Sample records for microwave-assisted polyol process

  1. Effect of lignin derivatives in the bio-polyols from microwave liquefied bamboo on the properties of polyurethane foams

    Treesearch

    Jiulong Xie; Jinqiu Qi; Chung-Yun Hse; Todd F. Shupe

    2014-01-01

    Bamboo residues were subjected to a microwave-assisted liquefaction process for the production of crude bio-polyols (CBP). The fractionated bio-polyols (FBP) were obtained by the removal of lignin derivatives from the crude bio-polyols (CBP) using a simple method. Polyurethane (PU) foams were successfully prepared from both CBP and FBP. The object of this study was to...

  2. 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 ( M W ) 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.

  3. 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

  4. The influences of microwave irradiation and polyol precursor pH on Cu/AC catalyst and its CO oxidation performance

    NASA Astrophysics Data System (ADS)

    Chuang, Kui-Hao; Shih, Kaimin; Wey, Ming-Yen

    2012-10-01

    This study evaluated the effects of microwave irradiation parameters and the pH of the polyol precursor on the morphological features and catalytic performances of Cu/activated carbon (AC) catalysts. Experimental results of carbon monoxide (CO) oxidation indicated that the highest catalytic activity is achieved when the Cu/AC catalyst is prepared with microwave irradiation at 700 W for 60 s. Scanning electron microscopy revealed the presence of beneficial small copper aciculae on the Cu/AC catalyst under such a microwave irradiation scheme. Further investigation of operational parameters found that the performance of Cu/AC catalysts is enhanced by adopting a pH = 12 polyol precursor solution. With the observation that small cube copper ( 16 nm) aggregates form when a pH = 12 polyol precursor solution is used, this study also demonstrated the importance of controlling the morphology of metal nanoparticles on Cu/AC catalysts when using the microwave-assisted polyol method.

  5. 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.

  6. Bio-based rigid polyurethane foam from liquefied products of wood in the presence of polyhydric alcohols

    Treesearch

    Zhifeng Zheng; Hui Pan; Yuanbo Huang; Chung Y. Hse

    2011-01-01

    Rigid polyurethane foams were prepared from the liquefied wood polyols, which was obtained by the liquefaction of southern pine wood in the presence of polyhydric alcohols with sulfuric acid catalyst by using microwave-assistant as an energy source. The properties of liquefied biomass-based polyols and the rigid polyurethane foams were investigated. The results...

  7. Rapid Polyol-Assisted Microwave Synthesis of Nanocrystalline LiFePO4/C Cathode for Lithium-Ion Batteries.

    PubMed

    Paul, Baboo Joseph; Gim, Jihyeon; Baek, Sora; Kang, Jungwon; Song, Jinju; Kim, Sungjin; Kim, Jaekook

    2015-08-01

    Nanocrystalline LiFePO4/C has been synthesized under a very short period of time (90 sec) using a polyol-assisted microwave heating synthesis technique. The X-ray diffraction (XRD) data indicates that the rapidly synthesized materials correspond to phase pure olivine. Post-annealing of the as-prepared sample at 600 °C in argon atmosphere yields highly crystalline LiFePO4/C. The morphology of the samples studied using scanning electron microscopy (SEM) reveals the presence of secondary particles formed from aggregation of primary particles in the range of 30-50 nm. Transmission electron microscopy (TEM) images reveal a thin carbon layer coating on the surface of the primary particle. The charge/discharge studies indicate that the as-prepared and annealed LiFePO4/C samples delivered initial discharge capacities of 126 and 160 mA h g-1, respectively, with good capacity retentions at 0.05 mA cm-2 current densities. The post-annealing process indeed improves the crystallinity of the LiFePO4 nanocrystals, which enhances the electrode performance of LiFePO4/C.

  8. Microwave-assisted polyol synthesis and characterization of pvp-capped cds nanoparticles for the photocatalytic degradation of tartrazine

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

    Darwish, Maher, E-mail: m-darwish@razi.tums.ac.ir; Mohammadi, Ali, E-mail: alimohammadi@tums.ac.ir; Nanotechnology Research Centre, Faculty of Pharmacy, Tehran University of Medical Sciences, Tehran

    2016-02-15

    Highlights: • PVP-stabilized CdS nanoparticles have been fabricated by a polyol-microwave method. • CdS nanoparticles were characterized and the size was approximately 48 ± 10 nm. • Catalytic activity of our nanoparticles was examined for tartrazine degradation. • Remarkable results were obtained under both UV and visible light irradiations. - Abstract: Polyvinylpyrrolidone capped cadmium sulfide nanoparticles have been successfully synthesized by a facile polyol method with ethylene glycol. Microwave irradiation and calcination were used to control the size and shape of nanoparticles. Characterization with scanning electron microscopy revealed a restricted nanoparticles growth comparing with the uncapped product, hexagonal phase andmore » 48 nm average particle size were confirmed by X-ray diffraction, and finally mechanism of passivation was suggested depending on Fourier transform infrared spectra. The efficiency of nanoparticles was evaluated by the photocatalytic degradation of tartrazine in aqueous solution under UVC and visible light irradiation. Complete degradation of the dye was observed after 90 min of UVC irradiation under optimized conditions. Kinetic of reaction fitted well to the pseudo-first-order kinetic and Langmuir–Hinshelwood models. Furthermore, 85% degradation of the dye in 9 h under visible light suggests that cadmium sulfide is a promising tool to work under visible light for environmental remediation.« less

  9. Structural, chemical and optical properties of SnO2 NPs obtained by three different synthesis routes

    NASA Astrophysics Data System (ADS)

    Drzymała, Elżbieta; Gruzeł, Grzegorz; Depciuch, Joanna; Budziak, Andrzej; Kowal, Andrzej; Parlinska-Wojtan, Magdalena

    2017-08-01

    Polyol (P), chemical precipitation (C) and microwave-assisted (M) syntheses were chosen to produce SnO2 nanoparticles with uniform size and minimum agglomeration. Their structural, chemical and optical properties were investigated using dynamic light scattering (DLS), scanning transmission electron microscopy (STEM), Raman, Fourier Transform Infrared (FTIR) using the Attenuated Total Reflectance (ATR) technique and Ultraviolet-Visible (UV-Vis) spectroscopies. STEM observations showed that the SnO2(P) and SnO2(C) nanoparticles (NPs) are combined into larger agglomerates with heterogeneous thickness, while the microwave-assisted NPs form a uniform thin layer across the TEM grid. The strongest agglomeration of the SnO2(C) NPs, observed by DLS, STEM and UV-Vis is explained by the very moderate amount of water present on the surface of the NPs identified by FTIR spectroscopy. High resolution STEM combined with SAED and X-ray diffraction (XRD) patterns confirmed the crystalline character of the NPs. In the nanoparticles from polyol synthesis, chlorine from the remains of metal precursors during reduction was detected by energy dispersive spectroscopy (EDS), contrary to the NPs obtained by the chemical precipitation and microwave-assisted methods. All three syntheses routes lead to small, 2-10 nm SnO2 NPs, which were the result of the low concentration of Cl ions in the solutions.

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

    Hachtel, J. A.; Yu, S.; Lupini, A. R.

    The combination of iron oxide and gold in a single nanoparticle results in both magnetic and plasmonic properties that can stimulate novel applications in bio-sensing, medical imaging, or therapeutics. Microwave assisted heating allows the fabrication of multi-component, multi-functional nanostructures by promoting selective heating at desired sites. Recently, we reported a microwave-assisted polyol route yielding gold nanotriangles decorated with iron oxide nanoparticles. Here, we present an in-depth microstructural and compositional characterization of the system by using scanning transmission electron microscopy (STEM) and electron energy loss (EELS) spectroscopy. A method to remove the iron oxide nanoparticles from the gold nanocrystals and somemore » insights on crystal nucleation and growth mechanisms are also provided.« less

  11. Gold nanotriangles decorated with superparamagnetic iron oxide nanoparticles: a compositional and microstructural study

    DOE PAGES

    Hachtel, J. A.; Yu, S.; Lupini, A. R.; ...

    2016-03-11

    The combination of iron oxide and gold in a single nanoparticle results in both magnetic and plasmonic properties that can stimulate novel applications in bio-sensing, medical imaging, or therapeutics. Microwave assisted heating allows the fabrication of multi-component, multi-functional nanostructures by promoting selective heating at desired sites. Recently, we reported a microwave-assisted polyol route yielding gold nanotriangles decorated with iron oxide nanoparticles. Here, we present an in-depth microstructural and compositional characterization of the system by using scanning transmission electron microscopy (STEM) and electron energy loss (EELS) spectroscopy. A method to remove the iron oxide nanoparticles from the gold nanocrystals and somemore » insights on crystal nucleation and growth mechanisms are also provided.« less

  12. Ultrafast synthesis and characterization of carbonated hydroxyapatite nanopowders via sonochemistry-assisted microwave process.

    PubMed

    Zou, Zhaoyong; Lin, Kaili; Chen, Lei; Chang, Jiang

    2012-11-01

    Herein, carbonated hydroxyapatite (CHAp) nanopowders were synthesized via sonochemistry-assisted microwave process. The influences of microwave and ultrasonic irradiation on the crystallinity, morphology, yield, Ca/P molar ratio, specific surface area and dispersibility were investigated and compared with the conventional precipitation method. The results showed that sonochemistry-assisted microwave process significantly increased the synthetic efficiency. The well-crystallized nanopowders could be obtained at high yield of 98.8% in ultra-short-period of 5min. In addition, the crystallization process was promoted with the increase of ultrasonic and microwave power and the reaction time during the sonochemistry-assisted microwave process. The sonochemistry assistance also remarkably increased the specific surface area and dispersibility of the as-obtained products. These results suggest that the sonochemistry-assisted microwave process is an effective approach to synthesize CHAp with high efficiency. Copyright © 2012 Elsevier B.V. All rights reserved.

  13. Polyols from microwave liquefied bagasse and its application to rigid polyurethane foam

    Treesearch

    Jiulong Xie; Xianglin Zhai; Chung Hse; Todd Shupe; Hui Pan

    2015-01-01

    Bagasse flour (BF) was liquefied using bi-component polyhydric alcohol (PA) as a solventand phosphoric acid as a catalyst in a microwave reactor. The effect of BF to solvent ratio andreaction temperatures on the liquefaction extent and characteristics of liquefied products wereevaluated. The results revealed that almost 75% of the...

  14. Citric acid functionalized carbon materials for fuel cell applications

    NASA Astrophysics Data System (ADS)

    Poh, Chee Kok; Lim, San Hua; Pan, Hui; Lin, Jianyi; Lee, Jim Yang

    Carbon materials can be easily functionalized using citric acid (CA) treatment. The CA modification of carbon materials is both simple and effective. It requires no prolonged heating, filtration and washing, and produces more functional groups such as carboxyl and hydroxide on CA-modified carbon nanotubes and XC72 carbon blacks than on HNO 3-H 2SO 4 oxidized carbon nanotubes and as-purchased XC72. Platinum nanoparticles are deposited on these functionalized carbon materials by means of a microwave-assisted polyol process. The investigations using TEM, XRD, FTIR and TGA indicate that CA modification creates more functional groups and thus deposits more Pt nanoparticles with smaller average particle size on the surface of carbon materials. Electrochemical studies of the Pt/C samples for methanol oxidation reveal higher activity for Pt on CA-modified carbon materials. It is therefore considered that this method can find important applications in reducing the cost and improving performance of proton-exchange membrane fuel cells.

  15. Fast and Simple Microwave Synthesis of TiO2/Au Nanoparticles for Gas-Phase Photocatalytic Hydrogen Generation.

    PubMed

    May-Masnou, Anna; Soler, Lluís; Torras, Miquel; Salles, Pol; Llorca, Jordi; Roig, Anna

    2018-01-01

    The fabrication of small anatase titanium dioxide (TiO 2 ) nanoparticles (NPs) attached to larger anisotropic gold (Au) morphologies by a very fast and simple two-step microwave-assisted synthesis is presented. The TiO 2 /Au NPs are synthesized using polyvinylpyrrolidone (PVP) as reducing, capping and stabilizing agent through a polyol approach. To optimize the contact between the titania and the gold and facilitate electron transfer, the PVP is removed by calcination at mild temperatures. The nanocatalysts activity is then evaluated in the photocatalytic production of hydrogen from water/ethanol mixtures in gas-phase at ambient temperature. A maximum value of 5.3 mmol·[Formula: see text]h -1 (7.4 mmol·[Formula: see text]h -1 ) of hydrogen is recorded for the system with larger gold particles at an optimum calcination temperature of 450°C. Herein we demonstrate that TiO 2 -based photocatalysts with high Au loading and large Au particle size (≈50 nm) NPs have photocatalytic activity.

  16. 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.

  17. Continuous monitoring of the progressive degradation of a liquid composite by means of a noninvasive microwave resonator

    NASA Astrophysics Data System (ADS)

    Catala-Civera, Jose M.; Canos-Marin, Antoni J.; de los Reyes, E.

    2000-07-01

    Microwave control capabilities have been used to monitor the degradation of polyol, an alcohol composite material commonly used in the footwear industry for polymerization purposes. The liquid flows continuously inside a thin pipe and its desirable properties are altered with time associated to moisture absorption processes. Consequently, variations in the dielectric properties are involved, and they can be detected by permittivity measurements. In this paper, in order to obtain high sensitivity and resolution, a rectangular cavity resonator working at a fixed frequency was designed using as sample holder a rectangular pipe containing the liquid going through. Changes in the liquid modify the original response of the cavity with a non- degraded liquid and these differences have been used to determine the degree of degradation of the material. The final response of the microwave resonator was experimentally validated with measurements in a continuous line.

  18. Soy-based polyols

    DOEpatents

    Suppes, Galen; Lozada, Zueica; Lubguban, Arnold

    2013-06-25

    The invention provides processes for preparing soy-based oligomeric polyols or substituted oligomeric polyols, as well as urethane bioelasteromers comprising the oligomeric polyols or substituted oligomeric polyols.

  19. Fast and simple microwave synthesis of TiO2/Au nanoparticles for gas-phase photocatalytic hydrogen generation

    NASA Astrophysics Data System (ADS)

    May-Masnou, Anna; Soler, Lluís; Torras, Miquel; Salles, Pol; Llorca, Jordi; Roig, Anna

    2018-04-01

    The fabrication of small anatase titanium dioxide (TiO2) nanoparticles (NPs) attached to larger anisotropic gold (Au) morphologies by a very fast and simple two-step microwave-assisted synthesis is presented. The TiO2/Au NPs are synthesized using polyvinylpyrrolidone (PVP) as reducing, capping and stabilizing agent through a polyol approach. To optimize the contact between the titania and the gold and facilitate electron transfer, the PVP is removed by calcination at mild temperatures. The nanocatalysts activity is then evaluated in the photocatalytic production of hydrogen from water/ethanol mixtures in gas-phase at ambient temperature. A maximum value of 5.3 mmol·gcat-1·h-1 (7.4 mmol·gTiO2-1·h-1) of hydrogen is recorded for the system with larger gold particles at an optimum calcination temperature of 450 °C. Herein we demonstrate that TiO2-based photocatalysts with high Au loading and large Au particle size (≈ 50 nm) NPs have photocatalytic activity.

  20. Water-based binary polyol process for the controllable synthesis of silver nanoparticles inhibiting human and foodborne pathogenic bacteria

    USDA-ARS?s Scientific Manuscript database

    The polyol process is a widely used strategy for producing nanoparticles from various reducible metallic precursors; however it requires a bulk polyol liquid reaction with additional protective agents at high temperatures. Here, we report a water-based binary polyol process using low concentrations ...

  1. Changes in non-volatile taste components of button mushroom (Agaricus bisporus) during different stages of freeze drying and freeze drying combined with microwave vacuum drying.

    PubMed

    Pei, Fei; Shi, Ying; Gao, Xingyang; Wu, Fangning; Mariga, Alfred Mugambi; Yang, Wenjian; Zhao, Liyan; An, Xinxin; Xin, Zhihong; Yang, Fangmei; Hu, Qiuhui

    2014-12-15

    Button mushroom slices were dehydrated using freeze drying (FD) or FD combined with microwave vacuum drying (FMVD), and the non-volatile component profiles were studied. The results showed that the level of non-volatile components in button mushroom firstly increased during sublimation of FD/FMVD process and then fell during desorption in FD process and MVD in FMVD process. Compared to FD products, the contents of soluble sugars and polyols in FMVD products were relatively low, whereas the contents of total free amino acids were significantly higher, close to the level of fresh mushroom. However, there was no significant difference in the contents of 5'-nucleotides and organic acids between FD and FMVD products. The equivalent umami concentration (EUC) values for FD and FMVD products did not differ from fresh, indicating that both drying methods could effectively preserve MSG (monosodium glutamate)-like components in button mushroom. Copyright © 2014 Elsevier Ltd. All rights reserved.

  2. Production of xylooligosaccharide from wheat bran by microwave assisted enzymatic hydrolysis.

    PubMed

    Wang, Tseng-Hsing; Lu, Shin

    2013-06-01

    The effective production of xylooligosaccharides (XOS) from wheat bran was investigated. Wheat bran contains rich hemicellulose which can be hydrolyzed by enzyme; the XOS were obtained by microwave assisted enzymatic hydrolysis. To improve the productivity of XOS, repeated microwave assisted enzymatic hydrolysis and activated carbon adsorption method was chosen to eliminate macromolecules in the XOS. On the basis of experimental data, an industrial XOS production process consisting of pretreatment, repeated microwave assisted enzymatic treatment and purification was designed. Using the designed process, 3.2g dry of purified XOS was produced from 50 g dry wheat bran powder. Copyright © 2012 Elsevier Ltd. All rights reserved.

  3. 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 spark technology will benefit from predictive models which include the plasma processes governing the observed combustion enhancement. This dissertation documents the development of a chemical kinetic mechanism for the plasma-assisted combustion processes relevant to microwave-assisted spark ignition. The mechanism includes an existing mechanism for gas-phase methane oxidation, supplemented with electron impact reactions, cation and anion chemical reactions, and reactions involving vibrationally-excited and electronically-excited species. Calculations using the presently-developed numerical model explain experimentally-observed trends, highlighting the relative importance of pressure, temperature, and mixture composition in determining the effectiveness of microwave-assisted ignition enhancement.

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

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

    Rao, Siddharth; Subhra Mukherjee, Sankha; Elyasi, Mehrdad

    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.

  5. Production of low-cost polyesters by microwaving heating of carboxylic acids and polyol blends

    USDA-ARS?s Scientific Manuscript database

    Numerous issues such as price uncertainty, manufacturing costs, environmental disposal, and geo-political issues affect the petroleum-based polymer industry. As an alternative, increasing interest in the development of biodegradable non-petroleum-based polymers has risen steadily since the 1980s. Ho...

  6. An efficient microwave-assisted synthesis method for the production of water soluble amine-terminated Si nanoparticles.

    PubMed

    Atkins, Tonya M; Louie, Angelique Y; Kauzlarich, Susan M

    2012-07-27

    Silicon nanoparticles can be considered a green material, especially when prepared via a microwave-assisted method without the use of highly reactive reducing agents or hydrofluoric acid. A simple solution synthesis of hydrogen-terminated Si- and Mn-doped Si nanoparticles via microwave-assisted synthesis is demonstrated. The reaction of the Zintl salt, Na(4)Si(4), or Mn-doped Na(4)Si(4), Na(4)Si(4(Mn)), with ammonium bromide, NH(4)Br, produces small dispersible nanoparticles along with larger particles that precipitate. Allylamine and 1-amino-10-undecene were reacted with the hydrogen-terminated Si nanoparticles to provide water solubility and stability. A one-pot, single-reaction process and a one-pot, two-step reaction process were investigated. Details of the microwave-assisted process are provided, with the optimal synthesis being the one-pot, two-step reaction procedure and a total time of about 15 min. The nanoparticles were characterized by transmission electron microscopy (TEM), x-ray diffraction, and fluorescence spectroscopies. The microwave-assisted method reliably produces a narrow size distribution of Si nanoparticles in solution.

  7. Plasma-assisted microwave processing of materials

    NASA Technical Reports Server (NTRS)

    Barmatz, Martin (Inventor); Jackson, Henry (Inventor); Ylin, Tzu-yuan (Inventor)

    1998-01-01

    A microwave plasma assisted method and system for heating and joining materials. The invention uses a microwave induced plasma to controllably preheat workpiece materials that are poorly microwave absorbing. The plasma preheats the workpiece to a temperature that improves the materials' ability to absorb microwave energy. The plasma is extinguished and microwave energy is able to volumetrically heat the workpiece. Localized heating of good microwave absorbing materials is done by shielding certain parts of the workpiece and igniting the plasma in the areas not shielded. Microwave induced plasma is also used to induce self-propagating high temperature synthesis (SHS) process for the joining of materials. Preferably, a microwave induced plasma preheats the material and then microwave energy ignites the center of the material, thereby causing a high temperature spherical wave front from the center outward.

  8. Process characteristics for microwave assisted hydrothermal carbonization of cellulose.

    PubMed

    Zhang, Junting; An, Ying; Borrion, Aiduan; He, Wenzhi; Wang, Nan; Chen, Yirong; Li, Guangming

    2018-07-01

    The process characteristics of microwave assisted hydrothermal carbonization of cellulose was investigated and a first order kinetics model based on carbon concentration was developed. Chemical properties analysis showed that comparing to conventional hydrothermal carbonization, hydrochar with comparable energy properties can be obtained with 5-10 times decrease in reaction time with assistance of microwave heating. Results from kinetics study was in great agreement with experimental analysis, that they both illustrated the predominant mechanism of the reaction depend on variations in the reaction rates of two co-existent pathways. Particularly, the pyrolysis-like intramolecular dehydration reaction was proved to be the predominant mechanism for hydrochar generation under high temperatures. Finally, the enhancement effects of microwave heating were reflected under both soluble and solid pathways in this research, suggesting microwave-assisted hydrothermal carbonization as a more attracting method for carbon-enriched hydrochar recovery. Copyright © 2018 Elsevier Ltd. All rights reserved.

  9. Process development of short-chain polyols synthesis from corn stover by combination of enzymatic hydrolysis and catalytic hydrogenolysis.

    PubMed

    Fang, Zhen-Hong; Zhang, Jian; Lu, Qi-Ming; Bao, Jie

    2014-09-01

    Currently short-chain polyols such as ethanediol, propanediol, and butanediol are produced either from the petroleum feedstock or from the starch-based food crop feedstock. In this study, a combinational process of enzymatic hydrolysis with catalytic hydrogenolysis for short-chain polyols production using corn stover as feedstock was developed. The enzymatic hydrolysis of the pretreated corn stover was optimized to produce stover sugars at the minimum cost. Then the stover sugars were purified and hydrogenolyzed into polyols products catalyzed by Raney nickel catalyst. The results show that the yield of short-chain polyols from the stover sugars was comparable to that of the corn-based glucose. The present study provided an important prototype for polyols production from lignocellulose to replace the petroleum- or corn-based polyols for future industrial applications.

  10. Preparation and characterization of Pt/C and Pt sbnd Ru/C electrocatalysts for direct ethanol fuel cells

    NASA Astrophysics Data System (ADS)

    Liu, Zhaolin; Ling, Xing Yi; Su, Xiaodi; Lee, Jim Yang; Gan, Leong Ming

    Nano-sized Pt and Pt sbnd Ru colloids are prepared by a microwave-assisted polyol process, and transferred to a toluene solution of decanthiol. Vulcan XC-72 is then added to the toluene solution to adsorb the thiolated Pt and Pt sbnd Ru colloids. Transmission electron microscopy examinations show nearly spherical particles and narrow size distributions for both supported and unsupported metals. The carbon-supported Pt and Pt sbnd Ru nanoparticles are activated by thermal treatment to remove the thiol stabilizing shell. All Pt and Pt sbnd Ru catalysts (except Pt 23sbnd Ru 77) give the X-ray diffraction pattern of a face-centered cubic (fcc) crystal structure, whereas the Pt 23sbnd Ru 77 alloy is more typical of the hexagonal close packed (hcp) structure. The electro-oxidation of liquid ethanol on these catalysts is investigated at room temperature by cyclic voltammetry. The results demonstrate that the alloy catalyst is catalytically more active than pure platinum. Preliminary tests on a single cell of a direct ethanol fuel cell (DEFC) indicate that a Pt 52sbnd Ru 48/C anode catalyst gives the best electrocatalytic performance among all the carbon-supported Pt and Pt sbnd Ru catalysts.

  11. Gold nanoparticle decorated multi-walled carbon nanotubes as counter electrode for dye sensitized solar cells.

    PubMed

    Kaniyoor, Adarsh; Ramaprabhu, Sundara

    2012-11-01

    A novel counter electrode material for dye sensitized solar cells (DSSCs) composed of nanostructured Au particles decorated on functionalized multi-walled carbon nanotubes (f-MWNTs) is demonstrated for the first time. MWNTs synthesized by catalytic chemical vapor deposition technique are purified and functionalized by treating with concentrated acids. Au nanoparticles are decorated on f-MWNTs by a rapid and facile microwave assisted polyol reduction method. The materials are characterized by X-ray diffractometry, Fourier transform infra red spectroscopy and electron microscopy. The DSSC fabricated with Au/f-MWNTs based counter electrode shows enhanced power conversion efficiency (eta) of 4.9% under AM 1.5G simulated solar radiation. In comparison, the reference DSSCs fabricated with f-MWNTs and Pt counter electrodes show eta of 2.1% and 4.5%. This high performance of Au/f-MWNTs counter electrode is investigated using electrochemical impedance spectroscopy and cyclic voltammetry studies.

  12. 40 CFR 63.1425 - Process vent control requirements.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... Standards for Hazardous Air Pollutant Emissions for Polyether Polyols Production § 63.1425 Process vent... operators of all affected sources using epoxides in the production of polyether polyols are subject to the... (c) of this section only if epoxides are used in the production of polyether polyols and nonepoxide...

  13. Magnetic carbon nanostructures: microwave energy-assisted pyrolysis vs. conventional pyrolysis.

    PubMed

    Zhu, Jiahua; Pallavkar, Sameer; Chen, Minjiao; Yerra, Narendranath; Luo, Zhiping; Colorado, Henry A; Lin, Hongfei; Haldolaarachchige, Neel; Khasanov, Airat; Ho, Thomas C; Young, David P; Wei, Suying; Guo, Zhanhu

    2013-01-11

    Magnetic carbon nanostructures from microwave assisted- and conventional-pyrolysis processes are compared. Unlike graphitized carbon shells from conventional heating, different carbon shell morphologies including nanotubes, nanoflakes and amorphous carbon were observed. Crystalline iron and cementite were observed in the magnetic core, different from a single cementite phase from the conventional process.

  14. 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...

  15. 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.

  16. Rigid Polyurethane Foams from Lignin Based-Polyols

    NASA Astrophysics Data System (ADS)

    Cateto, Carolina; Barreiro, Filomena; Rodrigues, Alírio; Belgacem, Naceur

    2008-08-01

    Rigid polyurethane (RPU) foams were synthesized using lignin-based polyols obtained by an oxypropylation process. Alcell, Indulin AT, Curan 27-11P and Sarkanda lignins have been oxypropylated using formulations deduced from an optimization study with Alcell. L/PO/C (ratio between lignin, PO and catalyst content) of 30/70/2 and 20/80/5 were used to obtain the desired polyols. The resulting RPU foams were characterized in terms of density, mechanical properties, conductivity and morphology. All Sarkanda lignin based polyols and the 30/70/2 Curan 27-11P polyol were found inadequate for RPU formulations. Alcell and Indulin AT based polyols and the 20/80/5 Curan 27-11P polyol resulted in RPU foams with properties very similar to those obtained from conventional commercial polyols. RPU foams produced with the 30/70/2 Alcell and the 30/70/2 Indulin AT polyols exhibited improved properties compared with those from 20/80/5 based formulations.

  17. Catalysts and process for hydrogenolysis of sugar alcohols to polyols

    DOEpatents

    Chopade, Shubham P [East Lansing, MI; Miller, Dennis J [Okemos, MI; Jackson, James E [Haslett, MI; Werpy, Todd A [West Richland, WA; Frye, Jr., John G [Richland, WA; Zacher, Alan H [Richland, WA

    2001-09-18

    The present invention provides a process for preparation of low molecular weight polyols from high molecular weight polyols in a hydrogenolysis reaction under elevated temperature and hydrogen pressure. The process comprises providing in a reaction mixture the polyols, a base, and a metal catalyst prepared by depositing a transition metal salt on an inert support, reducing the metal salt to the metal with hydrogen, and passivating the metal with oxygen, and wherein the catalyst is reduced with hydrogen prior to the reaction. In particular, the process provides for the preparation of glycerol, propylene glycol, and ethylene glycol from sugar alcohols such as sorbitol or xylitol. In a preferred process, the metal catalyst comprises ruthenium which is deposited on an alumina, titania, or carbon support, and the dispersion of the ruthenium on the support increases during the hydrogenolysis reaction.

  18. Gram-level synthesis of core-shell structured catalysts for the oxygen reduction reaction in proton exchange membrane fuel cells

    NASA Astrophysics Data System (ADS)

    Luo, Mingchuan; Wei, Lingli; Wang, Fanghui; Han, Kefei; Zhu, Hong

    2014-12-01

    Over the past decade, Pt based core-shell structured alloys have been studied extensively as oxygen reduction reaction (ORR) catalysts for proton exchange membrane fuel cells (PEMFCs) because of their distinctive electrochemical performance and low Pt loading. In this paper, a facile route based on microwave-assisted polyol method and chemical dealloying process is proposed to synthesize carbon supported core-shell structured nanoparticles (NPs) in gram-level for ORR electrocatalysis in PEMFCs. The obtained samples are characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDX), inductively coupled plasma atomic emission spectroscopy (ICP-AES), and X-ray photoelectron spectroscopy (XPS). These physical characterization indicate that the final synthesized NPs are highly dispersed on the carbon support, and in a core-shell structure with CuPt alloy as the core and Pt as the shell. Electrochemical measurements, conducted by cyclic voltammetry (CV) and rotating disk electrode (RDE) tests, show the core-shell structured catalyst exhibit a 3× increase in mass activity and a 2× increase in specific activity over the commercial Pt/C catalyst, respectively. These results demonstrate that this route can be a reliable way to synthesize low-Pt catalyst in large-scale for PEMFCs.

  19. Synthesis of hexagonal wurtzite Cu{sub 2}ZnSnS{sub 4} prisms by an ultrasound-assisted microwave solvothermal method

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

    Long, Fei, E-mail: long.drf@gmail.com; Chi, Shangsen; Institute of Advanced Materials and Technology, University of Science and Technology Beijing, Beijing 100083

    Wurtzite Cu{sub 2}ZnSnS{sub 4} (CZTS) hexagonal prisms were synthesized by a simple ultrasound-microwave solvothermal method. The product was characterized by XRD, FESEM, EDS, TEM, Raman and UV–vis spectrometer. The hexagonal prisms were 0.5–2 μm wide and 5–12 μm long. The PVP played an important role in the formation of the CZTS hexagonal prisms. In addition, the ultrasound-assisted microwave process was helpful for synthesis of wurtzite rather than kesterite phase CZTS. A nucleation–dissolution–recrystallization mechanism was also proposed to explain the growth of the CZTS hexagonal prisms. - Graphical abstract: Wurtzite Cu{sub 2}ZnSnS{sub 4} hexagonal prisms were synthesized by ultrasound-microwave solvothermal method.more » The ultrasound-assisted microwave process and PVP were useful to the growth of CZTS. A nucleation–dissolution–recrystallization growth mechanism was also proposed. - Highlights: • Wurtzite Cu{sub 2}ZnSnS{sub 4} was prepared by ultrasound-assisted microwave solvothermal method. • The wurtzite CZTS hexagonal prisms are demonstrated a band gap of 1.49 eV. • Synergistic effect of ultrasound and microwave is helpful to prepare Wurtzite CZTS. • PVP plays an important role in the formation of the CZTS hexagonal prisms. • Nucleation–dissolution–recrystallization growth mechanism of the CZTS was proposed.« less

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

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

    Li, Shan; Jiangsu Key Laboratory of Advanced Catalytic Materials and Technology, Changzhou University, Changzhou 213164; Wang, Fei

    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 evaporationmore » 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.« less

  1. Catalytic activity of CuOn-La2O3/gamma-Al2O3 for microwave assisted ClO2 catalytic oxidation of phenol wastewater.

    PubMed

    Bi, Xiaoyi; Wang, Peng; Jiang, Hong

    2008-06-15

    In order to develop a catalyst with high activity and stability for microwave assisted ClO2 catalytic oxidation, we prepared CuOn-La2O3/gamma-Al2O3 by impregnation-deposition method, and determined its properties using BET, XRF, XPS and chemical analysis techniques. The test results show that, better thermal ability of gamma-Al2O3 and high loading of Cu in the catalyst can be achieved by adding La2O3. The microwave assisted ClO2 catalytic oxidation process with CuOn-La2O3/gamma-Al2O3 used as catalyst was also investigated, and the results show that the catalyst has an excellent catalytic activity in treating synthetic wastewater containing 100 mg/L phenol, and 91.66% of phenol and 50.35% of total organic carbon (TOC) can be removed under the optimum process conditions. Compared with no catalyst process, CuOn-La2O3/gamma-Al2O3 can effectively degrade contaminants in short reaction time and with low oxidant dosage, extensive pH range. The comparison of phenol removal efficiency in the different process indicates that microwave irradiation and catalyst work together to oxidize phenol effectively. It can therefore be concluded from results and discussion that CuOn-La2O3/gamma-Al2O3 is a suitable catalyst in microwave assisted ClO2 catalytic oxidation process.

  2. 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...

  3. Microwave-Assisted Synthesis of a MK2 Inhibitor by Suzuki-Miyaura Coupling for Study in Werner Syndrome Cells.

    PubMed

    Bagley, Mark C; Baashen, Mohammed; Chuckowree, Irina; Dwyer, Jessica E; Kipling, David; Davis, Terence

    2015-06-03

    Microwave-assisted Suzuki-Miyaura cross-coupling reactions have been employed towards the synthesis of three different MAPKAPK2 (MK2) inhibitors to study accelerated aging in Werner syndrome (WS) cells, including the cross-coupling of a 2-chloroquinoline with a 3-pyridinylboronic acid, the coupling of an aryl bromide with an indolylboronic acid and the reaction of a 3-amino-4-bromopyrazole with 4-carbamoylphenylboronic acid. In all of these processes, the Suzuki-Miyaura reaction was fast and relatively efficient using a palladium catalyst under microwave irradiation. The process was incorporated into a rapid 3-step microwave-assisted method for the synthesis of a MK2 inhibitor involving 3-aminopyrazole formation, pyrazole C-4 bromination using N-bromosuccinimide (NBS), and Suzuki-Miyaura cross-coupling of the pyrazolyl bromide with 4-carbamoylphenylboronic acid to give the target 4-arylpyrazole in 35% overall yield, suitable for study in WS cells.

  4. Microwave-assisted extraction of pectin from cocoa peel

    NASA Astrophysics Data System (ADS)

    Sarah, M.; Hanum, F.; Rizky, M.; Hisham, M. F.

    2018-02-01

    Pectin is a polymer of d-galacturonate acids linked by β-1,4 glycosidic bond. This study isolates pectin from cocoa peel (Theobroma cacao) using citric acid as solvent by microwave-assisted extraction method. Cocoa peels (moisture content of 10%) with citric acid solution (pH of 1.5) irradiated by microwave energy at various microwave power (180, 300, 450 and 600 W) for 10, 15, 20, 25 and 30 minutes respectively. Pectin obtained from this study was collected and filtrated by adding 96% ethanol to precipitate the pectin. The best results obtained from extraction process using microwave power of 180 Watt for 30 minutes. This combination of power and time yielded 42.3% pectin with moisture content, ash content, weight equivalent, methoxyl content and galacturonate levels were 8.08%, 5%, 833.33 mg, 6.51% and 58,08%, respectively. The result finding suggested that microwave-assisted extraction method has a great potency on the commercial pectin production.

  5. 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...

  6. 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....

  7. 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...

  8. A comparison of essential oils obtained from lavandin via different extraction processes: Ultrasound, microwave, turbohydrodistillation, steam and hydrodistillation.

    PubMed

    Périno-Issartier, Sandrine; Ginies, Christian; Cravotto, Giancarlo; Chemat, Farid

    2013-08-30

    A total of eight extraction techniques ranging from conventional methods (hydrodistillation (HD), steam distillation (SD), turbohydrodistillation (THD)), through innovative techniques (ultrasound assisted extraction (US-SD) and finishing with microwave assisted extraction techniques such as In situ microwave-generated hydrodistillation (ISMH), microwave steam distillation (MSD), microwave hydrodiffusion and gravity (MHG), and microwave steam diffusion (MSDf)) were used to extract essential oil from lavandin flowers and their results were compared. Extraction time, yield, essential oil composition and sensorial analysis were considered as the principal terms of comparison. The essential oils extracted using the more innovative processes were quantitatively (yield) and qualitatively (aromatic profile) similar to those obtained from the conventional techniques. The method which gave the best results was the microwave hydrodiffusion and gravity (MHG) method which gave reduced extraction time (30min against 220min for SD) and gave no differences in essential oil yield and sensorial perception. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. Optimisation of microwave-assisted processing in production of pineapple jam

    NASA Astrophysics Data System (ADS)

    Ismail, Nur Aisyah Mohd; Abdullah, Norazlin; Muhammad, Norhayati

    2017-10-01

    Pineapples are available all year round since they are unseasonal fruits. Due to the continuous harvesting of the fruit, the retailers and farmers had to find a solution such as the processing of pineapple into jam, to treat the unsuccessfully sold pineapples. The direct heating of pineapple puree during the production of pineapple jam can cause over degradation of quality of the fresh pineapple. Thus, this study aims to optimise the microwave-assisted processing conditions for producing pineapple jam which could reduce water activity and meets minimum requirement for pH and total soluble solids contents of fruit jam. The power and time of the microwave processing were chosen as the factors, while the water activity, pH and total soluble solids (TSS) content of the pineapple jam were determined as responses to be optimised. The microwave treatment on the pineapple jam was able to give significant effect on the water activity and TSS content of the pineapple jam. The optimum power and time for the microwave processing of pineapple jam is 800 Watt and 8 minutes, respectively. The use of domestic microwave oven for the pineapple jam production results in acceptable pineapple jam same as conventional fruit jam sold in the marketplace.

  10. Biotechnological and in situ food production of polyols by lactic acid bacteria.

    PubMed

    Ortiz, Maria Eugenia; Bleckwedel, Juliana; Raya, Raúl R; Mozzi, Fernanda

    2013-06-01

    Polyols such as mannitol, erythritol, sorbitol, and xylitol are naturally found in fruits and vegetables and are produced by certain bacteria, fungi, yeasts, and algae. These sugar alcohols are widely used in food and pharmaceutical industries and in medicine because of their interesting physicochemical properties. In the food industry, polyols are employed as natural sweeteners applicable in light and diabetic food products. In the last decade, biotechnological production of polyols by lactic acid bacteria (LAB) has been investigated as an alternative to their current industrial production. While heterofermentative LAB may naturally produce mannitol and erythritol under certain culture conditions, sorbitol and xylitol have been only synthesized through metabolic engineering processes. This review deals with the spontaneous formation of mannitol and erythritol in fermented foods and their biotechnological production by heterofermentative LAB and briefly presented the metabolic engineering processes applied for polyol formation.

  11. [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.

  12. Microwave-induced biomimetic approach for hydroxyapatite coatings of chitosan scaffolds.

    PubMed

    Kaynak Bayrak, Gökçe; Demirtaş, T Tolga; Gümüşderelioğlu, Menemşe

    2017-02-10

    Simulated body fluid (SBF) can form calcium phosphates on osteoinductive materials, so it is widely used for coating of bone scaffolds to mimic natural extracellular matrix (ECM). However, difficulties of bulk coating in 3D scaffolds and the necessity of long process times are the common problems for coating with SBF. In the present study, a microwave-assisted process was developed for rapid and internal coating of chitosan scaffolds. The scaffolds were fabricated as superporous hydrogel (SPH) by combining microwave irradiation and gas foaming methods. Then, they were immersed into 10x  SBF-like solution and homogenous bone-like hydroxyapatite (HA) coating was achieved by microwave treatment at 600W without the need of any nucleating agent. Cell culture studies with MC3T3-E1 preosteoblasts showed that microwave-assisted biomimetic HA coating process could be evaluated as an efficient and rapid method to obtain composite scaffolds for bone tissue engineering. Copyright © 2016 Elsevier Ltd. All rights reserved.

  13. Access to small size distributions of nanoparticles by microwave-assisted synthesis. Formation of Ag nanoparticles in aqueous carboxymethylcellulose solutions in batch and continuous-flow reactors

    NASA Astrophysics Data System (ADS)

    Horikoshi, Satoshi; Abe, Hideki; Torigoe, Kanjiro; Abe, Masahiko; Serpone, Nick

    2010-08-01

    This article examines the effect(s) of the 2.45-GHz microwave (MW) radiation in the synthesis of silver nanoparticles in aqueous media by reduction of the diaminesilver(i) complex, [Ag(NH3)2]+, with carboxymethylcellulose (CMC) in both batch-type and continuous-flow reactor systems with a particular emphasis on the characteristics of the microwaves in this process and the size distributions. This microwave thermally-assisted synthesis is compared to a conventional heating (CH) method, both requiring a reaction temperature of 100 °C to produce the nanoparticles, in both cases leading to the formation of silver colloids with different size distributions. Reduction of the diaminesilver(i) precursor complex, [Ag(NH3)2]+, by CMC depended on the solution temperature. Cooling the reactor during the heating process driven with 390-Watt microwaves (MW-390W/Cool protocol) yielded silver nanoparticles with sizes spanning the range 1-2 nm. By contrast, the size distribution of Ag nanoparticles with 170-Watt microwaves (no cooling; MW-170W protocol) was in the range 1.4-3.6 nm (average size ~3 nm). The overall results suggest the potential for a scale-up process in the microwave-assisted synthesis of nanoparticles. Based on the present data, a flow-through microwave reactor system is herein proposed for the continuous production of silver nanoparticles. The novel flow reactor system (flow rate, 600 mL min-1) coupled to 1200-Watt microwave radiation generated silver nanoparticles with a size distribution 0.7-2.8 nm (average size ca. 1.5 nm).

  14. Photonic crystal nanocavity assisted rejection ratio tunable notch microwave photonic filter

    PubMed Central

    Long, Yun; Xia, Jinsong; Zhang, Yong; Dong, Jianji; Wang, Jian

    2017-01-01

    Driven by the increasing demand on handing microwave signals with compact device, low power consumption, high efficiency and high reliability, it is highly desired to generate, distribute, and process microwave signals using photonic integrated circuits. Silicon photonics offers a promising platform facilitating ultracompact microwave photonic signal processing assisted by silicon nanophotonic devices. In this paper, we propose, theoretically analyze and experimentally demonstrate a simple scheme to realize ultracompact rejection ratio tunable notch microwave photonic filter (MPF) based on a silicon photonic crystal (PhC) nanocavity with fixed extinction ratio. Using a conventional modulation scheme with only a single phase modulator (PM), the rejection ratio of the presented MPF can be tuned from about 10 dB to beyond 60 dB. Moreover, the central frequency tunable operation in the high rejection ratio region is also demonstrated in the experiment. PMID:28067332

  15. Photonic crystal nanocavity assisted rejection ratio tunable notch microwave photonic filter

    NASA Astrophysics Data System (ADS)

    Long, Yun; Xia, Jinsong; Zhang, Yong; Dong, Jianji; Wang, Jian

    2017-01-01

    Driven by the increasing demand on handing microwave signals with compact device, low power consumption, high efficiency and high reliability, it is highly desired to generate, distribute, and process microwave signals using photonic integrated circuits. Silicon photonics offers a promising platform facilitating ultracompact microwave photonic signal processing assisted by silicon nanophotonic devices. In this paper, we propose, theoretically analyze and experimentally demonstrate a simple scheme to realize ultracompact rejection ratio tunable notch microwave photonic filter (MPF) based on a silicon photonic crystal (PhC) nanocavity with fixed extinction ratio. Using a conventional modulation scheme with only a single phase modulator (PM), the rejection ratio of the presented MPF can be tuned from about 10 dB to beyond 60 dB. Moreover, the central frequency tunable operation in the high rejection ratio region is also demonstrated in the experiment.

  16. Photonic crystal nanocavity assisted rejection ratio tunable notch microwave photonic filter.

    PubMed

    Long, Yun; Xia, Jinsong; Zhang, Yong; Dong, Jianji; Wang, Jian

    2017-01-09

    Driven by the increasing demand on handing microwave signals with compact device, low power consumption, high efficiency and high reliability, it is highly desired to generate, distribute, and process microwave signals using photonic integrated circuits. Silicon photonics offers a promising platform facilitating ultracompact microwave photonic signal processing assisted by silicon nanophotonic devices. In this paper, we propose, theoretically analyze and experimentally demonstrate a simple scheme to realize ultracompact rejection ratio tunable notch microwave photonic filter (MPF) based on a silicon photonic crystal (PhC) nanocavity with fixed extinction ratio. Using a conventional modulation scheme with only a single phase modulator (PM), the rejection ratio of the presented MPF can be tuned from about 10 dB to beyond 60 dB. Moreover, the central frequency tunable operation in the high rejection ratio region is also demonstrated in the experiment.

  17. Microwave-Assisted Synthesis of a MK2 Inhibitor by Suzuki-Miyaura Coupling for Study in Werner Syndrome Cells

    PubMed Central

    Bagley, Mark C.; Baashen, Mohammed; Chuckowree, Irina; Dwyer, Jessica E.; Kipling, David; Davis, Terence

    2015-01-01

    Microwave-assisted Suzuki-Miyaura cross-coupling reactions have been employed towards the synthesis of three different MAPKAPK2 (MK2) inhibitors to study accelerated aging in Werner syndrome (WS) cells, including the cross-coupling of a 2-chloroquinoline with a 3-pyridinylboronic acid, the coupling of an aryl bromide with an indolylboronic acid and the reaction of a 3-amino-4-bromopyrazole with 4-carbamoylphenylboronic acid. In all of these processes, the Suzuki-Miyaura reaction was fast and relatively efficient using a palladium catalyst under microwave irradiation. The process was incorporated into a rapid 3-step microwave-assisted method for the synthesis of a MK2 inhibitor involving 3-aminopyrazole formation, pyrazole C-4 bromination using N-bromosuccinimide (NBS), and Suzuki-Miyaura cross-coupling of the pyrazolyl bromide with 4-carbamoylphenylboronic acid to give the target 4-arylpyrazole in 35% overall yield, suitable for study in WS cells. PMID:26046488

  18. 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...

  19. 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...

  20. Microwave-assisted efficient conjugation of nanodiamond and paclitaxel.

    PubMed

    Hsieh, Yi-Han; Liu, Kuang-Kai; Sulake, Rohidas S; Chao, Jui-I; Chen, Chinpiao

    2015-01-01

    Nanodiamond has recently received considerable attention due to the various possible applications in medical field such as drug delivery and bio-labeling. For this purpose suitable and effective surface functionalization of the diamond material are required. A versatile and reproducible surface modification method of nanoscale diamond is essential for functionalization. We introduce the input of microwave energy to assist the functionalization of nanodiamond surface. The feasibility of such a process is illustrated by comparing the biological assay of ND-paclitaxel synthesized by conventional and microwave irradiating. Using a microwave we manage to have approximately doubled grafted molecules per nanoparticle of nanodiamond. Copyright © 2015 Elsevier Ltd. All rights reserved.

  1. Carbon supported Pt-NiO nanoparticles for ethanol electro-oxidation in acid media

    NASA Astrophysics Data System (ADS)

    Comignani, Vanina; Sieben, Juan Manuel; Brigante, Maximiliano E.; Duarte, Marta M. E.

    2015-03-01

    In the present work, the influence of nickel oxide as a co-catalyst of Pt nanoparticles for the electro-oxidation of ethanol in the temperature range of 23-60 °C was investigated. The carbon supported nickel oxide and platinum nanoparticles were prepared by hydrothermal synthesis and microwave-assisted polyol process respectively, and characterized by XRD, EDX, TEM and ICP analysis. The electrocatalytic activity of the as-prepared materials was studied by cyclic voltammetry and chronoamperometry. Small metal nanoparticles with sizes in the range of 3.5-4.5 nm were obtained. The nickel content in the as-prepared Pt-NiO/C catalysts was between 19 and 35 at.%. The electrochemical experiments showed that the electrocatalytic activity of the Pt-NiO/C materials increase with NiO content in the entire temperature range. The apparent activation energy (Ea,app) for the overall ethanol oxidation reaction was found to decrease with NiO content (24-32 kJ mol-1 at 0.3 V), while for Pt/C the activation energy exceeds 48 kJ mol-1. The better performance of the Pt-NiO/C catalysts compared to Pt/C sample is ascribed to the activation of both the C-H and O-H bonds via oxygen-containing species adsorbed on NiO molecules and the modification of the surface electronic structure (changes in the density of states near the Fermi level).

  2. Trace detection of tetrahydrocannabinol (THC) with a SERS-based capillary platform prepared by the in situ microwave synthesis of AgNPs.

    PubMed

    Yüksel, Sezin; Schwenke, Almut M; Soliveri, Guido; Ardizzone, Silvia; Weber, Karina; Cialla-May, Dana; Hoeppener, Stephanie; Schubert, Ulrich S; Popp, Jürgen

    2016-10-05

    In the present study, an ultra-sensitive and highly reproducible novel SERS-based capillary platform was developed and utilized for the trace detection of tetrahydrocannabinol (THC). The approach combines the advantages of microwave-assisted nanoparticle synthesis, plasmonics and capillary forces. By employing a microwave-assisted preparation method, glass capillaries were reproducibly coated with silver nanoparticles in a batch fabrication process that required a processing time of 3 min without needing to use any pre-surface modifications or add surfactants. The coated capillaries exhibited an excellent SERS activity with a high reproducibility and enabled the detection of low concentrations of target molecules. At the same time, only a small amount of analyte and a short and simple incubation process was required. The developed platform was applied to the spectroscopic characterization of tetrahydrocannabinol (THC) and its identification at concentration levels down to 1 nM. Thus, a highly efficient detection system for practical applications, e.g., in drug monitoring/detection, is introduced, which can be fabricated at low cost by using microwave-assisted batch synthesis techniques. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Optimization of ultrasound and microwave assisted extractions of polyphenols from black rice (Oryza sativa cv. Poireton) husk.

    PubMed

    Jha, Pankaj; Das, Arup Jyoti; Deka, Sankar Chandra

    2017-11-01

    Phenolic compounds were extracted from the husk of milled black rice (cv. Poireton) by using a combination of ultrasound assisted extraction and microwave assisted extraction. Extraction parameters were optimized by response surface methodology according to a three levels, five variables Box-Behnken design. The appropriate process variables (extraction temperature and extraction time) to maximize the ethanolic extraction of total phenolic compounds, flavonoids, anthocyanins and antioxidant activity of the extracts were obtained. Extraction of functional components with varying ethanol concentration and microwave time were significantly affected by the process variables. The best possible conditions obtained by RSM for all the factors included 10.02 min sonication time, 49.46 °C sonication temperature, 1:40.79 (w/v) solute solvent ratio, 67.34% ethanol concentration, and 31.11 s microwave time. Under the given solutions, the maximum extraction of phenolics (1.65 mg/g GAE), flavonoids (3.04 mg/100 g), anthocyanins (3.39 mg/100 g) and antioxidants (100%) were predicted, while the experimental values included 1.72 mg/g GAE of total phenolics, 3.01 mg/100 g of flavonoids, 3.36 mg/100 g of anthocyanins and 100% antioxidant activity. The overall results indicated positive impact of co-application of microwave and ultrasound assisted extractions of phenolic compounds from black rice husk.

  4. HNO₃-assisted polyol synthesis of ultralarge single-crystalline Ag microplates and their far propagation length of surface plasmon polariton.

