasma optical emission spectrometry (ICP OES). Efficiency of digestion was evaluated taking into account the residual carbon content (RCC) and residual acidity in digests. Samples were digested using nitric acid solutions (2, 3, 7, and 14 mol L(-1) HNO(3)) and the effect of gas phase composition inside the reaction vessels by purging the vessel with Ar (inert atmosphere, 1 bar), air (20% of oxygen, 1 bar) and pure O(2) (100% of oxygen, 1 bar) was evaluated. The influence of oxygen pressure was studied using pressures of 5, 10, 15 and 20 bar. It was demonstrated that a diluted nitric acid solution as low as 3 mol L(-1) was suitable for an efficient digestion of sample masses up to 500 mg of botanical samples using 5 bar of oxygen pressure. The residual acidities in final digests were lower than 45% in relation to the initial amount of acid used for digestion (equivalent to 1.3 mol L(-1) HNO(3)). The accuracy of the proposed procedure was evaluated using certified reference materials of olive leaves, apple leaves, peach leaves and pine needles. Using the optimized conditions for sample digestion, the results obtained were in agreement with certified values. The limit of quantification was improved up to a factor of 14.5 times for the analytes evaluated. In addition, the proposed procedure was in agreement with the recommendations of the green chemistry once it was possible to obtain relatively high digestion efficiency (RCC<5%) using only diluted HNO(3), which is important to minimize the generation of laboratory residues.

  7. Cadmium and lead in grey wolf liver samples: optimisation of a microwave-assisted digestion method.

    PubMed

    Vihnanek Lazarus, Maja; Sekovanić, Ankica; Kljaković-Gašpić, Zorana; Orct, Tatjana; Jurasović, Jasna; Kusak, Josip; Reljić, Slaven; Huber, Duro

    2013-09-01

    A microwave-assisted digestion method for the determination of cadmium (Cd) and lead (Pb) by inductively coupled plasma mass spectrometry (ICP-MS) was optimised on certified reference material (CRM) (bovine liver, BCR-185R) and wolf liver samples. Different factors influencing digestion efficiency (temperature, time, composition of the digestion mixture, sample mass) were tested. Validation included linearity (up to 200 μg L(-1) for Cd and Pb), detection (0.003 μg L(-1) for Cd and 0.035 μg L(-1) for Pb), and quantification (0.008 μg L(-1) for Cd and 0.081 μg L(-1) for Pb) limits. Good agreement between measured and certified values was achieved in all conditions, with recoveries ranging from 94 % to 111 % for Cd and from 95 % to 105 % for Pb. The precision of the method, expressed as relative standard deviation, was up to 3 % for Cd and 8 % for Pb. The best digestion parameters (260 °C, 30 min, 1 mL HNO3+4 mL H2O, 0.1 g of CRM) based on accuracy and precision were applied on two wolf liver samples to evaluate the need for the predigestion step (freeze-drying) and appropriate mass of the sample. Freeze-drying improved precision and minimising the tissue mass to 0.1 g reduced the matrix effect. Using these optimised digestion conditions, we determined Cd and Pb in 40 wolf livers collected in Croatia, and their medians (0.055 μg g(-1) and 0.107 μg g(-1), respectively) were in the range of previously reported data for the grey wolf.

  8. DNA quantification via traceable phosphorus measurement through microwave-assisted UV digestion-ion chromatography.

    PubMed

    Dash, K; Rastogi, L; Arunachalam, J

    2012-02-07

    Accurate quantification of deoxyribonucleic acid (DNA) is critical for many analyses in molecular biology and genetic tests. We present a method in which the stoichiometrically existing phosphorus content in purified genomic DNA is quantitatively converted into orthophosphate ions by microwave assisted-UV digestion in the presence of microlitre quantities of dilute reagents (HCl, HNO(3), H(2)O(2)). The tandem use of microwave energy and ultraviolet photons for DNA digestion in pressurized quartz vessels enables a maximum reaction temperature of 240 °C resulting in efficient and fast mineralization of high molecular weight DNA within 30 minutes. Compared to hotplate digestion, the digestion time is reduced by a factor of 32. The MW-UV sample preparation approach coupled with the ion chromatographic measurement of phosphate using a high performance (HP) methodology provides an accurate quantitation of phosphorus mass fractions as low as 0.3 μg g(-1), corresponding to a DNA mass of 25 μg. The relative expanded uncertainties (% U) expressed at 95% confidence for these analyses range from 0.2 to 0.6%. Critically, the matrix of the calibrant solution is also matched with respect to the digested matrix anions (chloride, nitrate), without which significant bias in IC performance is observed. The phosphorus content of the calf thymus DNA was also measured using high-performance inductively coupled plasma optical emission spectroscopy (HP-ICP-OES), which provided independent data for comparison with the MW-UV digestion-IC based approach. Ion chromatography requires smaller volume of materials to perform the analysis and could be useful for characterizing primary calibration standards and certified reference materials with low uncertainties.

  9. Accelerated, microwave-assisted, and conventional solvent extraction methods affect anthocyanin composition from colored grains.

    PubMed

    Abdel-Aal, El-Sayed M; Akhtar, Humayoun; Rabalski, Iwona; Bryan, Michael

    2014-02-01

    Anthocyanins are important dietary components with diverse positive functions in human health. This study investigates effects of accelerated solvent extraction (ASE) and microwave-assisted extraction (MAE) on anthocyanin composition and extraction efficiency from blue wheat, purple corn, and black rice in comparison with the commonly used solvent extraction (CSE). Factorial experimental design was employed to study effects of ASE and MAE variables, and anthocyanin extracts were analyzed by spectrophotometry, high-performance liquid chromatography-diode array detector (DAD), and liquid chromatography-mass spectrometry chromatography. The extraction efficiency of ASE and MAE was comparable with CSE at the optimal conditions. The greatest extraction by ASE was achieved at 50 °C, 2500 psi, 10 min using 5 cycles, and 100% flush. For MAE, a combination of 70 °C, 300 W, and 10 min in MAE was the most effective in extracting anthocyanins from blue wheat and purple corn compared with 50 °C, 1200 W, and 20 min for black rice. The anthocyanin composition of grain extracts was influenced by the extraction method. The ASE extraction method seems to be more appropriate in extracting anthocyanins from the colored grains as being comparable with the CSE method based on changes in anthocyanin composition. The method caused lower structural changes in anthocaynins compared with the MAE method. Changes in blue wheat anthocyanins were lower in comparison with purple corn or black rice perhaps due to the absence of acylated anthocyanin compounds in blue wheat. The results show significant differences in anthocyanins among the 3 extraction methods, which indicate a need to standardize a method for valid comparisons among studies and for quality assurance purposes.

  10. Supercritical Carbon Dioxide and Microwave-Assisted Extraction of Functional Lipophilic Compounds from Arthrospira platensis.

    PubMed

    Esquivel-Hernández, Diego A; López, Víctor H; Rodríguez-Rodríguez, José; Alemán-Nava, Gibrán S; Cuéllar-Bermúdez, Sara P; Rostro-Alanis, Magdalena; Parra-Saldívar, Roberto

    2016-05-05

    Arthrospira platensis biomass was used in order to obtain functional lipophilic compounds through green extraction technologies such as supercritical carbon dioxide fluid extraction (SFE) and microwave-assisted extraction (MAE). The temperature (T) factor was evaluated for MAE, while for SFE, pressure (P), temperature (T), and co-solvent (ethanol) (CS) were evaluated. The maximum extraction yield of the obtained oleoresin was (4.07% ± 0.14%) and (4.27% ± 0.10%) for SFE and MAE, respectively. Extracts were characterized by gas chromatography mass spectrometry (GC-MS) and gas chromatography flame ionization detector (GC-FID). The maximum contents of functional lipophilic compounds in the SFE and MAE extracts were: for carotenoids 283 ± 0.10 μg/g and 629 ± 0.13 μg/g, respectively; for tocopherols 5.01 ± 0.05 μg/g and 2.46 ± 0.09 μg/g, respectively; and for fatty acids 34.76 ± 0.08 mg/g and 15.88 ± 0.06 mg/g, respectively. In conclusion, the SFE process at P 450 bar, T 60 °C and CS 53.33% of CO₂ produced the highest yield of tocopherols, carotenoids and fatty acids. The MAE process at 400 W and 50 °C gives the best extracts in terms of tocopherols and carotenoids. For yield and fatty acids, the MAE process at 400 W and 70 °C produced the highest values. Both SFE and MAE showed to be suitable green extraction technologies for obtaining functional lipophilic compounds from Arthrospira platensis.

  11. Synthesis and characterization of nano ZnO rods via microwave assisted chemical precipitation method

    SciTech Connect

    Uma Sangari, N.; Chitra Devi, S.

    2013-01-15

    A microwave assisted chemical precipitation method has been employed for the synthesis of nano zinc oxide rods by reacting zinc nitrate and potassium hydroxide. The amount of potassium hydroxide was adjusted for three different pHs to achieve ZnO nano rods with varying aspect ratio. The mechanism of growth of nano rods is explained briefly. The average crystallite size of the as synthesized samples was analyzed by means of powder XRD pattern and estimated to vary from 25.6 nm to 43.1 nm. The existence of rods was confirmed using scanning electron microscopy (SEM). The samples were also analyzed using FT-IR. The optical properties of the samples were also studied by means of UV-visible spectra and Room Temperature Photo Luminescence studies. The band gap of the samples was determined from the DRS spectrum. A strong near band emission peaks due to surface defects are observed in the PL spectrum. - Graphical abstract: At the solution pH of 11 and 9, tetrapod-like and flower-like ZnO nano rods were formed along with separated rods respectively due to the formation of activated nuclei of different sizes. Highlights: Black-Right-Pointing-Pointer Increase in alkalinity of the precursor solution results in longer rods. Black-Right-Pointing-Pointer Beyond a saturation limit, the excess of added OH{sup -} ions inhibited the growth of rods. Black-Right-Pointing-Pointer Keeping all parameters the same, the alkalinity can only modify the aspect ratio of the rods and not their morphology.

  12. Microwave-assisted chemical insertion: a rapid technique for screening cathodes for Mg-ion batteries

    SciTech Connect

    Kaveevivitchai, Watchareeya; Huq, Ashfia; Manthiram, Arumugam

    2016-12-19

    We report an ultrafast microwave-assisted solvothermal method for chemical insertion of Mg2+ ions into host materials using magnesium acetate [Mg(CH3COO)2] as a metal-ion source and diethylene glycol (DEG) as a reducing agent. For instance, up to 3 Mg ions per formula unit of a microporous host framework Mo2.5+yVO9+z could be inserted in as little as 30 min at 170–195 °C in air. This process is superior to the traditional method which involves the use of organometallic reagents, such as di-n-butylmagnesium [(C4H9)2Mg] and magnesium bis(2,6-di-tert-butylphenoxide) [Mg-(O-2,6-But2C6H3)2], and requires an inert atmosphere with extremely long reaction times. Considering the lack of robust electrolytes for Mg-ion batteries, this facile approach can be readily used as a rapid screening technique to identify potential Mg-ion electrode hosts without the necessity of fabricating electrodes and assembling electrochemical cells. Due to the mild reaction conditions, the overall structure and morphology of the Mg-ion inserted products are maintained and the compounds can be used successfully as a cathode in Mg-ion batteries. The combined synchrotron X-ray and neutron diffraction Rietveld analysis reveals the structure of the Mg-inserted compounds and gives an insight into the interactions between the Mg ions and the open-tunnel host framework.

  13. Microwave-assisted protein solubilization for mass spectrometry-based shotgun proteome analysis.

    PubMed

    Ye, Xiaoxia; Li, Liang

    2012-07-17

    Protein solubilization is a key step in mass spectrometry-based shotgun proteome analysis. We describe a microwave-assisted protein solubilization (MAPS) method to dissolve proteins in reagents, such as NH(4)HCO(3) and urea, with high efficiency and with an added benefit that the solubilized proteins are denatured to become more susceptible to trypsin digestion, compared to other conventional protein solubilization techniques. In this method, a sample vial containing proteins suspended in a solubilization reagent is placed inside a domestic microwave oven and subjected to microwave irradiation for 30 s, followed by cooling the sample on ice to room temperature (~40 s) and then intermittent homogenization by vortex for 2 min. This cycle of microwave irradiation, cooling, and homogenization is repeated six times. In this way, sample overheating can be avoided, and a maximum amount of protein can be dissolved. It was shown that in the case of trypsin digestion of bovine serum albumen (BSA) more peptides and higher sequence coverage could be obtained from the protein dissolved by the MAPS method than the conventional heating, sonication, or vortex method. Compared to the most commonly used vortex-assisted protein solubilization method, MAPS reduces the solubilization time significantly, increases the amount of protein dissolvable in a reagent, and increases the number of proteins and peptides identified from a proteome sample. For example, in the proteome analysis of an Escherichia coli K-12 integral membrane protein extract, the MAPS method in combination with sequential protein solubilization and shotgun two-dimensional liquid chromatography tandem mass spectrometry analysis identified a total of 1291 distinct proteins and 10363 peptides, compared to 1057 proteins and 6261 peptides identified using the vortex method. Because MAPS can be done using an inexpensive microwave oven, this method can be readily adopted.

  14. Optimization of microwave-assisted extraction for six inorganic and organic arsenic species in chicken tissues using response surface methodology.

    PubMed

    Zhang, Wenfeng; Hu, Yuanan; Cheng, Hefa

    2015-09-01

    Response surface methodology was applied to optimize the parameters for microwave-assisted extraction of six major inorganic and organic arsenic species (As(III), As(V), dimethyl arsenic acid, monomethyl arsenic acid, p-arsanilic acid, and roxarsone) from chicken tissues, followed by detection using a high-performance liquid chromatography with inductively coupled mass spectrometry detection method, which allows the simultaneous analysis of both inorganic and organic arsenic species in the extract in a single run. Effects of extraction medium, solution pH, liquid-to-solid ratio, and the temperature and time of microwave-assisted extraction on the extraction of the targeted arsenic species were studied. The optimum microwave-assisted extraction conditions were: 100 mg of chicken tissue, extracted by 5 mL of 22% v/v methanol, 90 mmol/L (NH4 )2 HPO4 , and 0.07% v/v trifluoroacetic acid (with pH adjusted to 10.0 by ammonium hydroxide solution), ramping for 10 min to 71°C, and holding for 11 min. The method has good extraction performance for total arsenic in the spiked and nonspiked chicken tissues (104.0 ± 13.8% and 91.6 ± 7.8%, respectively), except for the ones with arsenic contents close to the quantitation limits. Limits of quantitation (S/N = 10) for As(III), As(V), dimethyl arsenic acid, monomethyl arsenic acid, p-arsanilic acid, and roxarsone in chicken tissues using this method were 0.012, 0.058, 0.039, 0.061, 0.102, and 0.240 mg/kg (dry weight), respectively. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Optimized microwave-assisted extraction of 6-gingerol from Zingiber officinale Roscoeand evaluation of antioxidant activity in vitro.

    PubMed

    Liu, Wei; Zhou, Chun-Li; Zhao, Jing; Chen, Dong; Li, Quan-Hong

    2014-01-01

    6-Gingerol is one of the most pharmacologically active and abundant components in ginger, which has a wide array of biochemical and pharmacologic activities. In recent years, the application of microwave-assisted extraction (MAE) for obtaining bioactive compounds from plant materials has shown tremendous research interest and potential. In this study, an efficient microwave-assisted extraction (MAE) technique was developed to extract 6-gingerol from ginger. The extraction efficiency of MAE was also compared with conventional extraction techniques. Fresh gingers (Zingiber officinale Rose.) were harvested at commercial maturity (originally from Shandong, laiwu, China). In single-factor experiments for the recovery of 6-gingerol, proper ranges of ratio of liquid to solid, ethanol proportion, microwave power, extraction time were determined. Based on the values obtained in single-factor experiments, a Box-Behnken design (BBD) was applied to determine the best combination of extraction variables on the yield of 6-gingerol. The optimum extraction conditions were as follows: microwave power 528 W, ratio of liquid to solid 26 mL·g(-1), extraction time 31 s and ethanol proportion 78%. Furthermore, more 6-gingerol and total polyphenols contents were extracted by MAE than conventional methods including Maceration (MAC), Stirring Extraction (SE), Heat reflux extraction (HRE), Ultrasound-assisted extraction (UAE), as well as the antioxidant capacity. Microwave-assisted extraction showed obvious advantages in terms of high extraction efficiency and antioxidant activity of extract within shortest extraction time. Scanning electron microscopy (SEM) images of ginger powder materials after different extractions were obtained to provide visual evidence of the disruption effect. To our best knowledge, this is the first report about usage of MAE of 6-gingerol extraction from ginger, which could be referenced for the extraction of other active compounds from herbal plants.

  16. A new strategy to grow polymer brush on graphene oxide surface through microwave assisted polymer synthesis

    NASA Astrophysics Data System (ADS)

    Park, Min Su; Ramaraj, B.; Yoon, Kuk Ro

    2012-09-01

    Herein, we report a method for growing polymers directly from the surface of graphene oxide (GPO). In this method, surface-initiated, microwave irradiation supported polymerization of benzyl chloride carrying vinylates was carried out from the surface of graphene oxide (GPO) for tailoring surface properties of GPO. This synthetic method consists of two important steps: first, the graphene was converted into GPO, then vinylbenzyl chloride (VBC) was polymerized on the surface of GPO by microwave induced irradiation polymerization. The structure and properties of the resultant polymeric conjugates were characterized by a range of characterization techniques viz.: Fourier transform infrared (FT-IR) spectroscopy, thermogravimetric analysis (TGA), energy-dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The FT-IR analysis of polymeric conjugates shows infrared (IR) peaks characteristic of VBC on the surface of GPO. TGA reveals enhanced thermal stability for GPO surface polymerized with VBC. EDX and XPS analysis shows signal corresponding to the chloride with reduction in oxygen percentage and increase in carbon percentage. SEM and TEM images visually show the presence of PVBC polymer layer on GPO surface.

  17. Comparison of microwave-assisted and conventional hydrodistillation in the extraction of essential oils from mango (Mangifera indica L.) flowers.

    PubMed

    Wang, Hong-Wu; Liu, Yan-Qing; Wei, Shou-Lian; Yan, Zi-Jun; Lu, Kuan

    2010-10-29

    Microwave-assisted hydrodistillation (MAHD) is an advanced hydrodistillation (HD) technique, in which a microwave oven is used in the extraction process. MAHD and HD methods have been compared and evaluated for their effectiveness in the isolation of essential oils from fresh mango (Mangifera indica L.) flowers. MAHD offers important advantages over HD in terms of energy savings and extraction time (75 min against 4 h). The composition of the extracted essential oils was investigated by GC-FID and GC-MS. Results indicate that the use of microwave irradiation did not adversely influence the composition of the essential oils. MAHD was also found to be a green technology.

  18. cis-Apa: a practical linker for the microwave-assisted preparation of cyclic pseudopeptides via RCM cyclative cleavage.

    PubMed

    Baron, Alice; Verdié, Pascal; Martinez, Jean; Lamaty, Frédéric

    2011-02-04

    A new linker cis-5-aminopent-3-enoic acid (cis-Apa) was prepared for the synthesis of cyclic pseudopeptides by cyclization-cleavage by using ring-closing methatesis (RCM). We developed a new synthetic pathway for the preparation of the cis-Apa linker that was tested in the cyclization-cleavage process of different RGD peptide sequences. Different macrocyclic peptidomimetics were prepared by using this integrated microwave-assisted method, showing that the readily available cis-Apa amino acid is well adapted as a linker in the cyclization-cleavage process.

  19. Microwave-assisted aminocarbonylation of ynamides by using catalytic [Fe3(CO)12] at low pressures of carbon monoxide.

    PubMed

    Pizzetti, Marianna; Russo, Adele; Petricci, Elena

    2011-04-11

    The microwave-assisted aminocarbonylation of ynamides at low pressures of CO is reported. A new class of (E)-acrylamides that are potentially suitable for several applications has been regioselectively synthesized after microwave irradiation for only 20 min by using eco-friendly [Fe(3)(CO)(12)] as the catalyst precursor and triethylamine as the ligand. This transformation is atom economic as all reactants are used in stoichiometric quantities. Furthermore, the transformation is efficiently applied to the alkoxycarbonylation of alkynes as well. Moreover, running these reactions under microwave irradiation allows the simplification of the reaction conditions with remarkable reductions in time, temperature and gas pressure.

  20. [Determination of fatty acids in shark cartilage by GC-MS using microwave-assisted digestion and derivatization].

    PubMed

    Li, G K; He, X Q; Zhang, Z X

    2000-07-01

    A rapid microwave-assisted digestion and derivatization method for the determination of fatty acids in shark cartilage by GC-MS was developed. The optimum conditions for digestion and derivatization were studied in detail using orthogonal design. The digestion and derivatization were accomplished in 4 minutes at 600 W microwave power using HCl-methanol (1:4, V/V) as digestion and derivatization solvent, and the extraction of the target analytes could be carried out simultaneously. This method is rapid, solvent-saving, and particularly suitable for the rapid determination of fatty acids in solid samples.

  1. One-Pot Synthesis of Imidazole-4-Carboxylates by Microwave-Assisted 1,5-Electrocyclization of Azavinyl Azomethine Ylides

    PubMed Central

    Preti, Lisa; Attanasi, Orazio A.; Caselli, Emilia; Favi, Gianfranco; Ori, Claudia; Davoli, Paolo; Felluga, Fulvia

    2013-01-01

    Diversely functionalized imidazole-4-carboxylates were synthesized by microwave-assisted 1,5-eletrocyclization of 1,2-diaza-1,3-diene-derived azavinyl azomethine ylides. 1,2-Diaza-1,3-dienes were treated with primary aliphatic or aromatic amines and subjected to microwave irradiation in the presence of aldehydes. 3-Alkyl- and 3-arylimidazole-4-carboxylates were prepared in good yields through a one-pot multicomponent procedure. Modulation of the substituents at C-2, N-3 and C-5 was possible, and 2-unsubstituted imidazoles were obtained when paraformaldehyde was used. PMID:24273445

  2. Microwave assisted synthesis of polyacrylamide grafted starch (St-g-PAM) and its applicability as flocculant for water treatment.

    PubMed

    Mishra, Sumit; Mukul, Ankita; Sen, Gautam; Jha, Usha

    2011-01-01

    Polyacrylamide grafted starch (St-g-PAM) was made by a novel method of synthesis, involving combination of microwave radiation and a chemical free radical initiator (ceric ammonium nitrate) to initiate grafting reaction. This method (microwave assisted synthesis) is quick, highly reliable, reproducible and yields high quality product as compared to the conventional method (which uses a chemical free radical initiator alone to initiate the grafting reaction).The St-g-PAM grades synthesized were characterized by various physicochemical techniques. Further, its application as flocculant for wastewater treatment was investigated.

  3. Wax: A benign hydrogen-storage material that rapidly releases H2-rich gases through microwave-assisted catalytic decomposition.

    PubMed

    Gonzalez-Cortes, S; Slocombe, D R; Xiao, T; Aldawsari, A; Yao, B; Kuznetsov, V L; Liberti, E; Kirkland, A I; Alkinani, M S; Al-Megren, H A; Thomas, J M; Edwards, P P

    2016-10-19

    Hydrogen is often described as the fuel of the future, especially for application in hydrogen powered fuel-cell vehicles (HFCV's). However, its widespread implementation in this role has been thwarted by the lack of a lightweight, safe, on-board hydrogen storage material. Here we show that benign, readily-available hydrocarbon wax is capable of rapidly releasing large amounts of hydrogen through microwave-assisted catalytic decomposition. This discovery offers a new material and system for safe and efficient hydrogen storage and could facilitate its application in a HFCV. Importantly, hydrogen storage materials made of wax can be manufactured through completely sustainable processes utilizing biomass or other renewable feedstocks.

  4. Room Temperature Magnetic Behavior In Nanocrystalline Ni-Doped Zro2 By Microwave-Assisted Polyol Synthesis

    NASA Astrophysics Data System (ADS)

    Parimita Rath, Pragyan; Parhi, Pankaj Kumar; Ranjan Panda, Sirish; Priyadarshini, Barsharani; Ranjan Sahoo, Tapas

    2017-08-01

    This article, deals with a microwave-assisted polyol method to demonstrate a low temperature route < 250°C, to prepare a high temperature cubic zirconia phase. Powder XRD pattern shows broad diffraction peaks suggesting nanometric size of the particles. Magnetic behavior of 1-5 at% Ni doped samples show a threshold for substitutional induced room temperature ferromagnetism up to 3 at% of Ni. TGA data reveals that Ni-doped ZrO2 polyol precursors decompose exothermically below 300°C. IR data confirms the reduction of Zr(OH)4 precipitates to ZrO2, in agreement with the conclusions drawn from the TGA analysis.

  5. Microwave-assisted isolation of essential oils from Nepeta crispa and N. racemosa and comparisons with the conventional method.

    PubMed

    Daryasari, Ameneh Porgham; Soleimani, Mojtaba; Ghorbani, Azam; Kheiri, Homayon; Daryasarie, Mohammad Porgham

    2012-11-01

    In this study microwave-assisted hydrodistillation (MAHD) has been compared with the conventional method of hydrodistillation for the extraction of the essential oils from two Iranian Lamiaceae species: Nepeta crispa Willd and N. racemosa Lam. The essential oils extracted by MAHD for 40 min were quantitatively and qualitatively (aromatic profile) similar to those obtained by conventional hydrodistillation for 3.5 h. The MAHD method yields an essential oil with higher amounts of more valuable oxygenated compounds, and allows substantial savings of costs in terms of time, energy and plant material.

  6. One-step microwave-assisted asymmetric cyclisation/hydrogenation of citronellal to menthols using supported nanoparticles on mesoporous materials.

    PubMed

    Balu, Alina Mariana; Campelo, Juan Manuel; Luque, Rafael; Romero, Antonio Angel

    2010-06-21

    The selective conversion of citronellal to menthols, with good diastereoselectivities to (-)-menthol for the case of (+)-citronellal as starting material, can effectively be carried out in a one-step reaction under microwave irradiation catalysed by supported nanoparticles on mesoporous materials. 2% Pt/Ga-MCM-41 was found to be the optimum catalyst for the reaction, with a quantitative conversion of starting material and selectivities above 85% to menthols obtained in short reaction times (typically 15 min). These results constitute the first report of a simple microwave-assisted one-step cyclisation/hydrogenation process for the production of menthols.

  7. Influence of intergrain interactions and thermal agitation on microwave-assisted magnetization switching behavior of granular magnetic film

    NASA Astrophysics Data System (ADS)

    Okamoto, Satoshi; Kikuchi, Nobuaki; Kitakami, Osamu; Shimatsu, Takehito

    2017-02-01

    Microwave-assisted magnetization switching (MAS) in a granular magnetic film is examined by computer simulation. Contrary to the macrospin calculation and the experiments on single magnetic dots reported so far, in which the switching field linearly decreases with increasing rf frequency and then sharply increases at the critical frequency, the granular film exhibits considerably broad MAS behavior against the rf frequency. This broad MAS behavior is mainly caused by the dispersion of magnetic properties and thermal agitation. On the other hand, intergrain dipolar and exchange interactions enhance the MAS effect in the granular film and suppress the MAS broadening.

  8. Microwave-assisted rapid synthesis of methyl 2,4,5-trimethoxyphenylpropionate, a metabolite of Cordia alliodora.

    PubMed

    Sinha, A K; Joshi, B P; Sharma, A; Kumar, J K; Kaul, V K

    2003-12-01

    Microwave assisted condensation of asaronaldehyde (2) with malonic acid in piperidine-AcOH provides 2,4,5-trimethoxycinnamic acid (3) in 87% yield within 4 min, which upon further reduction with PdCl2- HCOOH-aq. NaOH gives 3-(2,4,5-trimethoxy)phenyl propionic acid (4) in 88% yield within 3 min. Esterification of 4 with MeOH-H+ gives methyl 2,4,5-trimethoxyphenylpropionate (1), a metabolite of Cordia alliodora, in 94% yield within 3 min (overall 69% yield).