    PubMed

    Chang, Cheng-Wei; Lin, Fan-Cheng; Chiu, Chun-Ya; Su, Chung-Yi; Huang, Jer-Shing; Perng, Tsong-Pyng; Yen, Ta-Jen

    2014-07-23

    We developed a HNO3-assisted polyol reduction method to synthesize ultralarge single-crystalline Ag microplates routinely. The edge length of the synthesized Ag microplates reaches 50 μm, and their top facets are (111). The mechanism for dramatically enlarging single-crystalline Ag structure stems from a series of competitive anisotropic growths, primarily governed by carefully tuning the adsorption of Ag(0) by ethylene glycol and the desorption of Ag(0) by a cyanide ion on Ag(100). Finally, we measured the propagation length of surface plasmon polaritons along the air/Ag interface under 534 nm laser excitation. Our single-crystalline Ag microplate exhibited a propagation length (11.22 μm) considerably greater than that of the conventional E-gun deposited Ag thin film (5.27 μm).

  5. 40 CFR 63.1428 - Process vent requirements for group determination of PMPUs using a nonepoxide organic HAP to make...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... Hazardous Air Pollutant Emissions for Polyether Polyols Production § 63.1428 Process vent requirements for... make or modify a polyether polyol for a PMPU are less than 11,800 kg/yr, the owner or operator of that...

  6. Determining the microwave coupling and operational efficiencies of a microwave plasma assisted chemical vapor deposition reactor under high pressure diamond synthesis operating conditions

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

    Nad, Shreya; Department of Physics and Astronomy, Michigan State University, East Lansing, Michigan 48824; Gu, Yajun

    2015-07-15

    The microwave coupling efficiency of the 2.45 GHz, microwave plasma assisted diamond synthesis process is investigated by experimentally measuring the performance of a specific single mode excited, internally tuned microwave plasma reactor. Plasma reactor coupling efficiencies (η) > 90% are achieved over the entire 100–260 Torr pressure range and 1.5–2.4 kW input power diamond synthesis regime. When operating at a specific experimental operating condition, small additional internal tuning adjustments can be made to achieve η > 98%. When the plasma reactor has low empty cavity losses, i.e., the empty cavity quality factor is >1500, then overall microwave discharge coupling efficienciesmore » (η{sub coup}) of >94% can be achieved. A large, safe, and efficient experimental operating regime is identified. Both substrate hot spots and the formation of microwave plasmoids are eliminated when operating within this regime. This investigation suggests that both the reactor design and the reactor process operation must be considered when attempting to lower diamond synthesis electrical energy costs while still enabling a very versatile and flexible operation performance.« less

  7. Microwave-assisted hydrolysis and extraction of tricyclic antidepressants from human hair.

    PubMed

    Wietecha-Posłuszny, Renata; Garbacik, Aneta; Woźniakiewicz, Michał; Kościelniak, Paweł

    2011-03-01

    The objective of this research was to develop, optimize, and validate a modern, rapid method of preparation of human hair samples, using microwave irradiation, for analysis of eight tricyclic antidepressants (TCADs): nordoxepin, nortriptyline, imipramine, amitriptyline, doxepin, desipramine, clomipramine, and norclomipramine. It was based on simultaneous alkaline hair microwave-assisted hydrolysis and microwave-assisted extraction (MAH-MAE). Extracts were analyzed by high-performance liquid chromatography with diode-array detection (HPLC-DAD). A mixture of n-hexane and isoamyl alcohol (99:1, v/v) was used as extraction solvent and the process was performed at 60°C. Application of 1.0 mol L(-1) NaOH and microwave irradiation for 40 min were found to be optimum for hair samples. Limits of detection ranged from 0.3 to 1.2 μg g(-1) and LOQ from 0.9 to 4.0 μg g(-1) for the different drugs. This enabled us to quantify them in hair samples within average therapeutic concentration ranges.

  8. Beneficial effects of rhodium and tin oxide on carbon supported platinum catalysts for ethanol electrooxidation

    NASA Astrophysics Data System (ADS)

    Soares, Layciane A.; Morais, Claudia; Napporn, Teko W.; Kokoh, K. Boniface; Olivi, Paulo

    2016-05-01

    This work investigates ethanol electrooxidation on Pt/C, PtxRhy/C, Pt-SnO2/C, and PtxRhy-SnO2/C catalysts synthesized by the Pechini and microwave-assisted polyol methods. The catalysts are characterized by energy dispersive X-ray analysis (EDX), transmission electron microscopy (TEM), and X-ray diffraction (XRD) techniques. The electrochemical properties of these electrode materials are examined by cyclic voltammetry and chronoamperometry experiments in acid medium. The products obtained during ethanol electrolysis are identified by high performance liquid chromatography (HPLC). The adsorbed intermediates are evaluated by an in situ reflectance Infrared Spectroscopy technique combined with cyclic voltammetry. Catalysts performance in a direct ethanol fuel cell (DEFC) is also assessed. The electrical performance of the electrocatalysts in a single DEFC at 80 °C decreases in the following order Pt70Rh30SnO2 > Pt80Rh20SnO2 > Pt60Rh40SnO2 ∼ PtSnO2 > PtxRhy ∼ Pt, showing that the presence of SnO2 enhances the ability of Pt to catalyze ethanol electrooxidation.

  9. Negligible degradation upon in situ voltage cycling of a PEMFC using an electrospun niobium-doped tin oxide supported Pt cathode.

    PubMed

    Savych, Iuliia; Subianto, Surya; Nabil, Yannick; Cavaliere, Sara; Jones, Deborah; Rozière, Jacques

    2015-07-14

    Novel platinum-catalysed, corrosion-resistant, loose-tube-structured electrocatalysts for proton exchange membrane fuel cells have been obtained using single-needle electrospinning associated with a microwave-assisted polyol method. Monodisperse platinum particles supported on Nb-SnO2 demonstrated higher electrochemical stability than conventional Pt/C electrodes during ex situ potential cycling and comparable activity in the oxygen reduction reaction. In situ fuel cell operation under accelerated stress test conditions of a membrane electrode assembly elaborated using a Pt/C anode and Pt/Nb-SnO2 cathode confirmed that the voltage loss is significantly lower for the novel cathode than for an MEA prepared using conventional Pt/C supported electrocatalysts. Furthermore, the Nb-SnO2 stabilised the supported platinum nanoparticles against dissolution, migration and reprecipitation in the membrane. Pt/Nb-SnO2 loose-tubes constitute a mitigation strategy for two known degradation mechanisms in PEMFC: corrosion of the carbon support at the cathode, and dissolution of Pt at high cell voltages.

  10. Microwave discharge electrodeless lamps (MDEL). V. Microwave-assisted photolytic disinfection of Bacillus subtilis in simulated electroplating wash wastewaters.

    PubMed

    Horikoshi, Satoshi; Tsuchida, Akihiro; Abe, Masahiko; Ohba, Naoki; Uchida, Masayoshi; Serpone, Nick

    2010-01-01

    This short article examines the microwave-assisted photolytic disinfection of aqueous solutions contaminated by Bacillus subtilis microorganisms using UV and vacuum-UV radiation emitted from a microwave discharge electrodeless lamp (MDEL), a device containing a Hg/Ar gas-fill that was proposed recently for use in Advanced Oxidation Processes (AOPs). Results of the disinfection are compared with those obtained from UV radiation emitted by a low-pressure electrode Hg lamp and by an excimer lamp. Also examined is the disinfection of B. subtilis aqueous media that contained Au3+ or Ni2+ ions, species often found in the treatment of electroplating wash wastewaters.

  11. 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.

  12. Synthesis of Lipid Based Polyols from 1-butene Metathesized Palm Oil for Use in Polyurethane Foam Applications

    NASA Astrophysics Data System (ADS)

    Sasidharan Pillai, Prasanth Kumar

    This thesis explores the use of 1-butene cross metathesized palm oil (PMTAG) as a feedstock for preparation of polyols which can be used to prepare rigid and flexible polyurethane foams. PMTAG is advantageous over its precursor feedstock, palm oil, for synthesizing polyols, especially for the preparation of rigid foams, because of the reduction of dangling chain effects associated with the omega unsaturated fatty acids. 1-butene cross metathesis results in shortening of the unsaturated fatty acid moieties, with approximately half of the unsaturated fatty acids assuming terminal double bonds. It was shown that the associated terminal OH groups introduced through epoxidation and hydroxylation result in rigid foams with a compressive strength approximately 2.5 times higher than that of rigid foams from palm and soybean oil polyols. Up to 1.5 times improvement in the compressive strength value of the rigid foams from the PMTAG polyol was further obtained following dry and/or solvent assisted fractionation of PMTAG in order to reduce the dangling chain effects associated with the saturated components of the PMTAG. Flexible foams with excellent recovery was achieved from the polyols of PMTAG and the high olein fraction of PMTAG indicating that these bio-derived polyurethane foams may be suitable for flexible foam applications. PMTAG polyols with controlled OH values prepared via an optimized green solvent free synthetic strategy provided flexible foams with lower compressive strength and higher recovery; i.e., better flexible foam potential compared to the PMTAG derived foams with non-controlled OH values. Overall, this study has revealed that the dangling chain issues of vegetable oils can be addressed in part using appropriate chemical and physical modification techniques such as cross metathesis and fractionation, respectively. In fact, the rigidity and the compressive strength of the polyurethane foams were in very close agreement with the percentage of terminal hydroxyl and OH value of the polyol. The results obtained from the study can be used to convert PMTAG like materials into industrially valuable materials.

  13. Polyols from Microwave Liquefied Bagasse and Its Application to Rigid Polyurethane Foam.

    PubMed

    Xie, Jiulong; Zhai, Xianglin; Hse, Chung Yun; Shupe, Todd F; Pan, Hui

    2015-12-08

    Bagasse flour (BF) was liquefied using bi-component polyhydric alcohol (PA) as a solvent and phosphoric acid as a catalyst in a microwave reactor. The effect of BF to solvent ratio and reaction temperatures on the liquefaction extent and characteristics of liquefied products were evaluated. The results revealed that almost 75% of the raw bagasse was converted into liquid products within 9 min at 150 °C with a BF to solvent ratio of 1/4. The hydroxyl and acid values of the liquefied bagasse (LB) varied with the liquefied conditions. High reaction temperature combining with low BF to solvent ratio resulted in a low hydroxyl number for the LB. The molecular weight and polydispersity of the LB from reactions of 150 °C was lower compared to that from 125 °C. Rigid polyurethane (PU) foams were prepared from LB and methylene diphenyl diisocyanate (MDI), and the structural, mechanical and thermal properties of the PU foam were evaluated. The PU foams prepared using the LB from high reaction temperature showed better physical and mechanical performance in comparison to those from low reaction temperature. The amount of PA in the LB has the ability of increasing thermal stability of LB-PU foams. The results in this study may provide fundamental information on integrated utilizations of sugarcane bagasse via microwave liquefaction process.

  14. Polyols from Microwave Liquefied Bagasse and Its Application to Rigid Polyurethane Foam

    PubMed Central

    Xie, Jiulong; Zhai, Xianglin; Hse, Chung Yun; Shupe, Todd F.; Pan, Hui

    2015-01-01

    Bagasse flour (BF) was liquefied using bi-component polyhydric alcohol (PA) as a solvent and phosphoric acid as a catalyst in a microwave reactor. The effect of BF to solvent ratio and reaction temperatures on the liquefaction extent and characteristics of liquefied products were evaluated. The results revealed that almost 75% of the raw bagasse was converted into liquid products within 9 min at 150 °C with a BF to solvent ratio of 1/4. The hydroxyl and acid values of the liquefied bagasse (LB) varied with the liquefied conditions. High reaction temperature combining with low BF to solvent ratio resulted in a low hydroxyl number for the LB. The molecular weight and polydispersity of the LB from reactions of 150 °C was lower compared to that from 125 °C. Rigid polyurethane (PU) foams were prepared from LB and methylene diphenyl diisocyanate (MDI), and the structural, mechanical and thermal properties of the PU foam were evaluated. The PU foams prepared using the LB from high reaction temperature showed better physical and mechanical performance in comparison to those from low reaction temperature. The amount of PA in the LB has the ability of increasing thermal stability of LB-PU foams. The results in this study may provide fundamental information on integrated utilizations of sugarcane bagasse via microwave liquefaction process. PMID:28793725

  15. Dynamic dielectric properties of a wood liquefaction system using polyethylene glycol and glycerol

    Treesearch

    Mengchao Zhou; Thomas L. Eberhardt; Bo Cai; Chung-Yun Hse; Hui Pan

    2017-01-01

    Microwave-assisted liquefaction has shown potential for rapid thermal processing of lignocellulosic biomass. The efficiency of microwave heating depends largely on the dielectric properties of the materials being heated. The objective of this study was to investigate the dynamic interactions between microwave energy and the reaction system during the liquefaction of a...

  16. A Review of Microwave-Assisted Reactions for Biodiesel Production

    PubMed Central

    Nomanbhay, Saifuddin; Ong, Mei Yin

    2017-01-01

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

  17. A Review of Microwave-Assisted Reactions for Biodiesel Production.

    PubMed

    Nomanbhay, Saifuddin; Ong, Mei Yin

    2017-06-15

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

  18. 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 -1)...

  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. Unlocking Potentials of Microwaves for Food Safety and Quality

    PubMed Central

    Tang, Juming

    2015-01-01

    Microwave is an effective means to deliver energy to food through polymeric package materials, offering potential for developing short-time in-package sterilization and pasteurization processes. The complex physics related to microwave propagation and microwave heating require special attention to the design of process systems and development of thermal processes in compliance with regulatory requirements for food safety. This article describes the basic microwave properties relevant to heating uniformity and system design, and provides a historical overview on the development of microwave-assisted thermal sterilization (MATS) and pasteurization systems in research laboratories and used in food plants. It presents recent activities on the development of 915 MHz single-mode MATS technology, the procedures leading to regulatory acceptance, and sensory results of the processed products. The article discusses needs for further efforts to bridge remaining knowledge gaps and facilitate transfer of academic research to industrial implementation. PMID:26242920

  1. Unlocking Potentials of Microwaves for Food Safety and Quality.

    PubMed

    Tang, Juming

    2015-08-01

    Microwave is an effective means to deliver energy to food through polymeric package materials, offering potential for developing short-time in-package sterilization and pasteurization processes. The complex physics related to microwave propagation and microwave heating require special attention to the design of process systems and development of thermal processes in compliance with regulatory requirements for food safety. This article describes the basic microwave properties relevant to heating uniformity and system design, and provides a historical overview on the development of microwave-assisted thermal sterilization (MATS) and pasteurization systems in research laboratories and used in food plants. It presents recent activities on the development of 915 MHz single-mode MATS technology, the procedures leading to regulatory acceptance, and sensory results of the processed products. The article discusses needs for further efforts to bridge remaining knowledge gaps and facilitate transfer of academic research to industrial implementation. © 2015 Institute of Food Technologists®

  2. Difference and similarity of dielectric relaxation processes among polyols

    NASA Astrophysics Data System (ADS)

    Minoguchi, Ayumi; Kitai, Kei; Nozaki, Ryusuke

    2003-09-01

    Complex permittivity measurements were performed on sorbitol, xylitol, and sorbitol-xylitol mixture in the supercooled liquid state in an extremely wide frequency range from 10 μHz to 500 MHz at temperatures near and above the glass transition temperature. We determined detailed behavior of the relaxation parameters such as relaxation frequency and broadening against temperature not only for the α process but also for the β process above the glass transition temperature, to the best of our knowledge, for the first time. Since supercooled liquids are in the quasi-equilibrium state, the behavior of all the relaxation parameters for the β process can be compared among the polyols as well as those for the α process. The relaxation frequencies of the α processes follow the Vogel-Fulcher-Tammann manner and the loci in the Arrhenius diagram are different corresponding to the difference of the glass transition temperatures. On the other hand, the relaxation frequencies of the β processes, which are often called as the Johari-Goldstein processes, follow the Arrhenius-type temperature dependence. The relaxation parameters for the β process are quite similar among the polyols at temperatures below the αβ merging temperature, TM. However, they show anomalous behavior near TM, which depends on the molecular size of materials. These results suggest that the origin of the β process is essentially the same among the polyols.

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

    Paulauskas, F.L.; Meek, T.T.

    Studies of microwave-assisted curing of neat resins (epoxy) and unidirectional glass and carbon fiber laminates have shown that a substantial reduction in the curing time was obtained. This may be explained by the penetration of microwave energy directly and throughout the laminate with enhancement of the kinetics of the chemical reaction. Results of this work indicate that the microwave assisted curing of glass fiber laminates also shows a substantial reduction of the required curing time. Microwave radiation of 2.45 GHz has been demonstrated to be an acceptable method to cure unidirectional carbon fiber laminates. Also, effective curing of crossply (0/90)more » laminates through this method was observed when proper rotation of the parts accompanied the curing process. This is in accordance with previous work. Multidirectional carbon fiber/epoxy laminates demonstrate a lack of coupling during the curing process. A direct curing of these laminates was not possible by microwave radiation with the experimental approach used, in agreement with previous work. Nevertheless, a moderate reduction in the curing time of these thin laminates was observed due to hybrid curing.« less

  4. Microwave Assisted Grafting of Gums and Extraction of Natural Materials.

    PubMed

    Singh, Inderbir; Rani, Priya; Kumar, Pradeep

    2017-01-01

    Microwave assisted modification of polymers has become an established technique for modifying the functionality of polymers. Microwave irradiation reduces reaction time as well as the use of toxic solvents with enhanced sensitivity and yields of quality products. In this review article instrumentation and basic principles of microwave activation have been discussed. Microwave assisted grafting of natural gums, characterization of grafted polymers and their toxicological parameters have also been listed. Pharmaceutical applications viz. drug release retardant, mucoahesion and tablet superdisintegrant potential of microwave assisted gums has also been discussed. An overview of microwave assisted extraction of plant based natural materials has also been presented. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  5. 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. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    DOEpatents

    White, Terry L; Paulauskas, Felix L; Bigelow, Timothy S

    2014-03-25

    A method for continuously processing carbon fiber including establishing a microwave plasma in a selected atmosphere contained in an elongated chamber having a microwave power gradient along its length defined by a lower microwave power at one end and a higher microwave power at the opposite end of the elongated chamber. The elongated chamber having an opening in each of the ends of the chamber that are adapted to allow the passage of the fiber tow while limiting incidental gas flow into or out of said chamber. A continuous fiber tow is introduced into the end of the chamber having the lower microwave power. The fiber tow is withdrawn from the opposite end of the chamber having the higher microwave power. The fiber to is subjected to progressively higher microwave energy as the fiber is being traversed through the elongated chamber.

  7. Development of high-performance biodegradable rigid polyurethane foams using all bioresource-based polyols: Lignin and soy oil-derived polyols.

    PubMed

    Luo, Xiaogang; Xiao, Yuqin; Wu, Qiangxian; Zeng, Jian

    2018-04-25

    Development of biodegradable polyurethane materials is the most promising in the wider context of the "greening" of industrial chemistry. To tackle this challenge, a novel biodegradable polyurethane foam from all bioresource-based polyols (lignin and soy oil-derived polyols) and polymeric methyldiphenyl diisocyanate (pMDI) have been synthesized via a one-pot and self-rising process. All these foam samples have the internal cellular morphology and microstructure. FTIR result exhibits characteristic peaks of polyurethane, and indicates covalent bonds between soy-based polyurethane and lignin, and the lignin powders can react with pMDI via active -H and -CNO. In addition, hydrogen bonding also plays an important role in forming the 3D structures. These interactions and chemical bonds made the prepared foam samples form the 3D macromolecular structure with improved mechanical, thermal, and biodegradable properties. The reaction process is time-saving and cost-effective as it requires no blowing agent and minimum processing steps, while exploring the potential of using the higher content of nature bioresource constituents. Copyright © 2018 Elsevier B.V. All rights reserved.

  8. 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.

  9. Microwave-Assisted Hydro-Distillation of Essential Oil from Rosemary: Comparison with Traditional Distillation

    PubMed Central

    Moradi, Sara; Fazlali, Alireza; Hamedi, Hamid

    Background: Hydro-distillation (HD) method is a traditional technique which is used in most industrial companies. Microwave-assisted Hydro-distillation (MAHD) is an advanced HD technique utilizing a microwave oven in the extraction process. Methods: In this research, MAHD of essential oils from the aerial parts (leaves) of rosemary (Rosmarinus officinalis L.) was studied and the results were compared with those of the conventional HD in terms of extraction time, extraction efficiency, chemical composition, quality of the essential oils and cost of the operation. Results: Microwave hydro-distillation was superior in terms of saving energy and extraction time (30 min, compared to 90 min in HD). Chromatography was used for quantity analysis of the essential oils composition. Quality of essential oil improved in MAHD method due to an increase of 17% in oxygenated compounds. Conclusion: Consequently, microwave hydro-distillation can be used as a substitute of traditional hydro-distillation. PMID:29296263

  10. Microwave-Assisted Hydro-Distillation of Essential Oil from Rosemary: Comparison with Traditional Distillation.

    PubMed

    Moradi, Sara; Fazlali, Alireza; Hamedi, Hamid

    2018-01-01

    Hydro-distillation (HD) method is a traditional technique which is used in most industrial companies. Microwave-assisted Hydro-distillation (MAHD) is an advanced HD technique utilizing a microwave oven in the extraction process. In this research, MAHD of essential oils from the aerial parts (leaves) of rosemary ( Rosmarinus officinalis L. ) was studied and the results were compared with those of the conventional HD in terms of extraction time, extraction efficiency, chemical composition, quality of the essential oils and cost of the operation. Microwave hydro-distillation was superior in terms of saving energy and extraction time (30 min , compared to 90 min in HD). Chromatography was used for quantity analysis of the essential oils composition. Quality of essential oil improved in MAHD method due to an increase of 17% in oxygenated compounds. Consequently, microwave hydro-distillation can be used as a substitute of traditional hydro-distillation.

  11. Determination of fat-soluble vitamins in vegetable oils through microwave-assisted high-performance liquid chromatography.

    PubMed

    Carballo, Silvia; Prats, Soledad; Maestre, Salvador; Todolí, José-Luis

    2015-04-01

    In this manuscript, a study of the effect of microwave radiation on the high-performance liquid chromatography separation of tocopherols and vitamin K1 was conducted. The novelty of the application was the use of a relatively low polarity mobile phase in which the dielectric heating effect was minimized to evaluate the nonthermal effect of the microwave radiation over the separation process. Results obtained show that microwave-assisted high-performance liquid chromatography had a shorter analysis time from 31.5 to 13.3 min when the lowest microwave power was used. Moreover, narrower peaks were obtained; hence the separation was more efficient maintaining or even increasing the resolution between the peaks. This result confirms that the increase in mobile phase temperature is not the only variable for improving the separation process but also other nonthermal processes must intervene. Fluorescence detection demonstrated better signal-to-noise compared to photodiode arrayed detection mainly due to the independent effect of microwave pulses on the baseline noise, but photodiode array detection was finally chosen as it allowed a simultaneous detection of nonfluorescent compounds. Finally, a determination of the content of the vitamin E homologs was carried out in different vegetable oils. Results were coherent with those found in the literature. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. 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.

  13. Photonics for microwave systems and ultra-wideband signal processing

    NASA Astrophysics Data System (ADS)

    Ng, W.

    2016-08-01

    The advantages of using the broadband and low-loss distribution attributes of photonics to enhance the signal processing and sensing capabilities of microwave systems are well known. In this paper, we review the progress made in the topical areas of true-time-delay beamsteering, photonic-assisted analog-to-digital conversion, RF-photonic filtering and link performances. We also provide an outlook on the emerging field of integrated microwave photonics (MWP) that promise to reduce the cost of MWP subsystems and components, while providing significantly improved form-factors for system insertion.

  14. Production of polyol oils from soybean oil through bioprocess

    USDA-ARS?s Scientific Manuscript database

    Soy-polyol oils (oxygenated acylglycerols) are important starting materials for the manufacture of polymers such as polyurethane. Currently, they are produced by a two-step chemical process involving epoxidation and then the subsequent opening of the oxirane ring. The objective of this study is to d...

  15. 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

  16. 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.

  17. Innovative thermoplastic chitosan obtained by thermo-mechanical mixing with polyol plasticizers.

    PubMed

    Matet, Marie; Heuzey, Marie-Claude; Pollet, Eric; Ajji, Abdellah; Avérous, Luc

    2013-06-05

    Chitosan shows a degradation temperature lower than its melting point, which prevents its development in several applications. One way to overcome this issue is the plasticization of the carbohydrate. In this work plasticized chitosan was prepared by a thermo-mechanical kneading approach. The effects of different non-volatile polyol plasticizers (glycerol, xylitol and sorbitol) were investigated. The microstructure and morphology were determined using FTIR, XRD, TEM and SEM in order to understand the plasticization mechanism. Sorbitol, which is the highest molecular weight polyol used, resulted in plasticized chitosan with the highest thermal, mechanical and rheological properties. On the other hand, the sample plasticized with glycerol, the lowest molecular weight polyol, had the most important amorphous phase content and the lowest thermal, mechanical and rheological properties. Also, when the polyol content increased in the formulation, the plasticized chitosan was more amorphous and consequently its processability easier, while its properties decreased. Copyright © 2013 Elsevier Ltd. All rights reserved.

  18. Ultra-fast microwave-assisted hydrothermal synthesis of long vertically aligned ZnO nanowires for dye-sensitized solar cell application.

    PubMed

    Mahpeykar, S M; Koohsorkhi, J; Ghafoori-Fard, H

    2012-04-27

    Long vertically aligned ZnO nanowire arrays were synthesized using an ultra-fast microwave-assisted hydrothermal process. Using this method, we were able to grow ZnO nanowire arrays at an average growth rate as high as 200 nm min(-1) for maximum microwave power level. This method does not suffer from the growth stoppage problem at long growth times that, according to our investigations, a normal microwave-assisted hydrothermal method suffers from. Longitudinal growth of the nanowire arrays was investigated as a function of microwave power level and growth time using cross-sectional FESEM images of the grown arrays. Effect of seed layer on the alignment of nanowires was also studied. X-ray diffraction analysis confirmed c-axis orientation and single-phase wurtzite structure of the nanowires. J-V curves of the fabricated ZnO nanowire-based mercurochrome-sensitized solar cells indicated that the short-circuit current density is increased with increasing the length of the nanowire array. According to the UV-vis spectra of the dyes detached from the cells, these increments were mainly attributed to the enlarged internal surface area and therefore dye loading enhancement in the lengthened nanowire arrays.

  19. Microwave Pasteurization of Cooked Pasta: Effect of Process Parameters on Texture and Quality for Heat-and-Eat and Ready-to-Eat Meals.

    PubMed

    Joyner Melito, Helen S; Jones, Kari E; Rasco, Barbara A

    2016-06-01

    Pasta presents a challenge to microwave processing due to its unique cooking requirements. The objective of this study was to determine the effects of microwave processing on pasta physicochemical and mechanical properties. Fettuccine pasta was parboiled for selected times, then pasteurized using a Microwave Assisted Pasteurization System and stored under refrigeration for 1 wk. Samples were analyzed using microscopy, mechanical testing, and chemical analyses after storage. While no significant differences were observed for free amylose among fresh samples, samples parboiled for ≤6 min had significantly higher free amylose, suggesting reduced starch retrogradation. Increased heat treatment increased degree of protein polymerization, observed in microstructures as increased gluten strand thickness and network density. Firmness and extensibility increased with increased parboil time; however, extension data indicated an overall weakening of microwave-treated pasta regardless of total cooking time. Overall, microwave pasteurization was shown to be a viable cooking method for pasta. © 2016 Institute of Food Technologists®

  20. Development of CVD Diamond for Industrial Applications Final Report CRADA No. TC-2047-02

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

    Caplan, M.; Olstad, R.; Jory, H.

    2017-09-08

    This project was a collaborative effort to develop and demonstrate a new millimeter microwave assisted chemical vapor deposition(CVD) process for manufacturing large diamond disks with greatly reduced processing times and costs from those now available. In the CVD process, carbon based gases (methane) and hydrogen are dissociated into plasma using microwave discharge and then deposited layer by layer as polycrystalline diamond onto a substrate. The available low frequency (2.45GHz) microwave sources used elsewhere (De Beers) result in low density plasmas and low deposition rates: 4 inch diamond disks take 6-8 weeks to process. The new system developed in this projectmore » uses a high frequency 30GHz Gyrotron as the microwave source and a quasi-optical CVD chamber resulting in a much higher density plasma which greatly reduced the diamond processing times (1-2 weeks)« less

  1. High growth rate homoepitaxial diamond film deposition at high temperatures by microwave plasma-assisted chemical vapor deposition

    NASA Technical Reports Server (NTRS)

    Vohra, Yogesh K. (Inventor); McCauley, Thomas S. (Inventor)

    1997-01-01

    The deposition of high quality diamond films at high linear growth rates and substrate temperatures for microwave-plasma chemical vapor deposition is disclosed. The linear growth rate achieved for this process is generally greater than 50 .mu.m/hr for high quality films, as compared to rates of less than 5 .mu.m/hr generally reported for MPCVD processes.

  2. Optimization of dynamic-microwave assisted enzymatic hydrolysis extraction of total ginsenosides from stems and leaves of panax ginseng by response surface methodology.

    PubMed

    Wang, Xiao-Yan; Ren, Hui

    2018-03-21

    Ginseng stems and leaves (GSAL) are abundant in ginsenosides compounds. For efficient utilization of GSAL and the enhancement of total ginsenosides (TG) compound yields in GSAL, TG from GSAL were extracted, using dynamic-microwave assisted extraction coupled with enzymatic hydrolysis (DMAE-EH) method. The extraction process has been simulated and its main influencing factors such as ethanol concentration, microwave temperature, microwave time and pump flow rate have been optimized by response surface methodology coupled with a Box-Behnken design(BBD). The experimental results indicated that optimal extraction conditions of TG from GSAL were as follows: ethanol concentration of 75%, microwave temperature of 60°C, microwave time of 20 min and pump flow rate of 38 r/min. After experimental verification, the experimental yields of TG was 60.62 ± 0.85 mg g -1 , which were well agreement with the predicted by the model. In general, the present results demonstrated that DMAE-EH method was successfully used to extract total ginsenosides in GSAL.

  3. Two-step fast microwave-assisted pyrolysis of biomass for bio-oil production using microwave absorbent and HZSM-5 catalyst.

    PubMed

    Zhang, Bo; Zhong, Zhaoping; Xie, Qinglong; Liu, Shiyu; Ruan, Roger

    2016-07-01

    A novel technology of two-step fast microwave-assisted pyrolysis (fMAP) of corn stover for bio-oil production was investigated in the presence of microwave absorbent (SiC) and HZSM-5 catalyst. Effects of fMAP temperature and catalyst-to-biomass ratio on bio-oil yield and chemical components were examined. The results showed that this technology, employing microwave, microwave absorbent and HZSM-5 catalyst, was effective and promising for biomass fast pyrolysis. The fMAP temperature of 500°C was considered the optimum condition for maximum yield and best quality of bio-oil. Besides, the bio-oil yield decreased linearly and the chemical components in bio-oil were improved sequentially with the increase of catalyst-to-biomass ratio from 1:100 to 1:20. The elemental compositions of bio-char were also determined. Additionally, compared to one-step fMAP process, two-step fMAP could promote the bio-oil quality with a smaller catalyst-to-biomass ratio. Copyright © 2016. Published by Elsevier B.V.

  4. Microwave-assisted combustion synthesis of nano iron oxide/iron-coated activated carbon, anthracite, cellulose fiber, and silica, with arsenic adsorption studies

    EPA Science Inventory

    Combustion synthesis of iron oxide/iron coated carbons such as activated carbon, anthracite, cellulose fiber and silica is described. The reactions were carried out in alumina crucibles using a Panasonic kitchen microwave with inverter technology, and the reaction process was com...

  5. Capability of Thai Mission grass (Pennisetum polystachyon) as a new weedy lignocellulosic feedstock for production of monomeric sugar.

    PubMed

    Tatijarern, Patomwat; Prasertwasu, Sirirat; Komalwanich, Tidarat; Chaisuwan, Thanyalak; Luengnaruemitchai, Apanee; Wongkasemjit, Sujitra

    2013-09-01

    Mission grass (Pennisetum polystachyon) grown in Pakchong District, Nakornratchasima Province, Thailand, with high cellulose and hemicellulose contents were harvested to determine the fermentable monomeric sugars for bioethanol production by two-stage microwave/chemical pretreatment process. Microwave-assisted NaOH pretreatment effectively removed approximately 85% lignin content in Mission grass, using 3% (w/v) NaOH, 15:1 liquid-to-solid ratio (LSR) at 120 °C temperatures for 10 min. As a result, in the second stage, microwave-assisted H2SO4 pretreatment of an alkaline-pretreated Mission grass solid releasedan impressively high fermentable sugar content (34.3±1.3 g per 100 g of dried biomass), consisting mainly of 31.1±0.8 g of glucose per 100 g of dried biomass, using 1% (w/v) H2SO4, 15:1 LSR at 200 °C temperature for a very short pretreatment time (5 min). The total monomeric sugar yield obtained via two-stage microwave/chemical process was 40.9 g per 100 g of dried biomass. Copyright © 2013 Elsevier Ltd. All rights reserved.

  6. Optimality in Microwave-Assisted Drying of Aloe Vera ( Aloe barbadensis Miller) Gel using Response Surface Methodology and Artificial Neural Network Modeling

    NASA Astrophysics Data System (ADS)

    Das, Chandan; Das, Arijit; Kumar Golder, Animes

    2016-10-01

    The present work illustrates the Microwave-Assisted Drying (MWAD) characteristic of aloe vera gel combined with process optimization and artificial neural network modeling. The influence of microwave power (160-480 W), gel quantity (4-8 g) and drying time (1-9 min) on the moisture ratio was investigated. The drying of aloe gel exhibited typical diffusion-controlled characteristics with a predominant interaction between input power and drying time. Falling rate period was observed for the entire MWAD of aloe gel. Face-centered Central Composite Design (FCCD) developed a regression model to evaluate their effects on moisture ratio. The optimal MWAD conditions were established as microwave power of 227.9 W, sample amount of 4.47 g and 5.78 min drying time corresponding to the moisture ratio of 0.15. A computer-stimulated Artificial Neural Network (ANN) model was generated for mapping between process variables and the desired response. `Levenberg-Marquardt Back Propagation' algorithm with 3-5-1 architect gave the best prediction, and it showed a clear superiority over FCCD.

  7. Enhancing the microwave absorption properties of amorphous CoO nanosheet-coated Co (hexagonal and cubic phases) through interfacial polarizations.

    PubMed

    Deng, Jiushuai; Li, Shimei; Zhou, Yuanyuan; Liang, Luyang; Zhao, Biao; Zhang, Xi; Zhang, Rui

    2018-01-01

    Core-shell flower-like composites were successfully prepared by a simple polyol method. These composites were formed by coating dual-phased (face-centered cubic [fcc] and hexagonal close-packed [hcp]) Co with amorphous CoO nanosheets. The microwave absorption properties of the flower-like Co@CoO paraffin composites with various Co@CoO amounts were then investigated. Results showed that the paraffin-based composite containing 70wt% flower-like Co@CoO displayed excellent microwave absorption properties (R E =24.74dB·GHz/mm). The minimum reflection loss of -30.4dB was obtained at 16.1GHz with a small thickness of 1.5mm, and 1.5mm bandwidth reached 4.6GHz (13.4-18GHz) below -10dB (90% microwave absorption). The excellent microwave absorption properties of flower-like Co@CoO are attributed to the synergetic effect between magnetic loss and dielectric loss, and the magnetic loss makes a main contribution to absorption. The core-shell flower-like structures with dual Co phases also contributed to microwave absorption. The amorphous CoO nanosheets were able to generate multiple reflections and exhibit scattering. In addition, the novel absorption mechanism that enhanced interfacial polarization was proposed. This enhancement resulted from the presence of interfaces between the hcp and fcc phases and between the core-shell Co@CoO composites. Copyright © 2017 Elsevier Inc. All rights reserved.

  8. Application of microwave energy in the control of DPM, oxides of nitrogen and VOC emissions

    NASA Astrophysics Data System (ADS)

    Pallavkar, Sameer M.

    The emissions of DPM (diesel particulate matter), NOx (oxides of nitrogen), and toxic VOCs (volatile organic compounds) from diesel engine exhaust gases and other sources such as chemical process industry and manufacturing industry have been a great environmental and health concern. Most control technologies for these emissions require elevated temperatures. The use of microwave energy as a source of heat energy, however, has not been fully explored. In this study, the microwave energy was used as the energy source in three separate emission control processes, namely, the regeneration of diesel particulate filter (DPF) for DPM control, the NOx reduction using a platinum catalyst, and the VOC destruction involving a ceramic based material. The study has demonstrated that microwave heating is an effective method in providing heat for the studied processes. The control efficiencies associated with the microwave-assisted processes have been observed to be high and acceptable. Further research, however, is required for the commercial use of these technologies.

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

    Paulauskas, F.L.

    The objective of this work was to investigate the beneficial effect of the variable frequency microwave (VFM) technology to cure thermosetting prepreg laminates. Further, it was to investigate the interrelationship and effect on the curing process of frequency, band width, and curing time with different types of laminates. Previous studies of microwave-assisted curing of neat resins (epoxy) and unidirectional glass and carbon fiber laminates with a fixed frequency of 2.45 GHz, have shown that a substantial reduction in the curing time was obtained. Results of this earlier work indicate that the microwave-assisted curing of multidirectional glass fiber laminates also showmore » a substantial reduction of the required curing time. This may be explained by the penetration of microwave energy directly and throughout the laminate with enhancement of the kinetics of the chemical reaction. The fixed frequency microwave radiation of 2.45 GHz has been demonstrated to be a partially acceptable method to cure unidirectional carbon fiber laminates. Multidirectional carbon fiber/epoxy laminates demonstrate a lack of coupling during the curing process. A direct curing of these laminates was not possible by microwave radiation with the experimental approach used in agreement with previous work. In addition to this short coming, the unidirectional laminate samples cured with the fixed frequency are visually nonuniform. Localized areas of darker colors (burn, hot spots, overheating) are attributed to the formation of standing waves within the microwave cavity. For this reason, the laminates are subject to proper rotation while curing through fixed frequency. The present research indicates that variable frequency microwave technology is a sound and acceptable processing method to effectively cure uni-, bi- or multi-directional thermosetting glass fiber laminates. Also, this methodology will effectively cure unidirectional thermosetting carbon fiber laminates. For all these cases, this technology yielded a substantial reduction in the required cure time of these laminates. Multidirectional carbon fiber laminates demonstrated a lack of coupling of VFM energy during the curing process.« less

  10. An absorbing microwave micro-solid-phase extraction device used in non-polar solvent microwave-assisted extraction for the determination of organophosphorus pesticides.

    PubMed

    Wang, Ziming; Zhao, Xin; Xu, Xu; Wu, Lijie; Su, Rui; Zhao, Yajing; Jiang, Chengfei; Zhang, Hanqi; Ma, Qiang; Lu, Chunmei; Dong, Deming

    2013-01-14

    A single-step extraction-cleanup method, including microwave-assisted extraction (MAE) and micro-solid-phase extraction (μ-SPE), was developed for the extraction of ten organophosphorus pesticides in vegetable and fruit samples. Without adding any polar solvent, only one kind of non-polar solvent (hexane) was used as extraction solvent in the whole extraction step. Absorbing microwave μ-SPE device, was prepared by packing activated carbon with microporous polypropylene membrane envelope, and used as not only the sorbent in μ-SPE, but also the microwave absorption medium. Some experimental parameters effecting on extraction efficiency was investigated and optimized. 1.0 g of sample, 8 mL of hexane and three absorbing microwave μ-SPE devices were added in the microwave extraction vessel, the extraction was carried out under 400 W irradiation power at 60°C for 10 min. The extracts obtained by MAE-μ-SPE were directly analyzed by GC-MS without any clean-up process. The recoveries were in the range of 93.5-104.6%, and the relative standard deviations were lower than 8.7%. Copyright © 2012 Elsevier B.V. All rights reserved.

  11. Biodegradation of polyether-polyol-based polyurethane elastomeric films: influence of partial replacement of polyether polyol by biopolymers of renewable origin.

    PubMed

    Obruca, Stanislav; Marova, Ivana; Vojtova, Lucy

    2011-07-01

    In this work we investigated the degradation process ofpolyether-polyol-based polyurethane (PUR) elastomeric films in the presence of a mixed thermophilic culture as a model of a natural bacterial consortium. The presence of PUR material in cultivation medium resulted in delayed but intensive growth of the bacterial culture. The unusually long lag phase was caused by the release of unreacted polyether polyol and tin catalyst from the material. The lag phase was significantly shortened and the biodegradability of PUR materials was enhanced by partial replacement (10%) of polyether polyol with biopolymers (carboxymethyl cellulose, hydroxyethyl cellulose, acetyl cellulose and actylated starch). The process of material degradation consisted of two steps. First, the materials were mechanically disrupted and, second, the bacterial culture was able to utilize abiotic degradation products, which resulted in supported bacterial growth. Direct utilization of PUR by the bacterial culture was observed as well, but the bacterial culture contributed only slightly to the total mass losses. The only exception was PUR material modified by acetyl cellulose. In this case, direct biodegradation represented the major mechanism of material decomposition. Moreover, PUR material modified by acetyl cellulose did not tend to undergo abiotic degradation. In conclusion, the modification of PUR by proper biopolymers is a promising strategy for reducing potential negative effects of waste PUR materials on the environment and enhancing their biodegradability.

  12. Selective leaching of Zn from spent alkaline batteries using environmentally friendly approaches.

    PubMed

    Maryam Sadeghi, S; Vanpeteghem, Guillaumme; Neto, Isabel F F; Soares, Helena M V M

    2017-02-01

    The main aim of this work was to evaluate the possibility of using microwave or ultrasound to assist the efficient and selective leaching of Zn from spent alkaline batteries and compare the results with those obtained using the conventional method. Two different strategies were applied: acid leaching of a washed residue and alkaline leaching of the original residue. In both (acid and alkaline) approaches, the use of microwave- or ultrasound-assisted leaching increased the extraction of Zn compared with the best results obtained using conventional leaching [acid leaching (1.5mol/L H 2 SO 4 , 3h, 80°C), 90% of Zn extracted; alkaline leaching (6mol/L NaOH, 3h, 80°C), 42% of Zn extracted]. With acid leaching, 94% of the Zn was extracted using microwave-assisted leaching (1 cycle, 30s, 1mol/L H 2 SO 4 ), and 92% of the Zn was extracted using ultrasound-assisted leaching (2min, 0.1p, 20% amplitude, 1mol/L H 2 SO 4 ). Ultrasound-assisted leaching resulted in a more selective (Zn/Mn ratio of 5.1) Zn extraction than microwave-assisted leaching (Zn/Mn ratio of 3.5); both processes generated a concentrated Zn solution (⩾18.7g/L) with a purity (83.3% and 77.7%, respectively) that was suitable for electrowinning. With alkaline leaching, microwave- (1 cycle, 3 min, 4mol/L NaOH) and ultrasound-assisted (14min, 0.1p, 20% amplitude, 4mol/L NaOH) leaching extracted about 80% of the Zn and less than 0.01% of the Mn, which resulted in lesser concentrated Zn solutions (approximately 16.5g/L) but with high purity (>99.5%) that was suitable for the recovery of Zn by precipitation. The microwave- and ultrasound-assisted leaching strategies used in this work proved to be efficient and environmentally-friendly approaches for the extraction of Zn from spent alkaline residues since a concentrated Zn solution with adequate purity for subsequent Zn recovery was obtained using significantly decreased leaching times and concentrations of chemicals. Copyright © 2017 Elsevier Ltd. All rights reserved.

  13. Bio-refinery of orange peels waste: a new concept based on integrated green and solvent free extraction processes using ultrasound and microwave techniques to obtain essential oil, polyphenols and pectin.

    PubMed

    Boukroufa, Meryem; Boutekedjiret, Chahrazed; Petigny, Loïc; Rakotomanomana, Njara; Chemat, Farid

    2015-05-01

    In this study, extraction of essential oil, polyphenols and pectin from orange peel has been optimized using microwave and ultrasound technology without adding any solvent but only "in situ" water which was recycled and used as solvent. The essential oil extraction performed by Microwave Hydrodiffusion and Gravity (MHG) was optimized and compared to steam distillation extraction (SD). No significant changes in yield were noticed: 4.22 ± 0.03% and 4.16 ± 0.05% for MHG and SD, respectively. After extraction of essential oil, residual water of plant obtained after MHG extraction was used as solvent for polyphenols and pectin extraction from MHG residues. Polyphenols extraction was performed by ultrasound-assisted extraction (UAE) and conventional extraction (CE). Response surface methodology (RSM) using central composite designs (CCD) approach was launched to investigate the influence of process variables on the ultrasound-assisted extraction (UAE). The statistical analysis revealed that the optimized conditions of ultrasound power and temperature were 0.956 W/cm(2) and 59.83°C giving a polyphenol yield of 50.02 mgGA/100 g dm. Compared with the conventional extraction (CE), the UAE gave an increase of 30% in TPC yield. Pectin was extracted by conventional and microwave assisted extraction. This technique gives a maximal yield of 24.2% for microwave power of 500 W in only 3 min whereas conventional extraction gives 18.32% in 120 min. Combination of microwave, ultrasound and the recycled "in situ" water of citrus peels allow us to obtain high added values compounds in shorter time and managed to make a closed loop using only natural resources provided by the plant which makes the whole process intensified in term of time and energy saving, cleanliness and reduced waste water. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Co-pyrolysis of microwave-assisted acid pretreated bamboo sawdust and soapstock.

    PubMed

    Wang, Yunpu; Wu, Qiuhao; Duan, Dengle; Zhang, Yayun; Ruan, Roger; Liu, Yuhuan; Fu, Guiming; Zhang, Shumei; Zhao, Yunfeng; Dai, Leilei; Fan, Liangliang

    2018-05-30

    Fast microwave-assisted co-pyrolysis of pretreated bamboo sawdust and soapstock was conducted. The pretreatment process was carried out under microwave irradiation. The effects of microwave irradiation temperature, irradiation time, and concentration of hydrochloric acid on product distribution from co-pyrolysis and the relative contents of the major components in bio-oil were investigated. A maximum bio-oil yield of 40.00 wt.% was obtained at 200 °C for 60 min with 0.5 M hydrochloric acid. As pretreatment temperature, reaction time and acid concentration increased, respectively, the relative contents of phenols, diesel fraction (C12 + aliphatics), and other oxygenates decreased. The gasoline fraction (including C5-C12 aliphatics and aromatics) ranged from 55.77% to 73.30% under various pretreatment conditions. Therefore, excessive reaction time and concentration of acid are not beneficial to upgrading bio-oil. Copyright © 2018 Elsevier Ltd. All rights reserved.

  15. Aromatics and phenols from catalytic pyrolysis of Douglas fir pellets in microwave with ZSM-5 as a catalyst

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

    Wang, Lu; Lei, Hanwu; Ren, Shoujie

    Microwave assisted catalytic pyrolysis was investigated to convert Douglas fir pellets to bio-oils by a ZSM-5 Zeolite catalyst. A central composite experimental design (CCD) was used to optimize the catalytic pyrolysis process. The effects of reaction time, temperature and catalyst to biomass ratio on the bio-oil, syngas, and biochar yields were determined. GC/MS analysis results showed that the bio-oil contained a series of important and useful chemical compounds. Phenols, guaiacols, and aromatic hydrocarbons were the most abundant compounds which were about 50-82 % in bio-oil depending on the pyrolysis conditions. Comparison between the bio-oils from microwave pyrolysis with and withoutmore » catalyst showed that the catalyst increased the content of aromatic hydrocarbons and phenols. A reaction pathway was proposed for microwave assisted catalyst pyrolysis of Douglas fir pellets.« less

  16. A comparison study on microwave-assisted extraction of Artemisia sphaerocephala polysaccharides with conventional method: Molecule structure and antioxidant activities evaluation.

    PubMed

    Wang, Junlong; Zhang, Ji; Wang, Xiaofang; Zhao, Baotang; Wu, Yiqian; Yao, Jian

    2009-12-01

    The conventional extraction methods for polysaccharides were time-consuming, laborious and energy-consuming. Microwave-assisted extraction (MAE) technique was employed for the extraction of Artemisia sphaerocephala polysaccharides (ASP), which is a traditional Chinese food. The extracting parameters were optimized by Box-Behnken design. In microwave heating process, a decrease in molecular weight (M(w)) was detected in SEC-LLS measurement. A d(f) value of 2.85 indicated ASP using MAE exhibited as a sphere conformation of branched clusters in aqueous solution. Furthermore, it showed stronger antioxidant activities compared with hot water extraction. The data obtained showed that the molecular weights played a more important role in antioxidant activities.

  17. 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...

  18. Microwave-assisted extraction of rutin and quercetin from the stalks of Euonymus alatus (Thunb.) Sieb.

    PubMed

    Zhang, Fan; Yang, Yi; Su, Ping; Guo, Zhenku

    2009-01-01

    Euonymus alatus (Thunb.) has been used as one of traditional Chinese medicines for several thousand years. Conventional methods for the extraction of rutin and quercetin from E. alatus, including solvent extraction, Soxhlet extraction and heat reflux extraction are characterised by long extraction times and consumption of large amounts of solvents. To develop a simple and rapid method for the extraction of rutin and quercetin from the stalks of Euonymus alatus (Thunb.) Sieb using microwave-assisted extraction (MAE) technique. MAE experiments were performed with a multimode microwave extraction system. The experimental variables that affect the MAE process, such as the concentration of ethanol solution, extractant volume, microwave power and extraction time were optimised. Yields were determined by HPLC. The results were compared with that obtained by classical Soxhlet and ultrasonic-assisted extraction (UAE). From the optimised conditions for MAE of rutin and quercetin it can be concluded that the solvent is 50% ethanol (v/v) solution, the extractant volume is 40 mL, microwave power is 170 W and irradiation time is 6 min. Compared with Soxhlet extraction and ultrasonic extraction, microwave extraction is a rapid method with a higher yield and lower solvent consumption. The results showed that MAE can be used as an efficient and rapid method for the extraction of the active components from plants.

  19. Rapid microwave assisted synthesis of YIn1-xMnxO3 blue pigments: Synthesis, microstructure and optical properties

    NASA Astrophysics Data System (ADS)

    Zhou, Yuncheng; Jiang, Peng; Kuang, Jianlei; Yang, Xueshan; Cao, Wenbin

    2018-07-01

    The YIn1-xMnxO3 (0.1 ≤x ≤ 0.5) blue pigment samples are successfully prepared through a sol-gel process followed by microwave assisted sintering process. All the samples are shown single phases in the X-ray diffraction results. In the morphology study from scanning electronic microscope, the samples are composed of loosely connected small particles. The oxidation state of Mn is confirmed to be 3 + from the results of X-ray photonelectronic scan. The optical properties are characterized by UV-Visible spectrum and UV-visible-NIR spectrum. The samples exhibit intense blue color and they show small absorption in infrared region.

  20. Microwave assisted preparation of magnesium phosphate cement (MPC) for orthopedic applications: a novel solution to the exothermicity problem.

    PubMed

    Zhou, Huan; Agarwal, Anand K; Goel, Vijay K; Bhaduri, Sarit B

    2013-10-01

    There are two interesting features of this paper. First, we report herein a novel microwave assisted technique to prepare phosphate based orthopedic cements, which do not generate any exothermicity during setting. The exothermic reactions during the setting of phosphate cements can cause tissue damage during the administration of injectable compositions and hence a solution to the problem is sought via microwave processing. This solution through microwave exposure is based on a phenomenon that microwave irradiation can remove all water molecules from the alkaline earth phosphate cement paste to temporarily stop the setting reaction while preserving the active precursor phase in the formulation. The setting reaction can be initiated a second time by adding aqueous medium, but without any exothermicity. Second, a special emphasis is placed on using this technique to synthesize magnesium phosphate cements for orthopedic applications with their enhanced mechanical properties and possible uses as drug and protein delivery vehicles. The as-synthesized cements were evaluated for the occurrences of exothermic reactions, setting times, presence of Mg-phosphate phases, compressive strength levels, microstructural features before and after soaking in (simulated body fluid) SBF, and in vitro cytocompatibility responses. The major results show that exposure to microwaves solves the exothermicity problem, while simultaneously improving the mechanical performance of hardened cements and reducing the setting times. As expected, the cements are also found to be cytocompatible. Finally, it is observed that this process can be applied to calcium phosphate cements system (CPCs) as well. Based on the results, this microwave exposure provides a novel technique for the processing of injectable phosphate bone cement compositions. © 2013.