  9. Microwave-assisted cyclizations promoted by polyphosphoric acid esters: a general method for 1-aryl-2-iminoazacycloalkanes

    PubMed Central

    Díaz, Jimena E; Mollo, María C

    2016-01-01

    Summary The first general procedure for the synthesis of 5 to 7-membered 1-aryl-2-iminoazacycloalkanes is presented, by microwave-assisted ring closure of ω-arylaminonitriles promoted by polyphosphoric acid (PPA) esters. 1-Aryl-2-iminopyrrolidines were easily prepared from the acyclic precursors employing a chloroformic solution of ethyl polyphosphate (PPE). The use of trimethylsilyl polyphosphate (PPSE) in solvent-free conditions allowed for the synthesis of 1-aryl-2-iminopiperidines and hitherto unreported 1-aryl-2-iminoazepanes. The cyclization reaction involves good to high yields and short reaction times, and represents a novel application of PPA esters in heterocyclic synthesis. PMID:27829907

  10. Microwave-assisted cyclizations promoted by polyphosphoric acid esters: a general method for 1-aryl-2-iminoazacycloalkanes.

    PubMed

    Díaz, Jimena E; Mollo, María C; Orelli, Liliana R

    2016-01-01

    The first general procedure for the synthesis of 5 to 7-membered 1-aryl-2-iminoazacycloalkanes is presented, by microwave-assisted ring closure of ω-arylaminonitriles promoted by polyphosphoric acid (PPA) esters. 1-Aryl-2-iminopyrrolidines were easily prepared from the acyclic precursors employing a chloroformic solution of ethyl polyphosphate (PPE). The use of trimethylsilyl polyphosphate (PPSE) in solvent-free conditions allowed for the synthesis of 1-aryl-2-iminopiperidines and hitherto unreported 1-aryl-2-iminoazepanes. The cyclization reaction involves good to high yields and short reaction times, and represents a novel application of PPA esters in heterocyclic synthesis.

  11. Wax: A benign hydrogen-storage material that rapidly releases H2-rich gases through microwave-assisted catalytic decomposition

    NASA Astrophysics Data System (ADS)

    Gonzalez-Cortes, S.; Slocombe, D. R.; Xiao, T.; Aldawsari, A.; Yao, B.; Kuznetsov, V. L.; Liberti, E.; Kirkland, A. I.; Alkinani, M. S.; Al-Megren, H. A.; Thomas, J. M.; Edwards, P. P.

    2016-10-01

    Hydrogen is often described as the fuel of the future, especially for application in hydrogen powered fuel-cell vehicles (HFCV’s). However, its widespread implementation in this role has been thwarted by the lack of a lightweight, safe, on-board hydrogen storage material. Here we show that benign, readily-available hydrocarbon wax is capable of rapidly releasing large amounts of hydrogen through microwave-assisted catalytic decomposition. This discovery offers a new material and system for safe and efficient hydrogen storage and could facilitate its application in a HFCV. Importantly, hydrogen storage materials made of wax can be manufactured through completely sustainable processes utilizing biomass or other renewable feedstocks.

  12. Thrust Stand Measurements Using Alternative Propellants in the Microwave Assisted Discharge Inductive Plasma Accelerator

    NASA Technical Reports Server (NTRS)

    Hallock, Ashley K.; Polzin, Kurt A.

    2011-01-01

    Storable propellants (for example water, ammonia, and hydrazine) are attractive for deep space propulsion due to their naturally high density at ambient interplanetary conditions, which obviates the need for a cryogenic/venting system. Water in particular is attractive due to its ease of handling and availability both terrestrially and extra-terrestrially. While many storable propellants are reactive and corrosive, a propulsion scheme where the propellant is insulated from vulnerable (e.g. metallic) sections of the assembly would be well-suited to process these otherwise incompatible propellants. Pulsed inductive plasma thrusters meet this criterion because they can be operated without direct propellant-electrode interaction. During operation of these devices, electrical energy is capacitively stored and then discharged through an inductive coil creating a time-varying current in the coil that interacts with a plasma covering the face of the coil to induce a plasma current. Propellant is accelerated and expelled at a high exhaust velocity (O(10-100 km/s)) by the Lorentz body force arising from the interaction of the magnetic field and the induced plasma current. While this class of thruster mitigates the life-limiting issues associated with electrode erosion, many pulsed inductive plasma thrusters require high pulse energies to inductively ionize propellant. The Microwave Assisted Discharge Inductive Plasma Accelerator (MAD-IPA) is a pulsed inductive plasma thruster that addressees this issue by partially ionizing propellant inside a conical inductive coil before the main current pulse via an electron cyclotron resonance (ECR) discharge. The ECR plasma is produced using microwaves and a static magnetic field from a set of permanent magnets arranged to create a thin resonance region along the inner surface of the coil, restricting plasma formation, and in turn current sheet formation, to a region where the magnetic coupling between the plasma and the theta

  13. Closed vessel microwave assisted extraction - An innovative method for determination of trace metals in plant materials

    NASA Astrophysics Data System (ADS)

    Oeztan, S.; Duering, R.-A.

    2012-04-01

    Determination of metal concentrations in plant samples is important for better understanding of effects of toxic metals that are biologically magnified through the food chain and compose a great danger to all living beings. In recent years the use of microwave assisted extraction for plant samples has shown tremendous research interest which will probably substitute conventional procedures in the future. Generally conventional procedures have disadvantages including consuming of time and solvents. The objective of this study is to investigate and compare a new closed vessel microwave extraction (MAE) method with the combination of EDTA (MAE-EDTA) for the determination of metal contents (Cd, Mn, Pb, Zn) in plant samples (Lolio-Cynosuretum) by ICP-OES. Validation of the method was done by comparison of the results with another MAE procedure (MAE-H) which is applied with the mixture of 69% nitric acid (HNO3) and 30% hydrogen peroxide (H2O2). Moreover, conventional plant extraction (CE) method, for which the dissolution of plant samples were handled in HNO3 after dry ashing at 420° C, was used as a reference method. Approximately 0.5 g of sample was digested in 5 ml HNO3, 3 ml H2O2, and 5 ml deionized H2O for MAE-H and in 8 ml EDTA solution for MAE-EDTA. Certified plant reference materials (CRMs) were used for comparison of recovery rates from different extraction protocols. Thereby, the applicability of both MAE-H and MAE-EDTA procedures could be demonstrated. For 58 plant samples MAE-H showed the same extraction yields as CE in the determination of trace metal contents of the investigated elements in plant samples. MAE-EDTA gave similar values when compared to MAE-H and highly linear relationships were found for determination of Cd, Mn, Pb and Zn amounts. The recoveries for the CRMs were within the range 89.6-115%. Finally, strategic characteristics of MAE-EDTA for determination metal contents (Cd, Mn, Pb, Zn) in plant samples are: (i) applicability to a large set

  14. Microwave assisted extraction, antioxidant potential and chromatographic studies of some Rasayana drugs.

    PubMed

    Mishra, Ashish; Mishra, Shilpi; Bhargav, Shilpi; Bhargava, Cs; Thakur, Mayank

    2015-07-01

    To study and compare the conventional extraction procedure with microwave assisted extraction (MAE) for some Ayurvedic Rasayana drugs and to evaluate their antioxidant potential and carry out the characterization of extracts by thin layer chromatography. Three Ayurvedic rasayana plants Allium sativum Linn., Bombax ceiba Linn. and Inula racemosa Hook. were evaluated for an improved MAE methodology by determining the effects of grinding degree, extraction solvent, effect of dielectric constant and duration of time on the extractive value. Antioxidant potential of all three drugs was evaluated with 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging activity and reducing power was determined by using Gallic acid as standard. Further thin layer chromatographic (TLC) analysis was performed on pre-activated Silica Gel G plates and Rf value were compared with those reported for the important biomarkers. The total extractive value for Allium sativum Linn. was 36.95% (w/w) and 49.95% (w/w) for ethanol extraction respectively. In case of Bombax ceiba Linn. the yield of aqueous extract by MAE was 50% (w/w) compared to 42% (w/w) in ethanol (50% v/v). Percent yield of Inula racemosa Hook. in aqueous extract was found to be 27.55% (w/w) which was better than ethanol extract (50%) where the yield was 25.95% (w/w). Upon antioxidant activity evaluation. sativum extract showed an absorbance of 0.980±0.92 at concentration of 500 μg with maximum reducing capacity. This was followed by. ceiba Linn. 0.825±0.98 and. racemosa Hook. with 0.799±2.01 at a concentration of 500 μg. TLC based standardization of. sativum Linn. extract shows single spot with Rf value of 0.38, B. ceiba Linn. extract shows Rf values were 0.23, 0.58, 0.77, 0.92 and I. racemosa Hook. extract spot had a Rf value of 0.72. A significant improvement in extractive values was observed as a factor of time and other advantages by using MAE technology. All three drugs have high antioxidant potential and a TLC

  15. Resilience of Oocyte Germinal Vesicles to Microwave-Assisted Drying in the Domestic Cat Model

    PubMed Central

    Lee, Pei-Chih; Paramore, Elisha; Van Vorst, Matthew; Comizzoli, Pierre

    2015-01-01

    The ability to compact and inject the cat germinal vesicle (GV) into a recipient cytoplast allows exploration of a new fertility preservation strategy that avoids whole oocyte freezing. The objective of the present study was to understand the impact of water loss and storage time on GV DNA integrity. Immature cat oocytes were exposed to 1.5 M trehalose for 10 min before microwave-assisted dehydration for 0, 5, 10, 15, 20, 25, 30, or 40 min. Oocytes then were rehydrated to assess chromatin configuration and the incidence of DNA fragmentation (TUNEL assay). The moisture content progressively decreased (p<0.05) from 1.7 to 0.1 gH2O/gDW over the first 30 min, but did not decrease further (p>0.05) after 40 min. Chromatin configuration was unaffected (p>0.05) over time. The percentage of GVs with DNA fragmentation was unaltered (p>0.05) from 0 to 30 min of treatment (range, 6.1%–12%), but increased (p<0.05) to 32.5% after 40 min. Next, the influence of storage at two different supra-zero temperatures after 30 min of drying was investigated. Oocyte-loaded, microwave-treated filters were individually sealed in Dri-Shield moisture barrier bags and stored at 4°C or ambient temperature for 0 to 8 weeks. Moisture contents gradually decreased (p<0.05) from 0.12 to 0.10 gH2O/gDW after 8 weeks of storage at 4°C or ambient temperature. The percentage of GVs with DNA fragmentation more than doubled (p<0.05) from 0 (14.3%) to 2 days (30.0%–33.0%), but remained stable (p>0.05) thereafter (1 through 4 weeks, 25.0%–35.0%). Collective results demonstrate the feasibility of using microwave processing to dehydrate the mammalian GV to a moisture content that is nonlethal and enables nonfrozen storage, an alternative approach for preserving the maternal genome at cool or ambient temperature. PMID:26035005

  16. Microwave-assisted biosynthesis of zinc nanoparticles and their cytotoxic and antioxidant activity.

    PubMed

    Salari, Zeinab; Ameri, Atefeh; Forootanfar, Hamid; Adeli-Sardou, Mahboubeh; Jafari, Mandana; Mehrabani, Mitra; Shakibaie, Mojtaba

    2017-01-01

    The present study was designed for microwave assisted synthesis of zinc nanoparticles (Zn NPs) using Lavandula vera leaf extract in the presence of ZnSO4 (1mM). The biogenic Zn NPs were then characterized using scanning electron microscopy (SEM), energy dispersive X-ray (EDX), X-ray diffraction spectroscopy (XRD), UV-visible spectroscopy, and Fourier transform infrared spectroscopy (FTIR) techniques. Thereafter, the cytotoxic effect of ZnSO4 and Zn NPs on different cell lines was investigated by MTT-based cytotoxicity assay and their antioxidant properties were assessed using DPPH scavenging activity and reducing power assay. The SEM micrograph showed that the Zn NPs had spherical shape with the size range of 30-80nm. For A549, MCF-7, HT-29, and Caco-2 cell lines treated with Zn NPs, the concentration necessary causing 50% cell death (IC50) was found to be 22.3±1.1μgmL(-1), 86±3.7μgmL(-1), 10.9±0.5μgmL(-1), and 56.2±2.8μgmL(-1), respectively. In the case of ZnSO4, the same results (IC50) were observed at concentration of 81.6±1.3μgmL(-1) (A549), 121.0±2.4μgmL(-1) (MCF-7), 43.0±1.4μgmL(-1) (HT-29), and 85.7±2.3μgmL(-1) (Caco-2). The obtained results of antioxidant activity showed that the IC50 values of butylated hydroxyanisole (BHA) and Zn NPs were 44μgmL(-1)and 65.3μgmL(-1), respectively, while ZnSO4 at concentration of 200μgmL(-1) exhibited only 10.9% DPPH radical scavenging effect. Moreover, the reducing power of Zn NPs and BHA were significantly higher than ZnSO4 (p<0.05). To sum up, application of L. vera leaf extract combined with microwave heating energy led to simple and fast formation of Zn nanostructures exhibited higher antioxidant and cytotoxic activity compared to soluble Zn(+2) ions. However, identification of the related mechanisms merit further studies. Copyright © 2016. Published by Elsevier GmbH.

  17. An effective negative pressure cavitation-microwave assisted extraction for determination of phenolic compounds in P. calliantha H. Andr.

    PubMed

    Zhang, Dong-Yang; Yao, Xiao-Hui; Duan, Ming-Hui; Luo, Meng; Wang, Wei; Fu, Yu-Jie; Zu, Yuan-Gang; Efferth, Thomas

    2013-08-21

    A novel negative pressure and microwave assisted extraction technique (NMAE) was first proposed and applied for extraction of phenolic compounds from pyrola. [C₄MIM]BF₄ aqueous solution was selected as extraction solvent. Optimal extraction conditions were microwave power 700 W, negative pressure -0.07 MPa, temperature 40 °C, liquid-solid ratio 20 : 1, ionic liquid (IL) concentration 0.5 M, extraction time 15 min. The predominance of NMAE was investigated by comparing with microwave-assisted extraction (MAE) and negative pressure cavitation extraction (NPCE) using a first-order kinetics equation. The C∞ values of the target compounds by NMAE were from 0.406 to 5.977 mg g⁻¹ higher than these by MAE and NPCE, which indicated that NMAE had higher extraction yields. The K values of NMAE were also the highest; it was testified that the target compounds could be transferred from matrix into solvent much more effectively by NMAE than by MAE and NPCE. In addition, the NMAE method was validated in terms of repeatability and reproducibility, the relative standard deviation for relative recovery was lower than 5.43 and 8.78%, respectively. Therefore, NMAE was a developed extraction technique for analytical sample preparation. The RP-HPLC-UV method was also successfully applied for the quantification of six target compounds in pyrola.

  18. Measurement of Dielectric Properties and Microwave-Assisted Homogeneous Acid-Catalyzed Transesterification in a Monomode Reactor.

    PubMed

    Dall'Oglio, Evandro L; de Sousa, Paulo T; Campos, Deibnasser C; de Vasconcelos, Leonardo Gomes; da Silva, Alan Cândido; Ribeiro, Fabilene; Rodrigues, Vaniomar; Kuhnen, Carlos Alberto

    2015-08-27

    Microwave heating technology is dependent on the dielectric properties of the materials being processed. The dielectric properties of H2SO4, H3PO4, ClSO3H, and H3CSO3H were investigated in this study using a vector network analyzer in an open-ended coaxial probe method at various temperatures. Phosphoric and sulfuric acids presented higher loss tangents in the frequency range 0.3-13 GHz, reflecting greater mobility of the ions and counterions. The acids were employed as catalysts in microwave-assisted homogeneous transesterification reactions for the production of methylic and ethylic biodiesel. The effects of catalyst concentration, alcohol to oil molar ratio, and irradiation time on biodiesel conversions were investigated. The results showed a significant reduction in the reaction time for microwave-assisted transesterification reactions as compared to times for conventional heating. Also, despite its higher loss tangent, it was observed that H3PO4 leads to lower conversion to biodiesel, which can be explained by its lower carbonyl protonation capacity.

  19. Fabrication and morphology control of BaWO{sub 4} thin films by microwave assisted chemical bath deposition

    SciTech Connect

    Wang Rui; Liu Chen; Zeng Jia; Li KunWei; Wang Hao

    2009-04-15

    Highly crystallized barium tungstate (BaWO{sub 4}) thin films with dumbbell-like, kernel-like, bowknot-like and cauliflower-like microstructure were synthesized from an aqueous solution containing barium nitrate, ethylenediamine tetraacetate acid disodium and sodium tungstate, via mild microwave assisted chemical bath deposition process. The resulting BaWO{sub 4} films with different morphologies were characterized by X-ray diffraction spectrum, scanning electron microscope, Raman and photoluminescence spectra. The results indicate that the morphologies of final products significantly depend on the reaction conditions including the reaction time, the initial concentration of precursor reagent and the physicochemical characteristics of the substrates. Furthermore, the oriented aggregation mechanism is proposed as a possible formation mechanism of the films with specific morphologies. - Graphical abstract: Highly crystallized BaWO{sub 4} thin films with controllable morphologies have been synthesized via mild microwave assisted chemical bath deposition. The oriented aggregation mechanism has been proposed as the possible formation mechanism of specific films.

  20. Microwave-assisted chemical reduction routes for direct synthesis of (fct) L1 phase of Fe-Pt.

    PubMed

    Acharya, Smita; Singh, Kamal

    2011-01-01

    Microwave-assisted chemical reduction route has been explored for the direct synthesis of fct L1(0) - phase of Fe-Pt nanoparticles in the present work. Effects of microwave power and irradiation time on the growth process are systematically studied. Using this facile and high yield technique we could tune particle size from 7 to 17 nm. Prepared Fe-Pt NPs exhibited ordered face centered tetragonal (fct) L1(0) phase without any post-synthesis treatment. The particle size and magnetic properties of the prepared Fe-Pt were found to be very sensitive to the microwave irradiation power, while influence of exposure time was insignificant. The hysteresis measurements were performed at 300 K to study magnetic properties of the synthesized Fe-Pt as a function of crystallite size. Coercivity and saturation magnetization were observed to be decreasing with diminishing particle size. The microwave-assisted route is found to be a simple technique for direct synthesis of metal alloys and may prove to be a potential tool of high density data storage materials such as Fe-Pt.

  1. 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

  2. Optimization of microwave-assisted extraction with saponification (MAES) for the determination of polybrominated flame retardants in aquaculture samples.

    PubMed

    Fajar, N M; Carro, A M; Lorenzo, R A; Fernandez, F; Cela, R

    2008-08-01

    The efficiency of microwave-assisted extraction with saponification (MAES) for the determination of seven polybrominated flame retardants (polybrominated biphenyls, PBBs; and polybrominated diphenyl ethers, PBDEs) in aquaculture samples is described and compared with microwave-assisted extraction (MAE). Chemometric techniques based on experimental designs and desirability functions were used for simultaneous optimization of the operational parameters used in both MAES and MAE processes. Application of MAES to this group of contaminants in aquaculture samples, which had not been previously applied to this type of analytes, was shown to be superior to MAE in terms of extraction efficiency, extraction time and lipid content extracted from complex matrices (0.7% as against 18.0% for MAE extracts). PBBs and PBDEs were determined by gas chromatography with micro-electron capture detection (GC-muECD). The quantification limits for the analytes were 40-750 pg g(-1) (except for BB-15, which was 1.43 ng g(-1)). Precision for MAES-GC-muECD (%RSD < 11%) was significantly better than for MAE-GC-muECD (%RSD < 20%). The accuracy of both optimized methods was satisfactorily demonstrated by analysis of appropriate certified reference material (CRM), WMF-01.

  3. Extending lean operating limit and reducing emissions of methane spark-ignited engines using a microwave-assisted spark plug

    DOE PAGES

    Rapp, Vi H.; DeFilippo, Anthony; Saxena, Samveg; ...

    2012-01-01

    Amore » microwave-assisted spark plug was used to extend the lean operating limit (lean limit) and reduce emissions of an engine burning methane-air. In-cylinder pressure data were collected at normalized air-fuel ratios of λ = 1.46, λ = 1.51, λ = 1.57, λ = 1.68, and λ = 1.75. For each λ, microwave energy (power supplied to the magnetron per engine cycle) was varied from 0 mJ (spark discharge alone) to 1600 mJ. At lean conditions, the results showed adding microwave energy to a standard spark plug discharge increased the number of complete combustion cycles, improving engine stability as compared to spark-only operation. Addition of microwave energy also increased the indicated thermal efficiency by 4% at λ = 1.68. At λ = 1.75, the spark discharge alone was unable to consistently ignite the air-fuel mixture, resulting in frequent misfires. Although microwave energy produced more consistent ignition than spark discharge alone at λ = 1.75, 59% of the cycles only partially burned. Overall, the microwave-assisted spark plug increased engine performance under lean operating conditions (λ = 1.68) but did not affect operation at conditions closer to stoichiometric.« less

  4. Fast preparation of LiFePO4 nanoparticles for lithium batteries by microwave-assisted hydrothermal method.

    PubMed

    Yang, Gang; Ji, Hongmei; Liu, Haidong; Huo, Kaifu; Fu, Jijiang; Chu, Paul K

    2010-02-01

    Nanomaterial for lithium batteries can decrease mechanical strain upon lithium intercalation/ deintercalation from lattice, and lead to high rate capability. The currently available microwave technology permits the development and implantation of a temperature-controlled microwave-assisted hydrothermal synthesis (TCMH) of nano-sized cathode material for lithium batteries. Unlike in previous reported traditional hydrothermal synthesis of cathode material LiFePO4, the pure phase of LiFePO4 can be simply and rapidly synthesized for 5 minutes in water under hydrothermal treatment with microwave irradiation. The homogeneous effects induced by microwave irradiation could create a uniform seeding condition. The colloid precursor Li3PO4 plays the key role to be the nucleation center for the new phase while the formation energy for LiFePO4 would be decreased during the following microwave irradiation. The as-prepared pristine LiFePO4 without carbon coating are characterized by X-ray diffraction, Raman, scanning and transmission electron microscopy, and tested as the cathode in lithium batteries. The particle sizes of pristine LiFePO4 are dependent on hydrothermal and microwave-assisted hydrothermal condition and the electrochemical performance are relatively determined.

  5. Computation of adsorption parameters for the removal of dye from wastewater by microwave assisted sawdust: Theoretical and experimental analysis.

    PubMed

    S, Suganya; P, Senthil Kumar; A, Saravanan; P, Sundar Rajan; C, Ravikumar

    2017-03-01

    In this research, the microwave assistance has been employed for the preparation of novel material from agro/natural bio-waste i.e. sawdust, for the effective removal of methylene blue (MB) dye from aqueous solution. The characterization of the newly prepared microwave assisted sawdust (MASD) material was performed by using FTIR, SEM and XRD analyses. In order to obtain the maximum removal of MB dye from wastewater, the adsorption experimental parameters such as initial dye concentration, contact time, solution pH and adsorbent dosage were optimized by trial and error approach. The obtained experimental results were applied to the different theoretical models to predict the system behaviour. The optimum conditions for the maximum removal MB dye from aqueous solution for an initial MB dye concentration of 25mg/L was calculated as: adsorbent dose of 3g/L, contact time of 90min, solution pH of 7.0 and at the temperature of 30°C. Freundlich and pseudo-second order models was best obeyed with the studied experimental data. Langmuir maximum monolayer adsorption capacity of MASD for MB dye removal was calculated as 58.14mg of MB dye/g of MASD. Adsorption diffusion model stated that the present adsorption system was controlled by intraparticle diffusion model. The obtained results proposed that, novel MASD was considered to be an effective and low-cost adsorbent material for the removal of dye from wastewater.

  6. [Optimization of microwave-assisted extraction with RSM and HPLC determination for three iridoid glycosides in Cornus officinalis].

    PubMed

    He, Juan-ni; Liu, Xiao; Mou, Zhao-li; Zhan, Han-ying; Zhang, Zhi-qi

    2011-07-01

    To establish a method of microwave-assisted extraction and high performance liquid chromatographic (HPLC) for simultaneous determination of three iridoid glycosides including loganin, sweroside and cornuside in Cornus officinalis. The extraction conditions of microwave power,ethanol concentration, liquid to sample ratio were optimized with a response surface methodology (RSM); Three constituents were separated on an Agilent TC-C18 column by gradient elution using acetonitrile and water as the mobile phase. The flow rate was 1.0 mL/min. The detection wave length was 240 nm. The optimal conditions of microwave extraction were as follows: microwave power 400 W, ethanol concentration 72%, liquid to sample ratio 15 mL/g, the extraction time 10 min, the extraction times 2; The HPLC peak areas of all the constituents showed good linearity (r>0.9994) in the range of the tested concentration,the average recoveries of the method were 98.68%, 98.24% and 98.29%, respectively. The established method of microwave-assisted extraction and HPLC simultaneously determination has the advantages of convenient, precision and reliability. It can be used in simultaneous determination of three iridoid glycosides in Cornus officinalis.

  7. Microwave-assisted formulation of solid lipid nanoparticles loaded with non-steroidal anti-inflammatory drugs.

    PubMed

    Shah, Rohan M; Eldridge, Daniel S; Palombo, Enzo A; Harding, Ian H

    2016-12-30

    Stearic acid-based solid lipid nanoparticles (SLNs) were prepared using the microwave assisted one-pot microemulsions procedure pioneered by our group. In this study, non-steroidal anti-inflammatory drugs (NSAIDs) including indomethacin, ketoprofen and nimesulide were selected as ideal "test" drugs, based on their poor water solubility. The model drugs were incorporated within the SLNs by the microwave-assisted procedure at the time of SLN production. The microwave-produced drug-loaded SLNs were evaluated in terms of their physicochemical characteristics, drug release behavior and their uptake into against A549 cell line (human lung epithelial cells). The microwave-produced drug-loaded SLNs had a small particle size distribution, negative zeta potential and high encapsulation efficiency. The drug release studies were consistent with a core-shell structure of SLNs (probably a drug-loaded shell) which results in biphasic drug release from the SLNs. The drug release kinetics suggested a good fit of the release data to the Makoid-Banakar model and was governed by Fickian diffusion. The drug-loaded SLNs showed concentration-dependent cytotoxicity and reduced IL-6 and IL-8 secretion in lipopolysaccharide-induced cells. All of the above findings suggest that the microwave-produced SLNs could be promising drug carriers of NSAIDs and will further facilitate their development for topical, oral and/or nasal administration. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Microwave-assisted rapid synthesis of birnessite-type MnO{sub 2} nanoparticles for high performance supercapacitor applications

    SciTech Connect

    Zhang, Xiong; Miao, Wang; Li, Chen; Sun, Xianzhong; Wang, Kai; Ma, Yanwei

    2015-11-15

    Highlights: • Birnessite-type MnO{sub 2} nanoparticles were prepared by the microwave-assisted reflux. • The microwave reaction duration was only 5 min. • A specific capacitance of 329 F g{sup −1} was obtained for birnessite-type MnO{sub 2}. - Abstract: Birnessite-type MnO{sub 2} nanoparticles have been successfully synthesized by the microwave-assisted reflux as short as 5 min. The microstructure and morphology of the products were characterized by X-ray diffraction, N{sub 2} adsorption–desorption isotherms, scanning electron microscopy, transmission electron microscopy. The electrochemical properties of the as-prepared MnO{sub 2} as an electrode material for supercapacitor were investigated by cyclic voltammetry and galvanostatic charge-discharge measurements in 1 M Na{sub 2}SO{sub 4} electrolyte, and a high specific capacitance of 329 F g{sup −1} was achieved at a current density of 0.2 A g{sup −1}. The specific capacitance retention was 92% after 1000 cycles at 2 A g{sup −1}, suggesting that it is a promising electrode material for supercapacitors.