  1. Value-added conversion of waste cooking oil and post-consumer PET bottles into biodiesel and polyurethane foams.

    PubMed

    Dang, Yu; Luo, Xiaolan; Wang, Feng; Li, Yebo

    2016-06-01

    A sustainable process of value-added utilization of wastes including waste cooking oil (WCO) and post-consumer PET bottles for the production of biodiesel and polyurethane (PU) foams was developed. WCO collected from campus cafeteria was firstly converted into biodiesel, which can be used as vehicle fuel. Then crude glycerol (CG), a byproduct of the above biodiesel process, was incorporated into the glycolysis process of post-consumer PET bottles collected from campus to produce polyols. Thirdly, PU foams were synthesized through the reaction of the above produced polyols with isocyanate in the presence of catalysts and other additives. The characterization of the produced biodiesel demonstrated that its properties meet the specification of biodiesel standard. The effect of crude glycerol loading on the properties of polyols and PU foams were investigated. All the polyols showed satisfactory properties for the production of rigid PU foams which had performance comparable to those of some petroleum-based analogs. A mass balance and a cost analysis for the conversion of WCO and waste PET into biodiesel and PU foams were also discussed. This study demonstrated the potential of WCO and PET waste for the production of value-added products. Copyright © 2016 Elsevier Ltd. All rights reserved.

  2. TiO2-coated mesoporous carbon: conventional vs. microwave-annealing process.

    PubMed

    Coromelci-Pastravanu, Cristina; Ignat, Maria; Popovici, Evelini; Harabagiu, Valeria

    2014-08-15

    The study of coating mesoporous carbon materials with titanium oxide nanoparticles is now becoming a promising and challenging area of research. To optimize the use of carbon materials in various applications, it is necessary to attach functional groups or other nanostructures to their surface. The combination of the distinctive properties of mesoporous carbon materials and titanium oxide is expected to be applied in field emission displays, nanoelectronic devices, novel catalysts, and polymer or ceramic reinforcement. But, their synthesis is still largely based on conventional techniques, such as wet impregnation followed by chemical reduction of the metal nanoparticle precursors, which takes time and money. The thermal heating based techniques are time consuming and often lack control of particle size and morphology. Hence, since there is a growing interest in microwave technology, an alternative way of power input into chemical reactions through dielectric heating is the use of microwaves. This work is focused on the advantages of microwave-assisted synthesis of TiO2-coated mesoporous carbon over conventional thermal heating method. The reviewed studies showed that the microwave-assisted synthesis of such composites allows processes to be completed within a shorter reaction time allowing the nanoparticles formation with superior properties than that obtained by conventional method. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. 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.

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

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

    Xia Lixin; Wang Haibo; Wang Jian

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

  5. The Synergize effect of Chain extender to Phosporic acid catalyst to the ultimate property of Soy-Polyurethane

    NASA Astrophysics Data System (ADS)

    Elvistia Firdaus, Flora

    2016-04-01

    The polyurethanes (PUs) foam were made from vegetable oil; a soybean based polyol. The foams were categorized into flexible and semi rigid. This research is manufacturally designed polyurethane foams by a process requiring the reaction of mixture of 2, 4- and 2, 6-Toluene di Isocyanate isomers, soy polyol in the presence of other ingredients. The objective of this work was to functionalized soy-polyol using phosporic acid catalyst and chain extender, study their collaborative reaction in producing ultimate property of PU foam. Correlates the foam morphology images in accordance to mechanical properties of foams.

  6. Green Pea and Garlic Puree Model Food Development for Thermal Pasteurization Process Quality Evaluation.

    PubMed

    Bornhorst, Ellen R; Tang, Juming; Sablani, Shyam S; Barbosa-Cánovas, Gustavo V; Liu, Fang

    2017-07-01

    Development and selection of model foods is a critical part of microwave thermal process development, simulation validation, and optimization. Previously developed model foods for pasteurization process evaluation utilized Maillard reaction products as the time-temperature integrators, which resulted in similar temperature sensitivity among the models. The aim of this research was to develop additional model foods based on different time-temperature integrators, determine their dielectric properties and color change kinetics, and validate the optimal model food in hot water and microwave-assisted pasteurization processes. Color, quantified using a * value, was selected as the time-temperature indicator for green pea and garlic puree model foods. Results showed 915 MHz microwaves had a greater penetration depth into the green pea model food than the garlic. a * value reaction rates for the green pea model were approximately 4 times slower than in the garlic model food; slower reaction rates were preferred for the application of model food in this study, that is quality evaluation for a target process of 90 °C for 10 min at the cold spot. Pasteurization validation used the green pea model food and results showed that there were quantifiable differences between the color of the unheated control, hot water pasteurization, and microwave-assisted thermal pasteurization system. Both model foods developed in this research could be utilized for quality assessment and optimization of various thermal pasteurization processes. © 2017 Institute of Food Technologists®.

  7. Microwave-assisted routes for rapid and efficient modification of layered perovskites.

    PubMed

    Akbarian-Tefaghi, S; Wiley, J B

    2018-02-27

    Recent advances in exploiting microwave radiation in the topochemical modification of layered oxide perovskites are presented. Such methods work well for rapid bulk synthetic steps used in the production of novel inorganic-organic hybrids (protonation, grafting, intercalation, and in situ click reactions), exfoliation to produce dispersed nanosheets, and post-exfoliation processing to rapidly vary nanosheet surface groups. Compared to traditional methods that often take days, microwave methods can produce quality products in as little as 1-2 h.

  8. 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...

  9. Numerical simulation of temperature distribution in cylindrical ilmenite (FeTiO3) due to microwave heating

    NASA Astrophysics Data System (ADS)

    Hidayat, Mas Irfan P.; Fellicia, Dian Mughni; Rafandi, Ferdiansyah Iqbal

    2018-04-01

    Microwave assisted heating has been extensively used in materials processing particularly in extraction of TiO2 from Ilmenite (FeTiO3) minerals. Nevertheless, this method could generate non-uniform temperature distribution during the heating process. The observation of this phenomena in cylindrical ilmenite has been conducted by numerical simulation using finite element method according to the Poynthing's theorem. Four different cylinders with variation on its height were simulated in ANSYS 17 with input microwave power of 5.5 Kw. The results indicated that height of heated object could vigorously influence the uniformity of temperature inside the body.

  10. Optimization of continuous and intermittent microwave extraction of pectin from banana peels.

    PubMed

    Swamy, Gabriela John; Muthukumarappan, Kasiviswanathan

    2017-04-01

    Continuous and intermittent microwave-assisted extractions were used to extract pectin from banana peels. Extraction parameters which were employed in the continuous process were microwave power (300-900W), time (100-300s), pH (1-3) and in the intermittent process were microwave power (300-900W), pulse ratio (0.5-1), pH (1-3). The independent factors were optimized with the Box-Behnken response surface design (BBD) (three factor three level) with the desirability function methodology. Results indicate that the independent factors have substantial effect on the pectin yield. Optimized solutions for highest pectin yield (2.18%) from banana peels were obtained with microwave power of 900W, time 100s and pH 3.00 in the continuous method while the intermittent process yielded the highest pectin content (2.58%) at microwave power of 900W, pulse ratio of 0.5 and pH of 3.00. The optimized conditions were validated and close agreement was observed with the validation experiment and predicted value. Copyright © 2016 Elsevier Ltd. All rights reserved.

  11. 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

  12. Microwave-assisted acid pretreatment of alkali lignin: Effect on characteristics and pyrolysis behavior.

    PubMed

    Duan, Dengle; Ruan, Roger; Wang, Yunpu; Liu, Yuhuan; Dai, Leilei; Zhao, Yunfeng; Zhou, Yue; Wu, Qiuhao

    2018-03-01

    This study performed microwave-assisted acid pretreatment on pure lignin. The effects of microwave temperature, microwave time, and hydrochloric acid concentration on characteristics and pyrolysis behavior of lignin were examined. Results of ultimate analysis revealed better properties of all pretreated samples than those of raw lignin. Fourier transform infrared spectroscopy analysis showed breakage of βO4 bond and aliphatic side chain, decrease in OH groups, and formation of CO groups in pretreatment. Microwave temperature exerted more significant influence on lignin structure. Thermal stability of treated lignin was improved and insensitive to short microwave time and acid concentration under mild conditions. Resulting from improved alkyl-phenols and decreased alkoxy-phenols, microwave-assisted acid pretreatment of lignin yielded bio-oil with excellent quality. Total yield of phenols in pyrolysis vapors (200 °C) improved to 14.15%, whereas that of guaiacols decreased to 22.36%. This study shows that microwave-assisted acid pretreatment is a promising technology for lignin conversion. Copyright © 2017 Elsevier Ltd. All rights reserved.

  13. Phase Transformation of VO2 Nanoparticles Assisted by Microwave Heating

    PubMed Central

    Sikong, Lek.

    2014-01-01

    The microwave assisted synthesis nowadays attracts a great deal of attention. Monoclinic phase VO2 (M) was prepared from NH4VO3 and H2C2O4 · 2H2O by a rapid microwave assisted technique. The synthesis parameters, microwave irradiation time, microwave power, and calcinations temperature were systematically varied and their influences on the structure and morphology were evaluated. The microwave power level has been carried out in range 180–600 W. TEM analysis demonstrated nanosized samples. The structural and morphological properties were measured using XRD, TEM, and thermal analyses. The variations of vanadium phase led to thermochromic properties. PMID:24688438

  14. Microwave and continuous flow technologies in drug discovery.

    PubMed

    Sadler, Sara; Moeller, Alexander R; Jones, Graham B

    2012-12-01

    Microwave and continuous flow microreactors have become mainstream heating sources in contemporary pharmaceutical company laboratories. Such technologies will continue to benefit from design and engineering improvements, and now play a key role in the drug discovery process. The authors review the applications of flow- and microwave-mediated heating in library, combinatorial, solid-phase, metal-assisted, and protein chemistries. Additionally, the authors provide a description of the combination of microwave and continuous flow platforms, with applications in the preparation of radiopharmaceuticals and in drug candidate development. Literature reviewed is chiefly 2000 - 2012, plus key citations from earlier reports. With the advent of microwave irradiation, reactions that normally took days to complete can now be performed in a matter of minutes. Coupled with the introduction of continuous flow microreactors, pharmaceutical companies have an easy way to improve the greenness and efficiency of many synthetic operations. The combined force of these technologies offers the potential to revolutionize discovery and manufacturing processes.

  15. 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.

  16. Microwave-Irradiation-Assisted HVAC Filtration for Inactivation of Viral Aerosols (Postprint)

    DTIC Science & Technology

    2012-02-01

    Baggiani, A. and Senesi, S. (2004). Effect of Microwave Radiation on Bacillus subtilis Spores . J. Appl. Microbiol. 97: 1220–1227. Damit, B., Lee, C.N...AFRL-RX-TY-TP-2012-0020 MICROWAVE-IRRADIATION-ASSISTED HVAC FILTRATION FOR INACTIVATION OF VIRAL AEROSOLS POSTPRINT Myung-Heui Woo and...12-APR-2011 -- 11-DEC-2011 Microwave Irradiation-Assisted HVAC Filtration for Inactivation of Viral Aerosols (POSTPRINT) FA8650-06-C-5913 0602102F

  17. 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. Copyright © 2014 Elsevier Ltd. All rights reserved.

  18. One-step solution combustion synthesis of pure Ni nanopowders with enhanced coercivity: The fuel effect

    NASA Astrophysics Data System (ADS)

    Khort, Alexander; Podbolotov, Kirill; Serrano-García, Raquel; Gun'ko, Yurii K.

    2017-09-01

    In this paper, we report a new modified one-step combustion synthesis technique for production of Ni metal nanoparticles. The main unique feature of our approach is the use of microwave assisted foam preparation. Also, the effect of different types of fuels (urea, citric acid, glycine and hexamethylenetetramine) on the combustion process and characteristics of resultant solid products were investigated. It is observed that the combination of microwave assisted foam preparation and using of hexamethylenetetramine as a fuel allows producing pure ferromagnetic Ni metal nanoparticles with enhanced coercivity (78 Oe) and high value of saturation magnetization (52 emu/g) by one-step solution combustion synthesis under normal air atmosphere without any post-reduction processing.

  19. Effects of microwave power and irradiation time on pectin extraction from watermelon rinds (Citrullus lanatus) with acetic acid using microwave assisted extraction method

    NASA Astrophysics Data System (ADS)

    Sari, A. M.; Ishartani, D.; Dewanty, P. S.

    2018-01-01

    The aims of this research are to study the effect of microwave power (119.7 W, 199.5 W and 279.3 W) and irradiation time (6, 9 and 12 min) on pectin extraction by using Microwave Assisted Extraction (MAE) with acetic acid and to do a preliminary characterization of pectin from watermelon rinds. A randomized factorial design with two factors was used to determine the effect of microwave power and processing time on the yield, equivalent weight, degree of methoxylation (DM), galacturonic acid content (GA) and the degree of esterification (DE) of extracted pectin. The results showed that extracted pectin from watermelon rinds using MAE method have yield ranged from 3.925% to 5.766%, with equivalent weight ranged from 1249.702 to 2007.756. Extracted pectin have a DM value ranged from 3.89% to 10.81%. Galacturonic acid content that meets with IPPA standard resulted from extraction condition of 279.3-watt microwave power for 9 min and 12 min. The degree of esterification (DE) value ranged from 56.86% to 85.76%, and this value exhibited a relatively high methoxyl pectin (>50%). The best pectin properties was obtained at a microwave power of 279.3 watts for 12 min.

  20. Influence of Polarity and Activation Energy in Microwave–Assisted Organic Synthesis (MAOS)

    PubMed Central

    Rodríguez, Antonio M; Prieto, Pilar; de la Hoz, Antonio; Díaz-Ortiz, Ángel; Martín, D Raúl; García, José I

    2015-01-01

    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. PMID:26246993

  1. The Production of Biodiesel and Bio-kerosene from Coconut Oil Using Microwave Assisted Reaction

    NASA Astrophysics Data System (ADS)

    SAIFUDDIN, N.; SITI FAZLILI, A.; KUMARAN, P.; PEI-JUA, N.; PRIATHASHINI, P.

    2016-03-01

    Biofuels including biodiesel, an alternative fuel, is renewable, environmentally friendly, non-toxic and low emissions. The raw material used in this work was coconut oil, which contained saturated fatty acids about 90% with high percentage of medium chain (C8-C12), especially lauric acid and myristic acid. The purpose of this research was to study the effect of power and NaOH catalyst in transesterification assisted by microwave for production of biofuels (biodiesel and bio-kerosene) derived from coconut oil. The reaction was performed with oil and methanol using mole ratio of 1:6, catalyst concentration of 0.6% with microwave power at 100W, 180W, 300W, 450W, 600W, and 850W. The reaction time was set at of 3, 5, 7, 10 and 15 min. The results showed that microwave could accelerate the transesterification process to produce biodiesel and bio-kerosene using NaOH catalyst. The highest yield of biodiesel was 97.17 %, or 99.05 % conversion at 5 min and 100W microwave power. Meanwhile, the bio-kerosene obtained was 65% after distillation.

  2. Physicochemical characterization of lignin recovered from microwave-assisted delignified lignocellulosic biomass for use in biobased materials

    Treesearch

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

    2015-01-01

    Lignocellulosic biomass (Moso Bamboo, Chinese tallow tree wood, switchgrass, and pine wood) was subjected to a novel delignification process using microwave energy in a binary glycerol/methanol solvent. The physicochemical properties of the recovered lignin were analyzed prior to its application in the fabrication of polylactic acid (PLA)–lignin composites. The results...

  3. Five-minute synthesis of silver nanowires and their roll-to-roll processing for large-area organic light emitting diodes.

    PubMed

    Sim, Hwansu; Kim, Chanho; Bok, Shingyu; Kim, Min Ki; Oh, Hwisu; Lim, Guh-Hwan; Cho, Sung Min; Lim, Byungkwon

    2018-06-18

    Silver (Ag) nanowires (NWs) are promising building blocks for flexible transparent electrodes, which are key components in fabricating soft electronic devices such as flexible organic light emitting diodes (OLEDs). Typically, Ag NWs have been synthesized using a polyol method, but it still remains a challenge to produce high-aspect-ratio Ag NWs via a simple and rapid process. In this work, we developed a modified polyol method and newly found that the addition of propylene glycol to ethylene glycol-based polyol synthesis facilitated the growth of Ag NWs, allowing the rapid production of long Ag NWs with high aspect ratios of about 2000 in a high yield (∼90%) within 5 min. Transparent electrodes fabricated with our Ag NWs exhibited performance comparable to that of an indium tin oxide-based electrode. With these Ag NWs, we successfully demonstrated the fabrication of a large-area flexible OLED with dimensions of 30 cm × 15 cm using a roll-to-roll process.

  4. Processing and characterization of polyols plasticized-starch reinforced with microcrystalline cellulose.

    PubMed

    Rico, M; Rodríguez-Llamazares, S; Barral, L; Bouza, R; Montero, B

    2016-09-20

    Biocomposites suitable for short-life applications such as food packaging were prepared by melt processing and investigated. Biocomposites studied are wheat starch plasticized with two different molecular weight polyols (glycerol and sorbitol) and reinforced with various amounts of microcrystalline cellulose. The effect of the plasticizer type and the filler amount on the processing properties, the crystallization behavior and morphology developed for the materials, and the influence on thermal stability, dynamic mechanical properties and water absorption behavior were investigated. Addition of microcrystalline cellulose led to composites with good filler-matrix adhesion where the stiffness and resistance to humidity absorption were improved. The use of sorbitol as a plasticizer of starch also improved the stiffness and water uptake behavior of the material as well as its thermal stability. Biodegradable starch-based materials with a wide variety of properties can be tailored by varying the polyol plasticizer type and/or by adding microcrystalline cellulose filler. Copyright © 2016 Elsevier Ltd. All rights reserved.

  5. Microwave-assisted regeneration of synthetic zeolite used in tritium removal systems

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

    Tanaka, M.; Takayama, S.; Sano, S.

    The regeneration process using synthetic honeycomb type 5A zeolite under microwave irradiation was experimentally investigated using a single-mode cavity at 2.46 GHz. In order to investigate the effect of electromagnetic fields, inductive heating by a magnetic field was applied to synthetic zeolite containing water. Because the microwave energy absorbed in the sample was less than 15 W, the zeolite sample was only heated to a temperature of 71 C. degrees. Water desorption was observed based on the increased temperature of the zeolite sample and the thermogravimetric curve that indicated a single step phenomenon. As a result, the regeneration process ofmore » zeolite was not complete over a period of 6000 s. A comparison of dielectric heating by an electric field with inductive heating by a magnetic field showed that the regeneration process by microwave irradiation was particularly beneficial in dielectric heating. (authors)« less

  6. Effect of alkaline microwaving pretreatment on anaerobic digestion and biogas production of swine manure.

    PubMed

    Yu, Tao; Deng, Yihuan; Liu, Hongyu; Yang, Chunping; Wu, Bingwen; Zeng, Guangming; Lu, Li; Nishimura, Fumitake

    2017-05-10

    Microwave assisted with alkaline (MW-A) condition was applied in the pretreatment of swine manure, and the effect of the pretreatment on anaerobic treatment and biogas production was evaluated in this study. The two main microwaving (MW) parameters, microwaving power and reaction time, were optimized for the pretreatment. Response surface methodology (RSM) was used to investigate the effect of alkaline microwaving process for manure pretreatment at various values of pH and energy input. Results showed that the manure disintegration degree was maximized of 63.91% at energy input of 54 J/g and pH of 12.0, and variance analysis indicated that pH value played a more important role in the pretreatment than in energy input. Anaerobic digestion results demonstrated that MW-A pretreatment not only significantly increased cumulative biogas production, but also shortened the duration for a stable biogas production rate. Therefore, the alkaline microwaving pretreatment could become an alternative process for effective treatment of swine manure.

  7. Studying the effect of microwave heating on the digestion process and identification of proteins.

    PubMed

    Devi, Shobha; Wu, Bo-Hung; Chu, Pei-Yu; Liu, Yue-Pei; Wu, Hsin-Lin; Ho, Yen-Peng

    2017-02-01

    The impact of microwave irradiation on the in-solution digestion processes and the detection limit of proteins are systematically studied. Kinetic processes of many peptides produced through the trypsin digestion of various proteins under microwave heating at 50°C were investigated with MALDI-MS. This study also examines the detection limits and digestion completeness of individual proteins under microwave heating at 50°C and at different time intervals (1, 5 and 30 min) using LC-MS. We conclude that if the peptides without missed cleavage dictate the detection limit, conventional digestion will lead to a better detection limit. The detection limit may not differ between the microwave and conventional heating if the peptides with missed cleavage sites and strong intensity are formed at the very early stage (i.e., less than 1 min) and are not further digested throughout the entire digestion process. The digestion of Escherichia coli lysate was compared under conventional and short time (microwave) conditions. The number of proteins identified under conventional heating exceeded that obtained from microwave heating over heating periods less than 5 min. The overall results show that the microwave-assisted digestion is not complete. Although the sequence coverage might be better, the detection limit might be worse than that under conventional heating. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. 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.

  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 cationic polymerization of palm olein and their urea inclusion products

    NASA Astrophysics Data System (ADS)

    Soegijono, Bambang; Farid, Muhamad; Alim Mas'ud, Zainal

    2018-01-01

    Cationic polymerization is affected by the relative amount of unsaturated bond (C=C) in the compound. The enrichment of an unsaturated triglyceride fraction from oils may be performed using urea inclusion techniques. In this study, palm olein was enriched-unsaturated fraction using urea-methanol system. The palm olein and its urea-inclusion products were cationic polymerized with ethereal boron trifluoride catalyst and followed by irradiation using a commercial microwave (microwave-assisted). The microwave irradiated products were cured at 110 °C for 24 hours. Fatty acid composition of the palm olein and its urea-inclusion products were analyzed by gas chromatography. Iodine numbers, functional groups, and ultraviolet absorption spectra of all palm olein origin, urea inclusion products and polymerization products were analyzed using titrimetric, ultraviolet spectrophotometric, and Fourier Transform infrared spectrophotometric methods. Differential scanning calorimetric (DSC) was used to observe the thermal characteristics of the polymer. Urea-inclusion process increased the unsaturated fatty acid components as indicated by the increased iodine number, intensity of alkene band absorptions in the infrared spectra, and the absorbance of the ultraviolet spectra. The polymer formation is converting the C=C group to C-C, which is indicated by the opposite of the urea inclusion process. The curing process results in reformation of new C=C bonds that were similar to that of the urea inclusion process. The DSC thermogram curve shows that the enrichment process improves the thermal stability of the polymer formed.

  11. Molecular basis for polyol-induced protein stability revealed by molecular dynamics simulations

    NASA Astrophysics Data System (ADS)

    Liu, Fu-Feng; Ji, Luo; Zhang, Lin; Dong, Xiao-Yan; Sun, Yan

    2010-06-01

    Molecular dynamics simulations of chymotrypsin inhibitor 2 in different polyols (glycerol, xylitol, sorbitol, trehalose, and sucrose) at 363 K were performed to probe the molecular basis of the stabilizing effect, and the data in water, ethanol, and glycol were compared. It is found that protein protection by polyols is positively correlated with both the molecular volume and the fractional polar surface area, and the former contributes more significantly to the protein's stability. Polyol molecules have only a few direct hydrogen bonds with the protein, and the number of hydrogen bonds between a polyol and the protein is similar for different polyols. Thus, it is concluded that the direct interactions contribute little to the stabilizing effect. It is clarified that the preferential exclusion of the polyols is the origin of their protective effects, and it increases with increasing polyol size. Namely, there is preferential hydration on the protein surface (2 Å), and polyol molecules cluster around the protein at a distance of about 4 Å. The preferential exclusion of polyols leads to indirect interactions that prevent the protein from thermal unfolding. The water structure becomes more ordered with increasing the polyol size. So, the entropy of water in the first hydration shell decreases, and a larger extent of decrease is observed with increasing polyol size, leading to larger transfer free energy. The findings suggest that polyols protect the protein from thermal unfolding via indirect interactions. The work has thus elucidated the molecular mechanism of structural stability of the protein in polyol solutions.

  12. 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.

  13. Impact of structure and functionality of core polyol in highly functional biobased epoxy resins.

    PubMed

    Pan, Xiao; Webster, Dean C

    2011-09-01

    Highly functional biobased epoxy resins were prepared using dipentaerythritol (DPE), tripentaerythritol (TPE), and sucrose as core polyols that were substituted with epoxidized soybean oil fatty acids, and the impact of structure and functionality of the core polyol on the properties of the macromolecular resins and their epoxy-anhydride thermosets was explored. The chemical structures, functional groups, molecular weights, and compositions of epoxies were characterized using nuclear magnetic resonance (NMR) spectroscopy, Fourier-transform infrared (FTIR) spectroscopy, gel permeation chromatography (GPC), and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI MS). The epoxies were also studied for their bulk viscosity, intrinsic viscosity, and density. Crosslinked with dodecenyl succinic anhydride (DDSA), epoxy-anhydride thermosets were evaluated using differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), tensile tests, and tests of coating properties. Epoxidized soybean oil (ESO) was used as a control. Overall, the sucrose-based thermosets exhibited the highest moduli, having the most rigid and ductile performance while maintaining the highest biobased content. DPE/TPE-based thermosets showed modestly better thermosetting performance than the control ESO thermoset. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Development and application of a continuous fast microwave pyrolysis system for sewage sludge utilization.

    PubMed

    Zhou, Junwen; Liu, Shiyu; Zhou, Nan; Fan, Liangliang; Zhang, Yaning; Peng, Peng; Anderson, Erik; Ding, Kuan; Wang, Yunpu; Liu, Yuhuan; Chen, Paul; Ruan, Roger

    2018-05-01

    A continuous fast microwave-assisted pyrolysis system was designed, fabricated, and tested with sewage sludge. The system is equipped with continuous biomass feeding, mixing of biomass and microwave absorbent, and separated catalyst upgrading. The effect of the sludge pyrolysis temperature (450, 500, 550, and 600 °C) on the products yield, distribution and potentially energy recovery were investigated. The physical, chemical, and energetic properties of the raw sewage sludge and bio-oil, char and gas products obtained were analyzed using elemental analyzer, GC-MS, Micro-GC, SEM and ICP-OES. While the maximum bio-oil yield of 41.39 wt% was obtained at pyrolysis temperature of 550 °C, the optimal pyrolysis temperature for maximum overall energy recovery was 500 °C. The absence of carrier gas in the process may be responsible for the high HHV of gas products. This work could provide technical support for microwave-assisted system scale-up and sewage sludge utilization. Copyright © 2018 Elsevier Ltd. All rights reserved.

  15. Oil extraction from sheanut (Vitellaria paradoxa Gaertn C.F.) kernels assisted by microwaves.

    PubMed

    Nde, Divine B; Boldor, Dorin; Astete, Carlos; Muley, Pranjali; Xu, Zhimin

    2016-03-01

    Shea butter, is highly solicited in cosmetics, pharmaceuticals, chocolates and biodiesel formulations. Microwave assisted extraction (MAE) of butter from sheanut kernels was carried using the Doehlert's experimental design. Factors studied were microwave heating time, temperature and solvent/solute ratio while the responses were the quantity of oil extracted and the acid number. Second order models were established to describe the influence of experimental parameters on the responses studied. Under optimum MAE conditions of heating time 23 min, temperature 75 °C and solvent/solute ratio 4:1 more than 88 % of the oil with a free fatty acid (FFA) value less than 2, was extracted compared to the 10 h and solvent/solute ratio of 10:1 required for soxhlet extraction. Scanning electron microscopy was used to elucidate the effect of microwave heating on the kernels' microstructure. Substantial reduction in extraction time and volumes of solvent used and oil of suitable quality are the main benefits derived from the MAE process.

  16. [Extraction Optimization of Rhizome of Curcuma longa by Response Surface Methodology and Support Vector Regression].

    PubMed

    Zhou, Pei-pei; Shan, Jin-feng; Jiang, Jian-lan

    2015-12-01

    To optimize the optimal microwave-assisted extraction method of curcuminoids from Curcuma longa. On the base of single factor experiment, the ethanol concentration, the ratio of liquid to solid and the microwave time were selected for further optimization. Support Vector Regression (SVR) and Central Composite Design-Response Surface Methodology (CCD) algorithm were utilized to design and establish models respectively, while Particle Swarm Optimization (PSO) was introduced to optimize the parameters of SVR models and to search optimal points of models. The evaluation indicator, the sum of curcumin, demethoxycurcumin and bisdemethoxycurcumin by HPLC, were used. The optimal parameters of microwave-assisted extraction were as follows: ethanol concentration of 69%, ratio of liquid to solid of 21 : 1, microwave time of 55 s. On those conditions, the sum of three curcuminoids was 28.97 mg/g (per gram of rhizomes powder). Both the CCD model and the SVR model were credible, for they have predicted the similar process condition and the deviation of yield were less than 1.2%.

  17. 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. 2010 American Society for Mass Spectrometry. Published by Elsevier Inc. All rights reserved.

  18. Effect of replacing polyol by organosolv and kraft lignin on the property and structure of rigid polyurethane foam.

    PubMed

    Pan, Xuejun; Saddler, Jack N

    2013-01-28

    Lignin is one of the three major components in plant cell walls, and it can be isolated (dissolved) from the cell wall in pretreatment or chemical pulping. However, there is a lack of high-value applications for lignin, and the commonest proposal for lignin is power and steam generation through combustion. Organosolv ethanol process is one of the effective pretreatment methods for woody biomass for cellulosic ethanol production, and kraft process is a dominant chemical pulping method in paper industry. In the present research, the lignins from organosolv pretreatment and kraft pulping were evaluated to replace polyol for producing rigid polyurethane foams (RPFs). Petroleum-based polyol was replaced with hardwood ethanol organosolv lignin (HEL) or hardwood kraft lignin (HKL) from 25% to 70% (molar percentage) in preparing rigid polyurethane foam. The prepared foams contained 12-36% (w/w) HEL or 9-28% (w/w) HKL. The density, compressive strength, and cellular structure of the prepared foams were investigated and compared. Chain extenders were used to improve the properties of the RPFs. It was found that lignin was chemically crosslinked not just physically trapped in the rigid polyurethane foams. The lignin-containing foams had comparable structure and strength up to 25-30% (w/w) HEL or 19-23% (w/w) HKL addition. The results indicated that HEL performed much better in RPFs and could replace more polyol at the same strength than HKL because the former had a better miscibility with the polyol than the latter. Chain extender such as butanediol could improve the strength of lignin-containing RPFs.

  19. In-liquid Plasma. A stable light source for advanced oxidation processes in environmental remediation

    NASA Astrophysics Data System (ADS)

    Tsuchida, Akihiro; Shimamura, Takeshi; Sawada, Seiya; Sato, Susumu; Serpone, Nick; Horikoshi, Satoshi

    2018-06-01

    A microwave-inspired device that generates stable in-liquid plasma (LP) in aqueous media and emits narrow light emission lines at 280-320 nm, 660 nm and 780 nm is examined as a light source capable of driving photochemical reactions and advanced oxidation processes in wastewater treatments. The microwave-driven lighting efficiency was improved by decompressing the inside of the reaction vessel, which resulted in lowering the incident power of the microwaves and suppressed the deterioration of the microwave irradiation antenna. This protocol made it possible to generate continuous stable plasma in water. Evaluation of the LP device was carried out by revisiting the decomposition of 1,4-dioxane in aqueous media against the use of such other conventional water treatment processes as (i) UV irradiation alone, (ii) TiO2-assisted photocatalysis with UV irradiation (UV/TiO2), (iii) oxidation with sodium hypochlorite (NaClO), and (iv) UV-assisted decomposition in the presence of NaClO (UV/NaClO). The in-liquid plasma technique proved superior to these four other methods. The influence of pH on the LP protocol was ascertained through experiments in acidified (HCl and H2SO4) and alkaline (NaOH and KOH) aqueous media. Except for H2SO4, decomposition of 1,4-dioxane was enhanced in both acidic and alkaline media.

  20. 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…

  1. Microwave assisted facile hydrothermal synthesis and characterization of zinc oxide flower grown on graphene oxide sheets for enhanced photodegradation of dyes

    NASA Astrophysics Data System (ADS)

    Kashinath, L.; Namratha, K.; Byrappa, K.

    2015-12-01

    Microwave assisted hydrothermal process of synthesis of ZnO-GO nanocomposite by using ZnCl2 and NaOH as precursors is being reported first time. In this investigation, a novel route to study on synthesis, interaction, kinetics and mechanism of hybrid zinc oxide-graphene oxide (ZnO-GO) nanocomposite using microwave assisted facile hydrothermal method has been reported. The results shows that the ZnO-GO nanocomposite exhibits an enhancement and acts as stable photo-response degradation performance of Brilliant Yellow under the UV light radiation better than pure GO and ZnO nanoparticles. The microwave exposure played a vital role in the synthesis process, it facilitates with well define crystalline structure, porosity and fine morphology of ZnO/GO nanocomposite. Different molar concentrations of ZnO precursors doped to GO sheets were been synthesized, characterized and their photodegradation performances were investigated. The optical studies by UV-vis and Photo Luminescence shows an increase in band gap of nanocomposite, which added an advantage in photodegradation performance. The in situ flower like ZnO nano particles are were densely decorated and anchored on the surfaces of graphene oxide sheets which aids in the enhancement of the surface area, adsorption, mass transfer of dyes and evolution of oxygen species. The nanocomposite having high surface area and micro/mesoporous in nature. This structure and morphology supports significantly in increasing photo catalytic performance legitimate to the efficient photosensitized electron injection and repressed electron recombination due to electron transfer process with GO as electron collector and transporter dependent on the proportion of GO in ZnO/GO composite.

  2. Emerging Trends in Microwave Processing of Spices and Herbs.

    PubMed

    Rahath Kubra, Ismail; Kumar, Devender; Jagan Mohan Rao, Lingamallu

    2016-10-02

    Today, spices are integral part of our food as they provide sensory attributes such as aroma, color, flavour and taste to food. Further their antimicrobial, antioxidant, pharmaceutical and nutritional properties are also well known. Since spices are seasonal so their availability can be extended year round by adopting different preservation techniques. Drying and extraction are most important methods for preservation and value addition to spices. There are different techniques for drying of spices with their own advantages and limitations. A novel, non-conventional technique for drying of spices is use of microwave radiation. This technique proved to be very rapid, and also provide a good quality product. Similarly, there are a number of non-conventional extraction methods in use that are all, in principle, solid-liquid extractions but which introduce some form of additional energy to the process in order to facilitate the transfer of analytes from sample to solvent. This paper reviews latest advances in the use of microwave energy for drying of spices and herbs. Also, the review describes the potential application of microwave energy for extraction of essential oil/bioactive components from spices and herbs and the advantages of microwave-assisted process over the other extraction processes generally employed for extraction. It also showcases some recent research results on microwave drying/extraction from spices and herbs.

  3. A microwave plasma torch and its applications

    NASA Astrophysics Data System (ADS)

    Uhm, H. S.; Hong, Y. C.; Shin, D. H.

    2006-05-01

    A portable microwave plasma torch at atmospheric pressure by making use of magnetrons operated at 2.45 GHz and used in a home microwave oven has been developed. This electrodeless torch can be used in various areas including commercial, environmental and military applications. For example, perfluorocompounds (PFCs), which have long lifetimes and serious global warming implications, are widely used during plasma etching and plasma-assisted chamber cleaning processes in chemical vapour deposition systems. The microwave torch effectively eliminates PFCs. Efficient decomposition of toluene gas indicates the effectiveness of volatile organic compound eliminations from industrial emission and the elimination of airborne chemical and biological warfare agents. The microwave torch has been used to synthesize carbon nanotubes in an on-line system, thereby providing the opportunity of mass production of the nanotubes. There are other applications of the microwave plasma torch.

  4. Heteropoly acid-catalyzed microwave-assisted three-component aza-Diels-Alder cyclizations: diastereoselective synthesis of potential drug candidates for Alzheimer's disease.

    PubMed

    Borkin, Dmitry; Morzhina, Elena; Datta, Silpi; Rudnitskaya, Aleksandra; Sood, Abha; Török, Marianna; Török, Béla

    2011-03-07

    A highly diastereoselective microwave-assisted three component synthesis of azabicyclo[2.2.2]octan-5-ones by a silicotungstic acid-catalyzed aza-Diels-Alder cyclization is described. The one-pot process involves the formation of the in situ generated Schiff base and its immediate cyclization with cyclohex-2-enone. The short reaction times, good yields and excellent diastereoselectivity make this annulation a practical and environmentally attractive method for the synthesis of the target compounds. Preliminary assays were carried out to determine the activity of the products in AChE as well as in amyloid β fibrillogenesis inhibition.

  5. Microwave assisted combustion synthesis of nanocrystalline CoFe2O4 for LPG sensing

    NASA Astrophysics Data System (ADS)

    Chaudhari, Prashant; Acharya, S. A.; Darunkar, S. S.; Gaikwad, V. M.

    2015-08-01

    A microwave-assisted citrate precursor method has been utilized for synthesis of nanocrystalline powders of CoFe2O4. The process takes only a few minutes to obtain as-synthesized CoFe2O4. 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 CoFe2O4 prepared by screen printing towards Liquid Petroleum Gas (LPG) revealed that CoFe2O4 thick films are sensitive and shows maximum sensitivity at 350°C for 2500 ppm of LPG.

  6. 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.

  7. Integrated microwave processing system for the extraction of organophosphorus pesticides in fresh vegetables.

    PubMed

    Wu, Lijie; Song, Ying; Hu, Mingzhu; Xu, Xu; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

    2015-03-01

    A simple and efficient integrated microwave processing system (IMPS) was firstly assembled and validated for the extraction of organophosphorus pesticides in fresh vegetables. Two processes under microwave irradiation, dynamic microwave-assisted extraction (DMAE) and microwave-accelerated solvent elution (MASE), were integrated for simplifying the pretreatment of the sample. Extraction, separation, enrichment and elution were finished in a simple step. The organophosphorus pesticides were extracted from the fresh vegetables into hexane with DMAE, and then the extract was directly introduced into the enrichment column packed with active carbon fiber (ACF). Subsequently, the organophosphorus pesticides trapped on the ACF were eluted with ethyl acetate under microwave irradiation. No further filtration or cleanup was required before analysis of the eluate by gas chromatography-mass spectrometry. Some experimental parameters affecting extraction efficiency were investigated and optimized, such as microwave output power, kind and volume of extraction solvent, extraction time, amount of sorbent, elution microwave power, kind and volume of elution solvent, elution solvent flow rate. Under the optimized conditions, the recoveries were in the range of 71.5-105.2%, and the relative standard deviations were lower than 11.6%. The experiment results prove that the present method is a simple and effective sample preparation method for the determination of pesticides in solid samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. Microwave-Assisted Organic Synthesis and Transformations using Benign Reaction Media

    EPA Science Inventory

    The nonclassical heating technique using microwaves, termed as 'Bunsen burner of the 21st century, is rapidly becoming popular and is dramatically reducing the reaction times. The significant outcomes of microwave (MW)-assisted green chemistry endeavors are summarized that have r...

  9. Pyro-synthesis of a high rate nano-Li3V2(PO4)3/C cathode with mixed morphology for advanced Li-ion batteries.

    PubMed

    Kang, Jungwon; Mathew, Vinod; Gim, Jihyeon; Kim, Sungjin; Song, Jinju; Im, Won Bin; Han, Junhee; Lee, Jeong Yong; Kim, Jaekook

    2014-02-10

    A monoclinic Li3V2(PO4)3/C (LVP/C) cathode for lithium battery applications was synthesized by a polyol-assisted pyro-synthesis. The polyol in the present synthesis acts not only as a solvent, reducing agent and a carbon source but also as a low-cost fuel that facilitates a combustion process combined with the release of ultrahigh exothermic energy useful for nucleation process. Subsequent annealing of the amorphous particles at 800°C for 5 h is sufficient to produce highly crystalline LVP/C nanoparticles. A combined analysis of X-ray diffraction (XRD) and neutron powder diffraction (NPD) patterns was used to determine the unit cell parameters of the prepared LVP/C. Electron microscopic studies revealed rod-type particles of length ranging from nanometer to micrometers dispersed among spherical particles with average particle-sizes in the range of 20-30 nm. When tested for Li-insertion properties in the potential windows of 3-4.3 and 3-4.8 V, the LVP/C cathode demonstrated initial discharge capacities of 131 and 196 mAh/g (~100% theoretical capacities) at 0.15 and 0.1 C current densities respectively with impressive capacity retentions for 50 cycles. Interestingly, the LVP/C cathode delivered average specific capacities of 125 and 90 mAh/g at current densities of 9.6 C and 15 C respectively within the lower potential window.

  10. 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...

  11. Bioinspired Design of Strong, Tough, and Highly Conductive Polyol-Polypyrrole Composites for Flexible Electronics.

    PubMed

    Gao, Fengxian; Zhang, Ning; Fang, Xiaodong; Ma, Mingming

    2017-02-22

    Inspired by the dynamic network structure of animal dermis, we have designed and synthesized a series of polyol-polypyrrole (polyol-PPy) composites. Polyols and polypyrrole are cross-linked by hydrogen bonding and electrostatic interactions to form a dynamic network, which helps to dissipate destructive energy. We have found a clear correlation between the mechanical properties of polyol-PPy composites and the polyols structure. Particularly, the PEE-PPy film shows both high strength and flexibility, leading to a remarkable tensile toughness comparable to cocoon silk. The combination of outstanding strength, ductility, and conductivity enables polyol-PPy composites (especially PEE-PPy) as potential electronic materials for making flexible electronics.

  12. Overall Quality of Fruits and Vegetables Products Affected by the Drying Processes with the Assistance of Vacuum-Microwaves.

    PubMed

    Figiel, Adam; Michalska, Anna

    2016-12-30

    The seasonality of fruits and vegetables makes it impossible to consume and use them throughout the year, thus numerous processing efforts have been made to offer an alternative to their fresh consumption and application. To prolong their availability on the market, drying has received special attention as currently this method is considered one of the most common ways for obtaining food and pharmaceutical products from natural sources. This paper demonstrates the weakness of common drying methods applied for fruits and vegetables and the possible ways to improve the quality using different drying techniques or their combination with an emphasis on the microwave energy. Particular attention has been drawn to the combined drying with the assistance of vacuum-microwaves. The quality of the dried products was ascribed by chemical properties including the content of polyphenols, antioxidant capacity and volatiles as well as physical parameters such as color, shrinkage, porosity and texture. Both these fields of quality classification were considered taking into account sensory attributes and energy aspects in the perspective of possible industrial applications. In conclusion, the most promising way for improving the quality of dried fruit and vegetable products is hybrid drying consisting of osmotic dehydration in concentrated fruit juices followed by heat pump drying and vacuum-microwave finish drying.

  13. Overall Quality of Fruits and Vegetables Products Affected by the Drying Processes with the Assistance of Vacuum-Microwaves

    PubMed Central

    Figiel, Adam; Michalska, Anna

    2016-01-01

    The seasonality of fruits and vegetables makes it impossible to consume and use them throughout the year, thus numerous processing efforts have been made to offer an alternative to their fresh consumption and application. To prolong their availability on the market, drying has received special attention as currently this method is considered one of the most common ways for obtaining food and pharmaceutical products from natural sources. This paper demonstrates the weakness of common drying methods applied for fruits and vegetables and the possible ways to improve the quality using different drying techniques or their combination with an emphasis on the microwave energy. Particular attention has been drawn to the combined drying with the assistance of vacuum-microwaves. The quality of the dried products was ascribed by chemical properties including the content of polyphenols, antioxidant capacity and volatiles as well as physical parameters such as color, shrinkage, porosity and texture. Both these fields of quality classification were considered taking into account sensory attributes and energy aspects in the perspective of possible industrial applications. In conclusion, the most promising way for improving the quality of dried fruit and vegetable products is hybrid drying consisting of osmotic dehydration in concentrated fruit juices followed by heat pump drying and vacuum-microwave finish drying. PMID:28042845

  14. Fast microwave-assisted acidolysis: a new biorefinery approach for the zero-waste utilisation of lignocellulosic biomass to produce high quality lignin and fermentable saccharides.

    PubMed

    Zhou, Long; Santomauro, Fabio; Fan, Jiajun; Macquarrie, Duncan; Clark, James; Chuck, Christopher J; Budarin, Vitaliy

    2017-09-21

    Generally, biorefineries convert lignocellulosic biomass into a range of biofuels and further value added chemicals. However, conventional biorefinery processes focus mainly on the cellulose and hemicellulose fractions and therefore produce only low quality lignin, which is commonly burnt to provide process heat. To make full use of the biomass, more attention needs to be focused on novel separation techniques, where high quality lignin can be isolated that is suitable for further valorisation into aromatic chemicals and fuel components. In this paper, three types of lignocellulosic biomass (softwood, hardwood and herbaceous biomass) were processed by microwave-assisted acidolysis to produce high quality lignin. The lignin from the softwood was isolated largely intact in the solid residue after acidolysis. For example, a 10 min microwave-assisted acidolysis treatment produced lignin with a purity of 93% and in a yield of 82%, which is superior to other conventional separation methods reported. Furthermore, py-GC/MS analysis proved that the isolated lignin retained the original structure of native lignin in the feedstock without severe chemical modification. This is a large advantage, and the purified lignin is suitable for further chemical processing. To assess the suitability of this methodology as part of a biorefinery system, the aqueous phase, produced after acidolysis of the softwood, was characterised and assessed for its suitability for fermentation. The broth contained some mono- and di-saccharides but mainly contained organic acids, oligosaccharides and furans. While this is unsuitable for S. cerevisiae and other common ethanol producing yeasts, two oleaginous yeasts with known inhibitor tolerances were selected: Cryptococcus curvatus and Metschnikowia pulcherrima. Both yeasts could grow on the broth, and demonstrated suitable catabolism of the oligosaccharides and inhibitors over 7 days. In addition, both yeasts were shown to be able to produce an oil with a similar composition to that of palm oil. This preliminary work demonstrates new protocols of microwave-assisted acidolysis and therefore offers an effective approach to produce high purity lignin and fermentable chemicals, which is a key step towards developing a zero-waste lignocellulosic biorefinery.

  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. Effect of microwave-assisted sintering on dielectric properties of CaCu3Ti4O12 ceramic

    NASA Astrophysics Data System (ADS)

    Rani, Suman; Ahlawat, Neetu; Punia, R.; Kundu, R. S.; Ahlawat, N.

    2016-05-01

    In this present work, CaCu3Ti4O12 (CCTO) was synthesized by conventional solid-state reaction technique. The synthesis process was carried out in two phases; by conventional process (calcination and sintering at 1080°C for 10 hours) and phase II involves the micro assisted pre sintering of conventionally calcined CCTO for very short soaking time of 30 min at 1080°C in a microwave furnace followed by sintering at 1080°C for 10 hours in conventional furnace. X-ray diffraction (XRD) patterns confirmed the formation of single phase ceramic. Dielectric properties were studied over the frequency range from 50Hz -5MHz at temperatures (273K-343K). It was observed that pre- microwave sintering enhance the dielectric constant values from 10900 to 11893 and respectively reduces the dielectric loss values from 0.49 to 0.34 at room temperature(1 KHz). CCTO ceramics which are found desirable for many technological applications. The effect is more pronounced at low frequencies of applied electric field.

  17. Influence of polyols on the formation of nanocrystalline nickel ferrite inside silica matrices

    NASA Astrophysics Data System (ADS)

    Stoia, Marcela; Barvinschi, Paul; Barbu-Tudoran, Lucian; Bunoiu, Mădălin

    2017-01-01

    We have synthesized nickel ferrite/silica nanocomposites, using a modified sol-gel method that combines the sol-gel processing with the thermal decomposition of metal-organic precursors, leading to a homogenous dispersion of ferrite nanoparticles within the silica matrix and a narrow size distribution. We used as starting materials tetraethyl orthosilicate (TEOS) as source of silica, Fe(III) and Ni(II) nitrates as sources of metal cations, and polyols as reducing agent (polyvinyl alcohol, 1,4-butanediol and their mixture). TG/DTA coupled technique evidenced the redox interaction between the polyol and the mixture of metal nitrates during the heating of the gel, with formation of nickel ferrite precursors in the pores of the silica-gels. FT-IR spectroscopy confirmed the formation of metal carboxylates inside the silica-gels and the interaction of the polyols with the Si-OH groups of the polysiloxane network. X-ray diffractometry evidenced that in case of nanocomposites obtained by using a single polyol, nickel ferrite forms as single crystalline phase inside the amorphous silica matrix, while in case of using a mixture of polyols the nickel oxide appears as a secondary phase. TEM microscopy and elemental mapping evidenced the fine nature of the obtained nickel ferrite nanoparticles that are homogenously dispersed within the silica matrix. The obtained nanocomposites exhibit magnetic behavior very close to superparamagnetism slightly depending on the presence and nature of the organic compounds used in synthesis; the magnetization reached at 5 kOe magnetic field was 7 emu/g for all composites.

  18. 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...

  19. Influence of microwaves on the leaching kinetics of uraninite from a low grade ore in dilute sulfuric acid.

    PubMed

    Madakkaruppan, V; Pius, Anitha; T, Sreenivas; Giri, Nitai; Sarbajna, Chanchal

    2016-08-05

    This paper describes a study on microwave assisted leaching of uranium from a low-grade ore of Indian origin. The host rock for uranium mineralization is chlorite-biotite-muscovite-quartzo-feldspathic schist. The dominant presence of siliceous minerals determined leaching of uranium values in sulfuric acid medium under oxidizing conditions. Process parametric studies like the effect of sulfuric acid concentration (0.12-0.50M), redox potential (400-500mV), particle size (600-300μm) and temperature (35°-95°C) indicated that microwave assisted leaching is more efficient in terms of overall uranium dissolution, kinetics and provide relatively less impurities (Si, Al, Mg and Fe) in the leach liquor compared to conventional conductive leaching. The kinetics of leaching followed shrinking core model with product layer diffusion as controlling mechanism. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Optimization of enzymes-microwave-ultrasound assisted extraction of Lentinus edodes polysaccharides and determination of its antioxidant activity.

    PubMed

    Yin, Chaomin; Fan, Xiuzhi; Fan, Zhe; Shi, Defang; Gao, Hong

    2018-05-01

    Enzymes-microwave-ultrasound assisted extraction (EMUE) method had been used to extract Lentinus edodes polysaccharides (LEPs). The enzymatic temperature, enzymatic pH, microwave power and microwave time were optimized by response surface methodology. The yields, properties and antioxidant activities of LEPs from EMUE and other extraction methods including hot-water extraction, enzymes-assisted extraction, microwave-assisted extraction and ultrasound-assisted extraction were evaluated. The results showed that the highest LEPs yield of 9.38% was achieved with enzymatic temperature of 48°C, enzymatic pH of 5.0, microwave power of 440W and microwave time of 10min, which correlated well with the predicted value of 9.79%. Additionally, LEPs from different extraction methods possessed typical absorption peak of polysaccharides, which meant different extraction methods had no significant effects on type of glycosidic bonds and sugar ring of LEPs. However, SEM images of LEPs from different extraction methods were significantly different. Moreover, the different LEPs all showed antioxidant activities, but LEPs from EMUE showed the highest reducing power when compared to other LEPs. The results indicated LEPs from EMUE can be used as natural antioxidant component in the pharmaceutical and functional food industries. Copyright © 2018 Elsevier B.V. All rights reserved.

  1. Microwave-Assisted Preparation of Activated Carbon from Eupatorium Adenophorum: Effects of Preparation Parameters

    NASA Astrophysics Data System (ADS)

    Cheng, Song; Zhang, Shengzhou; Zhang, Libo; Xia, Hongying; Peng, Jinhui; Wang, Shixing

    2017-09-01

    Eupatorium adenophorum, global exotic weeds, was utilized as feedstock for preparation of activated carbon (AC) via microwave-induced KOH activation. Influences of the three vital process parameters - microwave power, activation time and impregnation ratio (IR) - have been assessed on the adsorption capacity and yield of AC. The process parameters were optimized utilizing the Design Expert software and were identified to be a microwave power of 700 W, an activation time of 15 min and an IR of 4, with the resultant iodine adsorption number and yield being 2,621 mg/g and 28.25 %, respectively. The key parameters that characterize the AC such as the brunauer emmett teller (BET) surface area, total pore volume and average pore diameter were estimated to be 3,918 m2/g, 2,383 ml/g and 2.43 nm, respectively, under the optimized process conditions. The surface characteristics of AC were characterized by Fourier transform infrared spectroscopy, scanning electron microscope and Transmission electron microscope.