  9. Comparative study on open system digestion and microwave assisted digestion methods for metal determination in shrimp sludge compost.

    PubMed

    Nemati, Keivan; Abu Bakar, Nor Kartini; Bin Abas, Mhd Radzi; Sobhanzadeh, Elham; Low, Kah Hin

    2010-10-15

    The aim of this work was to evaluate two different digestion methods for the determination of the total concentration of metals (Zn, Cu, Cr, Ni, Pb and Cd) in shrimp sludge compost. The compost made from shrimp aquaculture sludge co-composted with organic materials (peat, crushed bark and manure) was used as an organic growing medium for crop. Open system digestion and microwave assisted digestion procedures were employed in sample preparation. Various combinations and volumes of hydrofluoric, nitric and hydrochloric acids were evaluated for the efficiency of both methods. A certified reference material (CRM 146) was used in the comparison of these two digestion methods. The results revealed a good agreement between both procedures and the certified valued. The best recoveries were found in the range between 95% and 99% for microwave assisted digestion with a mixture of 2 ml of HF, 6 ml of HNO(3) and 2 ml of HCl. This procedure was recommended as the method for digestion the compost herein based on the recovery analysis and time taken.

  10. Microwave-assisted synthesis of reduced graphene oxide/titania nanocomposites as an adsorbent for methylene blue adsorption

    NASA Astrophysics Data System (ADS)

    Wang, Huan; Gao, Haihuan; Chen, Mingxi; Xu, Xiaoyang; Wang, Xuefang; Pan, Cheng; Gao, Jianping

    2016-01-01

    In this study microwave-assisted reduction (MrGO) and direct reduction of graphene oxide (rGO) by Ti powders were established, and the effect of the reaction conditions on the reduction were discussed. The results showed that GO can be effectively reduced by both methods, however, microwave assistance can greatly shorten the reduction time. The produced Ti ions from the reaction of Ti powder with GO were transferred to TiO2 by hydrolysis and formed MrGO/TiO2 and rGO/TiO2. They were used as adsorbents for the removal of methylene blue (MB). MrGO/TiO2 showed a higher adsorption capacity (qmax, 845.6 mg/g) than rGO/TiO2 (qmax, 467.6 mg/g). Investigation on the adsorption MB onto MrGO/TiO2 was conducted and demonstrated that adsorption kinetics followed the pseudo second-order kinetics model and the adsorption isotherm was well described by the Langmuir isotherm model. The recycling of MrGO/TiO2 was achieved by photocatalytic degradation of MB catalyzed by MrGO/TiO2 itself.

  11. Rapid microwave-assisted synthesis of hierarchical ZnO hollow spheres and their application in Cr(VI) removal.

    PubMed

    Zhao, Xiaowei; Qi, Limin

    2012-06-15

    A rapid one-pot synthesis of hierarchical ZnO hollow spheres consisting of nanoparticles was realized by a facile microwave-assisted solvothermal method using ethanol as the solvent. According to the time-dependent observation of the formation process, a tentative mechanism based on ethyl acetate bubble-templating self-assembly of ZnO nanoparticles was proposed for the formation of the ZnO hollow spheres. Compared with the conventional heating, the microwave irradiation resulted in a significantly shortened reaction time (within 30 min) and considerably improved quality of the ZnO hollow spheres, such as narrower size distribution and more regular morphology, owing to the high heating rate and thus the accelerated reaction rate. It was shown that the microwave-assisted synthesis of ZnO nanostructures with tunable morphologies can be realized by judicious selection of appropriate solvents. The obtained ZnO hollow spheres exhibited an excellent adsorption capacity towards Cr(VI) ions in water because of their high surface area for adsorption and a good ability to preserve the accessible surface.

  12. Microwave-assisted boron and nitrogen co-doped reduced graphene oxide as a transparent conductive electrode

    NASA Astrophysics Data System (ADS)

    Umrao, Sima; Mishra, Himanshu; Srivastava, Anchal; Lee, Sungjoo

    2017-07-01

    A crystalline Boron (B)- and Nitrogen (N)-co-doped microwave-assisted reduced graphene oxide (BNMRGO) film was investigated as a potential transparent conducting electrode (TCE) material. X-ray diffraction results revealed the good crystallinity of the BNMRGO film, and the presence of a (0004) reflection plane indicated the formation of a few small domains of hexagonal boron nitride in the microwave assisted reduced graphene oxide (MRGO) sheets under the co-doping process. Raman and X-ray photoelectron spectroscopic results indicated a reduction of sp3 carbon centers upon co-doping. The ID/IG ratio decreased after co-doping from 0.89 to 0.24, indicating a low average defect density of ˜1.01 × 1010 cm-2. Optoelectronic characterization of the BNMRGO film on a glass substrate revealed a high optical transparency of 82% at 550 nm and a low sheet resistance (Rsh) of 355 Ω/sq, which was lower than that observed from the MRGO sheets (Rsh = 719 Ω/sq). BNMRGO provided a ratio between the direct conductivity (σdc) to the optical conductivity (σoc), that is, the figure of merit of a TCE material, of 5.96. Overall, this work paves the way toward developing a manufacturable TCE.

  13. Deep Eutectic Solvent-Based Microwave-Assisted Method for Extraction of Hydrophilic and Hydrophobic Components from Radix Salviae miltiorrhizae.

    PubMed

    Chen, Jue; Liu, Mengjun; Wang, Qi; Du, Huizhi; Zhang, Liwei

    2016-10-17

    Deep eutectic solvents (DESs) have attracted significant attention as a promising green media. In this work, twenty-five kinds of benign choline chloride-based DESs with microwave-assisted methods were applied to quickly extract active components from Radix Salviae miltiorrhizae. The extraction factors, including temperature, time, power of microwave, and solid/liquid ratio, were investigated systematically by response surface methodology. The hydrophilic and hydrophobic ingredients were extracted simultaneously under the optimized conditions: 20 vol% of water in choline chloride/1,2-propanediol (1:1, molar ratio) as solvent, microwave power of 800 W, temperature at 70 °C, time at 11.11 min, and solid/liquid ratio of 0.007 g·mL(-1). The extraction yield was comparable to, or even better than, conventional methods with organic solvents. The microstructure alteration of samples before and after extraction was also investigated. The method validation was tested as the linearity of analytes (r² > 0.9997 over two orders of magnitude), precision (intra-day relative standard deviation (RSD) < 2.49 and inter-day RSD < 2.96), and accuracy (recoveries ranging from 95.04% to 99.93%). The proposed DESs combined with the microwave-assisted method provided a prominent advantage for fast and efficient extraction of active components, and DESs could be extended as solvents to extract and analyze complex environmental and pharmaceutical samples.

  14. The physicochemical properties of microwave-assisted encapsulated anthocyanins from Ipomoea batatas as affected by different wall materials

    PubMed Central

    Mohd Nawi, Norazlina; Muhamad, Ida Idayu; Mohd Marsin, Aishah

    2015-01-01

    This study focuses on the impact of different wall materials on the physicochemical properties of microwave-assisted encapsulated anthocyanins from Ipomoea batatas. Using the powder characterization technique, purple sweet potato anthocyanin (PSPAs) powders were analysed for moisture content, water activity, dissolution time, hygroscopicity, color and morphology. PSPAs were produced using different wall materials: maltodextrin (MD), gum arabic (GA) and a combination of gum arabic and maltodextrin (GA + MD) at a 1:1 ratio. Each of the wall materials was homogenized to the core material at a core/wall material ratio of 5 and were microencapsulated by microwave-assisted drying at 1100 W. Results indicated that encapsulated powder with the GA and MD combination presented better quality of powder with the lowest value of moisture content and water activity. With respect to morphology, the microcapsule encapsulated with GA + MD showed several dents in coating surrounding its core material, whereas other encapsulated powders showed small or slight dents entrapped onto the bioactive compound. Colorimetric analysis showed changes in values of L, a*, b*, hue and chroma in the reconstituted powder compared to the initial powder. PMID:25838887

  15. Conventional and microwave-assisted synthesis of new 1H-benzimidazole-thiazolidinedione derivatives: A potential anticancer scaffold.

    PubMed

    Sharma, Pankaj; Reddy, T Srinivasa; Kumar, Niggula Praveen; Senwar, Kishna Ram; Bhargava, Suresh K; Shankaraiah, Nagula

    2017-09-29

    A series of new benzimidazole bearing thiazolidinedione derivatives has been designed, synthesized by using conventional as well as microwave-assisted methods. Microwave-assisted synthesis caused a significant reduction in the reaction times and improvement in the yields of all the derivatives. All the new synthesized compounds were evaluated for their in vitro cytotoxic potential against selected human cancer cell lines of breast (MDAMB-231), prostate (PC-3), cervical (HeLa), lung (A549) and bone (HT1080) along with a normal kidney cells (HeK-293T). The compounds 17n, 17p and 17q were found to be potent cytotoxic with IC50 values in the range of 0.096-0.63 μM on PC-3, HeLa, A549 and HT1080 cancer cells. Most of the compounds have found to be safe on normal HeK-293T kidney cells in comparison to cancer cells. The treatment of cells with 17p and 17q showed the typical apoptotic morphological features like fragmentation and shrinkage of nuclei. Further, test compounds resulted in inhibition of cell migration through disruption of F-actin protein assembly. Hoechst, DCFH-DA staining, mitochondrial membrane and annexin binding assays revealed that the cancer cell proliferation was inhibited through induction of apoptosis in A549 cells. Copyright © 2017 Elsevier Masson SAS. All rights reserved.

  16. Single-step microwave-assisted hot water extraction of hemicelluloses from selected lignocellulosic materials - A biorefinery approach.

    PubMed

    Mihiretu, Gezahegn T; Brodin, Malin; Chimphango, Annie F; Øyaas, Karin; Hoff, Bård H; Görgens, Johann F

    2017-10-01

    The viability of single-step microwave-induced pressurized hot water conditions for co-production of xylan-based biopolymers and bioethanol from aspenwood sawdust and sugarcane trash was investigated. Extraction of hemicelluloses was conducted using microwave-assisted pressurized hot water system. The effects of temperature and time on extraction yield and enzymatic digestibility of resulting solids were determined. Temperatures between 170-200°C for aspenwood and 165-195°C for sugarcane trash; retention times between 8-22min for both feedstocks, were selected for optimization purpose. Maximum xylan extraction yields of 66 and 50%, and highest cellulose digestibilities of 78 and 74%, were attained for aspenwood and sugarcane trash respectively. Monomeric xylose yields for both feedstocks were below 7%, showing that the xylan extracts were predominantly in non-monomeric form. Thus, single-step microwave-assisted hot water method is viable biorefinery approach to extract xylan from lignocelluloses while rendering the solid residues sufficiently digestible for ethanol production. Copyright © 2017 Elsevier Ltd. All rights reserved.

  17. Optimization of microwave-assisted extraction for anthocyanins, polyphenols, and antioxidants from raspberry (Rubus Coreanus Miq.) using response surface methodology.

    PubMed

    Teng, Hui; Lee, Won Young; Choi, Yong Hee

    2013-09-01

    Anthocyanins (Acys), polyphenols, and antioxidants were extracted from raspberry (Rubus Coreanus Miq.) using a highly efficient microwave-assisted extraction technique. Different solvents, including methanol, ethanol, and acetone, were tested. The colors of the extracts varied from light yellow to purple red or dark red. SEM and other nutrient analyses verified that ethanol was the most favorable medium for the microwave-assisted extraction of raspberry due to its high output and low toxicity. Effects of process parameters, including microwave power, irradiation time, and solvent concentration, were investigated through response surface methodology. Canonical analysis estimated that the highest total Acys content, total polyphenols content, and antioxidant activity of raspberry were 17.93 mg cyanidin-3-O-glucoside equivalents per gram dry weight, 38.57 mg gallic acid equivalents per gram dry weight, and 81.24%, respectively. The polyphenol compositions of raspberry extract were identified by HPLC with diode array detection, and nine kinds of polyphenols were identified and quantified, revealing that chlorogenic acid, syringic acid, and rutin are the major polyphenols contained in raspberry fruits. Compared with other fruits and vegetables, raspberry contains higher Acy and polyphenol contents with stronger antioxidant activity, suggesting that raspberry fruits are a good source of natural food colorants and antioxidants.

  18. Microwave assisted synthesis and characterization of Ni/NiO nanoparticles as electrocatalyst for methanol oxidation in alkaline solution

    NASA Astrophysics Data System (ADS)

    Arunachalam, Prabhakarn; Ghanem, Mohamed A.; Al-Mayouf, Abdullah M.; Al-shalwi, Matar; Hamed Abd-Elkader, Omar

    2017-02-01

    Nickel/Nickel oxide (Ni/NiO) nanoparticles catalyst is prepared by microwave-assisted liquid-phase deposition using ethylene glycol (EG) and water mixture under atmospheric conditions. The physicochemical characterizations of the catalyst carried out by surface area analyzer, x-ray diffraction (XRD), x-ray photoelectron spectroscopy (XPS), electron microscopes measurements suggest the formation of crystalline nanoparticles structure of NiO. The surface area of Ni/NiO prepared using EG/water mixture reaches 70 m2 g-1 which is 2-fold enhsancement in surface area in comparison with NiO prepared in pure EG and an order of magnitude higher than that of bulk nickel prepared in pure water. The methanol electro-oxidation activity of the Ni/NiO nanoparticles obtained in EG/water mixture displayed more than 4-fold increase in oxidation current at 1.7 V versus RHE in comparison with NiO nanoparticles obtained in EG and 20-fold increase compared to bulk nickel catalyst concord with the enhancement of electro-active surface area. The results show the Ni/NiO nanoparticles produced by microwave assisted synthesis has superior activity for methanol oxidation in alkaline solution over the other nickel based catalysts and has potential for mass production.