  2. Synthesis and Raman analysis of SnS nanoparticles synthesized by PVP assisted polyol method

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

    Baby, Benjamin Hudson; Mohan, D. Bharathi, E-mail: d.bharathimohan@gmail.com

    2015-06-24

    SnS film was prepared by a simple drop casting method after synthesizing SnS nanoparticles by using PVP assisted polyol method. Confocal Raman study was carried out for the as deposited and annealed (150, 300 and 400 °C) films at two different excitation wavelengths 514 and 785 nm. At the excitation wavelength of 514 nm, the Raman modes showed for a mixed phase of SnS and SnS{sub 2} up to 150 °C and then only a pure SnS phase was observed up to 400 °C due to the dissociation of SnS{sub 2} in to SnS by releasing S. The increase in intensity ofmore » Raman (A{sub g} and B{sub 3g}) as well as IR (B{sub 3u}) active modes of SnS are observed with increasing annealing temperature at excitation wavelength 785 nm due to the increased crystallinity and inactiveness of SnS{sub 2} modes. X-ray diffraction confirming the formation of a single phase of SnS while the greater homogeneity in both size and shape of SnS nanoparticles were confirmed through surface morphology from SEM.« less

  3. Extraction of bioactives from Orthosiphon stamineus using microwave and ultrasound-assisted techniques: Process optimization and scale up.

    PubMed

    Chan, Chung-Hung; See, Tiam-You; Yusoff, Rozita; Ngoh, Gek-Cheng; Kow, Kien-Woh

    2017-04-15

    This work demonstrated the optimization and scale up of microwave-assisted extraction (MAE) and ultrasonic-assisted extraction (UAE) of bioactive compounds from Orthosiphon stamineus using energy-based parameters such as absorbed power density and absorbed energy density (APD-AED) and response surface methodology (RSM). The intensive optimum conditions of MAE obtained at 80% EtOH, 50mL/g, APD of 0.35W/mL, AED of 250J/mL can be used to determine the optimum conditions of the scale-dependent parameters i.e. microwave power and treatment time at various extraction scales (100-300mL solvent loading). The yields of the up scaled conditions were consistent with less than 8% discrepancy and they were about 91-98% of the Soxhlet extraction yield. By adapting APD-AED method in the case of UAE, the intensive optimum conditions of the extraction, i.e. 70% EtOH, 30mL/g, APD of 0.22W/mL, AED of 450J/mL are able to achieve similar scale up results. Copyright © 2016 Elsevier Ltd. All rights reserved.

  4. Optimization of the Microwave-Assisted Ethanosolv Extraction of Lignocellulosic Compounds from the Bagasse of Agave angustifolia Haw Using the Response Methodology.

    PubMed

    Hernández, Yuliana Rosas; García Serrano, Luz Arcelia; Maruri, Daniel Tapia; Jiménez Aparicio, Antonio Ruperto; Camacho Díaz, Brenda Hildeliza; Arenas Ocampo, Martha Lucía

    2018-04-04

    The main objective of this work was to optimize the process of fractionation of the bagasse of Agave angustifolia Haw, applying organosolv assisted with microwaves. The DCC was used to evaluate the effect of independent variables such as ethanol concentration (40, 50, and 60%) and reaction time (1, 1.5, and 2 h) on yield, cellulose and lignin percentages. Lignocellulosic fractions (F1 and F2) were obtained by means of organosolv assisted with microwave in an open system (atmospheric pressure) and a closed system (controlled pressure). The lignocellulosic fractions were microstructurally characterized. The highest extraction yields (70.39%) were reached in the open system at 50% ethanol for 1.5 h. The highest percentages of LK (5.05%) were obtained in the closed system at 60% ethanol for 2 h. The SEM photomicrograph showed that the microstructure of F1 was retained even after treatment with 60% ethanol for 2 h, and the exposure of the fibrillar part was observed obtaining the disposition of pectin.

  5. Effect of replacing polyol by organosolv and kraft lignin on the property and structure of rigid polyurethane foam

    PubMed Central

    2013-01-01

    Background Lignin is one of the three major components in plant cell walls, and it can be isolated (dissolved) from the cell wall in pretreatment or chemical pulping. However, there is a lack of high-value applications for lignin, and the commonest proposal for lignin is power and steam generation through combustion. Organosolv ethanol process is one of the effective pretreatment methods for woody biomass for cellulosic ethanol production, and kraft process is a dominant chemical pulping method in paper industry. In the present research, the lignins from organosolv pretreatment and kraft pulping were evaluated to replace polyol for producing rigid polyurethane foams (RPFs). Results Petroleum-based polyol was replaced with hardwood ethanol organosolv lignin (HEL) or hardwood kraft lignin (HKL) from 25% to 70% (molar percentage) in preparing rigid polyurethane foam. The prepared foams contained 12-36% (w/w) HEL or 9-28% (w/w) HKL. The density, compressive strength, and cellular structure of the prepared foams were investigated and compared. Chain extenders were used to improve the properties of the RPFs. Conclusions It was found that lignin was chemically crosslinked not just physically trapped in the rigid polyurethane foams. The lignin-containing foams had comparable structure and strength up to 25-30% (w/w) HEL or 19-23% (w/w) HKL addition. The results indicated that HEL performed much better in RPFs and could replace more polyol at the same strength than HKL because the former had a better miscibility with the polyol than the latter. Chain extender such as butanediol could improve the strength of lignin-containing RPFs. PMID:23356502

  6. Ultrasonic Spray Drying vs High Vacuum and Microwaves Technology for Blueberries

    NASA Astrophysics Data System (ADS)

    Candia-Muñoz, N.; Ramirez-Bunster, M.; Vargas-Hernández, Y.; Gaete-Garretón, L.

    Interest in high quality foods: good taste and a high content of nutrients with healthy beneficial effects are increasing. Fruits have good properties but, they are lost because the oxidation process, additionally, for different reasons a 40% of harvested fruit are lost. To conserve the fruit properties an ultrasonic assisted spray dryer was developed and tested, comparing its results with microwave-vacuum drying technology. Results did shown taste, color, smell, particle shape and size distribution better than the conventional one. The antioxidants conservation were quite good except in the anthocyanins, in which the microwave and vacuum technology shown best results.

  7. Microwave-assisted ignition

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

    Bechtold, J.K.; Booty, M.R.; Kriegsmann, G.A.

    1996-12-31

    In recent years, microwave heating has been proposed as an alternative to ignite materials during the process of self-propagating high-temperature synthesis. The microwave heating and ignition of a combustible material is modeled and analyzed in the small Biot number and large activation energy regimes. Both the temporal and spatial evolution of the temperature within the material are described. The ignition characteristics are determined by a localized equation for the perturbation to the inert temperature, which is shown to exhibit thermal runaway behavior. Analysis of this local equation provides explicit ignition conditions in terms of the physical parameters in the problem.

  8. 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...

  9. Microwave-assisted solid phase conversion study of Meldrum's acid to ethylenetetracarboxylic dianhydride (C 6O 6)

    NASA Astrophysics Data System (ADS)

    Taherpour, Avat (Arman)

    2010-01-01

    Utilization of microwave irradiation provides an effective method for fast synthesizing of some important compounds. Microwave-assisted solid phase is an especial class in chemical synthesis. By the use of MW-irradiation on chemicals, sometimes interesting results can be seen. The synthesis of the interesting molecule ethylenetetracarboxylic dianhydride (C 6O 6) was attempted with a few different methods. In this study, the microwave-assisted solid phase conversion of Meldrum's acid to ethylenetetracarboxylic dianhydride was reported. This conversion was characterized by FT-IR, GC/MS and NMR spectroscopy results.

  10. Microwave-Assisted Extraction for Microalgae: From Biofuels to Biorefinery

    PubMed Central

    Pandhal, Jagroop

    2018-01-01

    The commercial reality of bioactive compounds and oil production from microalgal species is constrained by the high cost of production. Downstream processing, which includes harvesting and extraction, can account for 70–80% of the total cost of production. Consequently, from an economic perspective extraction technologies need to be improved. Microalgal cells are difficult to disrupt due to polymers within their cell wall such as algaenan and sporopollenin. Consequently, solvents and disruption devices are required to obtain products of interest from within the cells. Conventional techniques used for cell disruption and extraction are expensive and are often hindered by low efficiencies. Microwave-assisted extraction offers a possibility for extraction of biochemical components including lipids, pigments, carbohydrates, vitamins and proteins, individually and as part of a biorefinery. Microwave technology has advanced since its use in the 1970s. It can cut down working times and result in higher yields and purity of products. In this review, the ability and challenges in using microwave technology are discussed for the extraction of bioactive products individually and as part of a biorefinery approach. PMID:29462888

  11. 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…

  12. Preparation and properties of poly HTBN-based urethane-urea/organo reactive montmorillonite nanocomposites

    NASA Astrophysics Data System (ADS)

    Li, Zai-Feng; Wu, Yuan; Zhang, Fu-Tao; Cao, Yu-Yang; Wu, Shou-Peng; Wang, Ting

    2012-12-01

    With ultrasonic assistant mixing way, an intercalated mixture of polyol/organo reactive montmorillonite (ORMMT) was pretreated. The prepolymer composed MMT clay was prepared by reaction of polyol/ORMMT mixture with toluene diisocyanate (TDI). The resultant prepolymer reacted with extender (DMTDA) and then the polyurethane-urea/organo reactive montmorillonite (PUU/ORMMT) nanocomposites were obtained. The structure, morphology and properties of PUU/ORMMT nanocomposites were characterized by FT-IR, TEM, AFM, strain-stress machine, TGA, and dynamic mechanical analysis (DMA). The results showed that when the OMMT content is 3%, the PUU/ORMMT nanocomposities performed super mechanical properties. Because of the presence of ORMMT, both T g of the soft segment and tan δ of the PUU increased, and the decomposition temperature for the first step and the second step increased respectively. TEM images showed that the organophilic MMT particles in the PUU composite exhibit a high degree of intercalation and exfoliation.

  13. PETI-298 Prepared by Microwave Synthesis: Neat Resin and Composite Properties

    NASA Technical Reports Server (NTRS)

    Smith, Joseph G.; Connell, John W.; Li, Chao-Jun; Wu, Wei; Criss, Jim M., Jr.

    2004-01-01

    PETI-298 is a high temperature/high performance matrix resin that is processable into composites by resin transfer molding (RTM), resin infusion and vacuum assisted RTM techniques. It is typically synthesized in a polar aprotic solvent from the reaction of an aromatic anhydride and a combination of diamines and endcapped with phenylethynylphthalic anhydride. Microwave synthesis of PETI-298 was investigated as a means to eliminate solvent and decrease reaction time. The monomers were manually mixed and placed in a microwave oven for various times to determine optimum reaction conditions. The synthetic process was subsequently scaled-up to 330g. Three batches were synthesized and combined to give 1 kg of material that was characterized for thermal and rheological properties and compared to PETI-298 prepared by the classic solution based synthetic method. The microwave synthesized PETI-298 was subsequently used to fabricate flat laminates on T650 carbon fabric by RTM. The composite panels were analyzed and mechanical properties determined and compared with those fabricated from PETI-298 prepared by the classic solution method. The microwave synthesis process and characterization of neat resin and carbon fiber reinforced composites fabricated by RTM will be presented. KEY WORDS: Resin Transfer Molding, High Temperature Polymers, Phenylethynyl Terminated Imides, Microwave Synthesis

  14. Eco-friendly microwave-assisted protocol to prepare hyaluronan-fatty acid conjugates and to induce their self-assembly process.

    PubMed

    Calce, Enrica; Mercurio, Flavia Anna; Leone, Marilisa; Saviano, Michele; De Luca, Stefania

    2016-06-05

    An environmentally sustainable and energy-efficient synthetic process has been developed to prepare hyaluronan-based nano-sized material. It consists in a microwave-promoted acylation of the hydroxyl function of the polysaccharide with natural fatty acids, performed under solvent-free conditions. The efficient interaction of the solid reagents with the MW radiation accounts for the obtained high yielded products. The self-assembly process of the obtained compounds very fast occurred in an aqueous medium under MW-radiation, thus allowing the development of a green protocol for the nano-particles preparation. Copyright © 2016 Elsevier Ltd. All rights reserved.

  15. Role of polyols (erythritol, xylitol and sorbitol) on the structural stabilization of collagen

    NASA Astrophysics Data System (ADS)

    Usha, R.; Raman, S. Sundar; Subramanian, V.; Ramasami, T.

    2006-10-01

    The effect of erythritol, xylitol and sorbitol on monomeric collagen solution was evaluated with melting temperature, fluorescence studies, conformational stability and binding energy. The emission intensity and the melting temperature increase as the chain length of polyols increases. Circular dichroism (CD) results indicate the possibility of aggregation of collagen in the presence of polyols. The interaction between collagen and polyols were calculated using binding energy, RMS deviation with collagen like models. Molecular mechanics calculations suggest that polyols bind well with collagen models, that have serine in the X position. The stability of collagen decreases as the number of carbon atoms present in the polyols increases.

  16. Coupled microwave ECR and radio-frequency plasma source for plasma processing

    DOEpatents

    Tsai, Chin-Chi; Haselton, Halsey H.

    1994-01-01

    In a dual plasma device, the first plasma is a microwave discharge having its own means of plasma initiation and control. The microwave discharge operates at electron cyclotron resonance (ECR), and generates a uniform plasma over a large area of about 1000 cm.sup.2 at low pressures below 0.1 mtorr. The ECR microwave plasma initiates the second plasma, a radio frequency (RF) plasma maintained between parallel plates. The ECR microwave plasma acts as a source of charged particles, supplying copious amounts of a desired charged excited species in uniform manner to the RF plasma. The parallel plate portion of the apparatus includes a magnetic filter with static magnetic field structure that aids the formation of ECR zones in the two plasma regions, and also assists in the RF plasma also operating at electron cyclotron resonance.

  17. Coupled microwave ECR and radio-frequency plasma source for plasma processing

    DOEpatents

    Tsai, C.C.; Haselton, H.H.

    1994-03-08

    In a dual plasma device, the first plasma is a microwave discharge having its own means of plasma initiation and control. The microwave discharge operates at electron cyclotron resonance (ECR), and generates a uniform plasma over a large area of about 1000 cm[sup 2] at low pressures below 0.1 mtorr. The ECR microwave plasma initiates the second plasma, a radio frequency (RF) plasma maintained between parallel plates. The ECR microwave plasma acts as a source of charged particles, supplying copious amounts of a desired charged excited species in uniform manner to the RF plasma. The parallel plate portion of the apparatus includes a magnetic filter with static magnetic field structure that aids the formation of ECR zones in the two plasma regions, and also assists in the RF plasma also operating at electron cyclotron resonance. 4 figures.

  18. 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…

  19. 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.

  20. Production of polyol oils from soybean oil by Pseudomonas aeruginosa E03-12.

    USDA-ARS?s Scientific Manuscript database

    Soy-polyols are important starting materials for the manufacture of polymers such as polyurethane. We have been trying to develop a bioprocess for the production of polyol oils directly from soybean oil. We reported earlier the polyol products produced from soybean oil by Acinetobacter haemolyticus ...

  1. 40 CFR 721.7500 - Nitrate polyether polyol (generic name).

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 32 2012-07-01 2012-07-01 false Nitrate polyether polyol (generic name... Substances § 721.7500 Nitrate polyether polyol (generic name). (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance nitrate polyether polyol (PMN P88-2540) is...

  2. 40 CFR 721.7500 - Nitrate polyether polyol (generic name).

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 32 2013-07-01 2013-07-01 false Nitrate polyether polyol (generic name... Substances § 721.7500 Nitrate polyether polyol (generic name). (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance nitrate polyether polyol (PMN P88-2540) is...

  3. 40 CFR 721.7500 - Nitrate polyether polyol (generic name).

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 31 2011-07-01 2011-07-01 false Nitrate polyether polyol (generic name... Substances § 721.7500 Nitrate polyether polyol (generic name). (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance nitrate polyether polyol (PMN P88-2540) is...

  4. 40 CFR 721.7500 - Nitrate polyether polyol (generic name).

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 31 2014-07-01 2014-07-01 false Nitrate polyether polyol (generic name... Substances § 721.7500 Nitrate polyether polyol (generic name). (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance nitrate polyether polyol (PMN P88-2540) is...

  5. Organo- and nano-catalyst in greener reaction medium: Microwave-assisted expedient synthesis of fine chemicals

    EPA Science Inventory

    The use of emerging microwave (MW) -assisted chemistry techniques is dramatically reducing chemical waste and reaction times in several organic syntheses and chemical transformations. A brief account of our experiences in developing MW-assisted organic transformations, which invo...

  6. A new method for the preparation of a Fe{sub 3}O{sub 4}/graphene hybrid material and its applications in electromagnetic wave absorption

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

    Wu, Tsung-Yung; Lu, Kai-Tai; Peng, Cheng-Hsiung

    2015-10-15

    Graphical abstract: A microwave-assisted solvothermal process was used to prepare Fe{sub 3}O{sub 4} nanoparticles/graphene hybrids, which could be applied as an electromagnetic (EM) radiation absorbent. The absorber, composed of 20 wt% Fe{sub 3}O{sub 4}/graphene–epoxy, exhibited a dual-frequency reflection characteristic covering the C and Ku bands with maximum reflection losses of less than −20 dB at thicknesses of 4 and 5 mm. - Highlights: • Fe{sub 3}O{sub 4}/graphene composites were prepared by a microwave-assisted solvothermal route. • Uniform loading of Fe{sub 3}O{sub 4} nanoparticles on graphene was obtained. • The products as-synthesized show great promise as a microwave absorption material. •more » Synergistic effects of Fe{sub 3}O{sub 4} and graphene caused improved absorption efficiency. • The Fe{sub 3}O{sub 4}/graphene product possessed a dual-frequency reflection characteristic. - Abstract: A rapid, simple, and inexpensive process combining a microwave-assisted technique and a solvothermal method has been developed using graphene sheets and FeCl{sub 3}·6H{sub 2}O as the reactant to prepare graphene/Fe{sub 3}O{sub 4} nanoparticle hybrids, which can be applied as an electromagnetic radiation absorbent. The experimental factors (i.e., composition ratio, microwave power, and irradiation time) on the products’ characteristics were examined. Under optimal conditions, the morphological analysis revealed that the graphene sheet was homogeneously covered with Fe{sub 3}O{sub 4} nanoparticles (∼50 nm). The electromagnetic parameters of the composites made from 20 wt% Fe{sub 3}O{sub 4}/graphene–epoxy were measured by a vector network analyzer. It was found that the 4- and 5 mm-thick composites could attain a reflection loss below −20 dB in the dual-ranges of 4–8 and 12–18 GHz.« less

  7. The formation of hollow poly(methyl methacrylate)/multiwalled carbon nanotube nanocomposite cylinders by microwave irradiation.

    PubMed

    Wang, Huan; Feng, Jiyun; Hu, Xijun; Ming Ng, Ka

    2009-03-04

    Poly(methyl methacrylate) (PMMA)/multiwalled carbon nanotube (MWCNT) nanocomposite particles with 1, 2 and 4 wt% of MWCNTs were prepared by mechanical grinding of PMMA and MWCNT powders in a mortar at room temperature. Both scanning electron microscopy and Raman scattering characterizations revealed that these nanocomposite particles consist of a PMMA core and a MWCNT shell. The PMMA/MWCNT nanocomposite particles were used to fabricate the corresponding nanocomposites in the form of a hollow cylinder with various diameters and heights under 700 W microwave irradiation within 1 min. A mechanism for the fast microwave assisted forming process is proposed. These experimental results may lead to a new technology for forming hollow polymeric articles that is different from the conventional injection and blowing process.

  8. 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

  9. 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.

  10. Advancing microwave technology for dehydration processing of biologics.

    PubMed

    Cellemme, Stephanie L; Van Vorst, Matthew; Paramore, Elisha; Elliott, Gloria D

    2013-10-01

    Our prior work has shown that microwave processing can be effective as a method for dehydrating cell-based suspensions in preparation for anhydrous storage, yielding homogenous samples with predictable and reproducible drying times. In the current work an optimized microwave-based drying process was developed that expands upon this previous proof-of-concept. Utilization of a commercial microwave (CEM SAM 255, Matthews, NC) enabled continuous drying at variable low power settings. A new turntable was manufactured from Ultra High Molecular Weight Polyethylene (UHMW-PE; Grainger, Lake Forest, IL) to provide for drying of up to 12 samples at a time. The new process enabled rapid and simultaneous drying of multiple samples in containment devices suitable for long-term storage and aseptic rehydration of the sample. To determine sample repeatability and consistency of drying within the microwave cavity, a concentration series of aqueous trehalose solutions were dried for specific intervals and water content assessed using Karl Fischer Titration at the end of each processing period. Samples were dried on Whatman S-14 conjugate release filters (Whatman, Maidestone, UK), a glass fiber membrane used currently in clinical laboratories. The filters were cut to size for use in a 13 mm Swinnex(®) syringe filter holder (Millipore(™), Billerica, MA). Samples of 40 μL volume could be dehydrated to the equilibrium moisture content by continuous processing at 20% with excellent sample-to-sample repeatability. The microwave-assisted procedure enabled high throughput, repeatable drying of multiple samples, in a manner easily adaptable for drying a wide array of biological samples. Depending on the tolerance for sample heating, the drying time can be altered by changing the power level of the microwave unit.

  11. Spark-plasma-sintering magnetic field assisted compaction of Co{sub 80}Ni{sub 20} nanowires for anisotropic ferromagnetic bulk materials

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

    Ouar, Nassima; Schoenstein, Frédéric; Mercone, Silvana

    We developed a two-step process showing the way for sintering anisotropic nanostructured bulk ferromagnetic materials. A new reactor has been optimized allowing the synthesis of several grams per batch of nanopowders via a polyol soft chemistry route. The feasibility of the scale-up has been successfully demonstrated for Co{sub 80}Ni{sub 20} nanowires and a massic yield of ∼97% was obtained. The thus obtained nanowires show an average diameter of ∼6 nm and a length of ∼270 nm. A new bottom-up strategy allowed us to compact the powder into a bulk nanostructured system. We used a spark-plasma-sintering technique under uniaxial compression andmore » low temperature assisted by a permanent magnetic field of 1 T. A macroscopic pellet of partially aligned nanowire arrays has been easily obtained. This showed optimized coercive properties along the direction of the magnetic field applied during compaction (i.e., the nanowires' direction)« less

  12. Enhanced degradation of 4-nitrophenol by microwave assisted Fe/EDTA process.

    PubMed

    Liu, Bo; Li, Song; Zhao, Yongjun; Wu, Wenfei; Zhang, Xuxiang; Gu, Xueyuan; Li, Ruihua; Yang, Shaogui

    2010-04-15

    A microwave assisted zero-valent iron oxidation process was studied in order to investigate the synergetic effects of MW irradiation on Fe/EDTA system (Fe/EDTA/MW) treated 4-nitrophenol (4-NP) from aqueous solution. The results indicated that the thermal effect of microwave improved the removal effect of 4-NP and TOC through raising the temperature of the system, as well as the non-thermal effect generated by the interaction between the microwave and the Fe resulting in an increase in the hydrophobic character of Fe surface. During the degradation of 4-NP in Fe/EDTA/MW system, the optimum value for MW power, Fe, EDTA dosage was 400 W, 2 g and 0.4 mM, respectively. The possible pathway for degrading the 4-NP was proposed based on GC/MS and HPLC analysis of the degradation intermediates. The concentration change course of the main bio-refractory by-products, the aminophenol formed in the degradation of 4-NP suggested a more efficient degradation and mineralization in Fe/EDTA/MW system. Finally, BOD(5)/COD(Cr) of the solution increased from 0.237 to 0.635 after reaction for 18 min, indicating that the biodegradability of wastewater was greatly improved by Fe/EDTA/MW system and would benefit to further treatment by biochemical methods. Crown Copyright 2009. Published by Elsevier B.V. All rights reserved.

  13. Polyol-mediated thermolysis process for the synthesis of MgO nanoparticles and nanowires

    NASA Astrophysics Data System (ADS)

    Subramania, A.; Vijaya Kumar, G.; Sathiya Priya, A. R.; Vasudevan, T.

    2007-06-01

    The main aim of this work is to prepare MgO nanoparticles and nanowires by a novel polyol-mediated thermolysis (PMT) process. The influence of different mole concentration of magnesium acetate, polyvinyl pyrrolidone (PVP; capping agent) and ethylene glycol (EG; solvent as well as reducing agent) on the formation of nanoparticles and nanowires and the effect of calcination on the crystalline size of the samples were also examined. The resultant oxide structure, thermal behaviour, size and shape have been studied using x-ray diffraction (XRD) studies, thermal (TG/DTA) analysis and scanning electron microscopy (SEM)/transmission electron microscopy (TEM) respectively.

  14. Optimized microwave-assistant extraction combined ultrasonic pretreatment of flavonoids from Periploca forrestii Schltr. and evaluation of its anti-allergic activity.

    PubMed

    Liang, Qian; Chen, Huaguo; Zhou, Xin; Deng, Qingfang; Hu, Enming; Zhao, Chao; Gong, Xiaojian

    2017-04-01

    Microwave extraction combined ultrasonic pretreatment of flavonoids from Periploca forrestii Schltr. was investigated in this study, extraction process was first performed in an ultrasonic cleaner, then treated by microwave irradiation. The optimum ultrasonic time of 25 min was selected by single-factor experiments. A response surface methodology has been used to obtain a mathematical model that describes the process and analyzes the significant parameters ethanol concentration 59.92%, liquid to raw materials ratio 21.24 mL/g, microwave radiation time 209.53 s, and microwave power 274.14 w. In these optimum conditions, the yield of flavonoids from P. forrestii (TFPF) could be up to 9.11 ± 0.08%, which was increased by 14.30 and 19.86% compared microwave extraction and ultrasonic extraction, respectively. In vitro suppress hyaluronidase experimentation showed that TFPF purified using polyamide exhibited good anti-hyaluronidase ability with IC 50 value of 1.033 mg/mL, possessing certain anti-antiallergic and potential application prospect in pharmaceutical production of treating inflammation and other related fields. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. 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.

  16. Rapid and solvent-saving liquefaction of woody biomass using microwave-ultrasonic assisted technology.

    PubMed

    Lu, Zexiang; Wu, Zhengguo; Fan, Liwei; Zhang, Hui; Liao, Yiqiang; Zheng, Deyong; Wang, Siqun

    2016-01-01

    A novel process to rapidly liquefy sawdust using reduced quantities of solvent, was successfully carried out via microwave-ultrasonic assisted technology (MUAT) in a sulphuric acid/polyethylene glycol 400-glycerol catalytic system. The influences of some key parameters on the liquefaction yield were investigated. The results showed that compared with traditional liquefaction, the introduction of MUAT allowed the solvent dosage to be halved and shortened the liquefaction time from 60 to 20 min. The liquefaction yield reached 91% under the optimal conditions. However, the influence on the yield of some parameters such as catalyst concentration, was similar to that of traditional liquefaction, indicating that the application of MUAT possibly only intensified heat and mass transfer rather than altering either the degradation mechanism or pathway. The introduction of MUAT as a process intensification technology has good industrial application potential for woody biomass liquefaction. Copyright © 2015 Elsevier Ltd. All rights reserved.

  17. A multimodality imaging-compatible insertion robot with a respiratory motion calibration module designed for ablation of liver tumors: a preclinical study.

    PubMed

    Li, Dongrui; Cheng, Zhigang; Chen, Gang; Liu, Fangyi; Wu, Wenbo; Yu, Jie; Gu, Ying; Liu, Fengyong; Ren, Chao; Liang, Ping

    2018-04-03

    To test the accuracy and efficacy of the multimodality imaging-compatible insertion robot with a respiratory motion calibration module designed for ablation of liver tumors in phantom and animal models. To evaluate and compare the influences of intervention experience on robot-assisted and ultrasound-controlled ablation procedures. Accuracy tests on rigid body/phantom model with a respiratory movement simulation device and microwave ablation tests on porcine liver tumor/rabbit liver cancer were performed with the robot we designed or with the traditional ultrasound-guidance by physicians with or without intervention experience. In the accuracy tests performed by the physicians without intervention experience, the insertion accuracy and efficiency of robot-assisted group was higher than those of ultrasound-guided group with statistically significant differences. In the microwave ablation tests performed by the physicians without intervention experience, better complete ablation rate was achieved when applying the robot. In the microwave ablation tests performed by the physicians with intervention experience, there was no statistically significant difference of the insertion number and total ablation time between the robot-assisted group and the ultrasound-controlled group. The evaluation by the NASA-TLX suggested that the robot-assisted insertion and microwave ablation process performed by physicians with or without experience were more comfortable. The multimodality imaging-compatible insertion robot with a respiratory motion calibration module designed for ablation of liver tumors could increase the insertion accuracy and ablation efficacy, and minimize the influence of the physicians' experience. The ablation procedure could be more comfortable with less stress with the application of the robot.

  18. 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. Copyright © 2014 Elsevier Ltd. All rights reserved.

  19. Intensification of marrubiin concentration by optimization of microwave-assisted (low CO2 yielding) extraction process for Marrubium vulgare using central composite design and antioxidant evaluation.

    PubMed

    Mittal, Vineet; Nanda, Arun

    2017-12-01

    Marrubium vulgare Linn (Lamiaceae) was generally extracted by conventional methods with low yield of marrubiin; these processes were not considered environment friendly. This study extracts the whole plant of M. vulgare by microwave assisted extraction (MAE) and optimizes the effect of various extraction parameters on the marrubiin yield by using Central Composite Design (CCD). The selected medicinal plant was extracted using ethanol: water (1:1) as solvent by MAE. The plant material was also extracted using a Soxhlet and the various extracts were analyzed by HPTLC to quantify the marrubiin concentration. The optimized conditions for the microwave-assisted extraction of selected medicinal plant was microwave power of 539 W, irradiation time of 373 s and solvent to drug ratio, 32 mL per g of the drug. The marrubiin concentration in MAE almost doubled relative to the traditional method (0.69 ± 0.08 to 1.35 ± 0.04%). The IC 50 for DPPH was reduced to 66.28 ± 0.6 μg/mL as compared to conventional extract (84.14 ± 0.7 μg/mL). The scanning electron micrographs of the treated and untreated drug samples further support the results. The CCD can be successfully applied to optimize the extraction parameters (MAE) for M. vulgare. Moreover, in terms of environmental impact, the MAE technique could be assumed as a 'Green approach' because the MAE approach for extraction of plant released only 92.3 g of CO 2 as compared to 3207.6 g CO 2 using the Soxhlet method of extraction.

  20. Microwave-Assisted Hydrolysis of Chitosan from Shrimp Shell Waste for Glucosammine Hydrochlorid Production

    NASA Astrophysics Data System (ADS)

    Zaeni, Ahmad; Safitri, Endang; Fuadah, Badrotul; Nyoman Sudiana, I.

    2017-05-01

    Chitin is the most widespread renewable natural sources following cellulose as the main source of chitosan. Chitin is isolated from crustacean waste and shrimp shells. Chitosan is derived from chitin throuhgt demineralisation, deproteination, decolorisation and deacetylation process using chemicals such as sodium hydroxide, hydrogen chloride and acetone. Glucosamine hydrochloride (GlcN-Cl) can be produced by hydrolysis of chitosan by using hydrogen chloride. During deacetylation and hydrolysis the solution is heated by hotplate or furnace. In this paper we use microwave instead of hotplate for production chitosan and GlcN-Cl. The research investigates effect of microwaves to amount of rendemen and their property. The chitosan was characterized its moisture content, solubility, and degree of deacetylation (DDA). Whereas the glucosammine hydrochloride characterized its functional groups using FTIR and crystallization by using X-Ray Difraction (XRD). The experimental results show that the use of microwave energy on deacetilation of chitosan and hydrolisis processes can decrease time consuming and reactant concentration during production. the DDA value obtained was very high from 70 to 85%. The results also show that microwaves meet chitosan and GlcN-Cl standards.

  1. Microwave-assisted microemulsion technique for production of miconazole nitrate- and econazole nitrate-loaded solid lipid nanoparticles.

    PubMed

    Shah, Rohan M; Eldridge, Daniel S; Palombo, Enzo A; Harding, Ian H

    2017-08-01

    The microwave-assisted production of solid lipid nanoparticles (SLNs) is a novel technique reported recently by our group. The small particle size, solid nature and use of physiologically well-tolerated lipid materials make SLNs an interesting and potentially efficacious drug carrier. The main purpose of this research work was to investigate the suitability of microwave-assisted microemulsion technique to encapsulate selected ionic drug substances such as miconazole nitrate and econazole nitrate. The microwave-produced SLNs had a small size (250-300nm), low polydispersity (<0.20), high encapsulation efficiency (72-87%) and loading capacity (3.6-4.3%). Differential scanning calorimetry (DSC) and X-ray diffraction (XRD) studies suggested reduced crystallinity of stearic acid in SLNs. The release studies demonstrated a slow, sustained but incomplete release of drugs (<60% after 24h) from microwave-produced SLNs. Data fitting of drug release data revealed that the release of both drugs from microwave-produced SLNs was governed by non-Fickian diffusion indicating that drug release was both diffusion- and dissolution- controlled. Anti-fungal efficacy of drug-loaded SLNs was evaluated on C. albicans. The cell viability studies showed that cytotoxicity of SLNs was concentration-dependent. These encouraging results suggest that the microwave-assisted procedure is suitable for encapsulation of ionic drugs and that microwave-produced SLNs can act as potential carriers of antifungal drugs. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Synthesis of Transesterified Palm Olein-Based Polyol and Rigid Polyurethanes from this Polyol.

    PubMed

    Arniza, Mohd Zan; Hoong, Seng Soi; Idris, Zainab; Yeong, Shoot Kian; Hassan, Hazimah Abu; Din, Ahmad Kushairi; Choo, Yuen May

    Transesterification of palm olein with glycerol can increase the functionality by introducing additional hydroxyl groups to the triglyceride structure, an advantage compared to using palm olein directly as feedstock for producing palm-based polyol. The objective of this study was to synthesize transesterified palm olein-based polyol via a three-step reaction: (1) transesterification of palm olein, (2) epoxidation and (3) epoxide ring opening. Transesterification of palm olein yielded approximately 78 % monoglyceride and has an hydroxyl value of approximately 164 mg KOH g -1 . The effect of formic acid and hydrogen peroxide concentrations on the epoxidation reaction was studied. The relationships between epoxide ring-opening reaction time and residual oxirane oxygen content and hydroxyl value were monitored. The synthesized transesterified palm olein-based polyol has hydroxyl value between 300 and 330 mg KOH g -1 and average molecular weight between 1,000 and 1,100 Da. On the basis of the hydroxyl value and average molecular weight of the polyol, the transesterified palm olein-based polyol is suitable for producing rigid polyurethane foam, which can be designed to exhibit desirable properties. Rigid polyurethane foams were synthesized by substituting a portion of petroleum-based polyol with the transesterified palm olein-based polyol. It was observed that by increasing the amount of transesterified palm olein-based polyol, the core density and compressive strength were reduced but at the same time the insulation properties of the rigid polyurethane foam were improved.

  3. 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.

  4. A simple and rapid microwave-assisted hematoxylin and eosin staining method using 1,1,1 trichloroethane as a dewaxing and a clearing agent.

    PubMed

    Temel, S G; Noyan, S; Cavusoglu, I; Kahveci, Z

    2005-01-01

    The use and practicability of microwave-assisted staining procedures in routine histopathology has been well established for more than 17 years. In the study reported here, we aimed to examine an alternative approach that would shorten the duration of dewaxing and clearing steps of hematoxylin and eosin (H & E) staining of paraffin sections by using a microwave oven. Although xylene is one of the most popular dewaxing and clearing agents, its flammability restricts its use in a microwave oven; thus we preferred 1,1,1 trichloroethane, which is not flammable, as the dewaxing and clearing agent in the present study. In Group I and Group II (control groups), intestine was processed with xylene and 1,1,1 trichloroethane, respectively. The sections were then stained with H & E according to the conventional staining protocol at room temperature and subdivided into two groups according to the duration of dewaxing and clearing in xylene. In Groups III and IV (experimental groups) similar tissues were processed with xylene and 1,1,1 trichloroethane, respectively; however, sections from these groups were divided into four subgroups to study the period required for dewaxing and clearing in 1,1,1 trichloroethane, then stained with H & E in the microwave oven at 360 W for 30 sec. Our conventional H & E staining procedure, which includes dewaxing, staining and clearing of sections, requires approximately 90 min, while our method using 1,1,1 trichloroethane and microwave heating required only 2 min. Our alternative method for H & E staining not only reduced the procedure time significantly, but also yielded staining quality equal or superior to those stained the conventional way. Our results suggest that 1,1,1 trichloroethane can be used effectively and safely as a dewaxing and clearing agent for H & E staining in a microwave oven.

  5. Microwave-assisted chemical pre-treatment of waste sorghum leaves: Process optimization and development of an intelligent model for determination of volatile compound fractions.

    PubMed

    Rorke, Daneal C S; Suinyuy, Terence N; Gueguim Kana, E B

    2017-01-01

    This study reports the profiling of volatile compounds generated during microwave-assisted chemical pre-treatment of sorghum leaves. Compounds including acetic acid (0-186.26ng/g SL), furfural (0-240.80ng/g SL), 5-hydroxymethylfurfural (HMF) (0-19.20ng/g SL) and phenol (0-7.76ng/g SL) were detected. The reducing sugar production was optimized. An intelligent model based on Artificial Neural Networks (ANNs) was developed and validated to predict a profile of 21 volatile compounds under novel pre-treatment conditions. This model gave R 2 -values of up to 0.93. Knowledge extraction revealed furfural and phenol exhibited high sensitivity to acid- and alkali concentration and S:L ratio, while phenol showed high sensitivity to microwave duration and intensity. Furthermore, furfural production was majorly dependent on acid concentration and fit a dosage-response relationship model with a 2.5% HCl threshold. Significant non-linearities were observed between pre-treatment conditions and the profile of various compounds. This tool reduces analytical costs through virtual analytical instrumentation, improving process economics. Copyright © 2016 Elsevier Ltd. All rights reserved.

  6. Phosphorous and nitrogen dual heteroatom doped mesoporous carbon synthesized via microwave method for supercapacitor application

    NASA Astrophysics Data System (ADS)

    Nasini, Udaya B.; Bairi, Venu Gopal; Ramasahayam, Sunil Kumar; Bourdo, Shawn E.; Viswanathan, Tito; Shaikh, Ali U.

    2014-03-01

    Phosphorus (P) and nitrogen (N) dual heteroatom doped mesoporous carbon (PNDC) synthesized by microwave assisted carbonization of tannin cross-linked to melamine in the presence of polyphosphoric acid was evaluated electrochemically for supercapacitor application. Controlling the N content by varying the amount of tannin to melamine in the carbonization process produced varying nitrogen, phosphorus and oxygen functionalities along with different physical properties. Electrochemical characterization studies revealed that N content is responsible for pseudocapacitance and high surface area plays a vital role in improving the capacitative behavior by enhanced electric double layer formation. In 1.0 M H2SO4 and 6.0 M KOH, PNDC-2 showed a high specific capacitance of 271 F g-1 and 236 F g-1, respectively. XPS results demonstrate the presence of pyridinic-N, quaternary-N as well as quinone type oxygen functionalities, which accounts for redox reactions and likely play an important role in the transportation of electrons during the charge/discharge process. Thus, the microwave assisted synthesis of doped carbon can provide a novel method of synthesizing materials useful for the fabrication of cheap and high performance supercapacitors.

  7. Effect of microwave-assisted sintering on dielectric properties of CaCu{sub 3}Ti{sub 4}O{sub 12} ceramic

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

    Rani, Suman, E-mail: sumanranigju@gmail.com; Ahlawat, Neetu; Punia, R.

    2016-05-23

    In this present work, CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) was synthesized by conventional solid-state reaction technique. The synthesis process was carried out in two phases; by conventional process (calcination and sintering at 1080°C for 10 hours) and phase II involves the micro assisted pre sintering of conventionally calcined CCTO for very short soaking time of 30 min at 1080°C in a microwave furnace followed by sintering at 1080°C for 10 hours in conventional furnace. X-ray diffraction (XRD) patterns confirmed the formation of single phase ceramic. Dielectric properties were studied over the frequency range from 50Hz -5MHz at temperatures (273K-343K). It wasmore » observed that pre- microwave sintering enhance the dielectric constant values from 10900 to 11893 and respectively reduces the dielectric loss values from 0.49 to 0.34 at room temperature(1 KHz). CCTO ceramics which are found desirable for many technological applications. The effect is more pronounced at low frequencies of applied electric field.« less

  8. Comparison of Conventional and Microwave Assisted Heating on Carbohydrate Content, Antioxidant Capacity and Postprandial Glycemic Response in Oat Meals

    PubMed Central

    Olędzki, Remigiusz

    2018-01-01

    Minimally processed cereal breakfast products from whole grain entered the market due to consumer demand of more nutritional food with more controlled sugar release. However, the subsequent processing of such products with different cooking methods in the consumer’s kitchen may lead to significant differentiation of their nutritional value. Therefore, the evaluation of the impact of frequently used cooking methods on a final quality of breakfast cereals meal is needed. The present study investigates how the two different methods of heating, conventional and microwave (MW) assisted, affect the carbohydrate content, profile and resulting glycemic index of so prepared food as well as the antioxidant activity of meals. Two products available on the market—oat bran and flakes—were used. The highest starch content in fluid phase of oatmeal was detected in samples heated for 3 min with microwaves, regardless the type. The lowest starch content was obtained for 5 min MW heated flakes sample. The total content of glucose was about 1.5 times lower in bran vs. flakes oatmeal. The highest β-glucan content in fluid fraction was also observed for bran meal but its release was independent of applied conditions. PMID:29443904

  9. 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.

  10. Effects of moisture content in cigar tobacco on nicotine extraction. Similarity between soxhlet and focused open-vessel microwave-assisted techniques.

    PubMed

    Ng, Lay-Keow; Hupé, Michel

    2003-09-05

    The effects of tobacco moisture on nicotine yield were investigated in this study. Soxhlet and microwave-assisted techniques were used to extract nicotine from cigar fillers of varying moisture contents (5-20%), using a polar (methanol) and a non-polar (isooctane) solvent. The extracts were analyzed by a gas chromatograph equipped with a flame-ionization detector. For both extraction techniques, higher nicotine yields were consistently obtained with methanol than with isooctane from the same samples. Solubility of nicotine salts in methanol but not in isooctane is the major cause of this observation. Moreover, pronounced effects of the tobacco moisture content on extraction efficiency were observed with isooctane but not with methanol. For microwave assisted extraction (MAE) with isooctane, nicotine yield increased from 3 to 70% as the moisture level in tobacco was raised from 3 to 13%, and leveled off thereafter. Similar observations were made with Soxhlet extraction. While MAE results were rationalized by the known cell-rupture process, a mechanism based on the interaction between the solvents and the structural components of the plant cells has been proposed to account for the observations made with Soxhlet extraction.

  11. 40 CFR Table 4 to Subpart Ppp of... - Known Organic HAP From Polyether Polyol Products

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 11 2010-07-01 2010-07-01 true Known Organic HAP From Polyether Polyol... CATEGORIES National Emission Standards for Hazardous Air Pollutant Emissions for Polyether Polyols Production Pt. 63, Subpt. PPP, Table 4 Table 4 to Subpart PPP of Part 63—Known Organic HAP From Polyether Polyol...

  12. Efficiency of Osmotic Dehydration of Apples in Polyols Solutions.

    PubMed

    Cichowska, Joanna; Żubernik, Joanna; Czyżewski, Jakub; Kowalska, Hanna; Witrowa-Rajchert, Dorota

    2018-02-17

    The present study aimed to evaluate the influence of selected compounds from the polyol group, as well as other saccharides, on the osmotic dehydration process of apples. The following alternative solutions were examined: erythritol, xylitol, maltitol, inulin and oligofructose. Efficiency of the osmotic dehydration process was evaluated based on the kinetics of the process, and through comparison of the results obtained during the application of a sucrose solution. This innovative research utilizes alternative solutions in osmotic pretreatment, which until now, have not been commonly used in fruit processing by researchers worldwide. Results indicate that erythritol and xylitol show stronger or similar efficiency to sucrose; however, the use of inulin, as well as oligofructose, was not satisfactory due to the insufficient, small osmotic driving forces of the process, and the low values of mass transfer parameters.

  13. Wax: A benign hydrogen-storage material that rapidly releases H2-rich gases through microwave-assisted catalytic decomposition

    PubMed Central

    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.

    2016-01-01

    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. PMID:27759014

  14. Carbonaceous meteorites as a source of sugar-related organic compounds for the early Earth

    NASA Technical Reports Server (NTRS)

    Cooper, G.; Kimmich, N.; Belisle, W.; Sarinana, J.; Brabham, K.; Garrel, L.

    2001-01-01

    The much-studied Murchison meteorite is generally used as the standard reference for organic compounds in extraterrestrial material. Amino acids and other organic compounds important in contemporary biochemistry are thought to have been delivered to the early Earth by asteroids and comets, where they may have played a role in the origin of life. Polyhydroxylated compounds (polyols) such as sugars, sugar alcohols and sugar acids are vital to all known lifeforms-they are components of nucleic acids (RNA, DNA), cell membranes and also act as energy sources. But there has hitherto been no conclusive evidence for the existence of polyols in meteorites, leaving a gap in our understanding of the origins of biologically important organic compounds on Earth. Here we report that a variety of polyols are present in, and indigenous to, the Murchison and Murray meteorites in amounts comparable to amino acids. Analyses of water extracts indicate that extraterrestrial processes including photolysis and formaldehyde chemistry could account for the observed compounds. We conclude from this that polyols were present on the early Earth and therefore at least available for incorporation into the first forms of life.

  15. 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

  16. A novel method to augment extraction of mangiferin by application of microwave on three phase partitioning.

    PubMed

    Kulkarni, Vrushali M; Rathod, Virendra K

    2015-06-01

    This work reports a novel approach where three phase partitioning (TPP) was combined with microwave for extraction of mangiferin from leaves of Mangifera indica . Soxhlet extraction was used as reference method, which yielded 57 mg/g in 5 h. Under optimal conditions such as microwave irradiation time 5 min, ammonium sulphate concentration 40% w/v, power 272 W, solute to solvent ratio 1:20, slurry to t -butanol ratio 1:1, soaking time 5 min and duty cycle 50%, the mangiferin yield obtained was 54 mg/g by microwave assisted three phase partitioning extraction (MTPP). Thus extraction method developed resulted into higher extraction yield in a shorter span, thereby making it an interesting alternative prior to down-stream processing.

  17. Microwave-Assisted Synthesis of Goethite Nanoparticles Used for Removal of Cr(VI) from Aqueous Solution

    PubMed Central

    Kynicky, Jindrich; Adam, Vojtech

    2017-01-01

    The microwave-assisted synthesis of goethite nanoparticles has been studied. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), differential thermal analysis (DTA) and Brunauer–Emmett–Teller (BET) method. Goethite rod-like nanoparticles have been successfully synthesized in 10 min of microwave treating at 100 °C. Particle size is in the range from 30 to 60 nm in width and from 200 to 350 nm in length. BET analysis indicated that the surface area of the product is 158.31 m2g−1. The feasibility of Cr(VI) removal fromaqueous solution depends on the pH of the solution and contact time. The maximum adsorptionis reached at pH 4.0 and 540 min of contact time. The adsorption kinetics was analyzedby the pseudo-first- and second-order models and the results reveal that the adsorption process obeys the pseudo-second-order model. The adsorption data were fitted well with the Langmuir adsorption isotherm. PMID:28773142

  18. Ultrafast Microwave Nano-manufacturing of Fullerene-Like Metal Chalcogenides

    PubMed Central

    Liu, Zhen; Zhang, Lin; Wang, Ruigang; Poyraz, Selcuk; Cook, Jonathan; Bozack, Michael J.; Das, Siddhartha; Zhang, Xinyu; Hu, Liangbing

    2016-01-01

    Metal Chalcogenides (MCs) have emerged as an extremely important class of nanomaterials with applications ranging from lubrication to energy storage devices. Here we report our discovery of a universal, ultrafast (60 seconds), energy-efficient, and facile technique of synthesizing MC nanoparticles and nanostructures, using microwave-assisted heating. A suitable combination of chemicals was selected for reactions on Polypyrrole nanofibers (PPy-NF) in presence of microwave irradiation. The PPy-NF serves as the conducting medium to absorb microwave energy to heat the chemicals that provide the metal and the chalcogenide constituents separately. The MCs are formed as nanoparticles that eventually undergo a size-dependent, multi-stage aggregation process to yield different kinds of MC nanostructures. Most importantly, this is a single-step metal chalcogenide formation process that is much faster and much more energy-efficient than all the other existing methods and can be universally employed to produce different kinds of MCs (e.g., MoS2, and WS2). PMID:26931353

  19. Ultrafast Microwave Nano-manufacturing of Fullerene-Like Metal Chalcogenides

    NASA Astrophysics Data System (ADS)

    Liu, Zhen; Zhang, Lin; Wang, Ruigang; Poyraz, Selcuk; Cook, Jonathan; Bozack, Michael J.; Das, Siddhartha; Zhang, Xinyu; Hu, Liangbing

    2016-03-01

    Metal Chalcogenides (MCs) have emerged as an extremely important class of nanomaterials with applications ranging from lubrication to energy storage devices. Here we report our discovery of a universal, ultrafast (60 seconds), energy-efficient, and facile technique of synthesizing MC nanoparticles and nanostructures, using microwave-assisted heating. A suitable combination of chemicals was selected for reactions on Polypyrrole nanofibers (PPy-NF) in presence of microwave irradiation. The PPy-NF serves as the conducting medium to absorb microwave energy to heat the chemicals that provide the metal and the chalcogenide constituents separately. The MCs are formed as nanoparticles that eventually undergo a size-dependent, multi-stage aggregation process to yield different kinds of MC nanostructures. Most importantly, this is a single-step metal chalcogenide formation process that is much faster and much more energy-efficient than all the other existing methods and can be universally employed to produce different kinds of MCs (e.g., MoS2, and WS2).

  20. Ultrafast Microwave Nano-manufacturing of Fullerene-Like Metal Chalcogenides.

    PubMed

    Liu, Zhen; Zhang, Lin; Wang, Ruigang; Poyraz, Selcuk; Cook, Jonathan; Bozack, Michael J; Das, Siddhartha; Zhang, Xinyu; Hu, Liangbing

    2016-03-02

    Metal Chalcogenides (MCs) have emerged as an extremely important class of nanomaterials with applications ranging from lubrication to energy storage devices. Here we report our discovery of a universal, ultrafast (60 seconds), energy-efficient, and facile technique of synthesizing MC nanoparticles and nanostructures, using microwave-assisted heating. A suitable combination of chemicals was selected for reactions on Polypyrrole nanofibers (PPy-NF) in presence of microwave irradiation. The PPy-NF serves as the conducting medium to absorb microwave energy to heat the chemicals that provide the metal and the chalcogenide constituents separately. The MCs are formed as nanoparticles that eventually undergo a size-dependent, multi-stage aggregation process to yield different kinds of MC nanostructures. Most importantly, this is a single-step metal chalcogenide formation process that is much faster and much more energy-efficient than all the other existing methods and can be universally employed to produce different kinds of MCs (e.g., MoS2, and WS2).

  1. "In silico" mechanistic studies as predictive tools in microwave-assisted organic synthesis.

    PubMed

    Rodriguez, A M; Prieto, P; de la Hoz, A; Díaz-Ortiz, A

    2011-04-07

    Computational calculations can be used as a predictive tool in Microwave-Assisted Organic Synthesis (MAOS). A DFT study on Intramolecular Diels-Alder reactions (IMDA) indicated that the activation energy of the reaction and the polarity of the stationary points are two fundamental parameters to determine "a priori" if a reaction can be improved by using microwave irradiation.

  2. Recent developments in high efficient freeze-drying of fruits and vegetables assisted by microwave: A review.

    PubMed

    Fan, Kai; Zhang, Min; Mujumdar, Arun S

    2018-01-10

    Microwave heating has been applied in the drying of high-value solids as it affords a number of advantages, including shorter drying time and better product quality. Freeze-drying at cryogenic temperature and extremely low pressure provides the advantage of high product quality, but at very high capital and operating costs due partly to very long drying time. Freeze-drying coupled with a microwave heat source speeds up the drying rate and yields good quality products provided the operating unit is designed and operated to achieve the potential for an absence of hot spot developments. This review is a survey of recent developments in the modeling and experimental results on microwave-assisted freeze-drying (MFD) over the past decade. Owing to the high costs involved, so far all applications are limited to small-scale operations for the drying of high-value foods such as fruits and vegetables. In order to promote industrial-scale applications for a broader range of products further research and development efforts are needed to offset the current limitations of the process. The needs and opportunities for future research and developments are outlined.

  3. Photodetectors using III-V nitrides

    DOEpatents

    Moustakas, T.D.; Misra, M.

    1997-10-14

    A photodetector using a III-V nitride and having predetermined electrical properties is disclosed. The photodetector includes a substrate with interdigitated electrodes formed on its surface. The substrate has a sapphire base layer, a buffer layer formed from a III-V nitride and a single crystal III-V nitride film. The three layers are formed by electron cyclotron resonance microwave plasma-assisted molecular beam epitaxy (ECR-assisted MBE). Use of the ECR-assisted MBE process allows control and predetermination of the electrical properties of the photodetector. 24 figs.

  4. Photodetectors using III-V nitrides

    DOEpatents

    Moustakas, Theodore D.; Misra, Mira

    1997-01-01

    A photodetector using a III-V nitride and having predetermined electrical properties is disclosed. The photodetector includes a substrate with interdigitated electrodes formed on its surface. The substrate has a sapphire base layer, a buffer layer formed from a III-V nitride and a single crystal III-V nitride film. The three layers are formed by electron cyclotron resonance microwave plasma-assisted molecular beam epitaxy (ECR-assisted MBE). Use of the ECR-assisted MBE process allows control and predetermination of the electrical properties of the photodetector.

  5. Identification of molecular species of polyol oils produced from soybean oil by Pseudomonas aeruginosa e03-12 nrrl b-59991

    USDA-ARS?s Scientific Manuscript database

    The objective of this study is to develop a bioprocess for the production of polyol oils directly from soybean oil. We reported earlier methods for microbial screening and production of polyol oils from soybean oil (Hou and Lin, 2013). The polyol oil produced by Acinetobacter haemolyticus A01-35 (NR...

  6. A review on polyols: new frontiers for health-based bakery products.

    PubMed

    Ghosh, Soma; Sudha, M L

    2012-05-01

    Polyols or sugar alcohols, a group of reduced calorie sweeteners, are the natural and nutritive sweeteners. These are neither sugars nor alcohols; rather they are a group of low-digestible carbohydrates which can be used instead of sucrose. They occur naturally in foods and come from plant products such as fruit and berries. They are used in food as sweeteners and bulking agents. Polyols have slightly reduced sweetness and caloric values compared to sucrose. Polyols available as either in solid crystalline form or syrups are emerging as a sugar replacer as well as a sugar substitute. Low sugar or low calorie is a top ranked market trend for bakery sector. Polyols offer the baker a versatile range of ingredients to boost the available portfolio of products. They would provide the functional benefits to bakery goods when the sugars used are replaced with polyols. This review focuses on some recent studies carried out on sucrose replacement with polyols in baked products.

  7. Microwave assisted step-by-step process for the production of fucoidan, alginate sodium, sugars and biochar from Ascophyllum nodosum through a biorefinery concept.

    PubMed

    Yuan, Yuan; Macquarrie, Duncan J

    2015-12-01

    The biorefinery is an important concept for the development of alternative routes to a range of interesting and important materials from renewable resources. It ensures that the resources are used fully and that all parts of them are valorized. This paper develops this concept, using brown macroalgae Ascophyllum nodosum as an example, by assistance of microwave technology. A step-by-step process was designed to obtain fucoidan, alginates, sugars and biochar (alga residue) consecutively. The yields of fucoidan, alginates, sugars and biochar were 14.09%, 18.24%, 10.87% and 21.44%, respectively. To make an evaluation of the biorefinery process, seaweed sample was also treated for fucoidan extraction only, alginate extraction only and hydrothermal treatment for sugars and biochar only. The chemical composition and properties of each product were also analyzed. The results indicated that A. nodosum could be potentially used as feedstock for a biorefinery process to produce valuable chemicals and fuels. Copyright © 2015 Elsevier Ltd. All rights reserved.

  8. Kinetic modeling of microscopic processes during electron cyclotron resonance microwave plasma-assisted molecular beam epitaxial growth of GaN/GaAs-based heterostructures

    NASA Astrophysics Data System (ADS)

    Bandić, Z. Z.; Hauenstein, R. J.; O'Steen, M. L.; McGill, T. C.

    1996-03-01

    Microscopic growth processes associated with GaN/GaAs molecular beam epitaxy (MBE) are examined through the introduction of a first-order kinetic model. The model is applied to the electron cyclotron resonance microwave plasma-assisted MBE (ECR-MBE) growth of a set of δ-GaNyAs1-y/GaAs strained-layer superlattices that consist of nitrided GaAs monolayers separated by GaAs spacers, and that exhibit a strong decrease of y with increasing T over the range 540-580 °C. This y(T) dependence is quantitatively explained in terms of microscopic anion exchange, and thermally activated N surface-desorption and surface-segregation processes. N surface segregation is found to be significant during GaAs overgrowth of GaNyAs1-y layers at typical GaN ECR-MBE growth temperatures, with an estimated activation energy Es˜0.9 eV. The observed y(T) dependence is shown to result from a combination of N surface segregation/desorption processes.

  9. Comparison of Conventional and Microwave-assisted Synthesis of Benzimidazole Derivative from Citronellal in Kaffir lime oil (Citrus hystrix DC.)

    NASA Astrophysics Data System (ADS)

    Warsito, W.; Noorhamdani, A. S.; Suratmo; Dwi Sapri, R.; Alkaroma, D.; Azhar, A. Z.

    2018-04-01

    Simple method has been used for the synthesis of benzimidazole derivative from citronellal in kaffir lime oil under microwave irradiation. These compounds were synthesized also by conventional heating for comparison. In addtion, microwave-assited synthesis was also compared between using to dichloromethane and methanol solvents with variation of reaction time for 30 to 70 minutes and 4 to 12 h for conventional heating. The 2-citronellyl benzimidazole compound synthesized were characterised by FT-IR, GC-MS, 1H and 13C NMR spectroscopy. Comparison between conventional and microwave-assisted synthesis was done by comparing between correlation of reaction time and percentage yield. The time optimum of microwave-assisted and conventional synthesis using dichloromethane solvent respectively at 60 minutes (yield 19.23%) and 8 hours (yield 11.54%). In addition, microwave-assited synthesis increasing 157.81 times compared by conventional heating. While using methanol solvent tends to increase linearly however the percentage of yield only 0.77 times of synthesis using dichloromethane solvent.

  10. Catalytic Deoxydehydration of Carbohydrates and Polyols to Chemicals and Fuels

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

    Nicholas, Kenneth M.

    As the world's fossil fuel resources are being depleted and their costs increase, there is an urgent need to discover and develop new processes for the conversion of renewable, biomass resources into fuels and chemical feedstocks. Research and development in this area have been given high priority by both governmental agencies and industry. To increase the energy content and decrease the boiling points of biomass-derived carbohydrates and polyols to the useful liquid range it is necessary to chemically remove water (dehydrate) and, preferably, oxygen (deoxygenate/reduce). The poly-hydroxylic nature of carbohydrates is attractive for their use as functionalized chemical building blocks,more » but it presents a daunting challenge for their selective conversion to single product chemicals or fuels. The long term, practical objective of this project is to develop catalytic processes for the deoxydehydration (DODH) of biomass-derived carbohydrates and polyols to produce unsaturated alcohols and hydrocarbons of value as chemical feedstocks and fuels; DODH: polyol + reductant --(LMOx catalyst)--> unsaturate + oxidized reductant + H2O. Limited prior studies have established the viability of the DODH process with expensive phosphine reductants and rhenium-catalysts. Initial studies in the PI's laboratory have now demonstrated: 1) the moderately efficient conversion of glycols to olefins by the economical sulfite salts is catalyzed by MeReO3 and Z+ReO4-; 2) effective phosphine-based catalytic DODH of representative glycols to olefins by cheap LMoO2 complexes; and 3) computational studies (with K. Houk, UCLA) have identified several Mo-, W-, and V-oxo complexes that are likely to catalyze glycol DODH. Seeking practically useful DODH reactions of complex polyols and new understanding of the reactivity of polyoxo-metal species with biomass-oxygenates we will employ a two-pronged approach: 1) investigate experimentally the reactivity, both stoichiometric and catalytic, of polyoxo-complexes and practical reductants with representative polyols to establish structure/reactivity relationships and reaction mechanisms; and b) carry out parallel computational studies of these reactions and their mechanisms- both analytical and predictive. Our prioritized action plan is: (1) to optimize the catalytic efficiency, assess the substrate scope/selectivity, and address key mechanistic aspects of Re-catalyzed, sulfite-driven DODH reactions; (2) use the findings from (1), together with computational predictions, to discover new, effective non-precious metal catalysts for sulfite-driven DODH reactions; and 3) to initiate exploratory studies of CO- and H2-driven DODH. Successful execution of this research project will: 1) provide practical chemical processes for the conversion of biomass into useful chemicals and fuels: 2) bring fundamental new understanding of chemical reactions involving metal-oxo catalysts; and 3) provide educational and technical training of future energy scientists.« less

  11. 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.

  12. Investigation of catalytic activity towards oxygen reduction reaction of Pt dispersed on boron doped graphene in acid medium.

    PubMed

    Pullamsetty, Ashok; Sundara, Ramaprabhu

    2016-10-01

    Boron doped graphene was prepared by a facile method and platinum (Pt) decoration over boron doped graphene was done in various chemical reduction methods such as sodium borohydride (NaBH4), polyol and modified polyol. X-ray diffraction analysis indicates that the synthesized catalyst particles are present in a nanocrystalline structure and transmission and scanning electron microscopy were employed to investigate the morphology and particle distribution. The electrochemical properties were investigated with the help of the rotating disk electrode (RDE) technique and cyclic voltammetry. The results show that the oxygen reduction reaction (ORR) takes place by a four-electron process. The kinetics of the ORR was evaluated using K-L and Tafel plots. The electrocatalyst obtained in modified polyol reduction method has shown the better catalytic activity compared to other two electrocatalysts. Copyright © 2016 Elsevier Inc. All rights reserved.

  13. Ultrafast Formation of ZnO Nanorods via Seed-Mediated Microwave Assisted Hydrolysis Process

    NASA Astrophysics Data System (ADS)

    Tan, S. T.; Umar, A. A.; Yahaya, M.; Yap, C. C.; Salleh, M. M.

    2013-04-01

    One dimensional (1D) zinc oxide, ZnO nanostructures have shown promising results for usage in photodiode and optoelectronic device due to their high surface area. Faster and conventional method for synthesis ZnO nanorods has become an attention for researcher today. In this paper, ZnO nanorods have been successfully synthesized via two-step process, namely alcothermal seeding and seed-mediated microwave hydrolysis process. In typical process, the ZnO nanoseeds were grown in the growth solution that contained equimolar (0.04 M) of zinc nitrate hexahydrate, Zn (NO3).6H2O and hexamethylenetetramine, HMT. The growth process was carried inside the inverted microwave within 5- 20 s. The effect of growth parameters (i.e. concentration, microwave power, time reaction) upon the modification of ZnO morphology was studied. ZnO nanostructures were characterized by Field emission scanning electron microscope (FESEM) and X-ray diffraction (XRD). The densities of nanorods were evaluated by the Image J analysis. It was found that the morphology (e.g. shape and size) of nanostructures has changed drastically with the increment of growth solution concentration. The density of ZnO nanorods was proven to increase with the increasing of reaction time and microwave power. We hypothesize that the microwave power might enhance the rate of nucleation and promote the faster nanostructure growth as compared with the normal heating condition due to the superheating phenomenon. This method might promote a new and faster alternative way in nanostructure growth which can be applied in currently existing application.

  14. Microwave-assisted 'greener' synthesis of organics and nanomaterials

    EPA Science Inventory

    Microwave selective heating techniques in conjunction with 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 ...

  15. Polyols in grape berry: transport and metabolic adjustments as a physiological strategy for water-deficit stress tolerance in grapevine.

    PubMed

    Conde, Artur; Regalado, Ana; Rodrigues, Diana; Costa, J Miguel; Blumwald, Eduardo; Chaves, M Manuela; Gerós, Hernâni

    2015-02-01

    Polyols are important metabolites that often function as carbon and energy sources and/or osmoprotective solutes in some plants. In grapevine, and in the grape berry in particular, the molecular aspects of polyol transport and metabolism and their physiological relevance are virtually unknown to date. Here, the biochemical function of a grapevine fruit mesocarp polyol transporter (VvPLT1) was characterized after its heterologous expression in yeast. This H(+)-dependent plasma membrane carrier transports mannitol (K m=5.4mM) and sorbitol (K m=9.5mM) over a broad range of polyols and monosaccharides. Water-deficit stress triggered an increase in the expression of VvPLT1 at the fully mature stage, allowing increased polyol uptake into pulp cells. Plant polyol dehydrogenases are oxireductases that reversibly oxidize polyols into monosaccharides. Mannitol catabolism in grape cells (K m=30.1mM mannitol) and mature berry mesocarps (K m=79mM) was, like sorbitol dehydrogenase activity, strongly inhibited (50-75%) by water-deficit stress. Simultaneously, fructose reduction into polyols via mannitol and sorbitol dehydrogenases was stimulated, contributing to their higher intracellular concentrations in water-deficit stress. Accordingly, the concentrations of mannitol, sorbitol, galactinol, myo-inositol, and dulcitol were significantly higher in berry mesocarps from water-deficit-stressed Tempranillo grapevines. Metabolomic profiling of the berry pulp by GC-TOF-MS also revealed many other changes in its composition induced by water deficit. The impact of polyols on grape berry composition and plant response to water deficit stress, via modifications in polyol transport and metabolism, was analysed by integrating metabolomics with transcriptional analysis and biochemical approaches. © The Author 2014. Published by Oxford University Press on behalf of the Society for Experimental Biology. All rights reserved. For permissions, please email: journals.permissions@oup.com.

  16. Application of ionic liquids in vacuum microwave-assisted extraction followed by macroporous resin isolation of three flavonoids rutin, hyperoside and hesperidin from Sorbus tianschanica leaves.

    PubMed

    Gu, Huiyan; Chen, Fengli; Zhang, Qiang; Zang, Jing

    2016-03-01

    Rutin, hyperoside and hesperidin were effectively extracted from Sorbus tianschanica leaves by an ionic liquid vacuum microwave-assisted method. A series of ionic liquids with various anions and alkyl chain length of the cations were studied and the extraction was performed in [C6mim][BF4] aqueous solution. After optimization by a factorial design and response surface methodology, total extraction yield of 2.37mg/g with an error of 0.12mg/g (0.71±0.04mg/g, 1.18±0.06mg/g and 0.48±0.02 for rutin, hyperoside and hesperidin, respectively) was achieved under -0.08MPa for vacuum, 19min and 420W for microwave irradiation time and power, and 15mL/g for liquid-solid ratio. The proposed method here is more efficient and needs a shorter extraction time for rutin, hyperoside and hesperidin from S. tianschanica leaves than reference extraction techniques. In stability studies performed with standard rutin, hyperoside and hesperidin, the target analytes were stable under the optimum conditions. The proposed method had a high reproducibility and precision. In addition, separation of rutin, hyperoside and hesperidin from [C6mim][BF4] extraction solution was completed effectively by AB-8 macroporous resin adsorption and desorption process. Ionic liquid vacuum microwave-assisted extraction is a simple, rapid and efficient sample extraction technique. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. Gastrointestinal Disturbances Associated with the Consumption of Sugar Alcohols with Special Consideration of Xylitol: Scientific Review and Instructions for Dentists and Other Health-Care Professionals

    PubMed Central

    2016-01-01

    Sugar alcohols (polyols) are used in food manufacturing and in medical tests and examinations. d-Glucitol (sorbitol) and d-mannitol were previously the most common alditols used for these purposes. After the 1960s, xylitol became a common ingredient in noncariogenic confectioneries, oral hygiene products, and diabetic food. Erythritol, a polyol of the tetritol type, can be regarded as the sweetener of the “next generation.” The disaccharide polyols maltitol, lactitol, and isomalt have also been used in food manufacturing and in medical tests. Consumption of pentitol- and hexitol-type polyols and disaccharide polyols may cause gastrointestinal disturbances at least in unaccustomed subjects. The occurrence of disturbances depends on consumer properties and on the molecular size and configuration of the polyol molecule. Adaptation may take place as a result of enzyme induction in the intestinal flora. Some of the literature on xylitol has been difficult to access by health-care professionals and will be reviewed here. Research and clinical field experience have found no pathology in polyol-associated osmotic diarrhea—the intestinal mucosa having normal basic structure, except in extreme instances. Xylitol is better tolerated than hexitols or the disaccharide polyols. Erythritol, owing to its smaller molecular weight and configuration that differ from other alditols, normally avoids the gastrointestinal reactions encountered with other polyols. This review will also touch upon the FODMAPs diet concept. PMID:27840639

  18. Microwave-Assisted Resolution of α-Lipoic Acid Catalyzed by an Ionic Liquid Co-Lyophilized Lipase.

    PubMed

    Liu, Ning; Wang, Lei; Wang, Zhi; Jiang, Liyan; Wu, Zhuofu; Yue, Hong; Xie, Xiaona

    2015-05-29

    The combination of the ionic liquid co-lyophilized lipase and microwave irradiation was used to improve enzyme performance in enantioselective esterification of α-lipoic acid. Effects of various reaction conditions on enzyme activity and enantioselectivity were investigated. Under optimal condition, the highest enantioselectivity (E = 41.2) was observed with a high enzyme activity (178.1 μmol/h/mg) when using the ionic liquid co-lyophilized lipase with microwave assistance. Furthermore, the ionic liquid co-lyophilized lipase exhibited excellent reusability under low power microwave.

  19. Highly Efficient Erythritol Recovery from Waste Erythritol Mother Liquor by a Yeast-Mediated Biorefinery Process.

    PubMed

    Wang, Siqi; Wang, Hengwei; Lv, Jiyang; Deng, Zixin; Cheng, Hairong

    2017-12-20

    Erythritol, a natural sugar alcohol, is produced industrially by fermentation and crystallization, but this process leaves a large amount of waste erythritol mother liquor (WEML) which contains more than 200 g/L erythritol as well as other polyol byproducts. These impurities make it very difficult to crystallize more erythritol. In our study, an efficient process for the recovery of erythritol from the WEML is described. The polyol impurities were first identified by high-performance liquid chromatography and gas chromatography-mass spectrometry, and a yeast strain Candida maltosa CGMCC 7323 was then isolated to metabolize those impurities to purify erythritol. Our results demonstrated that the process could remarkably improve the purity of erythritol and thus make the subsequent crystallization easier. This newly developed strategy is expected to have advantages in WEML treatment and provide helpful information with regard to green cell factories and zero-waste processing.

  20. Microwave-Assisted Green Synthesis of Silver Nanostructures

    EPA Science Inventory

    This account summarizes a microwave (MW)-assisted synthetic approach for producing silver nanostructures. The rapid and in-core MW heating has received considerable attention as a promising new method for the one-pot synthesis of metallic nanostructures in solutions. Conceptually...

  1. The role of isocyanates in determining the viscoelastic properties of polyurethane

    NASA Astrophysics Data System (ADS)

    AqilahHamuzan, Hawa; Badri, Khairiah Haji

    2016-11-01

    Polyurethane (PU) has a unique structure that is dependent on the structure of the starting material used. This research focused on investigating the role of isocyanate groups (NCO) in the determination of the viscoelastic properties of the polymer. Monoester polyol was reacted with three different diisocyanates separately by prepolymerization method. The diisocyanates used were 2,4-diphenyl methane diisocyanate (MDI), toluene 2,4-diisocyanate (TDI) and isophoronediisocyanate (IPDI). Acetone was used as a solvent. IPDI, MDI and TDI were reacted with monoester polyol at ratios of 10:9, 10:10, 10:12 and 10:14 (polyol:diisocyanate). Then, the PU foams produced by the curing process were analyzed by Fourier Transform infrared spectroscopy (FTIR). The FTIR spectra showed the presence of the amide peak (-NH) and the absence of hydroxyl peak (-OH) indicated that the reaction between polyol and diisocyanate has occurred. However, the soxhlet extraction showed that only MDI-based PUs contain crosslinking bond. These cross-linking bond at the ratio of 10:10, 10:12 and 10:14 were 41.3 %,61.1 % and 74.1 % respectively. Thermal properties of the PU foams were determined by differential scanning calorimetry (DSC) and thermogravimetry (TGA) techniques. MDI-based PUs and TDI-based PUs show two values of Tg while IPDI-based PUs only show one Tg value. The tensile strains of PU foams decreased with increasing ratio of isocyanate. Meanwhile, PU foams with ratio of polyol to isocyanate at 10:12 showed the highest tensile stress and modulus compared to at 10:10 and 10:14.

  2. 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...

  3. Microwave-Assisted Synthesis – Catalytic Applications in Aqueous Media

    EPA Science Inventory

    The development of sustainable methods directed towards the synthesis of molecules is due to the heightened awareness and recognition of alternative eco-friendly and economical protocols that have minimum impact on environment. Among others, microwave (MW)-assisted methodology ha...

  4. Microwave-assisted extraction performed in low temperature and in vacuo for the extraction of labile compounds in food samples.

    PubMed

    Xiao, Xiaohua; Song, Wei; Wang, Jiayue; Li, Gongke

    2012-01-27

    In this study, low temperature vacuum microwave-assisted extraction, which simultaneous performed microwave-assisted extraction (MAE) in low temperature and in vacuo environment, was proposed. The influencing parameters including solid/liquid ratio, extraction temperature, extraction time, degree of vacuum and microwave power were discussed. The predominance of low temperature vacuum microwave-assisted extraction was investigated by comparing the extraction yields of vitamin C, β-carotene, aloin A and astaxanthin in different foods with that in MAE and solvent extraction, and 5.2-243% increments were obtained. On the other hand, the chemical kinetics of vitamin C and aloin A, which composed two different steps including the extraction step of analyte transferred from matrix into solvent and the decomposition step of analyte degraded in the extraction solvent, were proposed. All of the decomposition rates (K(2)) for the selected analyte in low temperature, in vacuo and in nitrogen atmosphere decreased significantly comparing with that in conventional MAE, which are in agreement with that obtained from experiments. Consequently, the present method was successfully applied to extract labile compound from different food samples. These results showed that low temperature and/or in vacuo environment in microwave-assisted extraction system was especially important to prevent the degradation of labile components and have good potential on the extraction of labile compound in foods, pharmaceutical and natural products. Copyright © 2011 Elsevier B.V. All rights reserved.

  5. 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.

  6. 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.

  7. Low-temperature-compatible tunneling-current-assisted scanning microwave microscope utilizing a rigid coaxial resonator.

    PubMed

    Takahashi, Hideyuki; Imai, Yoshinori; Maeda, Atsutaka

    2016-06-01

    We present a design for a tunneling-current-assisted scanning near-field microwave microscope. For stable operation at cryogenic temperatures, making a small and rigid microwave probe is important. Our coaxial resonator probe has a length of approximately 30 mm and can fit inside the 2-in. bore of a superconducting magnet. The probe design includes an insulating joint, which separates DC and microwave signals without degrading the quality factor. By applying the SMM to the imaging of an electrically inhomogeneous superconductor, we obtain the spatial distribution of the microwave response with a spatial resolution of approximately 200 nm. Furthermore, we present an analysis of our SMM probe based on a simple lumped-element circuit model along with the near-field microwave measurements of silicon wafers having different conductivities.

  8. Low-temperature-compatible tunneling-current-assisted scanning microwave microscope utilizing a rigid coaxial resonator

    NASA Astrophysics Data System (ADS)

    Takahashi, Hideyuki; Imai, Yoshinori; Maeda, Atsutaka

    2016-06-01

    We present a design for a tunneling-current-assisted scanning near-field microwave microscope. For stable operation at cryogenic temperatures, making a small and rigid microwave probe is important. Our coaxial resonator probe has a length of approximately 30 mm and can fit inside the 2-in. bore of a superconducting magnet. The probe design includes an insulating joint, which separates DC and microwave signals without degrading the quality factor. By applying the SMM to the imaging of an electrically inhomogeneous superconductor, we obtain the spatial distribution of the microwave response with a spatial resolution of approximately 200 nm. Furthermore, we present an analysis of our SMM probe based on a simple lumped-element circuit model along with the near-field microwave measurements of silicon wafers having different conductivities.

  9. 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.

  10. A brief understanding of process optimisation in microwave-assisted extraction of botanical materials: options and opportunities with chemometric tools.

    PubMed

    Das, Anup Kumar; Mandal, Vivekananda; Mandal, Subhash C

    2014-01-01

    Extraction forms the very basic step in research on natural products for drug discovery. A poorly optimised and planned extraction methodology can jeopardise the entire mission. To provide a vivid picture of different chemometric tools and planning for process optimisation and method development in extraction of botanical material, with emphasis on microwave-assisted extraction (MAE) of botanical material. A review of studies involving the application of chemometric tools in combination with MAE of botanical materials was undertaken in order to discover what the significant extraction factors were. Optimising a response by fine-tuning those factors, experimental design or statistical design of experiment (DoE), which is a core area of study in chemometrics, was then used for statistical analysis and interpretations. In this review a brief explanation of the different aspects and methodologies related to MAE of botanical materials that were subjected to experimental design, along with some general chemometric tools and the steps involved in the practice of MAE, are presented. A detailed study on various factors and responses involved in the optimisation is also presented. This article will assist in obtaining a better insight into the chemometric strategies of process optimisation and method development, which will in turn improve the decision-making process in selecting influential extraction parameters. Copyright © 2013 John Wiley & Sons, Ltd.

  11. The Successful Diagnosis and Typing of Systemic Amyloidosis Using A Microwave-Assisted Filter-Aided Fast Sample Preparation Method and LC/MS/MS Analysis

    PubMed Central

    Zou, Lili; Shen, Kaini; Zhong, Dingrong; Zhou, Daobin; Sun, Wei; Li, Jian

    2015-01-01

    Laser microdissection followed by mass spectrometry has been successfully used for amyloid typing. However, sample contamination can interfere with proteomic analysis, and overnight digestion limits the analytical throughput. Moreover, current quantitative analysis methods are based on the spectrum count, which ignores differences in protein length and may lead to misdiagnoses. Here, we developed a microwave-assisted filter-aided sample preparation (maFASP) method that can efficiently remove contaminants with a 10-kDa cutoff ultrafiltration unit and can accelerate the digestion process with the assistance of a microwave. Additionally, two parameters (P- and D-scores) based on the exponentially modified protein abundance index were developed to define the existence of amyloid deposits and those causative proteins with the greatest abundance. Using our protocol, twenty cases of systemic amyloidosis that were well-typed according to clinical diagnostic standards (training group) and another twenty-four cases without subtype diagnoses (validation group) were analyzed. Using this approach, sample preparation could be completed within four hours. We successfully subtyped 100% of the cases in the training group, and the diagnostic success rate in the validation group was 91.7%. This maFASP-aided proteomic protocol represents an efficient approach for amyloid diagnosis and subtyping, particularly for serum-contaminated samples. PMID:25984759

  12. Synthesis of BiFeO{sub 3} thin films on single-terminated Nb : SrTiO{sub 3} (111) substrates by intermittent microwave assisted hydrothermal method

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

    Velasco-Davalos, Ivan; Ambriz-Vargas, Fabian; Kolhatkar, Gitanjali

    We report on a simple and fast procedure to create arrays of atomically flat terraces on single crystal SrTiO{sub 3} (111) substrates and the deposition of ferroelectric BiFeO{sub 3} thin films on such single-terminated surfaces. A microwave-assisted hydrothermal method in deionized water and ammonia solution selectively removes either (SrO{sub 3}){sup 4−} or Ti{sup 4+} layers to ensure the same chemical termination on all terraces. Measured step heights of 0.225 nm (d{sub 111}) and uniform contrast in the phase image of the terraces confirm the single termination in pure and Nb doped SrTiO{sub 3} single crystal substrates. Multiferroic BiFeO{sub 3} thinmore » films were then deposited by the same microwave assisted hydrothermal process on Nb : SrTiO{sub 3} (111) substrates. Bi(NO{sub 3}){sub 3} and Fe(NO{sub 3}){sub 3} along with KOH served as the precursors solution. Ferroelectric behavior of the BiFeO{sub 3} films on Nb : SrTiO{sub 3} (100) substrates was verified by piezoresponse force microscopy.« less

  13. Fast preparation of flower-like Bi{sub 4}Ge{sub 3}O{sub 12} microstructures via a microwave-assisted hydrothermal process

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

    Li, Zhao-Qian; Zhang, Lei; Chen, Xue-Tai, E-mail: xtchen@netra.nju.edu.cn

    In the present paper, we report a facile and fast microwave-assisted solution-phase approach for the preparation of flower-like bismuth germanate (Bi{sub 4}Ge{sub 3}O{sub 12}) microstructures, employing bismuth nitrate pentahydrate (Bi(NO{sub 3}){sub 3}{center_dot}5H{sub 2}O) and germanium dioxide (GeO{sub 2}) as starting materials. The phase and morphology of the products were characterized by powder X-ray diffraction, X-ray photoelectron spectrum, energy dispersive spectrometry, and scanning electron microscopy. Some control experiments have been carried out to reveal the influencing factors involved in the formation, which suggested that reaction time, reaction temperature, the volume of ammonia and glycerol play crucial roles in the formation ofmore » the flower-like Bi{sub 4}Ge{sub 3}O{sub 12}. The optical absorption property of the product has been investigated. - Highlights: Black-Right-Pointing-Pointer Flower-like Bi4Ge3O12 was synthesized via a microwave-assisted solution route. Black-Right-Pointing-Pointer The phases and morphologies of the product have been characterized. Black-Right-Pointing-Pointer The optical property of the product has been studied.« less

  14. 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.

  15. Influences of the Ratio of Polyol and MDI on the Acoustic Parameters of Polyurethane

    NASA Astrophysics Data System (ADS)

    Wang, Yonghua; Liu, Zheming; Wu, Haiquan; Zhang, Chengchun; Yu, Huadong; Ren, Luquan; Ichchou, Mohamed

    2018-05-01

    In this paper, the influence of different ratio of polyol and MDI on the absorption coefficient and acoustic parameters of polyurethane was studied. Ratio of 100:40 and 100:45 show the best sound absorption performance, and the change trend of transmission loss and sound absorption coefficient are opposite. The flow resistance increased with the increasing of the ratio of polyol and MDI, the greater the flow resistance, the worse the high frequency sound absorption property of the polyurethane. When the ratio of polyol and MDI keep 100:45, the minimum porosity of sample, the polyurethane porosity increase with the ratio of polyol and MDI increase.

  16. Characteristics of the microwave pyrolysis and microwave CO2-assisted gasification of dewatered sewage sludge.

    PubMed

    Chun, Young Nam; Jeong, Byeo Ri

    2017-07-28

    Microwave drying-pyrolysis or drying-gasification characteristics were examined to convert sewage sludge into energy and resources. The gasification was carried out with carbon dioxide as a gasifying agent. The examination results were compared with those of the conventional heating-type electric furnace to compare both product characteristics. Through the pyrolysis or gasification, gas, tar, and char were generated as products. The produced gas was the largest component of each process, followed by the sludge char and the tar. During the pyrolysis process, the main components of the produced gas were hydrogen and carbon monoxide, with a small amount of hydrocarbons such as methane and ethylene. In the gasification process, however, the amount of carbon monoxide was greater than the amount of hydrogen. In microwave gasification, a large amount of heavy tar was produced. The largest amount of benzene in light tar was generated from the pyrolysis or gasification. Ammonia and hydrogen cyanide, which are precursors of NO x , were also generated. In the microwave heating method, the sludge char produced by pyrolysis and gasification had pores in the mesopore range. This could be explained that the gas obtained from the microwave pyrolysis or gasification of the wet sewage sludge can be used as an alternative fuel, but the tar and NO x precursors in the produced gas should be treated. Sludge char can be used as a biomass solid fuel or as a tar removal adsorbent if necessary.

  17. 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.

  18. Microwave-assisted extraction and a new determination method for total steroid saponins from Dioscorea zingiberensis C.H. Wright.

    PubMed

    Ren, Yao; Chen, Yu; Hu, Bohan; Wu, Hui; Lai, Furao; Li, Xiaofeng

    2015-12-01

    An efficient microwave-assisted extraction (MAE) technique was applied to isolate total steroid saponins from Dioscorea zingiberensis C.H. Wright (DZW). The optimal extracting conditions were established as 75% ethanol as solvent, ratio of solid/liquid 1:20 (g/ml), temperature 75 °C, irradiation power 600 W and three extraction cycles of 6 min each. Scanning electron microscopy (SEM) images of DZW processed by four different extractions provided visual evidence of the disruption effect on DZW. Diosgenin was quantified by HPLC and examined further by LC-ESI/MS after acid hydrolysis. Total steroid saponins were calculated using diosgenin from total steroid saponins. The MAE procedure was optimized, validated and compared with other conventional extraction processes. This report provides a convenient technology for the extraction and quantification of total saponins of DZW combining MAE with HPLC and LC-ESI/MS for the first time. Copyright © 2015 Elsevier Inc. All rights reserved.

  19. 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. Copyright © 2014 Elsevier Ltd. All rights reserved.

  20. Determining Optimal Microwave Antigen Retrieval Conditions for Microtubule-Associated Protein 2 Immunohistochemistry in the Guinea Pig Brain

    DTIC Science & Technology

    2002-12-01

    sections of formalin-fixed guinea pig brains using different MAP-2 monoclonal antibodies. Brain sections were boiled in sodium citrate, citric acid...citric acid solution at pH 6.0 is the optimal microwave-assisted AR method for immunolabeling MAP-2 in formalin-fixed, paraffin-processed guinea pig brain...studies on archival guinea pig brain paraffin blocks, ultimately relaxing the use of additional animals to evaluate changes in MAP-2 expression between chemical warfare nerve agent-treated and control samples.

  1. Process for the synthesis of unsaturated alcohols

    DOEpatents

    Maughon, Bob R.; Burdett, Kenneth A.; Lysenko, Zenon

    2007-02-13

    A process of preparing an unsaturated alcohol (olefin alcohol), such as, a homo-allylic mono-alcohol or homo-allylic polyol, involving protecting a hydroxy-substituted unsaturated fatty acid or fatty acid ester, such as methyl ricinoleate, derived from a seed oil, to form a hydroxy-protected unsaturated fatty acid or fatty acid ester; homo-metathesizing or cross-metathesizing the hydroxy-protected unsaturated fatty acid or fatty acid ester to produce a product mixture containing a hydroxy-protected unsaturated metathesis product; and deprotecting the hydroxy-protected unsaturated metathesis product under conditions sufficient to prepare the unsaturated alcohol. Preferably, methyl ricinoleate is converted by cross-metathesis or homo-metathesis into the homo-allylic mono-alcohol 1-decene-4-ol or the homo-allylic polyol 9-octadecene-7,12-diol, respectively.

  2. Utilizing commercial microwave for rapid and effective immunostaining.

    PubMed

    Owens, Katrina; Park, Ji H; Kristian, Tibor

    2013-09-30

    There is an accumulating literature demonstrating the application of microwaves across a wide spectrum of histological techniques. Although exposure to microwaves for short periods resulted in substantial acceleration of all procedures this technique still is not adopted widely. In part, this may be due to concerns over solutions that will avoid induction of thermal damage to the tissue when using standard microwave. Here, we offer a cooling setup that can be used with conventional microwave ovens. We utilized dry ice for effective cooling during microwave irradiation of tissue samples. To prevent overheating, the cups with tissue during exposure to microwaves were surrounded with powdered dry ice. Since the dry ice does not touch the walls of the cups, freezing is prevented. Overheating is avoided by alternating the microwave treatment with 1-2 min time periods when the cups are cooled outside of the microwave oven. This technique was used on mouse brain sections that were immunostained with microglia-specific CD68 antiserum and astrocyte labeling GFAP antibody. Both standard and microwave-assisted immonolabeling gave comparable results visualizing cells with fine processes and low background signal. Short incubation time in the microwave requires high concentrations of antibody for tissue immunostaining. We show that by prolonging the microwaving procedure we were able to reduce the antibody concentration to the levels used in standard immunostaining protocol. In summary, our technique gives a possibility to use a conventional microwave for rapid and effective immunolabeling resulting in reduced amount of antibody required for satisfactory immunostaining. Published by Elsevier B.V.

  3. Synthesis, characterization and oxidation of metallic cobalt (Co) thin film into semiconducting cobalt oxide (Co3O4)thin film using microwave plasma CVD

    NASA Astrophysics Data System (ADS)

    Rahman Ansari, Akhalakur; Hussain, Shahir; Imran, Mohd; Abdel-wahab, M. Sh; Alshahrie, Ahmed

    2018-06-01

    The pure cobalt thin film was deposited on the glass substrate by using DC magnetron sputtering and then exposed to microwave assist oxygen plasma generated in microwave plasma CVD. The oxidation process of Co thin film into Co3O4 thin films with different microwave power and temperature were studied. The influences of microwave power, temperature and irradiation time were investigated on the morphology and particle size of oxide thin films. The crystal structure, chemical conformation, morphologies and optical properties of oxidized Co thin films (Co3O4) were studied by using x-ray diffraction (XRD), Field emission scanning electron microscopy (FESEM), Raman Spectroscopy and UV–vis Spectroscopy. The data of these films showed complete oxidation pure metallic cobalt (Co) into cobalt oxide (Co3O4). The optical properties were studied for calculating the direct band gaps which ranges from 1.35 to 1.8 eV.

  4. Quantification of fructans, galacto-oligosacharides and other short-chain carbohydrates in processed grains and cereals.

    PubMed

    Biesiekierski, J R; Rosella, O; Rose, R; Liels, K; Barrett, J S; Shepherd, S J; Gibson, P R; Muir, J G

    2011-04-01

    Wholegrain grains and cereals contain a wide range of potentially protective factors that are relevant to gastrointestinal health. The prebiotics best studied are fructans [fructooligosaccharides (FOS), inulin] and galactooligosaccharides (GOS). These and other short-chain carbohydrates can also be poorly absorbed in the small intestine (named fermentable oligo-, di- and monosaccharides and polyols; FODMAPs) and may have important implications for the health of the gut. In the present study, FODMAPs, including fructose in excess of glucose, FOS (nystose, kestose), GOS (raffinose, stachyose) and sugar polyols (sorbitol, mannitol), were quantified using high-performance liquid chromatography with an evaporative light scattering detector. Total fructan was quantified using an enzymic hydrolysis method. Fifty-five commonly consumed grains, breakfast cereals, breads, pulses and biscuits were analysed. Total fructan were the most common short-chain carbohydrate present in cereal grain products and ranged (g per portion as eaten) from 1.12 g in couscous to 0 g in rice; 0.6 g in dark rye bread to 0.07 g in spelt bread; 0.96 g in wheat-free muesli to 0.11 g in oats; and 0.81 g in muesli fruit bar to 0.05 g in potato chips. Raffinose and stachyose were most common in pulses.   Composition tables including FODMAPs and prebiotics (FOS and GOS) that are naturally present in food will greatly assist research aimed at understanding their physiological role in the gut. © 2011 The Authors. Journal compilation © 2011 The British Dietetic Association Ltd.

  5. Determination of trace nickel in hydrogenated cottonseed oil by electrothermal atomic absorption spectrometry after microwave-assisted digestion.

    PubMed

    Zhang, Gai

    2012-01-01

    Microwave digestion of hydrogenated cottonseed oil prior to trace nickel determination by electrothermal atomic absorption spectrometry (ETAAS) is proposed here for the first time. Currently, the methods outlined in U.S. Pharmacopeia 28 (USP28) or British Pharmacopeia (BP2003) are recommended as the official methods for analyzing nickel in hydrogenated cottonseed oil. With these methods the samples may be pre-treated by a silica or a platinum crucible. However, the samples were easily tarnished during sample pretreatment when using a silica crucible. In contrast, when using a platinum crucible, hydrogenated cottonseed oil acting as a reducing material may react with the platinum and destroy the crucible. The proposed microwave-assisted digestion avoided tarnishing of sample in the process of sample pretreatment and also reduced the cycle of analysis. The programs of microwave digestion and the parameters of ETAAS were optimized. The accuracy of the proposed method was investigated by analyzing real samples. The results were compared with the ones by pressurized-PTFE-bomb acid digestion and ones obtained by the U.S. Pharmacopeia 28 (USP28) method. The new method involves a relatively rapid matrix destruction technique compared with other present methods for the quantification of metals in oil. © 2011 Institute of Food Technologists®

  6. Microwave-assisted extraction of herbacetin diglucoside from flax (Linum usitatissimum L.) seed cakes and its quantification using an RP-HPLC-UV system.

    PubMed

    Fliniaux, Ophélie; Corbin, Cyrielle; Ramsay, Aina; Renouard, Sullivan; Beejmohun, Vickram; Doussot, Joël; Falguières, Annie; Ferroud, Clotilde; Lamblin, Frédéric; Lainé, Eric; Roscher, Albrecht; Grand, Eric; Mesnard, François; Hano, Christophe

    2014-03-10

    Flax (Linum usitatissimum L.) seeds are widely used for oil extraction and the cold-pressed flaxseed (or linseed) cakes obtained during this process constitute a valuable by-product. The flavonol herbacetin diglucoside (HDG) has been previously reported as a constituent of the flaxseed lignan macromolecule linked through ester bonds to the linker molecule hydroxymethylglutaric acid. In this context, the development and validation of a new approach using microwave-assisted extraction (MAE) of HDG from flaxseed cakes followed by quantification with a reverse-phase HPLC system with UV detection was purposed. The experimental parameters affecting the HDG extraction yield, such as microwave power, extraction time and sodium hydroxide concentration, from the lignan macromolecule were optimized. A maximum HDG concentration of 5.76 mg/g DW in flaxseed cakes was measured following an irradiation time of 6 min, for a microwave power of 150 W using a direct extraction in 0.1 M NaOH in 70% (v/v) aqueous methanol. The optimized method was proven to be rapid and reliable in terms of precision, repeatability, stability and accuracy for the extraction of HDG. Comparison with a conventional extraction method demonstrated that MAE is more effective and less time-consuming.

  7. 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...

  8. 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...

  9. 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. Copyright © 2014 Elsevier Ltd. All rights reserved.

  10. 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

  11. Apparatus and method for investigation of energy consumption of microwave assisted drying systems.

    PubMed

    Göllei, Attila; Vass, András; Magyar, Attila; Pallai, Elisabeth

    2009-10-01

    Convective, hot air drying by itself is relatively efficient for removing water from the surface environment of agricultural seed products. However, moving internal moisture to the surface needs rather a long time, as a rule. The major research aim of the authors was to decrease the processing time and processing costs, to improve the quality of the dried product, and to increase drying efficiency. For this reason their research activities focused on the development of a special drying apparatus and a method suitable for measuring of energy conditions in a hybrid (microwave and convective) dryer. Experimental investigations were made with moistened wheat as model material. Experiments were carried out in microwave, convective and hybrid drying systems. The microwave drying alone was more efficient than the convective method. The lowest energy consumption and shortest drying time were obtained by the use of a hybrid method in which the waste energy of magnetron was utilized and the temperature was controlled. In this way, it was possible to keep the temperature of the dried product at a constant and safe value and to considerably decrease the energy consumption.

  12. Microwave Assisted Enzymatic Kinetic Resolution of (±)-1-Phenyl-2-propyn-1-ol in Nonaqueous Media

    PubMed Central

    Devendran, Saravanan; Yadav, Ganapati D.

    2014-01-01

    Kinetic resolution of 1-phenyl-2-propyn-1-ol, an important chiral synthon, was studied through trans-esterification with acyl acetate to investigate synergism between microwave irradiation and enzyme catalysis. Lipases from different microbial origins were employed for the kinetic resolution of (R/S)-1-phenyl-2-propyn-1-ol, among which Candida antarctica lipase B, immobilized on acrylic resin (Novozym 435), was found to be the best catalyst in n-hexane as solvent. Vinyl acetate was the most effective among different acyl esters studied. The effect of various parameters was studied in a systematic manner. Definite synergism between microwave and enzyme was observed. The initial rate was improved around 1.28 times under microwave irradiation than conventional heating. Under optimum conditions, maximum conversion (48.78%) and high enantiomeric excess (93.25%) were obtained in 2 h. From modeling studies, it is concluded that the reaction follows the Ping-Pong bi-bi mechanism with dead end alcohol inhibition. Kinetic parameters were obtained by using nonlinear regression. This process is green, clean, and easily scalable as compared to the chemical process. PMID:24707487

  13. 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. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. 40 CFR 721.7480 - Isocyanate terminated polyols.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... SUBSTANCES CONTROL ACT SIGNIFICANT NEW USES OF CHEMICAL SUBSTANCES Significant New Uses for Specific Chemical Substances § 721.7480 Isocyanate terminated polyols. (a) Chemical substances and significant new uses subject to reporting. (1) The chemical substances identified generically as isocyanate terminated polyols (P...

  15. 40 CFR 721.7480 - Isocyanate terminated polyols.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... SUBSTANCES CONTROL ACT SIGNIFICANT NEW USES OF CHEMICAL SUBSTANCES Significant New Uses for Specific Chemical Substances § 721.7480 Isocyanate terminated polyols. (a) Chemical substances and significant new uses subject to reporting. (1) The chemical substances identified generically as isocyanate terminated polyols (P...

  16. Removal of Hexavalent Chromium by Adsorption on Microwave Assisted Activated Carbon Prepared from Stems of Leucas Aspera

    NASA Astrophysics Data System (ADS)

    Shanmugalingam, A.; Murugesan, A.

    2018-05-01

    This study reports adsorption of Cr(VI) ions from aqueous solution using activated carbon that was prepared from stems of Leucas aspera. Eight hundred and fifty watts power of microwave radiation, 12 min of radiation time, 60% of ZnCl2 solution and 24 h of impregnation time are the optimal parameters to prepare efficient carbon effective activated carbon. It was designated as MWLAC (Microwave assisted Zinc chloride activated Leucas aspera carbon). Various adsorption characteristics such as dose of the adsorbent, agitation time, initial Cr(VI) ion concentration, pH of the solution and temperature on adsorption were studied for removal of Cr(VI) ions from aqueous solution by batch mode. Also the equilibrium adsorption was analyzed by the Langmuir, Freundlich, Tempkin and D-R isotherm models. The order of best describing isotherms was given based on R2 value. The pseudo-second-order kinetic model best fitted with the Cr(VI) adsorption data. Thermodynamic parameters were also determined and results suggest that the adsorption process is a spontaneous, endothermic and proceeded with increased randomness.

  17. Microwave-assisted inorganic salt pretreatment of sugarcane leaf waste: Effect on physiochemical structure and enzymatic saccharification.

    PubMed

    Moodley, Preshanthan; Kana, E B Gueguim

    2017-07-01

    This paper presents a method to pretreat sugarcane leaf waste using microwave-assisted (MA) inorganic salt to enhance enzymatic saccharification. The effects of process parameters of salt concentration, microwave power intensity and pretreatment time on reducing sugar yield from sugarcane leaf waste were investigated. Pretreatment models based on MA-NaCl, MA-ZnCl 2 and MA-FeCl 3 were developed with high coefficients of determination (R 2 >0.8) and optimized. Maximum reducing sugar yield of 0.406g/g was obtained with 2M FeCl 3 at 700W for 3.5min. Scanning electron microscopy (SEM), Fourier Transform Infrared analysis (FTIR) and X-ray diffraction (XRD) showed major changes in lignocellulosic structure after MA-FeCl 3 pretreatment with 71.5% hemicellulose solubilization. This regime was further assessed on sorghum leaves and Napier grass under optimal MA-FeCl 3 conditions. A 2-fold and 3.1-fold increase in sugar yield respectively were observed compared to previous reports. This pretreatment was highly effective for enhancing enzymatic saccharification of lignocellulosic biomass. Copyright © 2017. Published by Elsevier Ltd.

  18. Potential of activated carbon from waste rubber tire for the adsorption of phenolics: effect of pre-treatment conditions.

    PubMed

    Gupta, Vinod Kumar; Nayak, Arunima; Agarwal, Shilpi; Tyagi, Inderjeet

    2014-03-01

    Rubber tire activated carbon modification (RTACMC) and rubber tire activated carbon (RTAC) were prepared from waste rubber tire by microwave assisted chemical treatment and physical heating respectively. A greater improvement in porosity and total pore volume was achieved in RTACMC as compared to that of RTAC. But both have a predominantly mesoporous structure. Under identical operating conditions, an irradiation time of 10 min, chemical impregnation ratio of 1.50 and a microwave power of 600 W resulted in maximizing the efficiency of RTACMC for p-cresol (250 mg/g) at a contact time of 90 min while RTAC showed a 71.43 mg/g adsorption capacity at 150 min. Phenol, due to its higher solubility was adsorbed to a lesser extent by both adsorbents. Physical nature of interactions, pore diffusion mechanism and exothermicity of the adsorption process was operative in both adsorbents. The outcomes support the feasibility of preparing high quality activated carbon from waste rubber tire by microwave assisted chemical activation. Copyright © 2013 Elsevier Inc. All rights reserved.

  19. Optimization of microwave-assisted extraction for the characterization of olive leaf phenolic compounds by using HPLC-ESI-TOF-MS/IT-MS(2).

    PubMed

    Taamalli, Amani; Arráez-Román, David; Ibañez, Elena; Zarrouk, Mokhtar; Segura-Carretero, Antonio; Fernández-Gutiérrez, Alberto

    2012-01-25

    In the present work, a simple and rapid method for the extraction of phenolic compounds from olive leaves, using microwave-assisted extraction (MAE) technique, has been developed. The experimental variables that affect the MAE process, such as the solvent type and composition, microwave temperature, and extraction time, were optimized using a univariate method. The obtained extracts were analyzed by using high-performance liquid chromatography (HPLC) coupled to electrospray time-of-flight mass spectrometry (ESI-TOF-MS) and electrospray ion trap tandem mass spectrometry (ESI-IT-MS(2)) to prove the MAE extraction efficiency. The optimal MAE conditions were methanol:water (80:20, v/v) as extracting solvent, at a temperature equal to 80 °C for 6 min. Under these conditions, several phenolic compounds could be characterized by HPLC-ESI-MS/MS(2). As compared to the conventional method, MAE can be used as an alternative extraction method for the characterization of phenolic compounds from olive leaves due to its efficiency and speed.

  20. Electrically tunable materials for microwave applications

    NASA Astrophysics Data System (ADS)

    Ahmed, Aftab; Goldthorpe, Irene A.; Khandani, Amir K.

    2015-03-01

    Microwave devices based on tunable materials are of vigorous current interest. Typical applications include phase shifters, antenna beam steering, filters, voltage controlled oscillators, matching networks, and tunable power splitters. The objective of this review is to assist in the material selection process for various applications in the microwave regime considering response time, required level of tunability, operating temperature, and loss tangent. The performance of a variety of material types are compared, including ferroelectric ceramics, polymers, and liquid crystals. Particular attention is given to ferroelectric materials as they are the most promising candidates when response time, dielectric loss, and tunability are important. However, polymers and liquid crystals are emerging as potential candidates for a number of new applications, offering mechanical flexibility, lower weight, and lower tuning voltages.

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

    PubMed

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

    2014-04-15

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

  2. Enhancement of water removing and the quality of fried purple-fleshed sweet potato in the vacuum frying by combined power ultrasound and microwave technology.

    PubMed

    Su, Ya; Zhang, Min; Bhandari, Bhesh; Zhang, Weiming

    2018-06-01

    The combination of ultrasound and microwave in vacuum frying system was investigated to achieve higher drying efficiency and quality attributes of fried products. Purple-fleshed potato were used as test specimen and different power levels of microwave (0 W, 600 W, 800 W) and ultrasound (0 W, 300 W, 600 W) during vacuum frying. Drying kinetics, dielectric properties, moisture state variation and quality attributes of fried samples were measured in a vacuum frying (VF), and an innovatively designed ultrasound and microwave assisted vacuum frying (USMVF) equipment. The USMVF process markedly increased the moisture evaporation rate and effective moisture diffusivity compared to VF process. The oil uptake was reduced by about 16-34%, the water activity and the shrinkage was lowered, the texture (crispness) and the color of fried samples were greatly improved. The higher ultrasound and microwave power level in USMVF made a greater improvement. The total anthocyanin levels and retention of fried purple-fleshed potato chips was the highest (123.52 mg/100 g solids and 79.51% retention, respectively) among all treatments in US600M800VF process. The SEM analysis revealed a more porous and disruption microstructure in USMVF sample. Copyright © 2018 Elsevier B.V. All rights reserved.