  19. 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

  20. Microwave-assisted cross-linking of milk proteins induced by microbial transglutaminase

    PubMed Central

    Chen, Chun-Chi; Hsieh, Jung-Feng

    2016-01-01

    We investigated the combined effects of microbial transglutaminase (MTGase, 7.0 units/mL) and microwave irradiation (MI) on the polymerization of milk proteins at 30 °C for 3 h. The addition of MTGase caused the milk proteins to become polymerized, which resulted in the formation of components with a higher molecular-weight (>130 kDa). SDS-PAGE analysis revealed reductions in the protein content of β-lactoglobulin (β-LG), αS-casein (αS-CN), κ-casein (κ-CN) and β-casein (β-CN) to 50.4 ± 2.9, 33.5 ± 3.0, 4.2 ± 0.5 and 1.2 ± 0.1%, respectively. The use of MTGase in conjunction MI with led to a 3-fold increase in the rate of milk protein polymerization, compared to a sample that contained MTGase but did not undergo MI. Results of two-dimensional gel electrophoresis (2-DE) indicated that κ-CN, β-CN, a fraction of serum albumin (SA), β-LG, α-lactalbumin (α-LA), αs1-casein (αs1-CN), and αs2-casein (αs2-CN) were polymerized in the milk, following incubation with MTGase and MI at 30 °C for 1 h. Based on this result, the combined use of MTGase and MI appears to be a better way to polymerize milk proteins. PMID:27966639

  1. Microwave-assisted cross-linking of milk proteins induced by microbial transglutaminase

    NASA Astrophysics Data System (ADS)

    Chen, Chun-Chi; Hsieh, Jung-Feng

    2016-12-01

    We investigated the combined effects of microbial transglutaminase (MTGase, 7.0 units/mL) and microwave irradiation (MI) on the polymerization of milk proteins at 30 °C for 3 h. The addition of MTGase caused the milk proteins to become polymerized, which resulted in the formation of components with a higher molecular-weight (>130 kDa). SDS-PAGE analysis revealed reductions in the protein content of β-lactoglobulin (β-LG), αS-casein (αS-CN), κ-casein (κ-CN) and β-casein (β-CN) to 50.4 ± 2.9, 33.5 ± 3.0, 4.2 ± 0.5 and 1.2 ± 0.1%, respectively. The use of MTGase in conjunction MI with led to a 3-fold increase in the rate of milk protein polymerization, compared to a sample that contained MTGase but did not undergo MI. Results of two-dimensional gel electrophoresis (2-DE) indicated that κ-CN, β-CN, a fraction of serum albumin (SA), β-LG, α-lactalbumin (α-LA), αs1-casein (αs1-CN), and αs2-casein (αs2-CN) were polymerized in the milk, following incubation with MTGase and MI at 30 °C for 1 h. Based on this result, the combined use of MTGase and MI appears to be a better way to polymerize milk proteins.

  2. Microwave assisted synthesis of sheet-like Cu/BiVO{sub 4} and its activities of various photocatalytic conditions

    SciTech Connect

    Chen, Xi; Li, Li; Yi, Tingting; Zhang, WenZhi; Zhang, Xiuli; Wang, Lili

    2015-09-15

    The Cu/BiVO{sub 4} photocatalyst with visible-light responsivity was prepared by the microwave-assisted hydrothermal method. The phase structures, chemical composition and surface physicochemical properties were well-characterized via X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV–vis diffuse reflectance absorption (UV–vis/DRS), scanning electron microscopy (SEM), and N{sub 2} adsorption–desorption tests. Results indicate that the crystal structure of synthetic composite materials is mainly monoclinic scheelite BiVO{sub 4}, which is not changed with the increasing doping amount of Cu. In addition, the presence of Cu not only enlarges the range of the composite materials under the visible-light response, but also increases the BET value significantly. Compared to pure BiVO{sub 4}, 1% Cu/BiVO{sub 4}-160 performs the highest photocatalytic activity to degrade methylene blue under the irradiation of ultraviolet, visible and simulated sunlight. In addition, the capture experiments prove that the main active species was superoxide radicals during photocatalytic reaction. Moreover, the 1% Cu/BiVO{sub 4}-160 composite shows good photocatalytic stability after three times of recycling. - Graphical abstract: A series of BiVO{sub 4} with different amounts of Cu doping were prepared by the microwave-assisted method, moreover, which performed the high photocatalytic activities to degrade methylene blue under multi-mode. - Highlights: • A series of Cu/BiVO{sub 4} with different amounts of Cu doping were prepared by microwave-assisted synthesis. • The morphologies of as-samples were different with the amount of Cu doping increased. • Compared with pure BiVO{sub 4}, as-Cu/BiVO{sub 4} showed stronger absorption in the visible light region obviously. • 1% Cu/BiVO{sub 4}-160 performed the high photocatalytic activities to degrade methylene blue under multi-mode. • OH{sup •} and h{sup +} both play important roles in the photocatalytic reaction.

  3. Mathematical modeling and Monte Carlo simulation of thermal inactivation of non-proteolytic Clostridium botulinum spores during continuous microwave-assisted pasteurization

    USDA-ARS?s Scientific Manuscript database

    The objective of this study is to develop a mathematical method to simulate the internal temperature history of products processed in a prototype microwave-assisted pasteurization system (MAPS) developed by Washington State University. Two products (10 oz. beef meatball trays and 16 oz. salmon fill...

  4. Extraction of Maltol from Fraser Fir: A Comparison of Microwave-Assisted Extraction and Conventional Heating Protocols for the Organic Chemistry Laboratory

    ERIC Educational Resources Information Center

    Koch, Andrew S.; Chimento, Clio A.; Berg, Allison N.; Mughal, Farah D.; Spencer, Jean-Paul; Hovland, Douglas E.; Mbadugha, Bessie; Hovland, Allan K.; Eller, Leah R.

    2015-01-01

    Two methods for the extraction of maltol from Fraser fir needles are performed and compared in this two-week experiment. A traditional benchtop extraction using dichloromethane is compared to a microwave-assisted extraction using aqueous ethanol. Students perform both procedures and weigh the merits of each technique. In doing so, students see a…

  5. A NOVEL HIGH-SPEED METHOD FOR THE GENERATION OF 4-ARYLDIHYDROPYRIMIDINE COMPOUND LIBRARIES USING A MICROWAVE-ASSISTED BIGINELLI CONDENSATION PROTOCOL -

    EPA Science Inventory

    In this presentation we report the application of microwave assisted chemistry to the parallel synthesis of 4-aryl-3,4-dihydropyrimidin-2(1H)-ones employing a solventless Biginelli multicomponent condensation protocol. The novel method employs neat mixtures of B-ketoesters, aryl ...

  6. Process optimisation of microwave-assisted extraction of peony ( Paeonia suffruticosa Andr .) seed oil using hexane-ethanol mixture and its characterisation

    Treesearch

    Xiaoli Sun; Wengang Li; Jian Li; Yuangang Zu; Chung-Yun Hse; Jiulong Xie; Xiuhua Zhao

    2016-01-01

    Ethanol and hexane mixture agent microwave-assisted extraction (MAE) method was conducted to extract peony (Paeonia suffruticosa Andr.) seed oil (PSO). The aim of the study was to optimise the extraction for both yield and energy consumption in mixture agent MAE. The highest oil yield (34.49%) and lowest unit energy consumption (14 125.4 J g

  7. CATALYST-FREE REACTIONS UNDER SOLVENT-FEE CONDITIONS: MICROWAVE-ASSISTED SYNTHESIS OF HETEROCYCLIC HYDRAZONES BELOW THE MELTING POINT OF NEAT REACTANTS: JOURNAL ARTICLE

    EPA Science Inventory

    NRMRL-CIN-1437 Jeselnik, M., Varma*, R.S., Polanc, S., and Kocevar, M. Catalyst-free Reactions under Solvent-fee Conditions: Microwave-assisted Synthesis of Heterocyclic Hydrazones below the Melting Point of Neat Reactants. Published in: Chemical Communications 18:1716-1717 (200...

  8. Microwave-Assisted Synthesis of a Natural Insecticide on Basic Montmorillonite K10 Clay. Green Chemistry in the Undergraduate Organic Laboratory

    ERIC Educational Resources Information Center

    Dintzner, Matthew R.; Wucka, Paul R.; Lyons, Thomas W.

    2006-01-01

    A detailed investigation of the clay-catalyzed condensation of sesamol and other phenols with 3-methyl-2-butenal to give methylenedioxyprecocene (MDP) and other chromenes is presented. The clay-catalyzed microwave-assisted condensation of sesamol with 3-methyl-2-butenal is appropriate for incorporation into undergraduate organic laboratory…

  9. Microwave-Assisted Synthesis of a Natural Insecticide on Basic Montmorillonite K10 Clay. Green Chemistry in the Undergraduate Organic Laboratory

    ERIC Educational Resources Information Center

    Dintzner, Matthew R.; Wucka, Paul R.; Lyons, Thomas W.

    2006-01-01

    A detailed investigation of the clay-catalyzed condensation of sesamol and other phenols with 3-methyl-2-butenal to give methylenedioxyprecocene (MDP) and other chromenes is presented. The clay-catalyzed microwave-assisted condensation of sesamol with 3-methyl-2-butenal is appropriate for incorporation into undergraduate organic laboratory…

  10. CATALYST-FREE REACTIONS UNDER SOLVENT-FEE CONDITIONS: MICROWAVE-ASSISTED SYNTHESIS OF HETEROCYCLIC HYDRAZONES BELOW THE MELTING POINT OF NEAT REACTANTS: JOURNAL ARTICLE

    EPA Science Inventory

    NRMRL-CIN-1437 Jeselnik, M., Varma*, R.S., Polanc, S., and Kocevar, M. Catalyst-free Reactions under Solvent-fee Conditions: Microwave-assisted Synthesis of Heterocyclic Hydrazones below the Melting Point of Neat Reactants. Published in: Chemical Communications 18:1716-1717 (200...

  11. Extraction of Maltol from Fraser Fir: A Comparison of Microwave-Assisted Extraction and Conventional Heating Protocols for the Organic Chemistry Laboratory

    ERIC Educational Resources Information Center

    Koch, Andrew S.; Chimento, Clio A.; Berg, Allison N.; Mughal, Farah D.; Spencer, Jean-Paul; Hovland, Douglas E.; Mbadugha, Bessie; Hovland, Allan K.; Eller, Leah R.

    2015-01-01

    Two methods for the extraction of maltol from Fraser fir needles are performed and compared in this two-week experiment. A traditional benchtop extraction using dichloromethane is compared to a microwave-assisted extraction using aqueous ethanol. Students perform both procedures and weigh the merits of each technique. In doing so, students see a…

  12. A NOVEL HIGH-SPEED METHOD FOR THE GENERATION OF 4-ARYLDIHYDROPYRIMIDINE COMPOUND LIBRARIES USING A MICROWAVE-ASSISTED BIGINELLI CONDENSATION PROTOCOL -

    EPA Science Inventory

    In this presentation we report the application of microwave assisted chemistry to the parallel synthesis of 4-aryl-3,4-dihydropyrimidin-2(1H)-ones employing a solventless Biginelli multicomponent condensation protocol. The novel method employs neat mixtures of B-ketoesters, aryl ...

  13. Effect of deposition parameters on the structural properties of ZnO nanopowders prepared by microwave-assisted hydrothermal synthesis.

    PubMed

    Caglar, Yasemin; Gorgun, Kamuran; Aksoy, Seval

    2015-03-05

    ZnO nanopowders were synthesized via microwave-assisted hydrothermal method at different deposition (microwave irradiation) times and pH values. The effects of pH and deposition (microwave irradiation) time on the crystalline structure and orientation of the ZnO nanopowders have been investigated by X-ray diffraction (XRD) study. XRD observations showed that the crystalline quality of ZnO nanopowders increased with increasing pH value. The crystallite size and texture coefficient values of ZnO nanopowders were calculated. The structural quality of ZnO nanopowder was improved by deposition parameters. Field emission scanning electron microscope (FESEM) was used to analyze the surface morphology of the ZnO nanopowders. Microwave irradiation time and pH value showed a significant effect on the surface morphology.

  14. Microwave-assisted green synthesis of silver nanoparticles from Fraxinus excelsior leaf extract and its antioxidant assay

    NASA Astrophysics Data System (ADS)

    Parveen, Mehtab; Ahmad, Faheem; Malla, Ali Mohammed; Azaz, Shaista

    2016-02-01

    The biosynthesis of nanoparticles has been proposed as a cost effective and environmentally benevolent alternative to chemical and physical methods. In the present study, microwave assisted synthesis of silver nanoparticles (AgNPs) has been demonstrated using leaf extract of Fraxinus excelsior reducing aqueous AgNO3 solution. The synthesized nanoparticles have been characterized on the basis of fourier transform infrared spectroscopy (FT-IR), UV-Vis spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and energy dispersive X-ray (EDX) analysis. The presence of a characteristic surface plasmon resonance (SPR) absorption band at 425 nm in UV-Vis reveals the reduction of silver metal ions into silver nanoparticles. FT-IR analysis was carried out to probe the possible functional group involved in the synthesis of AgNPs. Further leaf extracts and AgNPs were evaluated for antiradical scavenging activity by 1,1-diphenyl-2-picryl-hydrazyl (DPPH) assay.

  15. Microwave assisted preparation of n-butylacrylate grafted chitosan and its application for Cr(VI) adsorption.

    PubMed

    Santhana Krishna Kumar, A; Uday Kumar, Chinta; Rajesh, Vidya; Rajesh, N

    2014-05-01

    Biopolymers such as chitosan possess excellent properties suited for varied applications. In this work, we describe a novel microwave assisted method for the preparation of n-butylacrylate grafted chitosan adsorbent and its utility for the adsorption of chromium(VI). A 3 min irradiation time was enough to prepare the adsorbent, and techniques such as FT-IR, powder XRD, SEM and EDS were used for comprehensive characterization. The adsorption was effective at pH 3.5 with 25 mL of 20 ppm Cr(VI) solution. Langmuir, Freundlich, Dubinin-Radushkevich, Temkin, Elovich and Redlich isotherms were studied in detail. The ΔG, ΔH and ΔS parameters were evaluated to understand the adsorption thermodynamics. The adsorption involves the interaction of Cr(VI) with the hydroxyl and amino groups in chitosan. Copyright © 2014 Elsevier B.V. All rights reserved.