  3. Microwave optimization of mucilage extraction from Opuntia ficus indica Cladodes.

    PubMed

    Felkai-Haddache, Lamia; Dahmoune, Farid; Remini, Hocine; Lefsih, Khalef; Mouni, Lotfi; Madani, Khodir

    2016-03-01

    In this study, microwave-assisted extraction (MAE) of polysaccharides from Opuntia ficus indica Cladodes were investigated using response surface methodology (RSM). The effects of three extraction factors on the yield of mucilage were examined. The results indicated that the optimum extraction conditions were determined as follows: microwave power X1, 700 W; extraction time X2, 5.15 minand ratio water/raw material X3, 4.83 mL/g at fixed pH 11. Under these optimal extraction conditions, mucilage yield was found to be Y, 25.6%. A comparison between the model results and experimental data gave a high correlation coefficient (R(2)=0.88), adjusted coefficient (Radj=0.83) and low root mean square error (RMSE=2.45) and showed that the two models were able to predict a mucilage yield by green extraction microwave process. Copyright © 2015 Elsevier B.V. All rights reserved.

  4. Conversion of agricultural residues to carboxymethylcellulose and carboxymethylcellulose acetate

    USDA-ARS?s Scientific Manuscript database

    In view of continuing interest in the use of agricultural by-products, we have converted cellulose, wheat straw, barley straw, and rice hull into carboxymethylcellulose (CMC). Microwave-assisted synthesis was found to be a partly effective alternative to the conventional heating process. The CMC thu...

  5. A facile microwave-assisted Diels-Alder reaction of vinylboronates.

    PubMed

    Sarotti, Ariel M; Pisano, Pablo L; Pellegrinet, Silvina C

    2010-11-21

    The Diels-Alder reaction of vinylboronates can be easily performed using microwave irradiation giving excellent yields of the cycloadducts. Pinacol vinylboronate was the reagent of choice due to its stability towards hydrolysis, operational simplicity and yields of Diels-Alder products. To the best of our knowledge, this is the first example of microwave-assisted Diels-Alder reaction of boron-substituted dienophiles. Subsequent in situ oxidation of the cycloadducts with alkaline hydrogen peroxide afforded the alcohols efficiently.

  6. Microwave assisted centrifuge and related methods

    DOEpatents

    Meikrantz, David H [Idaho Falls, ID

    2010-08-17

    Centrifuge samples may be exposed to microwave energy to heat the samples during centrifugation and to promote separation of the different components or constituents of the samples using a centrifuge device configured for generating microwave energy and directing the microwave energy at a sample located in the centrifuge.

  7. Rapeseed Oil as Renewable Resource for Polyol Synthesis

    NASA Astrophysics Data System (ADS)

    Stirna, Uldis; Fridrihsone, Anda; Misane, Marija; Vilsone, Dzintra

    2011-01-01

    Vegetable oils are one of the most important platform chemicals due to their accessibility, specific structure of oils and low price. Rapeseed oil (RO) polyols were prepared by amidization of RO with diethanolamine (DEA). To determine the kinetics of amidization reaction, experiments were carried out. Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), amine (NH) value was determined. Group contribution method by Fedor‵s was used to calculate solubility parameters, van der Waals volume was calculated by Askadskii. Obtained polyol‵s OH and NH value are from 304 up to 415 mg KOH/g. RO polyols synthesis meets the criteria of "green chemistry". In the present study, reaction of RO amidization with DEA was investigated, as well as optimum conditions for polyol synthesis was established to obtain polyols for polyurethane production. Calculations of solubility parameter and cohesion energy density were calculated, as RO polyols will be used as side chains in polymers, and solubility parameter will be used to explain properties of polymers.

  8. 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...

  9. Microwave-Assisted Chemistry: Synthetic Applications for Rapid Assembly of Nanomaterials and Organics

    EPA Science Inventory

    The magic of microwave (MW) heating technique, termed as the Bunsen burner of the 21th Century, has emerged as valuable alternative in synthesis of organics, polymers, inorganics, and nanomaterials. Important innovations in MW-assisted chemistry now enable chemists to prepare cat...

  10. 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...

  11. Ionic-liquid-based ultrasound/microwave-assisted extraction of 2,4-dihydroxy-7-methoxy-1,4-benzoxazin-3-one and 6-methoxy-benzoxazolin-2-one from maize (Zea mays L.) seedlings.

    PubMed

    Li, Chunying; Lu, Zhicheng; Zhao, Chunjian; Yang, Lei; Fu, Yujie; Shi, Kunming; He, Xin; Li, Zhao; Zu, Yuangang

    2015-01-01

    We evaluated an ionic-liquid-based ultrasound/microwave-assisted extraction method for the extraction of 2,4-dihydroxy-7-methoxy-1,4-benzoxazin-3-one and 6-methoxy-benzoxazolin-2-one from etiolated maize seedlings. We performed single-factor and central composite rotatable design experiments to optimize the most important parameters influencing this technique. The best results were obtained using 1.00 M 1-octyl-3-methylimidazolium bromide as the extraction solvent, a 50°C extraction temperature, a 20:1 liquid/solid ratio (mL/g), a 21 min treatment time, 590 W microwave power, and 50 W fixed ultrasonic power. We performed a comparison between ionic-liquid-based ultrasound/microwave-assisted extraction and conventional homogenized extraction. Extraction yields of 2,4-dihydroxy-7-methoxy-1,4-benzoxazin-3-one and 6-methoxy-benzoxazolin-2-one by the ionic-liquid-based ultrasound/microwave-assisted extraction method were 1.392 ± 0.051 and 0.205 ± 0.008 mg/g, respectively, which were correspondingly 1.46- and 1.32-fold higher than those obtained by conventional homogenized extraction. All the results show that the ionic-liquid-based ultrasound/microwave-assisted extraction method is therefore an efficient and credible method for the extraction of 2,4-dihydroxy-7-methoxy-1,4-benzoxazin-3-one and 6-methoxy-benzoxazolin-2-one from maize seedlings. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. 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.

  13. Optimization of microwave assisted extraction of essential oils from Iranian Rosmarinus officinalis L. using RSM.

    PubMed

    Akhbari, Maryam; Masoum, Saeed; Aghababaei, Fahimeh; Hamedi, Sepideh

    2018-06-01

    In this study, the efficiencies of conventional hydro-distillation and novel microwave hydro-distillation methods in extraction of essential oil from Rosemary officinalis leaves have been compared. In order to attain the best yield and also highest quality of the essential oil in the microwave assisted method, the optimal values of operating parameters such as extraction time, microwave irradiation power and water volume to plant mass ratio were investigated using central composite design under response surface methodology. Optimal conditions for obtaining the maximum extraction yield in the microwave assisted method were predicted as follows: extraction time of 85 min, microwave power of 888 W, and water volume to plant mass ratio of 0.5 ml/g. The extraction yield at these predicted conditions was computed as 0.7756%. The qualities of the obtained essential oils under designed experiments were optimized based on total contents of four major compounds (α-pinene, 1,8-cineole, camphor and verbenone) which determined by gas chromatography equipped with mass spectroscopy (GC-MS). The highest essential oil quality (55.87%) was obtained at extraction time of 68 min; microwave irradiation power of 700 W; and water volume to plant mass ratio of zero.

  14. 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

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

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

    Liu, Xiao-Lin, E-mail: liu_x_l@sina.cn; Zhu, Ying-Jie; Zhang, Qian

    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 thismore » 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).« less

  16. Microwave-assisted synthesis of cyclodextrin polyurethanes.

    PubMed

    Biswas, Atanu; Appell, Michael; Liu, Zengshe; Cheng, H N

    2015-11-20

    Cyclodextrin (CD) has often been incorporated into polyurethanes in order to facilitate its use in encapsulation or removal of organic species for various applications. In this work a microwave-assisted method has been developed to produce polyurethanes consisting of α-, β-, and γ-CD and three common diisocyanates. As compared to conventional heating, this new synthetic method saves energy, significantly reduces reaction time, and gets similar or improved yield. The reaction products have been fully characterized with (13)C, (1)H, and two-dimensional NMR spectroscopy. With suitable stoichiometry of starting CD and diisocyanate, the resulting CD polyurethane is organic-soluble and water-insoluble and is shown to remove Nile red dye and phenol from water. Possible applications include the removal of undesirable materials from process streams, toxic compounds from the environment, and encapsulation of color or fragrance molecules. Published by Elsevier Ltd.

  17. Degradation of atrazine by microwave-assisted electrodeless discharge mercury lamp in aqueous solution.

    PubMed

    Ta, Na; Hong, Jun; Liu, Tingfeng; Sun, Cheng

    2006-11-02

    The present study investigates the degradation of atrazine (2-chloro-4-(ethyl amino)-6-isopropyl amino-s-triazine) in aqueous solution by a developed new method, namely by means of a microwave-assisted electrodeless discharge mercury lamp (MW-EDML). An experimental design was conducted to assess the influence of various parameters: pH value, initial concentration, amount of EDML, initial volume and coexisted solvent. Atrazine was degraded completely by EDML in a relatively short time (i.e. t(1/2)=1.2 min for 10 mg/l). Additionally, the identification of main degradation products during atrazine degradation process was conducted by gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS). This study proposes the degradation mechanism including four possible pathways for atrazine degradation according to the degradation products.

  18. Understanding the electrocatalytic activity of Pt xSn y in direct ethanol fuel cells

    NASA Astrophysics Data System (ADS)

    Wang, Yi; Song, Shuqin; Andreadis, George; Liu, Hong; Tsiakaras, Panagiotis

    In the present work, the activity of Pt xSn y/C catalysts towards ethanol, acetaldehyde and acetic acid electrooxidation reactions is investigated for each one separately by means of cyclic voltammetry. To this purpose, a series of Pt xSn y/C catalysts with different atomic ratio (x: y = 2:1, 3:2, 1:1) and small particle size (∼3 nm) are fast synthesized by using the pulse microwave assisted polyol method. The catalysts are well dispersed over the carbon support based on the physicochemical characterization by means of XRD and TEM. Concerning the ethanol electrooxidation, it is found that the Sn addition strongly enhances Pt's electrocatalytic activity and the contributing effect of Sn depends on: (i) the Sn content and (ii) the operating temperature. More precisely, at lower temperatures, Sn-rich catalysts exhibit better ethanol electrooxidation performance while at higher temperatures Sn-poor catalysts give better performance. In the case of acetaldehyde electrooxidation, Pt 1Sn 1/C catalyst exhibits the highest activity at all the investigated temperatures; due to the role of Sn, which could effectively remove C 2 species and inhibit the poison formation by supplying oxygen-containing species. Finally, it is found that the Pt xSn y/C catalysts are almost inactive (little current was measured) towards the acetic acid electrooxidation. The above findings indicate that Sn cannot substantially promote the electrooxidation of acetic acid to C 1 species.

  19. 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...

  20. 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…

  1. 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...

  2. 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...

  3. MICROWAVE-ASSISTED PREPARATION OF DIALKYLIMIDAZOLIUM TETRACHLOROALUMINATES AND THEIR USE AS CATALYSTS IN THE SOLVENT-FREE TETRAHYDROPYRANYLATION OF ALCOHOLS AND PHENOLS

    EPA Science Inventory

    Microwave-assisted preparation of dialkylimidazolium tetrachloroaluminates and their application as recyclable catalysts for the efficient and eco-friendly protection of alcohols as tetrahydropyranyl (THP) ethers are described; the same catalyst can also be utilized for the depro...

  4. Development of novel high power-short time (HPST) microwave assisted commercial decontamination process for dried turmeric powder (Curcuma Longa L.).

    PubMed

    Behera, G; Sutar, P P; Aditya, S

    2017-11-01

    The commercially available dry turmeric powder at 10.34% d.b. moisture content was decontaminated using microwaves at high power density for short time. To avoid the loss of moisture from turmeric due to high microwave power, the drying kinetics were modelled and considered during optimization of microwave decontamination process. The effect of microwave power density (10, 33.5 and 57 W g -1 ), exposure time (10, 20 and 30 s) and thickness of turmeric layer (1, 2 and 3 mm) on total plate, total yeast and mold (YMC) counts, color change (∆E), average final temperature of the product (T af ), water activity (a w ), Page model rate constant (k) and total moisture loss (ML) was studied. The perturbation analysis was carried out for all variables. It was found that to achieve more than one log reduction in yeast and mold count, a substantial reduction in moisture content takes place leading to the reduced output. The microwave power density significantly affected the YMC, T af and a w of turmeric powder. But the thickness of sample and microwave exposure time showed effect only on T af , a w and ML. The colour of turmeric and Page model rate constant were not significantly changed during the process as anticipated. The numerical optimization was done at 57.00 W g -1 power density, 1.64 mm thickness of sample layer and 30 s exposure time. It resulted into 1.6 × 10 7 CFU g -1 YMC, 82.71 °C T af , 0.383 a w and 8.41% (d.b.) final moisture content.

  5. Microwave-assisted synthesis of medicinally relevant indoles.

    PubMed

    Patil, S A; Patil, R; Miller, D D

    2011-01-01

    Indoles represent an important structural class in medicinal chemistry with broad spectrum of biological activities. The synthesis of indoles, therefore, has attracted enormous attention from synthetic chemists. Microwave methods for the preparation of indole analogs have been developed to speed up the synthesis, therefore, microwave assisted organic synthesis (MAOS) in controlled conditions is an invaluable technique for medicinal chemistry. In this review, indole forming classical reactions such as Fischer, Madelung, Bischler-Mohlau, Batcho-Leimgruber, Hemetsberger-Knittel, Graebe-Ullmann, Diels-Alder and Wittig type reactions using microwave radiation has been summarized. In addition, metal mediated cyclizations along with solid phase synthesis of indoles have been discussed. © 2011 Bentham Science Publishers Ltd.

  6. 77 FR 20386 - Agency Information Collection Activities; Submission to OMB for Review and Approval; Comment...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-04-04

    ... Activities; Submission to OMB for Review and Approval; Comment Request; NESHAP for Polyether Polyols... electronic docket, go to www.regulations.gov . Title: NESHAP for Polyether Polyols Production (Renewal). ICR... Hazardous Air Pollutants (NESHAP) for Polyether Polyols Production (40 CFR part 63 subpart PPP) were...

  7. New biobased high functionality polyols and their use in polyurethane coatings.

    PubMed

    Pan, Xiao; Webster, Dean C

    2012-02-13

    High-functionality polyols for application in polyurethanes (PUs) were prepared by epoxide ring-opening reactions from epoxidized sucrose esters of soybean oil-epoxidized sucrose soyates-in which secondary hydroxyl groups were generated from epoxides on fatty acid chains. Ester polyols were prepared by using a base-catalyzed acid-epoxy reaction with carboxylic acids (e.g., acetic acid); ether polyols were prepared by using an acid-catalyzed alcohol-epoxy reaction with monoalcohols (e.g., methanol). The polyols were characterized by using gel permeation chromatography, FTIR spectroscopy, (1)H NMR spectroscopy, differential scanning calorimetry (DSC), and viscosity measurements. PU thermosets were prepared by using aliphatic polyisocyanates based on isophorone diisocyanate and hexamethylene diisocyanate. The properties of the PUs were studied by performing tensile testing, dynamic mechanical analysis, DSC, and thermogravimetric analysis. The properties of PU coatings on steel substrates were evaluated by using ASTM methods to determine coating hardness, adhesion, solvent resistance, and ductility. Compared to a soy triglyceride polyol, sucrose soyate polyols provide greater hardness and range of cross-link density to PU thermosets because of the unique structure of these macromolecules: well-defined compact structures with a rigid sucrose core coupled with high hydroxyl group functionality. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Two-steps microwave-assisted treatment on acid hydrolysis of sago pith for bioethanol production

    NASA Astrophysics Data System (ADS)

    Sunarti, T. C.; Yanti, S. D.; Ruriani, E.

    2017-05-01

    Sago is a genus of palm that can be utilized to produce fermentable sugars as substrate for bioethanol. Sago pith is a heterogeneous substrate consists of starch and fiber. Acid hydrolysis by microwave heating radiation can break down starch and fibers together in a very short time, so it is considered to be very efficient process. The use of microwave energy (as power level) and variation of heating time can produce fermentable sugar with certain characteristics. This study included the preparation and analysis of sago pith flour; process of acid hydrolysis (0.3 M and 0.5 M H2SO4) using two steps microwave heating, first with power level 30% (1, 2 and 3 min) and second with power level 70% (3 min); and ethanol production. The conventional treatment (autoclaving at 121°C for 15 min) was carried for the comparison. The highest fermentable sugar (105.7 g/l) was resulted from microwave heating with power level 30% for 2 min followed by the power level 70% for 3 min. This hydrolyzate then used as substrate for bioethanol fermentation and partially neutralized (pH 3, 4, 5) by using yeast Issatchenkia orientalis, and the highest ethanol (2.8 g/l) was produced in pH 5.

  9. Modeling and prediction of extraction profile for microwave-assisted extraction based on absorbed microwave energy.

    PubMed

    Chan, Chung-Hung; Yusoff, Rozita; Ngoh, Gek-Cheng

    2013-09-01

    A modeling technique based on absorbed microwave energy was proposed to model microwave-assisted extraction (MAE) of antioxidant compounds from cocoa (Theobroma cacao L.) leaves. By adapting suitable extraction model at the basis of microwave energy absorbed during extraction, the model can be developed to predict extraction profile of MAE at various microwave irradiation power (100-600 W) and solvent loading (100-300 ml). Verification with experimental data confirmed that the prediction was accurate in capturing the extraction profile of MAE (R-square value greater than 0.87). Besides, the predicted yields from the model showed good agreement with the experimental results with less than 10% deviation observed. Furthermore, suitable extraction times to ensure high extraction yield at various MAE conditions can be estimated based on absorbed microwave energy. The estimation is feasible as more than 85% of active compounds can be extracted when compared with the conventional extraction technique. Copyright © 2013 Elsevier Ltd. All rights reserved.

  10. A microwave field-driven transistor-like skyrmionic device with the microwave current-assisted skyrmion creation

    NASA Astrophysics Data System (ADS)

    Xia, Jing; Huang, Yangqi; Zhang, Xichao; Kang, Wang; Zheng, Chentian; Liu, Xiaoxi; Zhao, Weisheng; Zhou, Yan

    2017-10-01

    Magnetic skyrmion is a topologically protected domain-wall structure at nanoscale, which could serve as a basic building block for advanced spintronic devices. Here, we propose a microwave field-driven skyrmionic device with the transistor-like function, where the motion of a skyrmion in a voltage-gated ferromagnetic nanotrack is studied by micromagnetic simulations. It is demonstrated that the microwave field can drive the motion of a skyrmion by exciting the propagating spin waves, and the skyrmion motion can be governed by a gate voltage. We also investigate the microwave current-assisted creation of a skyrmion to facilitate the operation of the transistor-like skyrmionic device on the source terminal. It is found that the microwave current with an appropriate frequency can reduce the threshold current density required for the creation of a skyrmion from the ferromagnetic background. The proposed transistor-like skyrmionic device operated with the microwave field and current could be useful for building future skyrmion-based circuits.

  11. Accessing Stereochemically Rich Sultams via Microwave-Assisted, Continuous Flow Organic Synthesis (MACOS) Scale-out

    PubMed Central

    Organ, Michael G.; Hanson, Paul R.; Rolfe, Alan; Samarakoon, Thiwanka B.; Ullah, Farman

    2011-01-01

    The generation of stereochemically-rich benzothiaoxazepine-1,1′-dioxides for enrichment of high-throughput screening collections is reported. Utilizing a microwave-assisted, continuous flow organic synthesis platform (MACOS), scale-out of core benzothiaoxazepine-1,1′-dioxide scaffolds has been achieved on multi-gram scale using an epoxide opening/SNAr cyclization protocol. Diversification of these sultam scaffolds was attained via a microwave-assisted intermolecular SNAr reaction with a variety of amines. Overall, a facile, 2-step protocol generated a collection of benzothiaoxazepine-1,1′-dioxides possessing stereochemical complexity in rapid fashion, where all 8 stereoisomers were accessed from commercially available starting materials. PMID:22116791

  12. Stereodivergent Synthesis of 1,3-Syn-Polyol Natural Product for Stereochemical-Based Structure Activity Relationship Studies

    NASA Astrophysics Data System (ADS)

    Zheng, Jiamin

    The 1,3-syn-diol functionality is very common in many natural products. An important class containing this moiety are the 1,3-syn-polyol/pyranone natural products, which have been isolated from a variety of plant sources, and possess biological activities like plant growth inhibition as well as antifeedant, antifungal, antibacterial, and antitumor properties. The feature of this class is a 6-membered lactone where the lactoe oxygen is part of a 1,3-syn-diol motif. To pursue the 1,3-syn-polyol/pyranone natural products, an iterative hydration of polyene strategy was utilized to provide the 1,3- syn-diol functionality, and asymmetric synthetic strategies were explored to form the requisite stereochemistry. The versatility of the asymmetric approach was demonstrated in the synthesis of eupatorium pyranone and also in an ongoing project aimed at the synthesis of SIA7248. As an outgrowth of our work on the total syntheses of 1,3-syn -polyol natural products inspired a stereo-divergent synthesis of 1,3-syn-polyol natural products and their analogs for stereochemical-based structure-activity relationship (SSAR) studies. To identify the key structural factors important for the anticancer activity of the 1,3-syn-polyol/pyranones, a stereo-divergent 16-member library of pyranone/polyol congeners was designed, synthesized and tested with variations in both stereochemistry and numbers of polyol repeat units. Having access to stereochemical isomers of the biologically active natural products allowed us to design experiments that help illustrate their mechanisms of action.

  13. MALDI MS analysis of oligonucleotides: desalting by functional magnetite beads using microwave-assisted extraction.

    PubMed

    Chen, Wei-Yu; Chen, Yu-Chie

    2007-11-01

    The presence of alkali cation adductions of oligonucleotides commonly deteriorates matrix-assisted laser desorption/ionization (MALDI) mass spectra. Thus, desalting is required for oligonucleotide samples prior to MALDI MS analysis in order to prevent the mass spectra from developing poor quality. In this paper, we demonstrate a new approach to extract traces of oligonucleotides from aqueous solutions containing high concentrations of salts using microwave-assisted extraction. The C18-presenting magnetite beads, capable of absorbing microwave irradiation, are used as affinity probes for oligonucleotides with the addition of triethylammonium acetate as the counterions. This new microwave-assisted extraction approach using magnetite beads as the trapping agents and as microwave-absorbers has been demonstrated to be very effective in the selective binding of oligonucleotides from aqueous solutions. The extraction of oligonucleotides from solutions onto the C18-presenting magnetite beads takes only 30 s to enrich oligonucleotides in sufficient quantities for MALDI MS analysis. After using this desalting approach, alkali cation adductions of oligonucleotides are dramatically reduced in the MALDI mass spectra. The presence of saturated NaCl (approximately 6 M) in the oligonucleotide sample is tolerated without degrading the mass spectra. The detection limit for d(A)6 is approximately 2.8 fmol.

  14. Production of polyol oils from soybean oil by bioprocess: results of microbial screening and identification of positive cultures

    USDA-ARS?s Scientific Manuscript database

    Recently we reported methods for microbial screening and production of polyol oils from soybean oil through bioprocessing (Hou and Lin, 2013). Soy-polyol oils (oxygenated acylglycerols) are important starting materials for the manufacture of polymers such as polyurethane. Currently, they are produce...

  15. 40 CFR 721.10289 - Hexanedioic acid polymer with aliphatic polyol dihydrogen phosphate aromatic ester (generic).

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 32 2012-07-01 2012-07-01 false Hexanedioic acid polymer with... polymer with aliphatic polyol dihydrogen phosphate aromatic ester (generic). (a) Chemical substance and... acid polymer with aliphatic polyol dihydrogen phosphate aromatic ester (PMN P-11-333) is subject to...

  16. Microwave-Assisted Piloty-Robinson Synthesis of 3,4-Disubstituted Pyrroles

    PubMed Central

    Milgram, Benjamin C.; Eskildsen, Katrine; Richter, Steven M.; Scheidt, W. Robert; Scheidt, Karl A.

    2007-01-01

    The synthesis of N-acyl 3,4-disubstituted pyrroles can be accomplished directly from hydrazine and an aldehyde via a Piloty-Robinson pyrrole synthesis. The use of microwave radiation for the cyclization and pyrrole formation greatly reduces the time necessary for this process and facilitates moderate to good yields from hydrazine for the corresponding 3,4-disubstituted products (5–12). By simple hydrolysis, the free N–H pyrroles can be accessed after the Piloty-Robinson reaction and then used directly in the synthesis of octaethylporphyrin (H2OEP, 14) and octaethyltetraphenylporphyrin (H2OETPP, 15). PMID:17432915

  17. Utilization of microbial oil obtained from crude glycerol for the production of polyol and its subsequent conversion to polyurethane foams.

    PubMed

    Uprety, Bijaya K; Reddy, Jayanth Venkatarama; Dalli, Sai Swaroop; Rakshit, Sudip K

    2017-07-01

    We have demonstrated possible use of microbial oil in biopolymer industries. Microbial oil was produced from biodiesel based crude glycerol and subsequently converted into polyol. Fermentation of crude glycerol in a batch bioreactor using Rhodosporidium toruloides ATCC 10788 produced 18.69g/L of lipid at the end of 7days. The microbial oil was then chemically converted to polyol and characterized using FT-IR and 1 H NMR. For comparison, canola oil and palm oil were also converted into their respective polyols. The hydroxyl numbers of polyols from canola, palm and microbial oil were found to be 266.86, 222.32 and 230.30 (mgKOH/g of sample) respectively. All the polyols were further converted into rigid and semi-rigid polyurethanes (maintaining the molar -NCO/-OH ratio of 1.1) to examine their suitability in polymer applications. Conversion of microbial lipid to polyurethane foam also provides a new route for the production of polymers using biodiesel based crude glycerol. Copyright © 2017 Elsevier Ltd. All rights reserved.

  18. 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.

  19. Highly luminescent carbon nanodots by microwave-assisted pyrolysis.

    PubMed

    Zhai, Xinyun; Zhang, Peng; Liu, Changjun; Bai, Tao; Li, Wenchen; Dai, Liming; Liu, Wenguang

    2012-08-18

    Carbon nanodots (CDs) with a low cytotoxicity have been synthesized by one-step microwave-assisted pyrolysis of citric acid in the presence of various amine molecules. The primary amine molecules have been confirmed to serve dual roles as N-doping precursors and surface passivation agents, both of which considerably enhanced the fluorescence of the CDs.

  20. Solventless and One-Pot Synthesis of Cu(II) Phthalocyanine Complex: A Green Chemistry Experiment

    ERIC Educational Resources Information Center

    Sharma, R. K.; Sharma, Chetna; Sidhwani, Indu Tucker

    2011-01-01

    With the growing awareness of green chemistry, it is increasingly important for students to understand this concept in the context of laboratory experiments. Although microwave-assisted organic synthesis has become a common and invaluable technique in recent years, there have been few procedures published for microwave-assisted inorganic synthesis…

  1. 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...

  2. 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 ...

  3. Microwave-assisted hydrothermal synthesis of marigold-like ZnIn2S4 microspheres and their visible light photocatalytic activity

    NASA Astrophysics Data System (ADS)

    Chen, Zhixin; Li, Danzhen; Xiao, Guangcan; He, Yunhui; Xu, Yi-Jun

    2012-02-01

    Marigold-like ZnIn2S4 microspheres were synthesized by a microwave-assisted hydrothermal method with the temperature ranging from 80 to 195 °C. X-ray diffraction, X-ray photoelectron spectroscopy, nitrogen sorption analysis, UV-visible spectroscopy, scanning electron microscopy and transmission electron microscopy were used to characterize the products. It was found that the crystallographic structure and optical property of the products synthesized at different temperatures were almost the same. The degradation of methyl orange (MO) under the visible light irradiation has been used as a probe reaction to investigate the photocatalytic activity of as-prepared ZnIn2S4, which shows that the ZnIn2S4 sample synthesized at 195 °C shows the best photocatalytic activity for MO degradation. In addition, the photocatalytic activities of all the samples prepared by the microwave-assisted hydrothermal method are better than those prepared by a normal hydrothermal method, which could be attributed to the formation of more defect sites during the microwave-assisted hydrothermal treatment.

  4. 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.

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

    PubMed

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

    2011-03-14

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

  6. Electrically tunable materials for microwave applications

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

    Ahmed, Aftab, E-mail: aahmed@anl.gov; Goldthorpe, Irene A.; Khandani, Amir K.

    2015-03-15

    Microwave devices based on tunable materials are of vigorous current interest. Typical applications include phase shifters, antenna beam steering, filters, voltage controlled oscillators, matching networks, and tunable power splitters. The objective of this review is to assist in the material selection process for various applications in the microwave regime considering response time, required level of tunability, operating temperature, and loss tangent. The performance of a variety of material types are compared, including ferroelectric ceramics, polymers, and liquid crystals. Particular attention is given to ferroelectric materials as they are the most promising candidates when response time, dielectric loss, and tunability aremore » important. However, polymers and liquid crystals are emerging as potential candidates for a number of new applications, offering mechanical flexibility, lower weight, and lower tuning voltages.« less

  7. Magnetization Switching of a Co /Pt Multilayered Perpendicular Nanomagnet Assisted by a Microwave Field with Time-Varying Frequency

    NASA Astrophysics Data System (ADS)

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

    2018-05-01

    Microwave-assisted magnetization switching (MAS) is attracting attention as a method for reversing nanomagnets with a high magnetic anisotropy by using a small-amplitude magnetic field. We experimentally study MAS of a perpendicularly magnetized nanomagnet by applying a microwave magnetic field with a time-varying frequency. Because the microwave field frequency can follow the nonlinear decrease of the resonance frequency, larger magnetization excitation than that in a constant-frequency microwave field is induced, which enhances the MAS effect. The switching field decreases almost linearly as the start value of the time-varying microwave field frequency increases, and it becomes smaller than the minimum switching field in a constant-frequency microwave field. To obtain this enhancement of the MAS effect, the end value of the time-varying microwave field frequency needs to be almost the same as or lower than the critical frequency for MAS in a constant-frequency microwave field. In addition, the frequency change typically needs to take 1 ns or longer to make the rate of change slow enough for the magnetization to follow the frequency change. This switching behavior is qualitatively explained by the theory based on the macrospin model.

  8. Sugar-Related Organic Compounds in Carbonaceous Meteorites

    NASA Technical Reports Server (NTRS)

    Cooper, G.; Kimmich, N.; Belisle, W.; Sarinana, J.; Brabham, K.; Garrel, L.; DeVincenzi, Donald L. (Technical Monitor)

    2001-01-01

    Sugars and related polyols are critical components of all organisms and may have been necessary for the origin of life. To date, this class of organic compounds had not been definitively identified in meteorites. This study was undertaken to determine if polyols were present in the early Solar System as constituents of carbonaceous meteorites. Results of analyses of the Murchison and Murray meteorites indicate that formaldehyde and sugar chemistry may be responsible for the presence of a variety of polyols. We conclude that polyols were present on the early Earth through delivery by asteroids and possibly comets.

  9. DC transport in two-dimensional electron systems under strong microwave illumination

    NASA Astrophysics Data System (ADS)

    Chakraborty, Shantanu

    At low temperature (T) and weak magnetic field ( B), two dimensional electron systems (2DES) can exhibit strong 1/ B-periodic resistance oscillations on application of sufficiently strong microwave radiation. These oscillations are known as microwave induced resistance oscillations (MIROs), MIROs appearing near cyclotron resonance (CR) and its harmonics involve single photon processes and are called integer MIROs while the oscillations near CR subharmonics require multiphoton processes and are called fractional MIROs. Similar strong 1/B periodic resistance oscillations can occur due to strong dc current, and are known as Hall-field resistance oscillations (HIROs). Oscillations also occur for a combination of microwave radiation and strong dc current. In one prominent theory of MIROs, known as the displacement model, electrons make impurity-assisted transitions into higher or lower Landau levels by absorbing or emitting one or more (N) photons. In the presence of combined strong dc current and microwave radiation, electrons make transitions between Landau levels by absorbing or emitting photons followed by a space transition along the applied dc bias. The object of the dissertation is to explore how the different resistance oscillations area affected by strong microwave radiation when multiphoton processes are relevant. We used a coplanar waveguide (CPW) structure deposited on the sample, as opposed to simply placing the sample near the termination of a waveguide as is more the usual practice in this field. The CPW allows us to estimate the AC electric field (EAC) at the sample. In much of the work presented in this thesis we find that higher Nprocesses supersede the competing lower N processes as microwave power is increased. We show this in the presence and in the absence of a strong dc electric field. Finally, we look at the temperature evolution of fractional MIROs to compare the origin of the fractional MIROs with that of integer MIROs.

  10. Multiphysics numerical modeling of the continuous flow microwave-assisted transesterification process.

    PubMed

    Muley, Pranjali D; Boldor, Dorin

    2012-01-01

    Use of advanced microwave technology for biodiesel production from vegetable oil is a relatively new technology. Microwave dielectric heating increases the process efficiency and reduces reaction time. Microwave heating depends on various factors such as material properties (dielectric and thermo-physical), frequency of operation and system design. Although lab scale results are promising, it is important to study these parameters and optimize the process before scaling up. Numerical modeling approach can be applied for predicting heating and temperature profiles including at larger scale. The process can be studied for optimization without actually performing the experiments, reducing the amount of experimental work required. A basic numerical model of continuous electromagnetic heating of biodiesel precursors was developed. A finite element model was built using COMSOL Multiphysics 4.2 software by coupling the electromagnetic problem with the fluid flow and heat transfer problem. Chemical reaction was not taken into account. Material dielectric properties were obtained experimentally, while the thermal properties were obtained from the literature (all the properties were temperature dependent). The model was tested for the two different power levels 4000 W and 4700 W at a constant flow rate of 840ml/min. The electric field, electromagnetic power density flow and temperature profiles were studied. Resulting temperature profiles were validated by comparing to the temperatures obtained at specific locations from the experiment. The results obtained were in good agreement with the experimental data.

  11. Microwave-assisted hydrothermal synthesis of marigold-like ZnIn{sub 2}S{sub 4} microspheres and their visible light photocatalytic activity

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

    Chen Zhixin, E-mail: czx@fzu.edu.cn; Analysis and Test Center, Fuzhou University, Fuzhou 350002; Li Danzhen

    Marigold-like ZnIn{sub 2}S{sub 4} microspheres were synthesized by a microwave-assisted hydrothermal method with the temperature ranging from 80 to 195 Degree-Sign C. X-ray diffraction, X-ray photoelectron spectroscopy, nitrogen sorption analysis, UV-visible spectroscopy, scanning electron microscopy and transmission electron microscopy were used to characterize the products. It was found that the crystallographic structure and optical property of the products synthesized at different temperatures were almost the same. The degradation of methyl orange (MO) under the visible light irradiation has been used as a probe reaction to investigate the photocatalytic activity of as-prepared ZnIn{sub 2}S{sub 4}, which shows that the ZnIn{sub 2}S{submore » 4} sample synthesized at 195 Degree-Sign C shows the best photocatalytic activity for MO degradation. In addition, the photocatalytic activities of all the samples prepared by the microwave-assisted hydrothermal method are better than those prepared by a normal hydrothermal method, which could be attributed to the formation of more defect sites during the microwave-assisted hydrothermal treatment. - Graphical abstract: Marigold-like ZnIn{sub 2}S{sub 4} microspheres were synthesized by a fast microwave-assisted hydrothermal method at 80-195 Degree-Sign C with a very short reaction time of 10 min. The as-prepared ZnIn{sub 2}S{sub 4} sample can be used as visible light photocatalyst for degradation of organic dyes. Highlights: Black-Right-Pointing-Pointer ZnIn{sub 2}S{sub 4} microspheres were synthesized by microwave-assisted hydrothermal method. Black-Right-Pointing-Pointer The crystal structure and optical property of the products were almost the same. Black-Right-Pointing-Pointer Increment of the temperature renders high surface area due to the bubbling effect. Black-Right-Pointing-Pointer The ZnIn{sub 2}S{sub 4} synthesized at 195 Degree-Sign C shows the best visible catalytic activity for MO.« less

  12. Microwave assisted synthesis for A2E and development of LC-ESI-MS method for quantification of ocular bisretinoids in human retina.

    PubMed

    Kotnala, A; Senthilkumari, S; Halder, N; Kumar, A; Velpandian, T

    2018-01-15

    To develop a microwave assisted method for the rapid synthesis of A2E and also to develop a method to quantify N-retinylidene-N-retinylethanolamine(A2E), all-trans retinal dimer (ATRD), A2-glycerophospho ethanolamine (A2GPE), dihydropyridine phosphatidyl ethanolamine (A2DHPE) and monofuran A2E (MFA2E) in age matched retina. The development of microwave assisted synthesis of A2E, its purification and characterization for its utility in quantification in human retina. The semi-quantitative method development using LC-ESI-MS, LC-ESI-MS/MS and LC-APCI-MS/MS from pooled macula and peripheral retina for the bisretinoid analysis has been done. Maximum A2E conversion using microwave assisted process took place at 80°C for 45min with a yield of 55.01%. Highly sensitive and specific mass spectrometric method was developed using reverse phase C-18 separation with positive electrospray ionization and positive atmospheric phase chemical ionization of tandom mass spectrometry. A gradient mobile phase separation was achieved using water and methanol with 0.1% TFA. Multiple reaction monitoring acquisition for ESI and APCI was performed at ATRD m/z 551.2/522.2, A2GPE m/z 746.4/729.5, A2DHPEm/z 594.4/576.5, MFA2E m/z 608.2/591.2, A2E m/z 592.4/418.2. Method was validated using LC-ESI-SIM mode to determine selectivity, linearity, sensitivity, precision and accuracy. An attempt towards optimization of the synthetic procedure of A2E was made so as to reduce the lengthy reaction time without compromising the yield. Developed method was capable enough for the detection of low level of bisretinids in retina. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. A case for closed-loop recycling of post-consumer PET for automotive foams.

    PubMed

    Bedell, Matthew; Brown, Matthew; Kiziltas, Alper; Mielewski, Deborah; Mukerjee, Shakti; Tabor, Rick

    2018-01-01

    Striving to utilize sustainable material sources, polyester polyols made via glycolysis and esterification of recycled polyethylene terephthalate (rPET) scrap were used to synthesize flexible polyurethane (PU) foams typically found in automotive interior applications. The objective of this endeavor was to ascertain if a closed-loop model could be established with the discarded PET feedstock. In five separate formulations, up to 50% of the total polyol content (traditionally derived from petroleum-based feedstock) was replaced with the afore-mentioned sustainable recycled polyols. These foams underwent mechanical, thermal, morphological, and physical characterization testing to determine feasibility for use in an automotive interior. Young's modulus, tensile stress at maximum load, tear resistance, and compression modulus all increased by combined averages of 121%, 67%, 32%, and 150% over the control petroleum-based formulation, respectively, in foams possessing 50% rPET polyol content. Thermal stability also increased with sustainable polyol content; thermogravimetric analysis showed that 50% mass loss temperature increased by an average of 20 °C in foams containing 30% recycled polyol. Properties of density and SAG factor remained within 5% of the control petroleum-based reference foams. After comparing these findings to traditional polyols, a compelling argument can be made for the use of post-consumer automotive and industrial feedstocks in developing high-performing interior automotive PU foams. Copyright © 2017 Elsevier Ltd. All rights reserved.

  14. 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.

  15. GREENER SYNTHESIS OF HETEROCYCLIC COMPOUNDS USING MICROWAVE IRRADIATION

    EPA Science Inventory

    An introduction of our interest in the microwave-assisted greener synthesis of a variety of heterocyclic compounds will be presented. It involves microwave (MW) exposure of neat reactants (undiluted) catalyzed by the surfaces of recyclable mineral supports, such as alumina, sili...

  16. Cationic pentaheteroaryls as selective G-quadruplex ligands by solvent-free microwave-assisted synthesis.

    PubMed

    Petenzi, Michele; Verga, Daniela; Largy, Eric; Hamon, Florian; Doria, Filippo; Teulade-Fichou, Marie-Paule; Guédin, Aurore; Mergny, Jean-Louis; Mella, Mariella; Freccero, Mauro

    2012-11-05

    We report herein a solvent-free and microwaved-assisted synthesis of several water soluble acyclic pentaheteroaryls containing 1,2,4-oxadiazole moieties (1-7). Their binding interactions with DNA quadruplex structures were thoroughly investigated by FRET melting, fluorescent intercalator displacement assay (G4-FID) and CD spectroscopy. Among the G-quadruplexes considered, attention was focused on telomeric repeats together with the proto-oncogenic c-kit sequences and the c-myc oncogene promoter. Compound 1, and to a lesser extent 2 and 5, preferentially stabilise an antiparallel structure of the telomeric DNA motif, and exhibit an opposite binding behaviour to structurally related polyoxazole (TOxaPy), and do not bind duplex DNA. The efficiency and selectivity of the binding process was remarkably controlled by the structure of the solubilising moieties. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Effect of extraction method on the yield of furanocoumarins from fruits of Archangelica officinalis Hoffm.

    PubMed

    Waksmundzka-Hajnos, M; Petruczynik, A; Dragan, A; Wianowska, D; Dawidowicz, A L

    2004-01-01

    Optimal conditions for the extraction and analysis of furanocoumarins from fruits of Archangelica officinalis Hoffm. have been determined. The following extraction methods were used: exhaustive extraction in a Soxhlet apparatus, ultrasonication at 25 and 60 degrees C, microwave-assisted solvent extraction in open and closed systems, and accelerated solvent extraction (ASE). In most cases the yields of furanocoumarins were highest using the ASE method. The effects of extracting solvent, temperature and time of extraction using this method were investigated. The highest yield of furanocoumarins by ASE was obtained with methanol at 100-130 degrees C for 10 min. The extraction yields of furanocoumarins from plant material by ultrasonication at 60 degrees C and microwave-assisted solvent extraction in an open system were comparable to the extraction yields obtained in the time- and solvent-consuming exhaustive process involving the Soxhlet apparatus.

  18. Rapid and Facile Microwave-Assisted Surface Chemistry for Functionalized Microarray Slides

    PubMed Central

    Lee, Jeong Heon; Hyun, Hoon; Cross, Conor J.; Henary, Maged; Nasr, Khaled A.; Oketokoun, Rafiou; Choi, Hak Soo; Frangioni, John V.

    2011-01-01

    We describe a rapid and facile method for surface functionalization and ligand patterning of glass slides based on microwave-assisted synthesis and a microarraying robot. Our optimized reaction enables surface modification 42-times faster than conventional techniques and includes a carboxylated self-assembled monolayer, polyethylene glycol linkers of varying length, and stable amide bonds to small molecule, peptide, or protein ligands to be screened for binding to living cells. We also describe customized slide racks that permit functionalization of 100 slides at a time to produce a cost-efficient, highly reproducible batch process. Ligand spots can be positioned on the glass slides precisely using a microarraying robot, and spot size adjusted for any desired application. Using this system, we demonstrate live cell binding to a variety of ligands and optimize PEG linker length. Taken together, the technology we describe should enable high-throughput screening of disease-specific ligands that bind to living cells. PMID:23467787

  19. Microwave-assisted rapid photocatalytic degradation of malachite green in TiO2 suspensions: mechanism and pathways.

    PubMed

    Ju, Yongming; Yang, Shaogui; Ding, Youchao; Sun, Cheng; Zhang, Aiqian; Wang, Lianhong

    2008-11-06

    Microwave-assisted photocatalytic (MPC) degradation of malachite green (MG) in aqueous TiO2 suspensions was investigated. A 20 mg/L sample of MG was rapidly and completely decomposed in 3 min with the corresponding TOC removal efficiency of about 85%. To gain insight into the degradation mechanism, both GC-MS and LC-ESI-MS/MS techniques were employed to identify the major intermediates of MG degradation, including N-demethylation intermediates [(p-dimethylaminophenyl)(p-methylaminophenyl)phenylmethylium (DM-PM), (p-methylaminophenyl)(p-methylaminophenyl)phenylmethylium (MM-PM), (p-methylaminophenyl)(p-aminophenyl)phenylmethylium (M-PM)]; a decomposition compound of the conjugated structure (4-dimethylaminobenzophenone (DLBP)); products resulting from the adduct reaction of hydroxyl radical; products of benzene removal; and other open-ring intermediates such as phenol, terephthalic acid, adipic acid, benzoic acid, etc. The possible degradation mechanism of MG included five processes: the N-demethylation process, adduct products of the hydroxyl radical, the breakdown of chromophores such as destruction of the conjugated structure intermediate, removal of benzene, and an open-ring reaction. To the best of our knowledge, it is the first time the whole MG photodegradation processes have been reported.

  20. Production of polyol oils from soybean oil by bioprocess and Philippines edible medicinal wild mushrooms

    USDA-ARS?s Scientific Manuscript database

    We have been trying to develop a bioprocess for the production of polyol oils directly from soybean oil. We reported earlier the polyol products produced from soybean oil by Acinetobacter haemolyticus A01-35 (NRRL B-59985) (Hou and Lin, 2013). The objective of this study is to identify the chemical ...

  1. Study the Polyol Process of Preparing the ru Doped FePt Nanoparticles

    NASA Astrophysics Data System (ADS)

    Lee, Chih-Hao; Hsu, Jen-Ho; Su, Hui-Chia; Huang, Tzu Wen

    The structure of Ru doped FePt nanoparticles using polyol process was studied. The particle size grown is around 5 nm, and a shell structure might be formed. By selecting the time and temperature of adding the Ru precursors into solution, three different processes to synthesize the FePtRu particles were studied resulting in different growing mechanics. The possible models during the reaction process are also discussed. The phase transition temperature for the as-grown FCC FePt nanoparticle to transform into L10 FePt nanoparticle is about 823 K which is about the same as the one without doping Ru atoms. From the XAS study of each element, the possible scenario is that: although Ru atoms with the size close to the Pt, they do not totally replace the Pt sites in the FePt alloy. Instead, most of Ru formed a shell outside the FePt nanoparticles and Fe atoms are replaced.

  2. Microwave Hydrothermal Synthesis of Reduced Graphene Oxide: Effects of Microwave Power and Irradiation Time

    NASA Astrophysics Data System (ADS)

    Agusu, La; Ode Ahmad, La; Anggara, Desna; Alimin; Mitsudo, Seitaro; Fujii, Yutaka; Kikuchi, Hiromitsu

    2018-04-01

    Reduced graphene oxide has been synthesihzed by one-pot microwave assisted hydrothermal method. Effects of microwave power and irradiation time to its crystal structure and electrical conductivity were investigated. Here, graphene oxide, firstly, were synthesized by modified hummers method and subsequently mixed with Zn as a reducing agent. Then it was transferred to modified domestic microwave oven (800 watts) with glass distiller equipment for completely reduction process. Three different power levels (240, 400, 630 watts) and two cases of irradiation times (20 and 40 minutes) were treated. XRD study shows that irradiation time variation is more effective than the variation of power level. Power level of 270 watts and for 40 minutes microwave irradiation are enough for producing estimated bilayer rGO with graphene interlayer of ~0.4 nm. Bilayer graphene and water molecule (~0.3 nm) may vibrate the same manner and perhaps they are accepting the same temperature. Graphene seems to be re-arranged in unspecified way among the thermal pressure, temperature gradient and/or water surface tension between graphene and water induced by microwave, in order to achieve thermal equilibrium through out the system The electrical conductivity rGO/PVA (60/40 %w) paper are ranging from 15.6 to 43.4 mS/cm.

  3. Optimization of furfural and 5-hydroxymethylfurfural production from wheat straw by a microwave-assisted process.

    PubMed

    Yemiş, Oktay; Mazza, Giuseppe

    2012-04-01

    Optimization of acid-catalyzed conversion conditions of wheat straw into furfural, 5-hydroxymethylfurfural (HMF), glucose, and xylose was studied by response surface methodology (RSM). A central composite design (CCD) was used to determine the effects of independent variables, including reaction temperature (140-200 °C), residence time (1-41 min), pH (0.1-2.1), and liquid:solid ratio (15-195 mL/g) on furan and sugar production. The surface response analysis revealed that temperature, time and pH had a strong influence on the furfural, HMF, xylose and glucose yield, whereas liquid to solid ratio was found not to be significant. The initial pH of solution was the most important variable in acid-catalyzed conversion of wheat straw to furans. The maximum predicted furfural, HMF, xylose and glucose yields were 66%, 3.4%, 100%, and 65%, respectively. This study demonstrated that the microwave-assisted process was a very effective method for the xylose production from wheat straw by diluted acid catalysis. Crown Copyright © 2012. Published by Elsevier Ltd. All rights reserved.

  4. Production of bio-oil and biochar from soapstock via microwave-assisted co-catalytic fast pyrolysis.

    PubMed

    Dai, Leilei; Fan, Liangliang; Liu, Yuhuan; Ruan, Roger; Wang, Yunpu; Zhou, Yue; Zhao, Yunfeng; Yu, Zhenting

    2017-02-01

    In this study, production of bio-oil and biochar from soapstock via microwave-assisted co-catalytic fast pyrolysis combining the advantages of in-situ and ex-situ catalysis was performed. The effects of catalyst and pyrolysis temperature on product fractional yields and bio-oil chemical compositions were investigated. From the perspective of bio-oil yield, the optimal pyrolysis temperature was 550°C. The use of catalysts reduced the water content, and the addition of bentonite increased the bio-oil yield. Up to 84.16wt.% selectivity of hydrocarbons in the bio-oil was obtained in the co-catalytic process. In addition, the co-catalytic process can reduce the proportion of oxygenates in the bio-oil to 15.84wt.% and eliminate the N-containing compounds completely. The addition of bentonite enhanced the BET surface area of bio-char. In addition, the bio-char removal efficiency of Cd 2+ from soapstock pyrolysis in presence of bentonite was 27.4wt.% higher than without bentonite. Copyright © 2016 Elsevier Ltd. All rights reserved.

  5. Activated carbon as catalyst for microwave-assisted wet peroxide oxidation of aromatic hydrocarbons.

    PubMed

    Garcia-Costa, Alicia L; Lopez-Perela, Lucia; Xu, Xiyan; Zazo, Juan A; Rodriguez, Juan J; Casas, Jose A

    2018-05-21

    This paper addresses the removal of four aromatic hydrocarbons typically found in petrochemical wastewater: benzene (B), toluene (T), o-xylene (X), and naphthalene (N), by microwave-assisted catalytic wet peroxide oxidation (MW-CWPO) using activated carbon (AC) as catalyst. Under the studied conditions, complete pollutant elimination (B, 1.28 mM; T, 1.09 mM; X, 0.94 mM; and N, 0.78 mM) was achieved, with more than 90% TOC removal after only 15-min reaction time, working at 120 °C, pH 0  = 3, AC at 1 g L -1 , and H 2 O 2 at the stoichiometric dose. Furthermore, in the case of toluene, naphthalene, and xylene, the hydroxylation and breakdown of the ring is very rapid and toxic intermediates were not detected. The process follows two steps: (i) pollutant adsorption onto AC followed by (ii) adsorbed compounds oxidation. Thus, MW-CWPO with AC as catalyst appears a promising way for a fast and effective process for B, T, X, and N removal in aqueous phase.

  6. Optimization of preparation of activated carbon from cotton stalk by microwave assisted phosphoric acid-chemical activation.

    PubMed

    Deng, Hui; Zhang, Genlin; Xu, Xiaolin; Tao, Guanghui; Dai, Jiulei

    2010-10-15

    The preparation of activated carbon (AC) from cotton stalk was investigated in this paper. Orthogonal array experimental design method was used to optimize the preparation of AC using microwave assisted phosphoric acid. Optimized parameters were radiation power of 400 W, radiation time of 8 min, concentration of phosphoric acid of 50% by volume and impregnation time of 20 h, respectively. The surface characteristics of the AC prepared under optimized condition were examined by pore structure analysis, scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR). Pore structure analysis shows that mecropores constitute more of the porosity of the prepared AC. Compared to cotton stalk, different functionalities and morphology on the carbon surfaces were formed in the prepared process. The adsorption capacity of the AC was also investigated by removing methylene blue (MB) in aqueous solution. The equilibrium data of the adsorption was well fitted to the Langmuir isotherm. The maximum adsorption capacity of MB on the prepared AC is 245.70 mg/g. The adsorption process follows the pseudo-second-order kinetic model. 2010 Elsevier B.V. All rights reserved.