  16. Microwave assisted synthesis of porous ZnO/SnS heterojunction and its application in visible light degradation of ciprofloxacin

    SciTech Connect

    Makama, A. B. Salmiaton, A. Choong, T. S. Y. Abdullah, N.; Saion, E. B.

    2016-07-06

    Porous ZnO/SnS heterojunctions were successfully synthesized via microwave-assisted heating of aqueous solutions containing different amounts of SnS precursors (SnCl{sub 2} and Na{sub 2}S) in the presence of fixed amount of ZnCO{sub 3} nanoparticles. The experimental results revealed that the heterojunctions exhibited much higher visible light-driven photocatalytic activity for the degradation of the ciprofloxacin than pure SnS nanocrystals. The photocatalytic degradation efficiency (1-C{sub t}/C{sub 0}) of the pollutant for the most active heterogeneous nanostructure is about four times more efficient than pure SnS. The enhanced photocatalytic efficiency is ascribed to the synergic effect of high photon absorption and reduction in the recombination of electrons and holes because of efficient separation and electron transfer from the SnS to ZnO nanoparticles.

  17. Microwave-assisted extraction and ultrasonic slurry sampling procedures for cobalt determination in geological samples by electrothermal atomic absorption spectroscopy.

    PubMed

    Felipe-Sotelo, M; Carlosena, A; Fernández, E; López-Mahía, P; Muniategui, S; Prada, D

    2004-06-17

    Slurry sampling is compared to microwave-assisted acid digestion for cobalt determination in soil/sediment samples by electrothermal atomic absorption spectrometry (ETAAS). Furnace temperature programs and appropriate amounts of three chemical modifiers were optimised in order to get the highest signals and good separations between the atomic and background signals. Using nitric acid (0.5% (v/v)) as liquid medium, no chemical modifier was needed. The detection limit, based on integrated absorbance, was 0.04mugg(-1) for digests and slurries. Within-batch precision and analytical recoveries were satisfactory for both procedures. Accuracy was tested by analysing a reference soil and a sediment from IRMM. The methods were further compared employing a set of roadside soils and estuarine sediments. As no significant differences (95% confidence) were found, practical analytical properties were suggested in order to select one of them.

  18. Microwave-assisted synthesis, characterization and biological activities of organotin (IV) complexes with some thio Schiff bases

    NASA Astrophysics Data System (ADS)

    Singh, Ran Vir; Chaudhary, Pratibha; Chauhan, Shikha; Swami, Monika

    2009-03-01

    Microwave-assisted synthesis and characterization of the organotin (IV) complexes are reported. Trigonal bipyramidal and octahedral complexes of tin (IV) have been synthesized by the reaction of dimethyltin (IV) dichloride with 4-nitrobenzanilide- S-benzyldithiocarbazate (L 1H), 4-chlorobenzanilide- S-benzyldithiocarbazate (L 2H), 4-nitrobenzanilidebenzothiazoline (L 3H) and 4-chlorobenzanilidebenzothiazoline (L 4H). The complexes so formed were characterized by elemental analysis, conductance measurements, molecular weight determinations and spectral data viz. IR, UV-Visible, 1H and 13C NMR. The anti-microbial activities of the ligands and their corresponding organotin (IV) complexes have been screened against various strains of bacteria and fungi. Antifertility activity against male albino rats has also been reported.

  19. Microwave-assisted rapid synthesis of luminescent gold nanoclusters for sensing Hg2+ in living cells using fluorescence imaging.

    PubMed

    Shang, Li; Yang, Linxiao; Stockmar, Florian; Popescu, Radian; Trouillet, Vanessa; Bruns, Michael; Gerthsen, Dagmar; Nienhaus, G Ulrich

    2012-07-21

    A microwave-assisted strategy for synthesizing dihydrolipoic acid (DHLA) capped fluorescent gold nanoclusters (AuNCs) has been developed. Irradiation with microwaves during synthesis enhanced the fluorescence quantum yield (QY) of AuNCs by about five-fold and shortened the reaction time from hours to several minutes. The as-synthesized DHLA-AuNCs possessed bright near-infrared fluorescence (QY: 2.9%), ultrasmall hydrodynamic diameter (3.3 nm), good colloidal stability over the physiologically relevant pH range of 5-10 as well as low cytotoxicity toward HeLa cells. Moreover, these DHLA-AuNCs were capable of sensing Hg(2+) through the specific interaction between Hg(2+) and Au(+) on the surface of AuNCs; the limit of detection (LOD) was 0.5 nM. A potential application in imaging intracellular Hg(2+) in HeLa cells was demonstrated by using spinning disc confocal microscopy.

  20. Direct Synthesis of Fe-Pt Nanoparticles in Ordered Face Centered (fct) LIo Phase by Microwave Assisted Route

    NASA Astrophysics Data System (ADS)

    Acharya, S. A.; Khule, S. M.; Singh, K.; Bhoga, S. S.

    2011-07-01

    In the present work, microwave-assisted chemical reduction route has been explored for the direct synthesis of fct LIo-phase of Fe-Pt nanoparticles. Effects of microwave power and irradiation time on the growth process were investigated. Using this facile and high yield technique we could tune particle size from 7 to 17 nm. The as-prepared FePt were found to be sensitive to the microwave irradiation power, while influence of exposure time was insignificant. The hysteresis measurements were performed at room temperature (300 K) to study magnetic properties of as-synthesized Fe-Pt as a function of crystallize size. The coercivity and saturation magnetization was observed to be decrease with diminishing for direct synthesis of metal alloys.

  1. Microwave-assisted acid hydrolysis of toluene diamine conjugates in urine samples for biomarkers in toluene diisocyanate analysis.

    PubMed

    Yeh, Hui-Jung; Lin, Wei-Chao; Sheu, Shiann-Cherng; Shih, Tung-Sheng; Chen, Lien-Huei; Chang, Ho-Yuan

    2007-06-15

    Toluene diamines (TDAs) in urine have been used widely to determine the amount of toluene diisocyanate (TDI) absorbed by humans. Conventional hydrolysis to prepare a sample of urine takes approximately 16h. An attempt is made to apply microwave-assisted heating (MAH) to reduce the duration of analysis. Urine collected from rats exposed to a mixture of 2,4- and 2,6-TDI was diluted with non-exposed human urine 1/1250-, 1/500- and 1/250-fold. The urine samples were hydrolyzed by both conventional heating and MAH. The hydrolysis efficiency obtained using MAH significantly exceeded that obtained using conventional heating. Hydrolysis by MAH required only 20min, 48 times faster than with conventional heating. The use of the MAH method in hydrolysis was demonstrated to be reproducible, timesaving and efficient technique in measuring the concentration of urinary TDAs.

  2. Morphology-controlled synthesis of nanostructured zinc hydroxide fluoride via a microwave-assisted ionic liquid route

    NASA Astrophysics Data System (ADS)

    Zhang, Songtao; Zheng, Mingbo; Song, Jiakui; Li, Nianwu; Lu, Hongling; Cao, Jieming

    2014-12-01

    Zinc hydroxide fluoride (Zn(OH)F) with multiform morphologies such as flower-like particles, pumpkin-like aggregates, and hollow orange-like aggregates are prepared by a microwave-assisted ionic liquid method. During synthesis, microwave irradiation accelerates the reaction rate and shortens the reaction time. 1-Butyl-3-methylimidazolium tetrafluoroborate ([Bmim][BF4]) or 1-2-hydroxylethyl-3-methylimidazolium tetrafluoroborate ([C2OHmim][BF4]) is used as both reactant and template. Experimental results indicate that the morphology evolution of Zn(OH)F is mainly controlled by the concentration of zinc acetate solution. A possible mechanism underlying the formation of nanostructured Zn(OH)F with diverse morphologies is proposed. Furthermore, nanoporous ZnO is obtained by the thermal decomposition of as-prepared Zn(OH)F in air, and the morphology is well retained.

  3. Reduced leakage current and improved ferroelectricity in magneto-electric composite ceramics prepared with microwave assisted radiant hybrid sintering

    SciTech Connect

    Upadhyay, Sanjay Kumar; Reddy, V. Raghavendra E-mail: vrreddy.ugcdaecsr@nic.in; Gupta, S. M.; Chauhan, N.; Gupta, Ajay

    2015-04-15

    Structural, electrical and magnetic properties of magneto-electric composite ceramics viz., 0.9 BaTi{sub 0.95}Sn{sub 0.05}O{sub 3} (BTSO)- 0.1 Ni{sub 0.8}Zn{sub 0.2}Fe{sub 2}O{sub 4} (NZFO) prepared with microwave assisted radiant hybrid sintering (MARH) are reported. Phase purity and isovalent substitution of Ti{sup 4+} by Sn{sup 4+} of the samples is confirmed from x-ray diffraction and {sup 119}Sn Mossbauer measurements respectively. Significant suppression of leakage current and improvement of ferroelectricity is observed for the composites prepared with MARH. The observed results are explained in terms of uniform dispersion of ferrite (NZFO) phase in the ferroelectric (BTSO) matrix as evidenced from back-scattered scanning electron micrographs.

  4. Microwave-assisted synthesis of Gd3+ doped PbI2 hierarchical nanostructures for optoelectronic and radiation detection applications

    NASA Astrophysics Data System (ADS)

    Shkir, Mohd.; AlFaify, S.; Yahia, I. S.; Ganesh, V.; Shoukry, H.

    2017-03-01

    In this work, we report the simple, low temperature and rapid microwave-assisted synthesis of undoped and Gadolinium (III) doped lead iodide with different morphologies, i.e. nanorods of average diameter 200 nm and hierarchical (flower-shaped) nanosheets of thicknesses less than 100 nm. Prepared nanostructures were typify in details using a variety of analytical techniques that reveal the well crystallinity with hexagonal structure. We found that by changing the concentrations of Gadolinium (III) one can tailor the size and shape of nanostructures of lead iodide. The presence of Gadolinium (III) doping was assessed by energy dispersive X-ray analysis. Optical band gap and Photoluminescence intensity are found to be enhanced due to Gadolinium (III) doping. The value of Gamma linear absorption coefficient is found to be enriched with doping, which suggests its application in radiation detection.

  5. Optimization and comparison of ultrasound/microwave assisted extraction (UMAE) and ultrasonic assisted extraction (UAE) of lycopene from tomatoes.

    PubMed

    Lianfu, Zhang; Zelong, Liu

    2008-07-01

    The extracting technology including ultrasonic and microwave assisted extraction (UMAE) and ultrasonic assisted extraction (UAE) of lycopene from tomato paste were optimized and compared. The results showed that the optimal conditions for UMAE were 98 W microwave power together with 40 KHz ultrasonic processing, the ratio of solvents to tomato paste was 10.6:1 (V/W) and the extracting time should be 367 s; as for UAE, the extracting temperature was 86.4 degrees C, the ratio of the solvents to tomato paste was 8.0:1 (V/W) and the extracting time should be 29.1 min, while the percentage of lycopene yield was 97.4% and 89.4% for UMAE and UAE, respectively. These results implied that UMAE was far more efficient extracting method than UAE.

  6. Synthesis of an Isoindoline-Annulated, Tricyclic Sultam Library via Microwave-Assisted, Continuous-Flow Organic Synthesis (MACOS).

    PubMed

    Ullah, Farman; Zang, Qin; Javed, Salim; Porubsky, Patrick; Neuenswander, Benjamin; Lushington, Gerald H; Hanson, Paul R; Organ, Michael G

    2012-01-01

    A microwave-assisted, continuous-flow organic synthesis (MACOS) protocol for the synthesis of an isoindoline-annulat-ed, tricyclic sultam library, utilizing a Heck-aza-Michael (HaM) strategy, is reported. This sequence involves a Heck reaction on vi-nylsulfonamides with batch microwave heating followed by a one-pot, sequential intramolecular aza-Michael cyclization/Boc-deprot-ection using MACOS. Subsequent cyclization with either 1,1'-carbonyldiimidazole or chloromethyl pivalate using MACOS provided an array of tricyclic sultams. This efficient three-step protocol requires only a few hours to produce the target sultams starting from simple starting materials. Using this strategy, a 38-member library of isoindoline-annulated sultams was generated in good to excellent overall yields (53-87%).

  7. Ultrafast ammonia-driven, microwave-assisted synthesis of nitrogen-doped graphene quantum dots and their optical properties

    NASA Astrophysics Data System (ADS)

    Zheng, Binjie; Chen, Yuanfu; Li, Pingjian; Wang, Zegao; Cao, Bingqiang; Qi, Fei; Liu, Jinbo; Qiu, Zhiwen; Zhang, Wanli

    2017-01-01

    For the first time, a facile, ultrafast, ammonia-driven microwave-assisted synthesis of high-quality nitrogen-doped graphene quantum dots (NGQDs) at room temperature and atmospheric pressure is presented. This one-step method is very cheap, environment friendly, and suitable for large-scale production. The as-synthesized NGQDs consisting of one to three graphene monolayers exhibit highly crystalline quality with an average size of 5.3 nm. A new fluorescence (FL) emission peak at 390 nm is observed, which might be attributed to the doped nitrogen atoms into the GQDs. An interesting red-shift is observed by comparing the FL excitation spectra to the UV-visible absorption spectra. Based on the optical properties, the detailed Jablonski diagram representing the energy level structure of NGQDs is derived.

  8. Synthesis of an Isoindoline-Annulated, Tricyclic Sultam Library via Microwave-Assisted, Continuous-Flow Organic Synthesis (MACOS)

    PubMed Central

    Ullah, Farman; Zang, Qin; Javed, Salim; Porubsky, Patrick; Neuenswander, Benjamin; Lushington, Gerald H.

    2013-01-01

    A microwave-assisted, continuous-flow organic synthesis (MACOS) protocol for the synthesis of an isoindoline-annulat-ed, tricyclic sultam library, utilizing a Heck–aza-Michael (HaM) strategy, is reported. This sequence involves a Heck reaction on vi-nylsulfonamides with batch microwave heating followed by a one-pot, sequential intramolecular aza-Michael cyclization/Boc-deprot-ection using MACOS. Subsequent cyclization with either 1,1′-carbonyldiimidazole or chloromethyl pivalate using MACOS provided an array of tricyclic sultams. This efficient three-step protocol requires only a few hours to produce the target sultams starting from simple starting materials. Using this strategy, a 38-member library of isoindoline-annulated sultams was generated in good to excellent overall yields (53–87%). PMID:24244052

  9. Innovative biofilm inhibition and anti-microbial behavior of molybdenum sulfide nanostructures generated by microwave-assisted solvothermal route

    NASA Astrophysics Data System (ADS)

    Qureshi, Nilam; Patil, Rajendra; Shinde, Manish; Umarji, Govind; Causin, Valerio; Gade, Wasudev; Mulik, Uttam; Bhalerao, Anand; Amalnerkar, Dinesh P.

    2015-03-01

    The incessant use of antibiotics against infectious diseases has translated into a vicious circle of developing new antibiotic drug and its resistant strains in short period of time due to inherent nature of micro-organisms to alter their genes. Many researchers have been trying to formulate inorganic nanoparticles-based antiseptics that may be linked to broad-spectrum activity and far lower propensity to induce microbial resistance than antibiotics. The way-out approaches in this direction are nanomaterials based (1) bactericidal and (2) bacteriostatic activities. We, herein, present hitherto unreported observations on microbial abatement using non-cytotoxic molybdenum disulfide nanostructures (MSNs) which are synthesized using microwave assisted solvothermal route. Inhibition of biofilm formation using MSNs is a unique feature of our study. Furthermore, this study evinces antimicrobial mechanism of MSNs by reactive oxygen species (ROS) dependent generation of superoxide anion radical via disruption of cellular functions.

  10. Application of water as a solvent in microwave-assisted extraction for analysis of PCBs and CBzs in fly ash.

    PubMed

    Sun, Yifei; Takaoka, Masaki; Takeda, Nobuo; Matsumoto, Tadao; Oshita, Kazuyuki

    2005-04-01

    Polychlorinated biphenyls (PCBs) and chlorobenzenes (CBzs) are two classes of dioxin precursors formed in municipal solid waste incinerators (MSWIs); they produce negative health effects similar to those of dioxins. Reducing the analytical time required for determining the concentrations of these compounds in MSWIs is important for quickly evaluating their importance and assessing associated health risks. In the present study, water is used as a safe and environmentally friendly solvent in microwave-assisted extraction (MAE) for PCB and CBz analyses. MAE is compared with traditional Soxhlet extraction (SE) to determine the extraction efficiencies. The evaluation of extraction efficiencies shows that MAE has a high extraction efficiency compared with that of SE when water content is lower than 60%. Furthermore, the extraction time and organic solvent consumption are reduced with MAE compared with SE.

  11. Microwave-assisted synthesis of 3,5-disubstituted isoxazoles and evaluation of their anti-ageing activity.

    PubMed

    Koufaki, Maria; Fotopoulou, Theano; Kapetanou, Marianna; Heropoulos, Georgios A; Gonos, Efstathios S; Chondrogianni, Niki

    2014-08-18

    One-pot uncatalysed microwave-assisted 1,3-dipolar cycloaddition reactions between in situ generated nitrile oxides and alkynes bearing protected antioxidant substituents, were regioselectively afforded 3,5-disubstituted isoxazoles. The yields were moderate, based on the starting aldehydes, while the reaction times were in general shorter than those reported in the literature. The cytoprotective and anti-ageing effect of the final deprotected compounds was evaluated in vitro, on cellular survival following oxidative challenge and in vivo, on organismal longevity using the nematode Caenorhabditis elegans. The activity of the isoxazole analogues depends on the nature and the number of the antioxidant substituents. Analogue 17 bearing a phenolic group and a 6-OH-chroman group is a promising anti-ageing agent, since it increased survival of human primary fibroblasts following treatment with H2O2 and extended C. elegans lifespan.

  12. Microwave assisted synthesis of porous ZnO/SnS heterojunction and its application in visible light degradation of ciprofloxacin

    NASA Astrophysics Data System (ADS)

    Makama, A. B.; Salmiaton, A.; Saion, E. B.; Choong, T. S. Y.; Abdullah, N.

    2016-07-01

    Porous ZnO/SnS heterojunctions were successfully synthesized via microwave-assisted heating of aqueous solutions containing different amounts of SnS precursors (SnCl2 and Na2S) in the presence of fixed amount of ZnCO3 nanoparticles. The experimental results revealed that the heterojunctions exhibited much higher visible light-driven photocatalytic activity for the degradation of the ciprofloxacin than pure SnS nanocrystals. The photocatalytic degradation efficiency (1-Ct/C0) of the pollutant for the most active heterogeneous nanostructure is about four times more efficient than pure SnS. The enhanced photocatalytic efficiency is ascribed to the synergic effect of high photon absorption and reduction in the recombination of electrons and holes because of efficient separation and electron transfer from the SnS to ZnO nanoparticles.

  13. Microwave-assisted synthesis of novel 2H-chromene derivatives bearing phenylthiazolidinones and their biological activity assessment.

    PubMed

    El Azab, Islam H; Youssef, Mohamed M; Amin, Mahmoud A

    2014-11-26

    6-Hydroxy-2-oxo-2H-chromene-4-carbaldehyde (2), 6-chloro-2-oxo-2H-chromene-4-carbaldehyde (3) and 6-hydrazinyl-4-methyl-2H-chromen-2-one (5) were prepared as single-pharmacophore motif key intermediates. Compounds 2, 3 and 5 were incorporated in a series of multicomponent reactions (MCRs), under microwave assistance as well as conventional chemical synthesis processes, to afford a series of three and/or four-pharmacophoric-motif conjugates 8a,b, 11, 13, 16, 17, 19 and 20 in good yields. The newly synthesized compounds were characterized by IR, NMR, 13C-NMR, MS and elemental analyses. Finally the synthesized compounds have been screened for their biological activity whereupon they exhibited remarkable antimicrobial activity on different classes of bacteria and the fungus.

  14. Comparison of microwave-assisted hydrodistillation withthe traditional hydrodistillation method in the extractionof essential oils from Thymus vulgaris L.

    PubMed

    Golmakani, Mohammad-Taghi; Rezaei, Karamatollah

    2008-08-15

    Microwave-assisted hydrodistillation (MAHD) is an advanced hydrodistillation (HD) technique utilizing a microwave oven in the extraction process. MAHD of essential oils from the aerial parts (tops) of Thymus vulgaris L. (common thyme) was studied and the results were compared with those of the conventional HD in terms of extraction time, extraction yield/efficiency, chemical composition, quality of the essential oils and cost of the operation. MAHD was superior in terms of saving energy and extraction time (75min, compared to 4h in HD). Scanning electron microscopy (SEM) of thyme leaves undergone HD and MAHD provided evidences as to a sudden rupture of essential oil glands with MAHD. Gas chromatography-mass spectrometry analysis of the extracted essential oils indicated that the use of microwave irradiation did not adversely influence the composition of the essential oils. MAHD was found to be a green technology. Copyright © 2008 Elsevier Ltd. All rights reserved.

  15. Visible light-induced photocatalytic activity of Bi2O3 prepared via microwave-assisted method.

    PubMed

    Liu, Xinjuan; Pan, Likun; Li, Jinliang; Yu, Kai; Sun, Zhuo

    2013-07-01

    Bi2O3 was successfully synthesized via microwave-assisted reaction of Bi2O3 precursor in aqueous solution using a microwave system. Their morphologies, structures and photocatalytic performances in the degradation of methylene blue (MB) were characterized by scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction spectroscopy, photoluminescence spectroscopy and UV-vis absorption spectroscopy, respectively. The results show that Bi2O3 synthesized at pH value of 7 exhibits an optimal photocatalytic performance with the MB degradation rate of 76% at 240 min under visible light irradiation due to its higher visible light absorption and comparatively low electron-hole pair recombination.

  16. Microwave assisted combustion synthesis of nanocrystalline CoFe{sub 2}O{sub 4} for LPG sensing

    SciTech Connect

    Chaudhari, Prashant; Acharya, S. A. Darunkar, S. S.; Gaikwad, V. M.

    2015-08-28

    A microwave-assisted citrate precursor method has been utilized for synthesis of nanocrystalline powders of CoFe{sub 2}O{sub 4}. The process takes only a few minutes to obtain as-synthesized CoFe{sub 2}O{sub 4}. Structural properties of the synthesized material were investigated by X-ray diffraction; scanning electron microscopy, Thermogravimetric analysis (TGA) and Fourier transform infrared spectroscopy. The gas sensing properties of thick film of CoFe{sub 2}O{sub 4} prepared by screen printing towards Liquid Petroleum Gas (LPG) revealed that CoFe{sub 2}O{sub 4} thick films are sensitive and shows maximum sensitivity at 350°C for 2500 ppm of LPG.

  17. Evaluation of microwave-assisted and pressurized liquid extractions to obtain β-d-glucans from mushrooms.

    PubMed

    Smiderle, Fhernanda Ribeiro; Morales, Diego; Gil-Ramírez, Alicia; de Jesus, Liana Inara; Gilbert-López, Bienvenida; Iacomini, Marcello; Soler-Rivas, Cristina

    2017-01-20

    Microwave-assisted extraction (MAE) and pressurized liquid extraction (PLE) were compared as advanced technologies to obtain polysaccharides (particularly biologically active β-glucans) from Pleurotus ostreatus and Ganoderma lucidum fruiting bodies. Extraction effectiveness was compared by a full-factorial experimental design (response surface methodology, RSM), using water as extraction solvent. Total carbohydrate content of the obtained extracts and polysaccharide yields were the variable responses investigated, while temperature and extraction time were the experimental factors. Temperature showed stronger influence in the polysaccharide extraction than time. The latter factor slightly affected MAE but not PLE extractions. Optimal conditions within the studied range were determined for each extraction method and species based on the desirability functions. Regarding the polysaccharide composition, the main differences between the species were more quantitative rather than qualitative, since NMR analyses indicated that all extracts contained mainly β- and α-glucans and heteropolysaccharides. Both extraction systems were effective for polysaccharide extraction from mushrooms.

  18. Microwave-assisted synthesis of CdO-ZnO nanocomposite and its antibacterial activity against human pathogens.

    PubMed

    Karthik, K; Dhanuskodi, S; Gobinath, C; Sivaramakrishnan, S

    2015-03-15

    CdO-ZnO nanocomposite was prepared by microwave-assisted method and characterized by X-ray crystallography (XRD), Scanning Electron Microscopy (SEM) and Fourier Transform Infrared Spectroscopy (FT-IR). It exhibits hexagonal cubic structure with an average crystallite size of 27 nm. From the UV-Vis spectra, the bandgap is estimated as 2.92 eV. The fluorescence spectrum shows a near band edge emission at 422 nm. In addition the antibacterial activity of CdO-ZnO nanocomposite was carried out in-vitro against two kinds of bacteria: gram negative bacteria (G -ve) i.e. Escherichia coli, Pseudomonas aeruginosa, Klebsiella pneumoniae and gram positive bacteria (G +ve): Staphylococcus aureus, Proteus vulgaris and Bacillus spp. This study indicates the zone of inhibition of 40 mm has high antibacterial activity towards the gram positive bacterium S. aureus.

  19. Microwave-assisted synthesis and characterization of optically active poly (ester-imide)s incorporating L-alanine.

    PubMed

    Zahmatkesh, Saeed; Hajipour, Abdol R

    2010-04-01

    Pyromellitic dianhydride (1) was reacted with L-alanine (2) to result [N,N'-(pyromellitoyl)-bis-L-alanine diacid] (3). This compound (3) was converted to N,N'-(pyromellitoyl)-bis-L-alanine diacyl chloride (4) by reaction with thionyl chloride. The microwave-assisted polycondensation of this diacyl chloride (4) with polyethyleneglycol-diol (PEG-200) and/or three synthetic aromatic diols furnish a series of new PEIs and Co-PEIs in a laboratory microwave oven (Milestone). The resulting polymers and copolymers have inherent viscosities in the range of 0.31-0.53 dl g(-1). These polymers are optically active, thermally stable and soluble in polar aprotic solvents such as DMF, DMSO, NMP, DMAc, and sulfuric acid. All of the above polymers were fully characterized by IR spectroscopy, (1)H NMR spectroscopy, elemental analyses, specific rotation and thermal analyses. Some structural characterizations and physical properties of these optically active PEIs and Co-PEIs have been reported.

  20. Microwave-assisted synthesis of CdO-ZnO nanocomposite and its antibacterial activity against human pathogens

    NASA Astrophysics Data System (ADS)

    Karthik, K.; Dhanuskodi, S.; Gobinath, C.; Sivaramakrishnan, S.

    2015-03-01

    CdO-ZnO nanocomposite was prepared by microwave-assisted method and characterized by X-ray crystallography (XRD), Scanning Electron Microscopy (SEM) and Fourier Transform Infrared Spectroscopy (FT-IR). It exhibits hexagonal cubic structure with an average crystallite size of 27 nm. From the UV-Vis spectra, the bandgap is estimated as 2.92 eV. The fluorescence spectrum shows a near band edge emission at 422 nm. In addition the antibacterial activity of CdO-ZnO nanocomposite was carried out in-vitro against two kinds of bacteria: gram negative bacteria (G -ve) i.e. Escherichia coli, Pseudomonas aeruginosa, Klebsiella pneumoniae and gram positive bacteria (G +ve): Staphylococcus aureus, Proteus vulgaris and Bacillus spp. This study indicates the zone of inhibition of 40 mm has high antibacterial activity towards the gram positive bacterium S. aureus.