  7. Microwave synthesis of noncentrosymmetric BaTiO3 truncated nanocubes for charge storage applications.

    PubMed

    Swaminathan, V; Pramana, Stevin S; White, T J; Chen, L; Chukka, Rami; Ramanujan, R V

    2010-11-01

    Truncated nanocubes of barium titanate (BT) were synthesized using a rapid, facile microwave-assisted hydrothermal route. Stoichiometric composition of pellets of nanocube BT powders was prepared by two-stage microwave process. Characterization by powder XRD, Rietveld refinement, SEM, TEM, and dielectric and polarization measurements was performed. X-ray diffraction revealed a polymorphic transformation from cubic Pm3̅m to tetragonal P4mm after 15 min of microwave irradiation, arising from titanium displacement along the c-axis. Secondary electron images were examined for nanocube BT synthesis and annealed at different timings. Transmission electron microscopy showed a narrow particle size distribution with an average size of 70 ± 9 nm. The remanence and saturation polarization were 15.5 ± 1.6 and 19.3 ± 1.2 μC/cm(2), respectively. A charge storage density of 925 ± 47 nF/cm(2) was obtained; Pt/BT/Pt multilayer ceramic capacitor stack had an average leakage current density of 5.78 ± 0.46 × 10(-8) A/cm(2) at ±2 V. The significance of this study shows an inexpensive and facile processing platform for synthesis of high-k dielectric for charge storage applications.

  8. Using x-ray mammograms to assist in microwave breast image interpretation.

    PubMed

    Curtis, Charlotte; Frayne, Richard; Fear, Elise

    2012-01-01

    Current clinical breast imaging modalities include ultrasound, magnetic resonance (MR) imaging, and the ubiquitous X-ray mammography. Microwave imaging, which takes advantage of differing electromagnetic properties to obtain image contrast, shows potential as a complementary imaging technique. As an emerging modality, interpretation of 3D microwave images poses a significant challenge. MR images are often used to assist in this task, and X-ray mammograms are readily available. However, X-ray mammograms provide 2D images of a breast under compression, resulting in significant geometric distortion. This paper presents a method to estimate the 3D shape of the breast and locations of regions of interest from standard clinical mammograms. The technique was developed using MR images as the reference 3D shape with the future intention of using microwave images. Twelve breast shapes were estimated and compared to ground truth MR images, resulting in a skin surface estimation accurate to within an average Euclidean distance of 10 mm. The 3D locations of regions of interest were estimated to be within the same clinical area of the breast as corresponding regions seen on MR imaging. These results encourage investigation into the use of mammography as a source of information to assist with microwave image interpretation as well as validation of microwave imaging techniques.

  9. 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. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. 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.

  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. Microwave assisted synthesis of luminescent carbonaceous nanoparticles from silk fibroin for bioimaging.

    PubMed

    Gao, Hongzhi; Teng, Choon Peng; Huang, Donghong; Xu, Wanqing; Zheng, Chaohui; Chen, Yisong; Liu, Minghuan; Yang, Da-Peng; Lin, Ming; Li, Zibiao; Ye, Enyi

    2017-11-01

    Bombyx mori silk as a natural protein based biopolymer with high nitrogen content, is abundant and sustainable because of its mass product all over the world per year. In this study, we developed a facile and fast microwave-assisted synthesis of luminescent carbonaceous nanoparticles using Bombyx mori silk fibroin and silk solution as the precursors. As a result, the obtained carbonaceous nanoparticles exhibit a photoluminescence quantum yield of ~20%, high stability, low cytotoxicity, high biocompatibility. Most importantly, we successfully demonstrated bioimaging using these luminescent carbonaceous nanoparticles with excitation dependent luminescence. In addition, the microwave-assisted hydrothermal method can be extended to convert other biomass into functional nanomaterials. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Evaluation and application of microwave-assisted extraction and dispersive liquid-liquid microextraction followed by high-performance liquid chromatography for the determination of polar heterocyclic aromatic amines in hamburger patties.

    PubMed

    Aeenehvand, Saeed; Toudehrousta, Zahra; Kamankesh, Marzieh; Mashayekh, Morteza; Tavakoli, Hamid Reza; Mohammadi, Abdorreza

    2016-01-01

    This study developed an analytical method based on microwave-assisted extraction and dispersive liquid-liquid microextraction followed by high-performance liquid chromatography for the determination of three polar heterocyclic aromatic amines from hamburger patties. Effective parameters controlling the performance of the microextraction process, such as the type and volume of extraction and disperser solvents, microwave time, nature of alkaline aqueous solution, pH and salt amount, were optimized. The calibration graphs were linear in the range of 1-200 ng g(-1), with a coefficient of determination (R(2)) better than 0.9993. The relative standard deviations (RSD) for seven analyses were between 3.2% and 6.5%. The recoveries of those compounds in hamburger patties were from 90% to 105%. Detection limits were between 0.06 and 0.21 ng g(-1). A comparison of the proposed method with the existing literature demonstrates that it is a simple, rapid, highly selective and sensitive, and it gives good enrichment factors and detection limits for determining HAAs in real hamburger patties samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

  14. Optimization of microwave-assisted extraction of total extract, stevioside and rebaudioside-A from Stevia rebaudiana (Bertoni) leaves, using response surface methodology (RSM) and artificial neural network (ANN) modelling.

    PubMed

    Ameer, Kashif; Bae, Seong-Woo; Jo, Yunhee; Lee, Hyun-Gyu; Ameer, Asif; Kwon, Joong-Ho

    2017-08-15

    Stevia rebaudiana (Bertoni) consists of stevioside and rebaudioside-A (Reb-A). We compared response surface methodology (RSM) and artificial neural network (ANN) modelling for their estimation and predictive capabilities in building effective models with maximum responses. A 5-level 3-factor central composite design was used to optimize microwave-assisted extraction (MAE) to obtain maximum yield of target responses as a function of extraction time (X 1 : 1-5min), ethanol concentration, (X 2 : 0-100%) and microwave power (X 3 : 40-200W). Maximum values of the three output parameters: 7.67% total extract yield, 19.58mg/g stevioside yield, and 15.3mg/g Reb-A yield, were obtained under optimum extraction conditions of 4min X 1 , 75% X 2 , and 160W X 3 . The ANN model demonstrated higher efficiency than did the RSM model. Hence, RSM can demonstrate interaction effects of inherent MAE parameters on target responses, whereas ANN can reliably model the MAE process with better predictive and estimation capabilities. Copyright © 2017. Published by Elsevier Ltd.

  15. Solvent-Free Microwave-Assisted Extraction of Polyphenols from Olive Tree Leaves: Antioxidant and Antimicrobial Properties.

    PubMed

    Şahin, Selin; Samli, Ruya; Tan, Ayşe Seher Birteksöz; Barba, Francisco J; Chemat, Farid; Cravotto, Giancarlo; Lorenzo, José M

    2017-06-24

    Response surface methodology (RSM) and artificial neural networks (ANN) were evaluated and compared in order to decide which method was the most appropriate to predict and optimize total phenolic content (TPC) and oleuropein yields in olive tree leaf ( Olea europaea ) extracts, obtained after solvent-free microwave-assisted extraction (SFMAE). The SFMAE processing conditions were: microwave irradiation power 250-350 W, extraction time 2-3 min, and the amount of sample 5-10 g. Furthermore, the antioxidant and antimicrobial activities of the olive leaf extracts, obtained under optimal extraction conditions, were assessed by several in vitro assays. ANN had better prediction performance for TPC and oleuropein yields compared to RSM. The optimum extraction conditions to recover both TPC and oleuropein were: irradiation power 250 W, extraction time 2 min, and amount of sample 5 g, independent of the method used for prediction. Under these conditions, the maximal yield of oleuropein (0.060 ± 0.012 ppm) was obtained and the amount of TPC was 2.480 ± 0.060 ppm. Moreover, olive leaf extracts obtained under optimum SFMAE conditions showed antibacterial activity against S. aureus and S. epidermidis , with a minimum inhibitory concentration (MIC) value of 1.25 mg/mL.

  16. Focused microwave-assisted solvent extraction and HPLC determination of effective constituents in Eucommia ulmodies Oliv. (E. ulmodies).

    PubMed

    Li, Hui; Chen, Bo; Zhang, Zhaohui; Yao, Shouzhuo

    2004-06-17

    A new focused microwave-assisted solvent extraction method using water as solvent has been developed for leaching geniposidic and chlorogenic acids from Eucommia ulmodies Oliv. The extraction procedures were optimized using a two indexes orthogonal experimental design and graphical analysis, by varying irradiation time, solvent volume, solvent composition and microwave power. The optimum extraction conditions were obtained: for geniposidic acid, 50% micorwave power, 40s irradiation, and 80% (v/v) aqueous methanol as extraction solvent (20mlg(-1) sample); and for chlorogenic acid, 50% micorwave power, 30s irradiation, and 20% aqueous methanol (20mlg(-1) sample). The composition of the extraction solvent was optimized and can be directly used as the mobile phase in the HPLC separation. Quantification of organic acids was done by HPLC at room temperature using Spherigel C(18) chromatographic column (250 mm x4.6 mm , i.d. 5mum), the methanol:water:acetic acid (20:80:1.0, v/v) mobile phase and UV detection at 240nm. The R.S.D. of the extraction process for geniposidic and chlorogenic acid were 3.8 and 4.1%, respectively.

  17. 40 CFR Table 4 to Subpart Ppp of... - Known Organic HAP From Polyether Polyol Products

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 12 2014-07-01 2014-07-01 false Known Organic HAP From Polyether Polyol Products 4 Table 4 to Subpart PPP of Part 63 Protection of Environment ENVIRONMENTAL PROTECTION... Polyether Polyols Production Pt. 63, Subpt. PPP, Table 4 Table 4 to Subpart PPP of Part 63—Known Organic HAP...

  18. 40 CFR Table 4 to Subpart Ppp of... - Known Organic HAP From Polyether Polyol Products

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 12 2013-07-01 2013-07-01 false Known Organic HAP From Polyether Polyol Products 4 Table 4 to Subpart PPP of Part 63 Protection of Environment ENVIRONMENTAL PROTECTION... Polyether Polyols Production Pt. 63, Subpt. PPP, Table 4 Table 4 to Subpart PPP of Part 63—Known Organic HAP...

  19. 40 CFR Table 4 to Subpart Ppp of... - Known Organic HAP From Polyether Polyol Products

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 12 2012-07-01 2011-07-01 true Known Organic HAP From Polyether Polyol Products 4 Table 4 to Subpart PPP of Part 63 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY... Pt. 63, Subpt. PPP, Table 4 Table 4 to Subpart PPP of Part 63—Known Organic HAP From Polyether Polyol...

  20. Nanocrystalline hydroxyapatite ceramics prepared by hydrolysis in polyol medium

    NASA Astrophysics Data System (ADS)

    Mechay, Abderrahmen; Feki, Hafed E. L.; Schoenstein, Fréderic; Jouini, Noureddine

    2012-07-01

    This Letter describes a new approach for the synthesis of hydroxyapatite nanoparticles, which involves precipitation and hydrolysis reactions conducted in polyol medium. In fact, ammonium-hydrogen phosphate and calcium nitrate were dissolved in polyol, and then heated at the boiling point of the polyol (ethane1, 2diol or propane1, 2diol). Besides, the phase and composition of the polycrystalline were studied by TGA/DTA, FT-IR, TEM and XRD techniques. The nanoparticles thus obtained present interesting morphological characters varying from needle to very thin platelet. Moreover, the hydroxyapatite prepared in ployol shows higher cristallinity in comparison with that obtained by other 'chimie douce' methods.

  1. Effects of the Acrylic Polyol Structure and the Selectivity of the Employed Catalyst on the Performance of Two-Component Aqueous Polyurethane Coatings

    PubMed Central

    Cakic, Suzana; Lacnjevac, Caslav; Stamenkovic, Jakov; Ristic, Nikola; Takic, Ljiljana; Barac, Miroljub; Gligoric, Miladin

    2007-01-01

    Two kinds of aqueous acrylic polyols (single step and multi step synthesis type) have been investigated for their performance in the two-component aqueous polyurethane application, by using more selective catalysts. The aliphatic polyfunctional isocyanates based on hexamethylen diisocyanates have been employed as suitable hardeners. The complex of zirconium, commercially known as K-KAT®XC-6212, and manganese (III) complexes with mixed ligands based on the derivative of maleic acid have been used as catalysts in this study. Both of the aqueous polyols give good results, in terms of application and hardness, when elevated temperatures and more selective catalysts are applied. A more selective catalyst promotes the reaction between the isocyanate and polyol component. This increases the percentage of urethane bonds and the degree of hardness in the films formed from the two components of aqueous polyurethane lacquers. The polyol based on the single step synthesis route is favourable concerning potlife and hardness. The obtained results show that the performance of the two-component aqueous polyurethane coatings depends on the polymer structure of the polyols as well as on the selectivity of the employed catalyst.

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

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

    Preda, Silviu, E-mail: predas01@yahoo.co.uk; Rutar, Melita; Jožef Stefan International Postgraduate School, Jamova cesta 39, SI-1000 Ljubljana

    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 electronmore » 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.« less

  3. 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.

  4. Characterization and antibacterial properties of stable silver substituted hydroxyapatite nanoparticles synthesized through surfactant assisted microwave process

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

    Iqbal, Nida; Abdul Kadir, Mohammed Rafiq, E-mail: rafiq@biomedical.utm.my; Nik Malek, Nik Ahmad Nazim

    Highlights: • Stable nano sized silver substitute hydroxyapatite is prepared under surfactant assisted microwave process at 600 W power for 7 min. • The nanoparticles are in the size range of 58–72 nm and exert uniform elongated spheroid morphology. • Increase in silver concentration resulted in better dielectric properties. • Good antibacterial activity and silver release. - Abstract: The present study reports a relatively simple method for the synthesis of stable silver substituted hydroxyapatite nanoparticles with controlled morphology and particle size. In order to achieve this, CTAB is included as a surfactant in the microwave refluxing process (600 W formore » 7 min). The nanoparticles produced with different silver ion concentrations (0.05, 0.1 and 0.2 wt%) were characterized using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, field emission scanning electron microscope (FESEM), energy dispersive X-ray (EDX) and Brunauer–Emmett–Teller (BET) analysis. XRD and FTIR analyses reveal that the Ag-HA nanoparticles were phase pure at 1000 °C. FESEM images showed that the produced nanoparticles are in the size range of 58–72 nm and exert uniform elongated spheroid morphology. The dielectric properties suggest that the increase in dielectric constant (ε′) and dissipation factor (D) values with increasing Ag concentrations. Antibacterial performance of the Ag-HA samples elucidated using disk diffusion technique (DDT) and minimum inhibitory concentration (MIC) demonstrates anti-bacterial activity against Staphylococcus aureus, Bacillus subtilis, Pseudomonas aeruginosa and Escherichia coli. This effect was dose dependent and was more pronounced against Gram-negative bacteria than Gram-positive organisms.« less

  5. A study on experimental characteristic of microwave-assisted pyrolysis of microalgae.

    PubMed

    Hu, Zhifeng; Ma, Xiaoqian; Chen, Chunxiang

    2012-03-01

    The microwave-assisted pyrolysis of Chlorella vulgaris was carried out under different microwave power levels, catalysts and contents of activated carbon and solid residue. The products, pyrolysis temperature and temperature rising rate were analyzed in order to obtain the optimal conditions. The results indicated that the higher the microwave power level was, the higher the maximum temperature rising rate and pyrolysis temperature were. The maximum bio-oil yield (35.83 wt.%) and gas yield (52.37%) were achieved under the microwave power of 1500 W and 2250 W, respectively. And 2250 W was the optimal power to obtain bio-fuel product. High microwave power level and catalyst can enhance the production of gas. Catalysts can promote the pyrolysis of C. vulgaris, and activated carbon was the best among the tested catalysts followed by the solid residue. The optimal content of activated carbon is 5% with the maximum bio-fuel yield of 87.47%. Copyright © 2011 Elsevier Ltd. All rights reserved.

  6. Silicon carbide passive heating elements in microwave-assisted organic synthesis.

    PubMed

    Kremsner, Jennifer M; Kappe, C Oliver

    2006-06-09

    Microwave-assisted organic synthesis in nonpolar solvents is investigated utilizing cylinders of sintered silicon carbide (SiC)--a chemically inert and strongly microwave absorbing material--as passive heating elements (PHEs). These heating inserts absorb microwave energy and subsequently transfer the generated thermal energy via conduction phenomena to the reaction mixture. The use of passive heating elements allows otherwise microwave transparent or poorly absorbing solvents such as hexane, carbon tetrachloride, tetrahydrofuran, dioxane, or toluene to be effectively heated to temperatures far above their boiling points (200-250 degrees C) under sealed vessel microwave conditions. This opens up the possibility to perform microwave synthesis in unpolar solvent environments as demonstrated successfully for several organic transformations, such as Claisen rearrangements, Diels-Alder reactions, Michael additions, N-alkylations, and Dimroth rearrangements. This noninvasive technique is a particularly valuable tool in cases where other options to increase the microwave absorbance of the reaction medium, such as the addition of ionic liquids as heating aids, are not feasible due to an incompatibility of the ionic liquid with a particular substrate. The SiC heating elements are thermally and chemically resistant to 1500 degrees C and compatible with any solvent or reagent.

  7. 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.

  8. Parallel and automated library synthesis of 2-long alkyl chain benzoazoles and azole[4,5-b]pyridines under microwave irradiation.

    PubMed

    Martínez-Palou, Rafael; Zepeda, L Gerardo; Höpfl, Herbert; Montoya, Ascensión; Guzmán-Lucero, Diego J; Guzmán, Javier

    2005-01-01

    A versatile route to 40-membered library of 2-long alkyl chain substituted benzoazoles (1 and 2) and azole[4,5-b]pyridines (3 and 4) via microwave-assisted combinatorial synthesis was developed. The reactions were carried out in both monomode and multimode microwave oven. With the latter, all reactions were performed in high-throughput experimental settings consisting of an 8 x 5 combinatorial library designed to synthesize 40 compounds. Each step, from the addition of reagents to the recovery of final products, was automated. The microwave-assisted N-long chain alkylation reactions of 2-alkyl-1H-benzimidazole (1) and 2-alkyl-1H-benzimidazole[4,5-b] pyridines (3) were also studied.

  9. 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.

  10. Microwave-assisted Derivatization of Fatty Acids for Its Measurement in Milk Using High-Performance Liquid Chromatography.

    PubMed

    Shrestha, Rojeet; Miura, Yusuke; Hirano, Ken-Ichi; Chen, Zhen; Okabe, Hiroaki; Chiba, Hitoshi; Hui, Shu-Ping

    2018-01-01

    Fatty acid (FA) profiling of milk has important applications in human health and nutrition. Conventional methods for the saponification and derivatization of FA are time-consuming and laborious. We aimed to develop a simple, rapid, and economical method for the determination of FA in milk. We applied a beneficial approach of microwave-assisted saponification (MAS) of milk fats and microwave-assisted derivatization (MAD) of FA to its hydrazides, integrated with HPLC-based analysis. The optimal conditions for MAS and MAD were determined. Microwave irradiation significantly reduced the sample preparation time from 80 min in the conventional method to less than 3 min. We used three internal standards for the measurement of short-, medium- and long-chain FA. The proposed method showed satisfactory analytical sensitivity, recovery and reproducibility. There was a significant correlation in the milk FA concentrations between the proposed and conventional methods. Being quick, economic, and convenient, the proposed method for the milk FA measurement can be substitute for the convention method.

  11. Solvothermal synthesis of selenium nano and microspheres deposited on silicon surface by microwave-assisted method

    NASA Astrophysics Data System (ADS)

    Ahmad, Muthanna

    2016-10-01

    This work describes a new application of the solvothermal method, based on the microwave heating, for the synthesis of nano and microparticles of selenium. The reaction of selenium with hydrofluoric acid on the silicon surface is induced by microwave irradiation under high pressure and temperature of 60 bar and 160 °C, respectively. This method allows the deposition of spherical-like particles on the in situ etched silicon surface. The size of deposited selenium spheres scales from tens of nanometers up to tens of micrometers. The morphology and composition of the deposited selenium were analyzed by various analytical techniques. The formation dynamic of spherical structure is explained on the base of reduction of selenium species by hydrogen inside gas bubbles which are generated on the silicon surface by the etching process.

  12. 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…

  13. Fast microwave-assisted extraction of rotenone for its quantification in seeds of yam bean (Pachyrhizus sp.).

    PubMed

    Lautié, Emmanuelle; Rasse, Catherine; Rozet, Eric; Mourgues, Claire; Vanhelleputte, Jean-Paul; Quetin-Leclercq, Joëlle

    2013-02-01

    The aim of this study was to find if fast microwave-assisted extraction could be an alternative to the conventional Soxhlet extraction for the quantification of rotenone in yam bean seeds by SPE and HPLC-UV. For this purpose, an experimental design was used to determine the optimal conditions of the microwave extraction. Then the values of the quantification on three accessions from two different species of yam bean seeds were compared using the two different kinds of extraction. A microwave extraction of 11 min at 55°C using methanol/dichloromethane (50:50) allowed rotenone extraction either equivalently or more efficiently than the 8-h-Soxhlet extraction method and was less sensitive to moisture content. The selectivity, precision, trueness, accuracy, and limit of quantification of the method with microwave extraction were also demonstrated. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. 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. Copyright © 2014 Elsevier B.V. All rights reserved.

  15. Methane Synthesis from Automotive Paint Sludge via Microwave Assisted Pyrolysis

    NASA Astrophysics Data System (ADS)

    Rosli, N. L.; Rahman, N. Abd; Kadri, A.

    2018-05-01

    Methane gas, which has one atom of carbon and four atoms of hydrogen, is a valuable energy resource, which can be used in the energy sector. The purpose of this research work is to identify methane synthesis from Automotive Paint Sludge (APS) using microwave assisted pyrolysis. APS is known as a hazardous waste since it contains various chemicals that categorized as heavy metals and toxic substances. A modified conventional kitchen microwave was used to pyrolise the APS. The microwave was set with the power level of 600 W and 50 minutes radiation time. Through the experiment, pyrogas was collected into tedlar bag and was analysed using Gas Chromatography with Flame Ionization Detector (GC-FID). Results from the GC-FID were shown that the retention time of 3.3583, 3.2733, and 3.2267 min are proved to be methane gas. The results obtained are resembled with the results from the literature. This indicates methane gas was presented in the pyrogas of pyrolysis of APS and there is a possibility of producing methane gas. The research study suggests that it is possible to synthesize methane gas from the APS via microwave assisted pyrolysis, and in the meantime reduce the volume of APS in the landfill.

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

    PubMed

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

    2012-06-30

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

  17. 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. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. GREENER AND CONTROLLED SYNTHESIS OF NOBLE NANOSTRUCTURES IN AQUEOUS MEDIA USING MICROWAVE IRRADIATION

    EPA Science Inventory

    Microwave-assisted spontaneous reduction of gold salts is described using sugar solutions such as alpha-D-glucose, sucrose and maltose, etc. The expeditious reactions are conducted in aqueous media using microwave irradiation wherein the reduction occurs within 30 to 60 seconds ...

  19. Carbohydrate conjugation through microwave-assisted functionalization of single-walled carbon nanotubes using perfluorophenyl azides.

    PubMed

    Kong, Na; Shimpi, Manishkumar R; Ramström, Olof; Yan, Mingdi

    2015-03-20

    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. Copyright © 2014 Elsevier Ltd. All rights reserved.

  20. Micro-PIXE and micro-RBS characterization of micropores in porous silicon prepared using microwave-assisted hydrofluoric acid etching.

    PubMed

    Ahmad, Muthanna; Grime, Geoffrey W

    2013-04-01

    Porous silicon (PS) has been prepared using a microwave-assisted hydrofluoric acid (HF) etching method from a silicon wafer pre-implanted with 5 MeV Cu ions. The use of microbeam proton-induced X-ray emission (micro-PIXE) and microbeam Rutherford backscattering techniques reveals for the first time the capability of these techniques for studying the formation of micropores. The porous structures observed from micro-PIXE imaging results are compared to scanning electron microscope images. It was observed that the implanted copper accumulates in the same location as the pores and that at high implanted dose the pores form large-scale patterns of lines and concentric circles. This is the first work demonstrating the use of microwave-assisted HF etching in the formation of PS.

  1. Studies of the Kaneda Reaction in the Synthesis of Oocydin A/Haterumalide NA and Polyurethanes from Renewable Resources: Polyols from Soybean Oil

    NASA Astrophysics Data System (ADS)

    Schmit, Amanda L.

    This thesis is broken down into two main projects. First, studies of the Kaneda reaction in the synthesis of oocydin A/haterumalide NA and, second, polyurethanes from renewable resources: polyols from soybean oil. In Chapter I, the stereoselectivity of the Kaneda reaction was studied. The driving interest stemmed from the hypothesis that one epimer of an acyclic precursor could give the desired bicyclic core of oocydin A/haterumalide NA. In Chapter II, the work toward new polyols from soybean oil is discussed. Renewable content in polyurethanes on the market is still low because of economics and performance. Our ideas for new polyol systems are presented.

  2. Modeling of electron behaviors under microwave electric field in methane and air pre-mixture gas plasma assisted combustion

    NASA Astrophysics Data System (ADS)

    Akashi, Haruaki; Sasaki, K.; Yoshinaga, T.

    2011-10-01

    Recently, plasma-assisted combustion has been focused on for achieving more efficient combustion way of fossil fuels, reducing pollutants and so on. Shinohara et al has reported that the flame length of methane and air premixed burner shortened by irradiating microwave power without increase of gas temperature. This suggests that electrons heated by microwave electric field assist the combustion. They also measured emission from 2nd Positive Band System (2nd PBS) of nitrogen during the irradiation. To clarify this mechanism, electron behavior under microwave power should be examined. To obtain electron transport parameters, electron Monte Carlo simulations in methane and air mixture gas have been done. A simple model has been developed to simulate inside the flame. To make this model simple, some assumptions are made. The electrons diffuse from the combustion plasma region. And the electrons quickly reach their equilibrium state. And it is found that the simulated emission from 2nd PBS agrees with the experimental result. Recently, plasma-assisted combustion has been focused on for achieving more efficient combustion way of fossil fuels, reducing pollutants and so on. Shinohara et al has reported that the flame length of methane and air premixed burner shortened by irradiating microwave power without increase of gas temperature. This suggests that electrons heated by microwave electric field assist the combustion. They also measured emission from 2nd Positive Band System (2nd PBS) of nitrogen during the irradiation. To clarify this mechanism, electron behavior under microwave power should be examined. To obtain electron transport parameters, electron Monte Carlo simulations in methane and air mixture gas have been done. A simple model has been developed to simulate inside the flame. To make this model simple, some assumptions are made. The electrons diffuse from the combustion plasma region. And the electrons quickly reach their equilibrium state. And it is found that the simulated emission from 2nd PBS agrees with the experimental result. This work was supported by KAKENHI (22340170).

  3. Preparation and properties of high storage stability polyester polyol dispersion for two-component waterborne polyurethane coating

    NASA Astrophysics Data System (ADS)

    Hao, H.; Hu, J. Q.; Wang, F.; Tu, W. P.

    2017-01-01

    A new type of polyester polyol dispersion with good storage stability was prepared based on a hydrophilic monomer 5-sodium sulfodimethyl isophthalate (5-SIPM), and frequently-used monomers such as neopentyl glycol (NPG), dimethyl terephthalate (DMT), dimethyl phthalate (DMP) and trimethylolpropane (TMP) by the transpolycondensation and polycondensation method. The polyester polyol dispersion was characterized by FTIR and GPC. The proper content of these monomers were determined by the performance of polyester dispersion: the content of TMP was 15wt%, the content of NPG was 7.5wt% and the hydrophilic monomer 5-SIPM content was 5wt%. Two-component waterborne polyurethane (2K-WPU) coatings were prepared by Bayhydur® XP2487/1 and polyester polyol dispersions, which were stored before and after at 40 ° for 6 weeks, the prepared films have no differences in drying time, adhesion, pencil hardness, gloss and chemical resistance, the result also reveals that the polyester polyol dispersion have excellent storage stability resistance.

  4. Structures and Properties of Polyurethanes. Part II,

    DTIC Science & Technology

    1979-03-23

    effect was observed for polymethyl methacrylate (222, 2721. The polyol, which contain fluorine , decrease adhesion, in spite DOC = 79011112 PAGE S4% of...small differences in the hardness of films on the basis of the fluorine -bearing polyol and generally accepted polyol. Is investigated the etfect ot...polyurethane, to rigid surface. DOC 79011112 P A * S The effect of the solvent, utilized for obtaining the varnish , on adhesion is investigated in

  5. Genetic engineering of Synechocystis PCC6803 for the photoautotrophic production of the sweetener erythritol.

    PubMed

    van der Woude, Aniek D; Perez Gallego, Ruth; Vreugdenhil, Angie; Puthan Veetil, Vinod; Chroumpi, Tania; Hellingwerf, Klaas J

    2016-04-08

    Erythritol is a polyol that is used in the food and beverage industry. Due to its non-caloric and non-cariogenic properties, the popularity of this sweetener is increasing. Large scale production of erythritol is currently based on conversion of glucose by selected fungi. In this study, we describe a biotechnological process to produce erythritol from light and CO2, using engineered Synechocystis sp. PCC6803. By functionally expressing codon-optimized genes encoding the erythrose-4-phosphate phosphatase TM1254 and the erythrose reductase Gcy1p, or GLD1, this cyanobacterium can directly convert the Calvin cycle intermediate erythrose-4-phosphate into erythritol via a two-step process and release the polyol sugar in the extracellular medium. Further modifications targeted enzyme expression and pathway intermediates. After several optimization steps, the best strain, SEP024, produced up to 2.1 mM (256 mg/l) erythritol, excreted in the medium.

  6. Leaf-Cutter Ant Fungus Gardens Are Biphasic Mixed Microbial Bioreactors That Convert Plant Biomass to Polyols with Biotechnological Applications

    PubMed Central

    Somera, Alexandre F.; Lima, Adriel M.; dos Santos-Neto, Álvaro J.; Lanças, Fernando M.

    2015-01-01

    Leaf-cutter ants use plant matter to culture the obligate mutualistic basidiomycete Leucoagaricus gongylophorus. This fungus mediates ant nutrition on plant resources. Furthermore, other microbes living in the fungus garden might also contribute to plant digestion. The fungus garden comprises a young sector with recently incorporated leaf fragments and an old sector with partially digested plant matter. Here, we show that the young and old sectors of the grass-cutter Atta bisphaerica fungus garden operate as a biphasic solid-state mixed fermenting system. An initial plant digestion phase occurred in the young sector in the fungus garden periphery, with prevailing hemicellulose and starch degradation into arabinose, mannose, xylose, and glucose. These products support fast microbial growth but were mostly converted into four polyols. Three polyols, mannitol, arabitol, and inositol, were secreted by L. gongylophorus, and a fourth polyol, sorbitol, was likely secreted by another, unidentified, microbe. A second plant digestion phase occurred in the old sector, located in the fungus garden core, comprising stocks of microbial biomass growing slowly on monosaccharides and polyols. This biphasic operation was efficient in mediating symbiotic nutrition on plant matter: the microbes, accounting for 4% of the fungus garden biomass, converted plant matter biomass into monosaccharides and polyols, which were completely consumed by the resident ants and microbes. However, when consumption was inhibited through laboratory manipulation, most of the plant polysaccharides were degraded, products rapidly accumulated, and yields could be preferentially switched between polyols and monosaccharides. This feature might be useful in biotechnology. PMID:25911490

  7. Leaf-cutter ant fungus gardens are biphasic mixed microbial bioreactors that convert plant biomass to polyols with biotechnological applications.

    PubMed

    Somera, Alexandre F; Lima, Adriel M; Dos Santos-Neto, Álvaro J; Lanças, Fernando M; Bacci, Maurício

    2015-07-01

    Leaf-cutter ants use plant matter to culture the obligate mutualistic basidiomycete Leucoagaricus gongylophorus. This fungus mediates ant nutrition on plant resources. Furthermore, other microbes living in the fungus garden might also contribute to plant digestion. The fungus garden comprises a young sector with recently incorporated leaf fragments and an old sector with partially digested plant matter. Here, we show that the young and old sectors of the grass-cutter Atta bisphaerica fungus garden operate as a biphasic solid-state mixed fermenting system. An initial plant digestion phase occurred in the young sector in the fungus garden periphery, with prevailing hemicellulose and starch degradation into arabinose, mannose, xylose, and glucose. These products support fast microbial growth but were mostly converted into four polyols. Three polyols, mannitol, arabitol, and inositol, were secreted by L. gongylophorus, and a fourth polyol, sorbitol, was likely secreted by another, unidentified, microbe. A second plant digestion phase occurred in the old sector, located in the fungus garden core, comprising stocks of microbial biomass growing slowly on monosaccharides and polyols. This biphasic operation was efficient in mediating symbiotic nutrition on plant matter: the microbes, accounting for 4% of the fungus garden biomass, converted plant matter biomass into monosaccharides and polyols, which were completely consumed by the resident ants and microbes. However, when consumption was inhibited through laboratory manipulation, most of the plant polysaccharides were degraded, products rapidly accumulated, and yields could be preferentially switched between polyols and monosaccharides. This feature might be useful in biotechnology. Copyright © 2015, American Society for Microbiology. All Rights Reserved.

  8. Microwave-assisted domino and multicomponent reactions with cyclic acylketenes: expeditious syntheses of oxazinones and oxazindiones.

    PubMed

    Presset, Marc; Coquerel, Yoann; Rodriguez, Jean

    2009-12-17

    The microwave-assisted Wolff rearrangement of cyclic 2-diazo-1,3-diketones in the presence of aldehydes and primary amines provides a straightforward access to functionalized bi- and pentacyclic oxazinones following an unprecedented three-component domino reaction. Alternatively, in the presence of acyl azides, an efficient Curtius/Wolff/hetero-Diels-Alder sequence allows the direct synthesis of oxazindiones.

  9. 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…

  10. Optimization of the microwave-assisted enzymatic extraction of Rosa roxburghii Tratt. polysaccharides using response surface methodology and its antioxidant and α-d-glucosidase inhibitory activity.

    PubMed

    Wang, Huizhu; Li, Yan; Ren, Zhihui; Cong, Zhongcheng; Chen, Mengjie; Shi, Lin; Han, Xu; Pei, Jin

    2018-06-01

    An extraction assay applying microwave-assisted enzymatic treatment for polysaccharides in Rosa roxburghii was developed using response surface methodology. The process parameters were optimized using Plackett-Burman (PB) design and central composite design to enhance the Rosa roxburghii polysaccharide extraction yield. Specific conditions (microwave power, 575W; microwave time, 18min; liquid-to-material ratio, 13.5:1mL/g; and enzyme dose, 6.5g/mL) generated an experimental yield of 36.21±0.62%, which closely agreed with the predicted value of 35.75%. Purification with a DEAE-52 cellulose column generated two fractions, PR-1 (from 6.2×10 3 to 7.4KDa) and PR-2 (from 559.8 to 106.6KDa). Subsequently, the antioxidant activity and α-d-glucosidase inhibitory activity of the two polysaccharide fractions were assessed; PR-1 exhibited stronger antioxidant activity and α-d-glucosidase inhibitory activity than PR-2. Finally, the monosaccharide composition of PR-1 was determined by HPLC using a 1-phenyl-3-methyl-5-pyrazolone precolumn derivatization method. The result showed that PR-1 contained mannose, ribose, rhamnose, glucosamine hydrochloride, glucuronic acid, galacturonic acid, glucose, galactose, arabinose and fucose with molar percentages of 2.1%, 0.54%, 2.1%, 0.26%, 1.5%, 22.7%, 24.0%, 26.4%, 19.6% and 0.89%, respectively. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. 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. Copyright © 2011 Elsevier Ltd. All rights reserved.

  12. Simple Microwave-Assisted Synthesis of Amphiphilic Carbon Quantum Dots from A3/B2 Polyamidation Monomer Set.

    PubMed

    Choi, Yujin; Jo, Seongho; Chae, Ari; Kim, Young Kwang; Park, Jeong Eun; Lim, Donggun; Park, Sung Young; In, Insik

    2017-08-23

    Highly fluorescent and amphiphilic carbon quantum dots (CQDs) were prepared by microwave-assisted pyrolysis of citric acid and 4,7,10-trioxa-1,13-tridecanediamine (TTDDA), which functioned as an A 3 and B 2 polyamidation type monomer set. Gram quantities of fluorescent CQDs were easily obtained within 5 min of microwave heating using a household microwave oven. Because of the dual role of TTDDA, both as a constituting monomer and as a surface passivation agent, TTDDA-based CQDs showed a high fluorescence quantum yield of 29% and amphiphilic solubility in various polar and nonpolar solvents. These properties enable the wide application of TTDDA-based CQDs as nontoxic bioimaging agents, nanofillers for polymer composites, and down-converting layers for enhancing the efficiency of Si solar cells.

  13. Microwave Energy Increases Fatty Acid Methyl Ester Yield in Human Whole Blood Due to Increased Sphingomyelin Transesterification.

    PubMed

    Metherel, Adam H; Aristizabal Henao, Juan J; Ciobanu, Flaviu; Taha, Ameer Y; Stark, Ken D

    2015-09-01

    Dried blood spots (DBS) by fingertip prick collection for fatty acid profiling are becoming increasingly popular due to ease of collection, minimal invasiveness and its amenability to high-throughput analyses. Herein, we assess a microwave-assisted direct transesterification method for the production of fatty acid methyl esters (FAME) from DBS. Technical replicates of human whole blood were collected and 25-μL aliquots were applied to chromatography strips prior to analysis by a standard 3-h transesterification method or microwave-assisted direct transesterification method under various power (variable vs constant), time (1-5 min) and reagent (1-10% H2SO4 in methanol) conditions. In addition, a standard method was compared to a 5-min, 30-W power microwave in 1% H2SO4 method for FAME yield from whole blood sphingomyelin, and sphingomyelin standards alone and spiked in whole blood. Microwave-assisted direct transesterification yielded no significant differences in both quantitative (nmol/100 µL) and qualitative (mol%) fatty acid assessments after as little as 1.5- and 1-min reaction times, respectively, using the variable power method and 5% H2SO4 in methanol. However, 30-W power for 5 min increased total FAME yield of the technical replicates by 14%. This increase appears largely due to higher sphingomyelin-derived FAME yield of up to 109 and 399% compared to the standard method when determined from whole blood or pure standards, respectively. In conclusion, microwave-assisted direct transesterification of DBS achieved in as little as 1-min, and 5-min reaction times increase total fatty acids primarily by significantly improving sphingomyelin-derived fatty acid yield.

  14. Design of experiment approach for the process optimisation of microwave assisted extraction of lupeol from Ficus racemosa leaves using response surface methodology.

    PubMed

    Das, Anup Kumar; Mandal, Vivekananda; Mandal, Subhash C

    2013-01-01

    Triterpenoids are a group of important phytocomponents from Ficus racemosa (syn. Ficus glomerata Roxb.) that are known to possess diverse pharmacological activities and which have prompted the development of various extraction techniques and strategies for its better utilisation. To develop an effective, rapid and ecofriendly microwave-assisted extraction (MAE) strategy to optimise the extraction of a potent bioactive triterpenoid compound, lupeol, from young leaves of Ficus racemosa using response surface methodology (RSM) for industrial scale-up. Initially a Plackett-Burman design matrix was applied to identify the most significant extraction variables amongst microwave power, irradiation time, particle size, solvent:sample ratio loading, varying solvent strength and pre-leaching time on lupeol extraction. Among the six variables tested, microwave power, irradiation time and solvent-sample/loading ratio were found to have a significant effect (P < 0.05) on lupeol extraction and were fitted to a Box-Behnken-design-generated quadratic polynomial equation to predict optimal extraction conditions as well as to locate operability regions with maximum yield. The optimal conditions were microwave power of 65.67% of 700 W, extraction time of 4.27 min and solvent-sample ratio loading of 21.33 mL/g. Confirmation trials under the optimal conditions gave an experimental yield (18.52 µg/g of dry leaves) close to the RSM predicted value of 18.71 µg/g. Under the optimal conditions the mathematical model was found to be well fitted with the experimental data. The MAE was found to be a more rapid, convenient and appropriate extraction method, with a higher yield and lower solvent consumption when compared with conventional extraction techniques. Copyright © 2012 John Wiley & Sons, Ltd.

  15. New microwave-integrated Soxhlet extraction. An advantageous tool for the extraction of lipids from food products.

    PubMed

    Virot, Matthieu; Tomao, Valérie; Colnagui, Giulio; Visinoni, Franco; Chemat, Farid

    2007-12-07

    A new process of Soxhlet extraction assisted by microwave was designed and developed. The process is performed in four steps, which ensures complete, rapid and accurate extraction of the samples. A second-order central composite design (CCD) has been used to investigate the performance of the new device. The results provided by analysis of variance and Pareto chart, indicated that the extraction time was the most important factor followed by the leaching time. The response surface methodology allowed us to determine optimal conditions for olive oil extraction: 13 min of extraction time, 17 min of leaching time, and 720 W of irradiation power. The proposed process is suitable for lipids determination from food. Microwave-integrated Soxhlet (MIS) extraction has been compared with a conventional technique, Soxhlet extraction, for the extraction of oil from olives (Aglandau, Vaucluse, France). The oils extracted by MIS for 32 min were quantitatively (yield) and qualitatively (fatty acid composition) similar to those obtained by conventional Soxhlet extraction for 8 h. MIS is a green technology and appears as a good alternative for the extraction of fat and oils from food products.

  16. Microwave-Assisted Drying for the Conservation of Honeybee Pollen.

    PubMed

    Canale, Angelo; Benelli, Giovanni; Castagna, Antonella; Sgherri, Cristina; Poli, Piera; Serra, Andrea; Mele, Marcello; Ranieri, Annamaria; Signorini, Francesca; Bientinesi, Matteo; Nicolella, Cristiano

    2016-05-12

    Bee pollen is becoming an important product thanks to its nutritional properties, including a high content of bioactive compounds such as essential amino acids, antioxidants, and vitamins. Fresh bee pollen has a high water content (15%-30% wt %), thus it is a good substrate for microorganisms. Traditional conservation methods include drying in a hot air chamber and/or freezing. These techniques may significantly affect the pollen organoleptic properties and its content of bioactive compounds. Here, a new conservation method, microwave drying, is introduced and investigated. The method implies irradiating the fresh pollen with microwaves under vacuum, in order to reduce the water content without reaching temperatures capable of thermally deteriorating important bioactive compounds. The method was evaluated by taking into account the nutritional properties after the treatment. The analyzed parameters were phenols, flavonoids, with special reference to rutin content, and amino acids. Results showed that microwave drying offers important advantages for the conservation of bee pollen. Irrespective of microwave power and treatment time, phenol and flavonoid content did not vary over untreated fresh pollen. Similarly, rutin content was unaffected by the microwave drying, suggesting that the microwave-assisted drying could be a powerful technology to preserve bioprotective compounds in fresh pollen.

  17. Microwave-assisted liquefaction of wood with polyhydric alcohols and its application in preparation of polyurethane (PU) foams

    Treesearch

    Hui Pan; Zhifeng Zheng; Chung Y. Hse

    2011-01-01

    Microwave radiation was used as the heating source in southern pine wood liquefaction with PEG/glycerin binary solvent. It was found that microwave heating was more efficient than conventional oil bath heating for wood liquefaction. The wood residue content of the H2SO4 catalyzed liquefied wood dropped to zero within 5 min with microwave heating. The resulting...

  18. Microwave-assisted liquefaction of wood with polyhydric alcohols and its application in preparation of polyurethane (PU) foams

    Treesearch

    Hui Pan; Zhifeng Zheng; Chung-Yun Hse

    2012-01-01

    Microwave radiation was used as the heating source in southern pine wood liquefaction with PEG/ glycerin binary solvent. It was found that microwave heating was more efficient than conventional oil bath heating for wood liquefaction. The wood residue content of the H2SO4 catalyzed liquefied wood dropped to zero within 5 min with microwave heating. The resulting...

  19. Dielectric characterization of Bentonite clay at various moisture contents and with mixtures of biomass in the microwave spectrum

    USDA-ARS?s Scientific Manuscript database

    This study assesses the potential for using bentonite as a microwave absorber for microwave-assisted biomass pyrolysis based on the dielectric properties. Dielectric properties of bentonite at different moisture contents were measured using a coaxial line dielectric probe and vector network analyzer...

  20. Microwave-Mediated Synthesis of Lophine: Developing a Mechanism to Explain a Product

    ERIC Educational Resources Information Center

    Crouch, R. David; Howard, Jessica L.; Zile, Jennifer L.; Barker, Kathryn H.

    2006-01-01

    The microwave-mediated preparation of lophine (2,4,5-triphenylimidazole) is described. This experiment allows for an introduction to the emerging technology of microwave-assisted organic synthesis while providing an opportunity for students to employ the principles of carbonyl chemistry in devising a mechanism to explain the formation of the…

  1. Ionic liquid-based ultrasonic/microwave-assisted extraction combined with UPLC-MS-MS for the determination of tannins in Galla chinensis.

    PubMed

    Lu, Chunxia; Wang, Hongxin; Lv, Wenping; Ma, Chaoyang; Lou, Zaixiang; Xie, Jun; Liu, Bo

    2012-01-01

    Ionic liquid was used as extraction solvents and applied to the extraction of tannins from Galla chinensis in the simultaneous ultrasonic- and microwave-assisted extraction (UMAE) technique. Several parameters of UMAE were optimised, and the results were compared with of the conventional extraction techniques. Under optimal conditions, the content of tannins was 630.2 ± 12.1 mg g⁻¹. Compared with the conventional heat-reflux extraction, maceration extraction, regular ultrasound- and microwave-assisted extraction, the proposed approach exhibited higher efficiency (11.7-22.0% enhanced) and shorter extraction time (from 6 h to 1 min). The tannins were then identified by ultraperformance liquid chromatography tandem mass spectrometry. This study suggests that ionic liquid-based UMAE is an efficient, rapid, simple and green sample preparation technique.

  2. Preparation of cashew gum-based flocculants by microwave- and ultrasound-assisted methods.

    PubMed

    Klein, Jalma Maria; de Lima, Vanessa Silva; da Feira, José Manoel Couto; Camassola, Marli; Brandalise, Rosmary Nichele; Forte, Maria Madalena de Camargo

    2018-02-01

    In this work, copolymers based on cashew gum (CG) grafted with polyacrylamide (PAM) were synthesized by microwave- and ultrasound-assisted methods, using potassium persulfate as an initiator in aqueous medium. The graft copolymers were characterized by Fourier-transform infrared spectroscopy, nuclear magnetic resonance spectroscopy, and thermogravimetric analysis. The efficiency of the graft copolymers (CG-g-PAM) in flocculation of a kaolin suspension was studied. Results indicated that the graft copolymers synthesized by ultrasound energy had better flocculation properties than the ones synthesized by the microwave-assisted method. The biodegradability of the graft copolymers was tested by inoculation with the basidiomycete Trametes villosa in liquid medium. The higher formation of biomass than that observed with the commercial flocculant Flonex-9045 indicated that the graft copolymer was accessible to enzymatic attack. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Applied mathematical problems in modern electromagnetics

    NASA Astrophysics Data System (ADS)

    Kriegsman, Gregory

    1994-05-01

    We have primarily investigated two classes of electromagnetic problems. The first contains the quantitative description of microwave heating of dispersive and conductive materials. Such problems arise, for example, when biological tissue are exposed, accidentally or purposefully, to microwave radiation. Other instances occur in ceramic processing, such as sintering and microwave assisted chemical vapor infiltration and other industrial drying processes, such as the curing of paints and concrete. The second class characterizes the scattering of microwaves by complex targets which possess two or more disparate length and/or time scales. Spatially complex scatterers arise in a variety of applications, such as large gratings and slowly changing guiding structures. The former are useful in developing microstrip energy couplers while the later can be used to model anatomical subsystems (e.g., the open guiding structure composed of two legs and the adjoining lower torso). Temporally complex targets occur in applications involving dispersive media whose relaxation times differ by orders of magnitude from thermal and/or electromagnetic time scales. For both cases the mathematical description of the problems gives rise to complicated ill-conditioned boundary value problems, whose accurate solutions require a blend of both asymptotic techniques, such as multiscale methods and matched asymptotic expansions, and numerical methods incorporating radiation boundary conditions, such as finite differences and finite elements.

  4. Hydrogen production from alcohol reforming in a microwave ‘tornado’-type plasma

    NASA Astrophysics Data System (ADS)

    Tatarova, E.; Bundaleska, N.; Dias, F. M.; Tsyganov, D.; Saavedra, R.; Ferreira, C. M.

    2013-12-01

    In this work, an experimental investigation of microwave plasma-assisted reforming of different alcohols is presented. A microwave (2.45 GHz) ‘tornado’-type plasma with a high-speed tangential gas injection (swirl) at atmospheric pressure is applied to decompose alcohol molecules, namely methanol, ethanol and propanol, and to produce hydrogen-rich gas. The reforming efficiency is investigated both in Ar and Ar+ water vapor plasma environments. The hydrogen yield dependence on the partial alcohol flux is analyzed. Mass spectrometry and Fourier transform infrared spectroscopy are used to detect the outlet gas products from the decomposition process. Hydrogen, carbon monoxide, carbon dioxide and solid carbon are the main decomposition by-products. A significant increase in the hydrogen production rate is observed with the addition of a small amount of water. Furthermore, optical emission spectroscopy is applied to detect the radiation emitted by the plasma and to estimate the gas temperature and electron density.

  5. 40 CFR 63.1426 - Process vent requirements for determining organic HAP concentration, control efficiency, and...

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... National Emission Standards for Hazardous Air Pollutant Emissions for Polyether Polyols Production § 63... percent reduction may be measured as total epoxide, total organic HAP, or as TOC minus methane and ethane... TOC (minus methane and ethane) concentrations in all process vent streams and primary and secondary...

  6. 40 CFR 63.1426 - Process vent requirements for determining organic HAP concentration, control efficiency, and...

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... National Emission Standards for Hazardous Air Pollutant Emissions for Polyether Polyols Production § 63... percent reduction may be measured as total epoxide, total organic HAP, or as TOC minus methane and ethane... TOC (minus methane and ethane) concentrations in all process vent streams and primary and secondary...

  7. Application of BiFeO3-based on nickel foam composites with a highly efficient catalytic activity and easily recyclable in Fenton-like process under microwave irradiation

    NASA Astrophysics Data System (ADS)

    Li, Shuo; Zhang, Guangshan; Zheng, Heshan; Zheng, Yongjie; Wang, Peng

    2018-05-01

    In this study, BiFeO3 (BFO) powders decorated on nickel foam (NF) with a high catalytic activity are prepared via a one-step microwave-assisted hydrothermal method. The factors that influence the degradation of bisphenol A (BPA) with BFO/NFs as catalysts are optimized to improve the catalytic activity in a microwave-enhanced Fenton-like process. BFO/NF exhibit a superior catalytic activity with a high BPA removal ratio (98.4%) and TOC removal ratio (69.5%) within 5 min. Results indicate that NF significantly affect the improvement of the catalytic activity of BFO because it served as a source of hydroxyl radicals (•OH) during degradation. The amount of •OH generated by BFO/NF is approximately 1.65-fold higher than that by pure BFO. After six reaction cycles, the stability and reusability of •OH remain high. These findings provide new insights into the synthesis of composites on heterogeneous catalysts with high efficiency and easy recyclability for water treatment applications.

  8. Microwave blanching and drying characteristics of Centella asiatica (L.) urban leaves using tray and heat pump-assisted dehumidified drying.

    PubMed

    Trirattanapikul, W; Phoungchandang, S

    2014-12-01

    The appropriate stage of maturity of Centella asiatica (L.) Urban leaves was investigated. Mature leaves with large diameter contained high total phenolics and % inhibition. Microwave blanching for 30 s retained the highest total phenolics and the microwave blanching for 30 s and 45 s retained the highest % inhibition. Modified Henderson and Modified Chung-Pfost models showed the best fit to both fresh and blanched leaves for equilibrium moisture content, Xe = f(RHe, T) and equilibrium relative humidity, RHe = f(Xe, T), respectively. The Modified Page model was the most effective model in describing the leaf drying. All drying was in the falling rate period. The drying constant was related to drying air temperature using the Arrhenius model. Effective moisture diffusivities increased with increasing temperature and blanching treatments as well as dehumidification by heat pump-assisted dehumidified dryer. The heat pump-assited dehumidified drying incorporated by the microwave blanching could reduce the drying time at 40 °C by 31.2 % and increase % inhibition by 6.1 %. Quality evaluation by total phenolics, % inhibition and rehydration ratio showed the best quality for C. asiatica leaves pretreated by microwave blanching and dried at 40 °C in heat pump-assisted dehumidified dryer.

  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. Copyright © 2015 Elsevier Inc. All rights reserved.

  10. 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%...

  11. Microwave assisted facile green synthesis of silver and gold nanocatalysts using the leaf extract of Aerva lanata.

    PubMed

    Joseph, Siby; Mathew, Beena

    2015-02-05

    Herein, we report a simple microwave assisted method for the green synthesis of silver and gold nanoparticles by the reduction of aqueous metal salt solutions using leaf extract of the medicinal plant Aerva lanata. UV-vis., FTIR, XRD, and HR-TEM studies were conducted to assure the formation of nanoparticles. XRD studies clearly confirmed the crystalline nature of the synthesized nanoparticles. From the HR-TEM images, the silver nanoparticles (AgNPs) were found to be more or less spherical and gold nanoparticles (AuNPs) were observed to be of different morphology with an average diameter of 18.62nm for silver and 17.97nm for gold nanoparticles. In order to evaluate the effect of microwave heating upon rate of formation, the synthesis was also conducted under ambient condition without the assistance of microwave radiation and the former method was found to be much faster than the later. The synthesized nanoparticles were used as nanocatalysts in the reduction of 4-nitrophenol to 4-aminophenol by NaBH4. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. 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.

  13. Determination of cobalt species in nutritional supplements using ICP-OES after microwave-assisted extraction and solid-phase extraction.

    PubMed

    Bartosiak, Magdalena; Jankowski, Krzysztof; Giersz, Jacek

    2018-06-05

    Cobalt content (as vitamin B 12 and inorganic cobalt) in two nutritional supplements, namely Spirulina platensis and Saccharomyces cerevisiae known as a "superfood", has been determined using inductively coupled plasma optical emission spectrometry (ICP-OES). Several sample pre-treatment protocols have been applied and compared. Microwave-assisted acid digestion efficiently decomposed all cobalt-containing compounds, thus allowed obtaining total cobalt content in supplements examined. Vitamin B 12 was extracted from the samples with acetate buffer and potassium cyanide solution exposed to mild microwave radiation for 30 min, and cyanocobalamin was separated from the extract by on-column solid phase extraction using C-18 modified silica bed. About 100% of cobalt species was extracted using the triple microwave-assisted extraction procedure. Total cobalt content was 20-fold greater in Spirulina tablets than the declared cobalamin content (as Co). The ICP-OES method precision was about 3% and detection limit was 1.9 and 2.7 ng Co mL -1 for inorganic cobalt or cyanocobalamin, respectively. Copyright © 2018 Elsevier B.V. All rights reserved.

  14. Comparison of microwave, ultrasound and accelerated-assisted solvent extraction for recovery of polyphenols from Citrus sinensis peels.

    PubMed

    Nayak, Balunkeswar; Dahmoune, Farid; Moussi, Kamal; Remini, Hocine; Dairi, Sofiane; Aoun, Omar; Khodir, Madani

    2015-11-15

    Peel of Citrus sinensis contains significant amounts of bioactive polyphenols that could be used as ingredients for a number of value-added products with health benefits. Extraction of polyphenols from the peels was performed using a microwave-assisted extraction (MAE) technique. The effects of aqueous acetone concentration, microwave power, extraction time and solvent-to-solid ratio on the total phenolic content (TPC), total antioxidant activity (TAA) (using DPPH and ORAC-values) and individual phenolic acids (IPA) were investigated using a response surface method. The TPC, TAA and IPA of peel extracts using MAE was compared with conventional, ultrasound-assisted and accelerated solvent extraction. The maximum predicted TPC under the optimal MAE conditions (51% acetone concentration in water (v/v), 500 W microwave power, 122 s extraction time and 25 mL g(-1) solvent to solid ratio), was 12.20 mg GAE g(-1) DW. The TPC and TAA in MAE extracts were higher than the other three extracts. Copyright © 2015 Elsevier Ltd. All rights reserved.

  15. The Utilization of Bark to Make Rigid Polyurethane Foams

    NASA Astrophysics Data System (ADS)

    D'Souza, Jason

    This work focused on the characterization of polyols derived from the liquefaction or alkoxylation of bark. Regarding liquefaction, it was found that both temperature and solvent structure played a significant role in polyol properties. High temperature liquefaction resulted in the degradation of sugars, while liquefaction at mild temperatures preserved sugar structures as shown by 31P-NMR. It was also shown that liquefaction at 130°C was ideal in terms of producing a polyol with a relatively at, broad, plateau of molecular weight distribution, whereas liquefaction at 90 and 160°C produced polyols with a large amount of low molecular weight compounds. Regarding solvent structure, it was found that polyhydric alcohols with short chain primary hydroxyls resulted in less sugar degradation products and less formation of condensation side-products. It is proposed that the highly polar environment promoted grafting and prevented condensation onto other biopolymers. Using organic solvents it was found that ketonic solvents like acetyl acetone and cyclohexanone, through their highly polar carbonyl group could engage in hydrogen bonding through electron donation/proton accepting interactions. These enabled the solvent to reduce the amount of condensation reactions and improve liquefaction yield. The liquefied bark-based polyols were then used to make polyurethane foams. It was found that when a diversity of hydroxyl groups were present the foaming rate was reduced and this may react a slower rate of curing and explain why the bark foams had a greater amount of cells that underwent coalescence. It was also observed that the bark foams had a low amount of closed-cell content. Since closed-cell content plays a role in dictating elastic compression, this may explain why the bark foams exhibited a lower elastic modulus. Finally, as a contrast to liquefaction, bark was alkoxylated. It was observed that the conversion yield was higher than liquefaction. The polyols had a high average molecular weight with a broad distribution and far greater solubility. It is proposed that alkoxylation is far less degradative than liquefaction. This may explain why the foams showed improved compressive behaviour compared to the foams made from liqueed bark-based polyols. Through greater characterization of the structure of polyols produced via liquefaction and alkoxylation the relationships between reaction parameters, polyol structure, and foam properties can be better understood. This is an important step towards the utilization of bark to make polyurethane foams.

  16. Structure-property studies of thermoplastic and thermosetting polyurethanes using palm and soya oils-based polyols.

    PubMed

    Mohammed, Issam Ahmed; Al-Mulla, Emad Abbas Jaffar; Kadar, Nurul Khizien Abdul; Ibrahim, Mazlan

    2013-01-01

    Palm and soya oils were converted to monoglycerides via transesterification of triglycerides with glycerol by one step process to produce renewable polyols. Thermoplastic polyurethanes (TPPUs) were prepared from the reaction of the monoglycerides which act as polyol with 4,4'-methylenediphenyldiisocyanate (MDI) whereas, thermosetting polyurethanes (TSPUs) were prepared from the reaction of glycerol, MDI and monoglycerides in one pot. Characterization of the polyurethanes was carried out by FT-IR, (1)H NMR, and iodine value and sol-gel fraction. The TSPUs showed good thermal properties compared to TPPUs as well as TSPUs exhibits good properties in pencil hardness and adhesion, however poorer in flexural and impact strength compared to TPPUs. The higher percentage of cross linked fraction, the higher degree of cross linking occurred, which is due to the higher number of double bond presents in the TSPUs. These were reflected in iodine value test as the highest iodine value of the soya-based thermosetting polyurethanes confirmed the highest degree of cross linking. Polyurethanes based on soya oil showed better properties compared to palm oil. This study is a breakthrough development of polyurethane resins using palm and soya oils as one of the raw materials.

  17. Polyurethane nanocomposites incorporating biobased polyols and reinforced with a low fraction of cellulose nanocrystals.

    PubMed

    Kong, Xiaohua; Zhao, Liyan; Curtis, Jonathan M

    2016-11-05

    High solids content polyurethane (PU) nanocomposites with enhanced thermal and mechanical properties were produced by incorporating of low fractions of cellulose nanocrystals (CNC) in a solvent-free process. This involved the use of a simple procedure to produce well dispersed and stable suspensions of CNC in biobased polyols, which were then used to produce PU-CNC nanocomposites. Transmission electron microscopy revealed that individual CNC particles were dispersed homogenously within the PU matrix. FTIR results suggested that CNC particles are covalently bonded to the PU molecular chains during polymerization. The thermal mechanical properties of the nanocomposites are significantly improved over pure PU as indicated by differential scanning calorimetry and dynamic mechanical analysis. Compared to pure PU, the PU nanocomposites made with the addition of only 0.5% of CNC had glass transition temperatures that were 6°C higher, their Young's moduli were about 10% higher and their abrasion resistance was higher by about 25%. The optimal composition contains only 0.5% CNC (w/w) which indicates that there is good potential for utilization of low levels of CNC for reinforcement of PU composites made using biobased polyols. Copyright © 2016 Elsevier Ltd. All rights reserved.

  18. Microwave-assisted preparation of flower-like cobalt phosphate and its application as a new heterogeneous Fenton-like catalyst

    NASA Astrophysics Data System (ADS)

    Hu, Xiaoxia; Li, Rong; Zhao, Shuyu; Xing, Yanjun

    2017-02-01

    A novel flower-like 3D hierarchical cobalt phosphate Co3(PO4)2·8H2O (fCoP), and a plate-like cobalt phosphate (pCoP) were successfully synthesized via a microwave-assisted method at low temperature under atmospheric pressure using hexamethylene tetramine (HMTA) or urea as a template. All CoPs were characterized using XRD, FESEM, TEM, DRS and surface photovoltage spectra (SPS). The performance of the photocatalytic degradation of Rhodamine B (RhB) via a Fenton-like process on CoPs was evaluated both in the dark and under illumination. The results showed that the morphology and composition of the CoPs affected the RhB degradation. The flower-like hierarchical fCoP favored the photo degradation of RhB. fCoP was also confirmed to have the merits of easy recycling and good stability based on successive degradation experiments. The active species trapping experiments showed that the superoxide radical (rad O2-) was the dominant active species in the Fenton-like process. The catalytic activation was confirmed to be related to both the Co(II) on the surface and the fCoP framework.

  19. Microwave-assisted extraction for Hibiscus sabdariffa bioactive compounds.

    PubMed

    Pimentel-Moral, Sandra; Borrás-Linares, Isabel; Lozano-Sánchez, Jesús; Arráez-Román, David; Martínez-Férez, Antonio; Segura-Carretero, Antonio

    2018-07-15

    H. sabdariffa has demonstrated positive results against chronic diseases due to the presence of phytochemicals, mainly phenolic compounds. The extraction process of bioactive compounds increases the efficient collection of extracts with high bioactivity. Microwave-Assisted Extraction (MAE) constituted a "green technology" widely employed for plant matrix. In this work, the impact of temperature (50-150 °C), composition of extraction solvent (15-75% EtOH) and extraction time (5-20 min) on the extraction yield and individual compounds concentrations were evaluated. Furthermore, the characterization of 16 extracts obtained was performed by HPLC-ESI-TOF-MS. The results showed that 164 °C, 12.5 min, 45% ethanol was the best extraction condition, although glycoside flavonoids were degraded. Besides that, the optimal conditions for extraction yield were 164 °C, 60% ethanol and 22 min. Thus, temperature and solvent concentration have demonstrated to be potential factors in MAE for obtaining bioactive compounds from H. sabdariffa. Copyright © 2018 Elsevier B.V. All rights reserved.

  20. 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.

  1. Simultaneous determination of 14 disinfection by-products in meat products using microwave-assisted extraction and static headspace coupled to gas chromatography-mass spectrometry.

    PubMed

    Cardador, Maria Jose; Gallego, Mercedes

    2017-08-04

    This paper described the first analytical method to simultaneously determine 14 disinfection by-products (DBPs) in meat products using microwave-assisted extraction (MAE) and static headspace (SHS) followed by gas chromatography-mass spectrometry (GC-MS). The DBPs included were 4 trihalomethanes, 7 haloacetic acids, 2 haloacetonitriles and trichloronitromethane, which are commonly formed as a consequence of the disinfection process of water. The combination of the MAE and SHS techniques allows meat samples to be analysed in two sequential steps into the same HS vial in spite of the sample's complexity. Detection limits were obtained within the range of 0.06-0.70ng/g, and the average relative standard deviation was 7.4%. Recoveries throughout the whole process were between 86 and 95%. The SHS-GC-MS method was applied to determine DBPs in meat products with different industrial processing which could be contaminated through contact with disinfectants and/or treated water employed in the factory either for washing or for the cooking of meat. Up to 5 DBPs were found at ng/g levels in about 36% of the samples analysed, cooked ham being the most contaminated meat product because of the brine solutions employed in its manufacturing process. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Polyol concentrations in Aspergillus repens grown under salt stress.

    PubMed

    Kelavkar, U P; Chhatpar, H S

    1993-09-01

    Na(+), K(+) and the ratio of Na(+)/K(+) were higher in cells of the halotolerant Aspergillus repens grown with 2 M NaCl than without NaCl. The osmolytes, proline, glycerol, betaine and glutamate, did not affect the Na(+)/K(+) ratio, nor the polyol content of cells under any conditions. The concentrations of polyols, consisting of glycerol, arabitol, erythritol and mannitol, changed markedly during growth, indicating that they have a crucial role in osmotic adaptation.

  3. Orthogonal protection of saccharide polyols through solvent-free one-pot sequences based on regioselective silylations

    PubMed Central

    Traboni, Serena; Bedini, Emiliano

    2016-01-01

    tert-Butyldimethylsilyl (TBDMS) and tert-butyldiphenylsilyl (TBDPS) are alcohol protecting groups widely employed in organic synthesis in view of their compatibility with a wide range of conditions. Their regioselective installation on polyols generally requires lengthy reactions and the use of high boiling solvents. In the first part of this paper we demonstrate that regioselective silylation of sugar polyols can be conducted in short times with the requisite silyl chloride and a very limited excess of pyridine (2–3 equivalents). Under these conditions, that can be regarded as solvent-free conditions in view of the insolubility of the polyol substrates, the reactions are faster than in most examples reported in the literature, and can even be further accelerated with a catalytic amount of tetrabutylammonium bromide (TBAB). The strategy proved also useful for either the selective TBDMS protection of secondary alcohols or the fast per-O-trimethylsilylation of saccharide polyols. In the second part of the paper the scope of the silylation approach was significantly extended with the development of unprecedented “one-pot” and “solvent-free” sequences allowing the regioselective silylation/alkylation (or the reverse sequence) of saccharide polyols in short times. The developed methodologies represent a very useful and experimentally simple tool for the straightforward access to saccharide building-blocks useful in organic synthesis. PMID:28144345

  4. Electric-field assisted spin torque nano-oscillator and binary frequency shift keying modulation

    NASA Astrophysics Data System (ADS)

    Zhang, Xiangli; Chen, Hao-Hsuan; Zhang, Zongzhi; Liu, Yaowen

    2018-04-01

    Electric-controlled magnetization precession introduces technologically relevant possibility for developing spin torque nano-oscillators (STNO) with potential applications in microwave emission. Using the perpendicularly magnetized magnetic tunnel junction (MTJ), we show that the magnetization oscillation frequency can be tuned by the co-action of electric field and spin polarized current. The dynamical phase diagram of MTJ-based STNO is analytically predicted through coordinate transformation from the laboratory frame to the rotation frame, by which the nonstationary out-of-plane magnetization precession process is therefore transformed into the stationary process in the rotation frame. Furthermore, using this STNO as a microwave source, we numerically demonstrate that the bit signal can be transmitted by a binary frequency shift keying (BFSK) modulation technique. The BFSK scheme shows good modulation features with no transient state.

  5. Hydrogenolysis of Glycerol to Propylene Glycol on Nanosized Cu-Zn-Al Catalysts Prepared Using Microwave Process.

    PubMed

    Kim, Dong Won; Ha, Sang Ho; Moon, Myung Jun; Lim, Kwon Taek; Ryu, Young Bok; Lee, Sun Do; Lee, Man Sig; Hong, Seong-Soo

    2015-01-01

    Cu-Zn-Al catalysts were prepared using microwave-assisted process and co-precipitation methods. The prepared catalysts were characterized by XRD, BET, XPS and TPD of ammonia and their catalytic activity for the hydrogenolysis of glycerol to propylene glycol was also examined. The XRD patterns of Cu/Zn/Al mixed catalysts show CuO and ZnO crystalline phase regardless of preparation method. The highest glycerol hydrogenolysis conversion is obtained with the catalyst having a Cu/Zn/Al ratio of 2:2:1. Hydrogen pre-reduction of catalysts significantly enhanced both glycerol conversions and selectivity to propylene glycol. The glycerol conversion increased with an increase of reaction temperature. However, the selectivity to propylene glycol increased with an increase of temperature, and then declined to 30.5% at 523 K.

  6. Preparation of High Surface Area Activated Carbon from Spent Phenolic Resin by Microwave Heating and KOH Activation

    NASA Astrophysics Data System (ADS)

    Cheng, Song; Zhang, Libo; Zhang, Shengzhou; Xia, Hongying; Peng, Jinhui

    2018-01-01

    The spent phenolic resin is as raw material for preparing high surface area activated carbon (HSAAC) by microwave-assisted KOH activation. The effects of microwave power, activation duration and impregnation ratio (IR) on the iodine adsorption capability and yield of HSAAC were investigated. The surface characteristics of HSAAC were characterized by nitrogen adsorption isotherms, FTIR, SEM and TEM. The operating variables were optimized utilizing the response surface methodology (RSM) and were identified to be microwave power of 700 W, activation duration of 15 min and IR of 4, corresponding to a yield of 51.25 % and an iodine number of 2,384 mg/g. The pore structure parameters of the HSAAC, i. e., Brunauer-Emmett-Teller (BET) surface area, total pore volume, and average pore diameter were estimated to be 4,269 m2/g, 2.396 ml/g and 2.25 nm, respectively, under optimum conditions. The findings strongly support the feasibility of microwave-assisted KOH activation for preparation of HSAAC from spent phenolic resin.

  7. 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.

  8. Comparison of heat and mass transfer of different microwave-assisted extraction methods of essential oil from Citrus limon (Lisbon variety) peel.

    PubMed

    Golmakani, Mohammad-Taghi; Moayyedi, Mahsa

    2015-11-01

    Dried and fresh peels of Citrus limon were subjected to microwave-assisted hydrodistillation (MAHD) and solvent-free microwave extraction (SFME), respectively. A comparison was made between MAHD and SFME with the conventional hydrodistillation (HD) method in terms of extraction kinetic, chemical composition, and antioxidant activity. Higher yield results from higher extraction rates by microwaves and could be due to a synergy of two transfer phenomena: mass and heat acting in the same way. Gas chromatography/mass spectrometry (GC/MS) analysis did not indicate any noticeable differences between the constituents of essential oils obtained by MAHD and SFME, in comparison with HD. Antioxidant analysis of the extracted essential oils indicated that microwave irradiation did not have adverse effects on the radical scavenging activity of the extracted essential oils. The results of this study suggest that MAHD and SFME can be termed as green technologies because of their less energy requirements per ml of essential oil extraction.

  9. Catalytic routes and oxidation mechanisms in photoreforming of polyols

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

    Sanwald, Kai E.; Berto, Tobias F.; Eisenreich, Wolfgang

    2016-12-01

    Photocatalytic reforming of biomass-derived oxygenates leads to H 2 generation and evolution of CO 2 via parallel formation of organic intermediates through anodic oxidations on a Rh/TiO 2 photocatalyst. The reaction pathways and kinetics in the photoreforming of C 3–C 6 polyols were explored. Polyols are converted via direct and indirect hole transfer pathways resulting in (i) oxidative rupture of C–C bonds, (ii) oxidation to a-oxygen functionalized aldoses and ketoses (carbonyl group formation) and (iii) light-driven dehydration. Direct hole transfer to chemisorbed oxygenates on terminal Ti(IV)-OH groups, generating alkoxy-radicals that undergo ß-C–C-cleavage, is proposed for the oxidative C–C rupture. Carbonylmore » group formation and dehydration are attributed to indirect hole transfer at surface lattice oxygen sites [Ti_ _ _O_ _ _Ti] followed by the generation of carbon-centered radicals. Polyol chain length impacts the contribution of the oxidation mechanisms favoring the C–C bond cleavage (internal preferred over terminal) as the dominant pathway with higher polyol carbon number.« less

  10. Directed-energy process technology efforts

    NASA Technical Reports Server (NTRS)

    Alexander, P.

    1985-01-01

    A summary of directed-energy process technology for solar cells was presented. This technology is defined as directing energy or mass to specific areas on solar cells to produce a desired effect in contrast to exposing a cell to a thermal or mass flow environment. Some of these second generation processing techniques are: ion implantation; microwave-enhanced chemical vapor deposition; rapid thermal processing; and the use of lasers for cutting, assisting in metallization, assisting in deposition, and drive-in of liquid dopants. Advantages of directed energy techniques are: surface heating resulting in the bulk of the cell material being cooler and unchanged; better process control yields; better junction profiles, junction depths, and metal sintering; lower energy consumption during processing and smaller factory space requirements. These advantages should result in higher-efficiency cells at lower costs. The results of the numerous contracted efforts were presented as well as the application potentials of these new technologies.

  11. Mass transfer coefficient in ginger oil extraction by microwave hydrotropic solution

    NASA Astrophysics Data System (ADS)

    Handayani, Dwi; Ikhsan, Diyono; Yulianto, Mohamad Endy; Dwisukma, Mandy Ayulia

    2015-12-01

    This research aims to obtain mass transfer coefficient data on the extraction of ginger oil using microwave hydrotropic solvent as an alternative to increase zingiberene. The innovation of this study is extraction with microwave heater and hydrotropic solvent,which able to shift the phase equilibrium, and the increasing rate of the extraction process and to improve the content of ginger oil zingiberene. The experiment was conducted at the Laboratory of Separation Techniques at Chemical Engineering Department of Diponegoro University. The research activities carried out in two stages, namely experimental and modeling work. Preparation of the model postulated, then lowered to obtain equations that were tested and validated using data obtained from experimental. Measurement of experimental data was performed using microwave power (300 W), extraction temperature of 90 ° C and the independent variable, i.e.: type of hydrotropic, the volume of solvent and concentration in order, to obtain zingiberen levels as a function of time. Measured data was used as a tool to validate the postulation, in order to obtain validation of models and empirical equations. The results showed that the mass transfer coefficient (Kla) on zingiberene mass transfer models ginger oil extraction at various hydrotropic solution attained more 14 ± 2 Kla value than its reported on the extraction with electric heating. The larger value of Kla, the faster rate of mass transfer on the extraction process. To obtain the same yields, the microwave-assisted extraction required one twelfth time shorter.

  12. Microwave-assisted solvothermal synthesis of hierarchical TiO2 microspheres for efficient electro-field-assisted-photocatalytic removal of tributyltin in tannery wastewater.

    PubMed

    Zhao, Yang; Huang, Zhiding; Chang, Wenkai; Wei, Chao; Feng, Xugen; Ma, Lin; Qi, Xiaoxia; Li, Zenghe

    2017-07-01

    Organotin compounds have been widely used in recent decades, however, the residential tributyltin (TBT) in environment has potential harmful effects on human health due to the disruption of endocrine system even at trace level. Herein, this work reports on an effective electro-field-assisted-photocatalytic technique for removal of TBT by applying an electric field to photocatalysis of as-prepared hierarchical TiO 2 microspheres. The synthesis of catalytic materials is based on a self-assembly process induced by microwave-assisted solvothermal reaction. Hierarchical TiO 2 microspheres consisting of nanowires can be obtained in short time with this facile method and possess high surface area and superior optical properties. As the catalyst, it was found that the reaction rate constant of electro-field-assisted-photocatalytic removal (0.0488 min -1 ) of TBT exhibited almost a 9 fold improvement as compared to that of photocatalysis (0.0052 min -1 ). The proposed mechanism of electro-field-assisted-photocatalytic removal of TBT was verified by using 117 Sn-enriched TBT spike solution as an isotopic tracer. In addition, varying impacts from some key reaction conditions, such as voltage of potential, pH value and the presence of Cr and formaldehyde were also discussed. The overall satisfactory TBT removal performance of the proposed electro-field-assisted-photocatalysis procedure with hierarchical TiO 2 microspheres, which was validated using actual tannery wastewater samples from three different kinds of tanning procedures. These attributes suggest that this electro-field-assisted-photocatalysis may have broad applications for the treatment of tannery wastewater. Copyright © 2017 Elsevier Ltd. All rights reserved.

  13. Peroxide-assisted microwave activation of pyrolysis char for adsorption of dyes from wastewater.

    PubMed

    Nair, Vaishakh; Vinu, R

    2016-09-01

    In this study, mesoporous activated biochar with high surface area and controlled pore size was prepared from char obtained as a by-product of pyrolysis of Prosopis juliflora biomass. The activation was carried out by a simple process that involved H2O2 treatment followed by microwave pyrolysis. H2O2 impregnation time and microwave power were optimized to obtain biochar with high specific surface area and high adsorption capacity for commercial dyes such as Remazol Brilliant Blue and Methylene Blue. Adsorption parameters such as initial pH of the dye solution and adsorbent dosage were also optimized. Pore size distribution, surface morphology and elemental composition of activated biochar were thoroughly characterized. H2O2 impregnation time of 24h and microwave power of 600W produced nanostructured biochar with narrow and deep pores of 357m(2)g(-1) specific surface area. Langmuir and Langmuir-Freundlich isotherms described the adsorption equilibrium, while pseudo second order model described the kinetics of adsorption. Copyright © 2016 Elsevier Ltd. All rights reserved.

  14. Rapid microwave-assisted synthesis of polydextrose and identification of structure and function.

    PubMed

    Wang, Haisong; Shi, Yonghui; Le, Guowei

    2014-11-26

    Microwave irradiation is a rapid and efficient method to synthesize oligomers and can be employed in polysaccharides production. As an artificial polysaccharide, polydextrose is known for its solid performance in food processing and its additional health benefits. This study was aimed at producing polydextrose by microwave irradiation using glucose and sorbitol as substrates; water and phosphoric acid as initiator and catalyst. The actual maximum yield was 99%. Synthetic polydextrose were purified by ethanol elution and Sepherdex G-25 column chromatography. Its purity was demonstrated by the high-performance gel-permeation chromatography as a single symmetrical sharp peak, additionally the average molecular weight was calculated to be 2.131 kDa. FT-IR spectra showed that the synthesized polydextrose has the structural feature similar to Polydextrose-Litesse(®). In vitro fermentation revealed that polydextrose possesses the biological function similar to Polydextrose-Litesse(®) in increasing the concentration of short chain fatty acid and decreasing pH. This research demonstrated the feasibility of a rapid and efficient microwave mediated method to synthesize polydextrose and potentially other value added carbohydrate polymers. Copyright © 2014 Elsevier Ltd. All rights reserved.

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

    Ding, Ling; Song, Yu, E-mail: songyu@dlpu.edu.cn; Yang, Wei

    Open-framework zinc phosphates were synthesized by microwave-assisted technique, and it was shown that the morphology of as-prepared materials could be easily tailored by changing synthesis temperature, reaction time and pH value. During the synthesis, when the reaction temperature increases from 130 °C to 220 °C, the products transformed from hexagonal prisms to polyhedron along with the disappearance of the hexagonal prisms vertical plane. Simultaneously, both the reaction time and pH value could promote the nucleation and growth of crystal particles. More interestingly, the target products with different morphologies could be obtained by varying the usage of NaOH or NH{sub 3}·H{submore » 2}O at 130 °C during the microwave synthesis process. - Graphical abstract: Zinc phosphates with variable morphologies can be obtained by simply tuning the microwave-heating temperatures. Display Omitted - Highlights: • Synthesis of open-framework Zn{sub 4} (H{sub 3}O) (NH{sub 4}){sub 3}(PO{sub 4}){sub 4} compounds employing microwave technique. • Dependence of morphology on the reaction conditions. • Morphology transformation from hexagonal prisms to polyhedron was observed.« less

  16. Presidential Green Chemistry Challenge: 2007 Designing Greener Chemicals Award

    EPA Pesticide Factsheets

    Presidential Green Chemistry Challenge 2007 award winner, Cargill, developed biobased polyols for polyurethane applications, including flexible foams. Cargill makes BiOH polyols from vegetable oils, not petroleum products.

  17. 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

  18. 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.

  19. 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.

  20. Comparison of solid phase extraction, saponification and gel permeation chromatography for the clean-up of microwave-assisted biological extracts in the analysis of polycyclic aromatic hydrocarbons.

    PubMed

    Navarro, P; Cortazar, E; Bartolomé, L; Deusto, M; Raposo, J C; Zuloaga, O; Arana, G; Etxebarria, N

    2006-09-22

    The feasibility of different clean-up procedures was studied for the determination of polycyclic aromatic hydrocarbons (PAHs) in biota samples such as oysters, mussels and fish liver. In this sense, once the samples were extracted--essentially with acetone and in a microwave system--and before they could be analysed by gas chromatography-mass spectrometry (GC-MS), three different approaches were studied for the clean-up step: solid phase extraction (SPE), microwave-assisted saponification (MAS) and gel permeation chromatography (GPC). The main aim of this work was to maximise the recoveries of PAHs and to minimise the presence of interfering compounds in the last extract. In the case of SPE, Florisil cartridges of 1, 2 and 5 g, and silica cartridges of 5 g were studied. In that case, and with oysters and mussels, microwave-assisted extraction and 5 g Florisil cartridges provided good results. In addition, the concentrations obtained for Standard Reference Material (SRM) NIST 2977 (mussel tissue) were in good agreement with the certified values. In the case of microwave-assisted saponification, the extracts were not as clean as those obtained with 5 g Florisil and this fact lead to overestimate the concentration of the heaviest PAHs. Finally, the cleanest extracts were obtained by GPC. The method was successfully applied to mussels, oysters and hake liver, and the results obtained for NIST 2977 (mussel tissue) were within the confidence interval of the certified reference material for most of the certified analytes.

  1. The effect of pressure on microwave-enhanced Diels-Alder reactions. A case study.

    PubMed

    Kaval, Nadya; Dehaen, Wim; Kappe, C Oliver; Van der Eycken, Erik

    2004-01-21

    It is demonstrated that microwave-assisted Diels-Alder reactions of substituted 2(1H)-pyrazinones with ethylene are significantly more effective utilizing pre-pressurized (up to 10 bar) reaction vessels.

  2. Microwave-assisted generation of standard gas mixtures.

    PubMed

    Xiong, Guohua; Pawliszyn, Janusz

    2002-05-15

    Microwave heating was employed for preparation of the standard gas of volatile organic compounds (VOCs) and semivolatile organic compounds (semi-VOCs) by using a 1000 W commercial domestic microwave oven and 1 L gas-sampling bulbs. The VOCs investigated were benzene, chloroform, 1,3-dichlorobenzene, tetrachloroethylene, toluene, and 1,1,2-trichloroethane, and the semi-VOCs used were the polychlorinated biphenyls (PCBs) PCB 1016 and PCB 1248. Since these weakly or nonpolar molecules are very poor absorbers of microwave energy, an appropriate amount of water was introduced to accept microwave radiation and act as the thermal source to accelerate their evaporation. The glass bulb may also contribute thermal energy to the VOCs/semi-VOCs by accepting microwave energy to a small degree. For 0.5 microL of liquid VOCs on 10 mg of glass wool, it was shown that 15 microL of H2O and 60 s of microwave heating yielded a very efficient evaporation [97.2-106.4%, compared with a classic method (Muller, L; Gorecki, T.; Pawliszyn, J. Fresenius' J. Anal. Chem. 1999, 364, 610-616)]. For 1 microL of PCB solution (1000 microg/mL in hexane), 15 microL of H2O and 90 s of microwave heating also provided a complete evaporation. The addition of water was particularly significant for microwave-assisted evaporation of PCBs because semi-VOCs are much more difficult to evaporate than VOCs. This developed microwave technique proved to be quite simple, powerful, rapid, accurate, and safe for the preparation of VOC/semi-VOC standard gas. Solid- phase microextraction combined with gas chromatography was used for the gas analysis.

  3. Microwave Heating of Synthetic Skin Samples for Potential Treatment of Gout Using the Metal-Assisted and Microwave-Accelerated Decrystallization Technique

    PubMed Central

    2016-01-01

    Physical stability of synthetic skin samples during their exposure to microwave heating was investigated to demonstrate the use of the metal-assisted and microwave-accelerated decrystallization (MAMAD) technique for potential biomedical applications. In this regard, optical microscopy and temperature measurements were employed for the qualitative and quantitative assessment of damage to synthetic skin samples during 20 s intermittent microwave heating using a monomode microwave source (at 8 GHz, 2–20 W) up to 120 s. The extent of damage to synthetic skin samples, assessed by the change in the surface area of skin samples, was negligible for microwave power of ≤7 W and more extensive damage (>50%) to skin samples occurred when exposed to >7 W at initial temperature range of 20–39 °C. The initial temperature of synthetic skin samples significantly affected the extent of change in temperature of synthetic skin samples during their exposure to microwave heating. The proof of principle use of the MAMAD technique was demonstrated for the decrystallization of a model biological crystal (l-alanine) placed under synthetic skin samples in the presence of gold nanoparticles. Our results showed that the size (initial size ∼850 μm) of l-alanine crystals can be reduced up to 60% in 120 s without damage to synthetic skin samples using the MAMAD technique. Finite-difference time-domain-based simulations of the electric field distribution of an 8 GHz monomode microwave radiation showed that synthetic skin samples are predicted to absorb ∼92.2% of the microwave radiation. PMID:27917407

  4. Optimization of simultaneous microwave/ultrasonic-assisted extraction of phenolic compounds from walnut flour using response surface methodology.

    PubMed

    Luo, Yan; Wu, Wanxing; Chen, Dan; Lin, Yuping; Ma, Yage; Chen, Chaoyin; Zhao, Shenglan

    2017-12-01

    Walnut is a traditional food as well as a traditional medicine recorded in the Chinese Pharmacopoeia; however, the large amounts of walnut flour (WF) generated in walnut oil production have not been well utilized. This study maximized the total polyphenolic yield (TPY) from the walnut flour (WF) by optimizing simultaneous ultrasound/microwave-assisted hydroalcoholic extraction (SUMAE). Response surface methodology was used to optimize the processing parameters for the TPY, including microwave power (20-140 W), ultrasonic power (75-525 W), extraction temperature (25-55 °C), and time (0.5-9.5 min). The polyphenol components were analysed by LC-MS. A second-order polynomial model satisfactorily fit the experimental TPY data (R 2  = 0.9932, P < 0.0001 and R adj 2     = 0.9868). The optimized quick extraction conditions were microwave power 294.38 W, ultrasonic power 93.5 W, temperature 43.38 °C and time 4.33 min, with a maximum TPY of 34.91 mg GAE/g, which was a rapid extraction. The major phenolic components in the WF extracts were glansreginin A, ellagic acid, and gallic acid with peak areas of 22.15%, 14.99% and 10.96%, respectively, which might be used as functional components for health food, cosmetics and medicines. The results indicated that walnut flour, a waste product from the oil industry, was a rich source of polyphenolic compounds and thus could be used as a high-value functional food ingredient.

  5. Rapid, facile microwave-assisted synthesis of xanthan gum grafted polyaniline for chemical sensor.

    PubMed

    Pandey, Sadanand; Ramontja, James

    2016-08-01

    Grafting method, through microwave radiation procedure is extremely productive in terms of time consumption, cost effectiveness and environmental friendliness. In this study, conductive and thermally stable composite (mwXG-g-PANi) was synthesized by grafting of aniline (ANi) on to xanthan gum (XG) using catalytic weight of initiator, ammonium peroxydisulfate in the process of microwave irradiation in an aqueous medium. The synthesis of mwXG-g-PANi were confirm by FTIR, XRD, TGA, and SEM. The influence of altering the microwave power, exposure time of microwave, concentration of monomer and the amount of initiator of graft polymerization were studied over the grafting parameters, for example, grafting percentage (%G) and grafting efficiency (%E). The maximum %G and %E achieved was 172 and 74.13 respectively. The outcome demonstrates that the microwave irradiation strategy can increase the reaction rate by 72 times over the conventional method. Electrical conductivity of XG and mwXG-g-PANi composite film was performed. The fabricated grafted sample film were then examined for the chemical sensor. The mwXG-g-PANi, effectively integrated and handled, are NH3 sensitive and exhibit a rapid sensing in presence of NH3 vapor. Chemiresistive NH3 sensors with superior room temperature sensing performance were produced with sensor response of 905 at 1ppb and 90% recovery within few second. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Investigation on the mechanical properties of palm-based flexible polyurethane foam

    NASA Astrophysics Data System (ADS)

    On, Ahmad Zuhdi Mohd; Badri, Khairiah Haji

    2015-09-01

    A series of modification polyurethane (PU) system was prepared by introducing palm kernel based polyol (PKO-p) to progressively replaced commercial polyether polyol from petrochemical based material. This paper describes the effect of PKO-p on the physical-mechanical properties of polyurethane foams. Stress-strain analysis in tensile mode was conducted with physicochemical analysis by performing Fourier transform infrared (FTIR). The morphological studies were observed by the optical microscope. The foam showed an increment on the modulus up to 458.3kPa as more incorporation of PKO-p introduced to the system. In contrast, tensile strength of PU foam depicted the highest up to 162 kPa at 60:40. The elongation at break showed decrement as the composition of the renewable polyol increased to a ratio 60/40 of PKO-p to petrochemical based polyol.

  7. Conversion of calibration curves for accurate estimation of molecular weight averages and distributions of polyether polyols by conventional size exclusion chromatography.

    PubMed

    Xu, Xiuqing; Yang, Xiuhan; Martin, Steven J; Mes, Edwin; Chen, Junlan; Meunier, David M

    2018-08-17

    Accurate measurement of molecular weight averages (M¯ n, M¯ w, M¯ z ) and molecular weight distributions (MWD) of polyether polyols by conventional SEC (size exclusion chromatography) is not as straightforward as it would appear. Conventional calibration with polystyrene (PS) standards can only provide PS apparent molecular weights which do not provide accurate estimates of polyol molecular weights. Using polyethylene oxide/polyethylene glycol (PEO/PEG) for molecular weight calibration could improve the accuracy, but the retention behavior of PEO/PEG is not stable in THF-based (tetrahydrofuran) SEC systems. In this work, two approaches for calibration curve conversion with narrow PS and polyol molecular weight standards were developed. Equations to convert PS-apparent molecular weight to polyol-apparent molecular weight were developed using both a rigorous mathematical analysis and graphical plot regression method. The conversion equations obtained by the two approaches were in good agreement. Factors influencing the conversion equation were investigated. It was concluded that the separation conditions such as column batch and operating temperature did not have significant impact on the conversion coefficients and a universal conversion equation could be obtained. With this conversion equation, more accurate estimates of molecular weight averages and MWDs for polyether polyols can be achieved from conventional PS-THF SEC calibration. Moreover, no additional experimentation is required to convert historical PS equivalent data to reasonably accurate molecular weight results. Copyright © 2018. Published by Elsevier B.V.

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

    PubMed Central

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

    2018-01-01

    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 °C (25 W of microwave power) for 5 min. The deprotection reactions were carried out at 75 °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. PMID:20057380

  9. Microwave-assisted extraction of oxymatrine from Sophora flavescens.

    PubMed

    Xia, En-Qin; Cui, Bo; Xu, Xiang-Rong; Song, Yang; Ai, Xu-Xia; Li, Hua-Bin

    2011-08-30

    In this paper, microwave-assisted extraction (MAE) of oxymatrine from Sophora flavescens were studied by HPLC-photodiode array detection. Effects of several experimental parameters, such as concentration of extraction solvent, ratio of liquid to material, microwave power, extraction temperature, and extraction time on the extraction efficiencies of oxymatrine were evaluated. The optimal extraction conditions were 60% ethanol, a 20:1 (v/v) ratio of liquid to material and extraction for 10 min at 50 °C under 500 W microwave irradiation. Under the optimum conditions, the yield of oxymatrine was 14.37 mg/g. The crude extract obtained could be used as either a component of some complex traditional medicines or for further isolation and purification of bioactive compounds. The results, which indicated that MAE is a very useful tool for the extraction of important phytochemicals from plant materials, should prove helpful for the full utilization of Sophora flavescens.

  10. 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 ( r ² > 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.

  11. The Use of Mouse Models of Breast Cancer and Quantitative Image Analysis to Evaluate Hormone Receptor Antigenicity after Microwave-assisted Formalin Fixation

    PubMed Central

    Engelberg, Jesse A.; Giberson, Richard T.; Young, Lawrence J.T.; Hubbard, Neil E.

    2014-01-01

    Microwave methods of fixation can dramatically shorten fixation times while preserving tissue structure; however, it remains unclear if adequate tissue antigenicity is preserved. To assess and validate antigenicity, robust quantitative methods and animal disease models are needed. We used two mouse mammary models of human breast cancer to evaluate microwave-assisted and standard 24-hr formalin fixation. The mouse models expressed four antigens prognostic for breast cancer outcome: estrogen receptor, progesterone receptor, Ki67, and human epidermal growth factor receptor 2. Using pathologist evaluation and novel methods of quantitative image analysis, we measured and compared the quality of antigen preservation, percentage of positive cells, and line plots of cell intensity. Visual evaluations by pathologists established that the amounts and patterns of staining were similar in tissues fixed by the different methods. The results of the quantitative image analysis provided a fine-grained evaluation, demonstrating that tissue antigenicity is preserved in tissues fixed using microwave methods. Evaluation of the results demonstrated that a 1-hr, 150-W fixation is better than a 45-min, 150-W fixation followed by a 15-min, 650-W fixation. The results demonstrated that microwave-assisted formalin fixation can standardize fixation times to 1 hr and produce immunohistochemistry that is in every way commensurate with longer conventional fixation methods. PMID:24682322

  12. 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. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Magnetisation switching of ECC grains in microwave-assisted magnetic recording

    NASA Astrophysics Data System (ADS)

    Greaves, Simon John; Muraoka, Hiroaki; Kanai, Yasushi

    2018-05-01

    Microwave-assisted magnetic recording was investigated using a planar write head and exchange-coupled composite (ECC) media. When recording on ECC media using a planar head field distribution and the high frequency field generated by a spin torque oscillator it was possible to switch the media magnetisation into the opposite direction to the head field, i.e. the media effectively had a negative coercive field. The conditions for this effect to occur are discussed.

  14. Molecular interactions in the betaine monohydrate-polyol deep eutectic solvents: Experimental and computational studies

    NASA Astrophysics Data System (ADS)

    Zahrina, Ida; Mulia, Kamarza; Yanuar, Arry; Nasikin, Mohammad

    2018-04-01

    DES (deep eutectic solvents) are a new class of ionic liquids that have excellent properties. The strength of interaction between molecules in the DES affects their properties and applications. In this work, the strength of molecular interactions between components in the betaine monohydrate salt and polyol (glycerol or/and propylene glycol) eutectic mixtures was studied by experimental and computational studies. The melting point and fusion enthalpy of the mixtures were measured using STA (Simultaneous Thermal Analyzer). The nature and strength of intermolecular interactions were observed by FT-IR and NMR spectroscopy. The molecular dynamics simulation was used to determine the number of H-bonds, percent occupancy, and radial distribution functions in the eutectic mixtures. The interaction between betaine monohydrate and polyol is following order: betaine monohydrate-glycerol-propylene glycol > betaine monohydrate-glycerol > betaine monohydrate-propylene glycol, where the latter is the eutectic mixture with the lowest stability, strength and extent of the hydrogen bonding interactions between component molecules. The presence of intra-molecular hydrogen bonding interactions, the inter-molecular hydrogen bonding interactions between betaine molecule and polyol, and also interactions between polyol and H2O of betaine monohydrate in the eutectic mixtures.

  15. Controlled Microwave Heating Accelerates Rolling Circle Amplification.

    PubMed

    Yoshimura, Takeo; Suzuki, Takamasa; Mineki, Shigeru; Ohuchi, Shokichi

    2015-01-01

    Rolling circle amplification (RCA) generates single-stranded DNAs or RNA, and the diverse applications of this isothermal technique range from the sensitive detection of nucleic acids to analysis of single nucleotide polymorphisms. Microwave chemistry is widely applied to increase reaction rate as well as product yield and purity. The objectives of the present research were to apply microwave heating to RCA and indicate factors that contribute to the microwave selective heating effect. The microwave reaction temperature was strictly controlled using a microwave applicator optimized for enzymatic-scale reactions. Here, we showed that microwave-assisted RCA reactions catalyzed by either of the four thermostable DNA polymerases were accelerated over 4-folds compared with conventional RCA. Furthermore, the temperatures of the individual buffer components were specifically influenced by microwave heating. We concluded that microwave heating accelerated isothermal RCA of DNA because of the differential heating mechanisms of microwaves on the temperatures of reaction components, although the overall reaction temperatures were the same.

  16. 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-C 3 N 4 ) with decreased structural imperfections benefits from the suppression of electron-hole recombination, which enhances its hydrogen generation activity. However, producing such g-C 3 N 4 materials by conventional heating in an electric furnace has proven challenging. Herein, we report on the synthesis of high-quality g-C 3 N 4 with reduced structural defects by judiciously combining the implementation of melamine-cyanuric acid (MCA) supramolecular aggregates and microwave-assisted thermolysis. The g-C 3 N 4 material produced after optimizing the microwave reaction time can effectively generate H 2 under visible-light irradiation. The highest H 2 evolution rate achieved was 40.5 μmol h -1 , which is two times higher than that of a g-C 3 N 4 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-C 3 N 4 photocatalysts. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Ultrasound/microwave-assisted solid-liquid-solid dispersive extraction with high-performance liquid chromatography coupled to tandem mass spectrometry for the determination of neonicotinoid insecticides in Dendrobium officinale.

    PubMed

    Zheng, Shuilian; Wu, Huizhen; Li, Zuguang; Wang, Jianmei; Zhang, Hu; Qian, Mingrong

    2015-01-01

    A one-step ultrasound/microwave-assisted solid-liquid-solid dispersive extraction procedure was used for the simultaneous determination of eight neonicotinoids (dinotefuran, nitenpyram, thiamethoxam, clothianidin, imidacloprid, acetamiprid, thiacloprid, imidaclothiz) in dried Dendrobium officinale by liquid chromatography combined with electrospray ionization triple quadrupole tandem mass spectrometry in multiple reaction monitoring mode. The samples were quickly extracted by acetonitrile and cleaned up by the mixed dispersing sorbents including primary secondary amine, C18 , and carbon-GCB. Parameters that could influence the ultrasound/microwave-assisted extraction efficiency such as microwave irradiation power, ultrasound irradiation power, temperature, and solvent were investigated. Recovery studies were performing well (70.4-113.7%) at three examined spiking levels (10, 50, and 100 μg/kg). Meanwhile, the limits of quantification for the neonicotinoids ranged from 0.87 to 1.92 μg/kg. The method showed good linearity in the concentration range of 1-100 μg/L with correlation coefficients >0.99. This quick and useful analytical method could provide a basis for monitoring neonicotinoid insecticide residues in herbs. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Microwave-assisted micellar extraction of organic and inorganic iodines using zwitterionic surfactants.

    PubMed

    Wang, Shu-Ling; Yi, Ling; Ye, Li-Hong; Cao, Jun; Du, Li-Jing; Peng, Li-Qing; Xu, Jing-Jing; Zhang, Qi-Dong

    2017-08-04

    Zwitterionic surfactant, used as extractant in microwave-assisted extraction (MAE) was investigated for the first time to extract organic and inorganic iodines from kelp samples. Optimized conditions for the MAE were 200W of microwave irradiation power, 100°C of extraction temperature, 10min of microwave irradiation time, 1g of sample, and 20mL of solvent volume. Ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF/MS) was used for the quantitative and qualitative analyses of the iodines. Under the optimum experimental conditions, KI, MIT and DIT were identified in kelp samples, the limits of detection of these analytes were ranged between 3.39 and 6.31ng/mL. The recoveries for spiked samples obtained from different areas were all higher than 92.48%. Compared with the ultrasound-assisted extraction, the proposed method is faster and more effective. Thus, the combination of zwitterionic surfactant-MAE and UHPLC-Q-TOF/MS made up a simple, rapid and effective approach for extraction and determination of iodine compounds in complex seaweed materials. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Microwave-assisted rapid synthesis of birnessite-type MnO{sub 2} nanoparticles for high performance supercapacitor applications

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

    Zhang, Xiong; Miao, Wang; Li, Chen

    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 measurementsmore » 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.« less

  20. Nanosize Fe x O y @SBA-3: A Comparative Study Between Conventional and Microwave Assisted Synthesis.

    PubMed

    Barik, Sunita; Badamali, Sushanta K; Sahoo, Sagarika; Behera, Nandakishor; Dapurkar, Sudhir E

    2018-01-01

    The present study is focussed on development of highly dispersed nanosize iron oxide (FexOy) particles within the uniform mesopore channels of SBA-3. Herein we report a comparative study between conventional incipient wetness and microwave assisted synthesis routes adopted to devise nanoparticles. The developed materials are characterised by following X-ray diffraction, high resolution transmission electron microscopy, proton induced X-ray emission, diffuse reflectance UV-visible spectroscopy, thermogravimetry and Fourier transform infrared spectroscopy. Mesoporous siliceous SBA-3 was prepared at room temperature to obtain samples with good crystallinity and ordered pore structure. Pore channels of SBA-3 were used as nanoreactor for developing iron oxide nanoparticles. Iron oxide nanoparticles developed under microwave activation showed uniform distribution within the SBA-3 structure along with retaining the orderness of the pore architecture. On the contrary, iron oxides developed under incipient wetness method followed by conventional heating resulted in agglomeration of nanoparticles along with significant loss in SBA-3 pore structure. Proton induced X-ray emission studies revealed the extremely high purity of the samples and almost thrice higher amount of iron oxide particles are encapsulated within the host by microwave assisted preparation as compared to incipient/conventional heating method.

  1. Microwave-assisted Maillard reactions for the preparation of advanced glycation end products (AGEs).

    PubMed

    Visentin, Sonja; Medana, Claudio; Barge, Alessandro; Giancotti, Valeria; Cravotto, Giancarlo

    2010-05-21

    The application of microwaves as an efficient form of volumetric heating to promote organic reactions was recognized in the mid-1980 s. It has a much longer history in the food research and industry where microwave irradiation was studied in depth to optimize food browning and the development of desirable flavours from Maillard reactions. The microwave-promoted Maillard reaction is a challenging synthetic method to generate molecular diversity in a straightforward way. In this paper we present a new rapid and efficient one-pot procedure for the preparation of pentosidine and other AGEs under microwave irradiation.

  2. 40 CFR 63.1433 - Wastewater provisions.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 12 2012-07-01 2011-07-01 true Wastewater provisions. 63.1433 Section... for Hazardous Air Pollutant Emissions for Polyether Polyols Production § 63.1433 Wastewater provisions. (a) Process wastewater. Except as specified in paragraph (c) of this section, the owner or operator...

  3. 40 CFR 63.1433 - Wastewater provisions.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 11 2011-07-01 2011-07-01 false Wastewater provisions. 63.1433 Section... for Hazardous Air Pollutant Emissions for Polyether Polyols Production § 63.1433 Wastewater provisions. (a) Process wastewater. Except as specified in paragraph (c) of this section, the owner or operator...

  4. Structure and magnetic properties of Fe-Co nanoparticles prepared by polyol method

    NASA Astrophysics Data System (ADS)

    Lam, Nguyen Mau; Thi, Tran Minh; Thanh, Pham Thi; Yen, Nguyen Hai; Dan, Nguyen Huy

    2018-03-01

    Fe100-xCox (x = 25 - 45) nanoparticles have been successfully prepared from FeCl2 and Co(C2H3O2)2 by thermal decomposition process in solution of polyethylene glycol and NaOH (polyol method). The influence of pH level and Co concentration on structure and magnetic properties of the Fe-Co nanoparticles were investigated. The X-Ray Diffraction (XRD) results confirm the formation of a body centered cubic single phase of the Fe(Co) nanoparticles. The Scanning Electron Microscopy (SEM) images show the grain size of the samples is about 60 nm. Saturation magnetization the Fe-Co nanoparticles strongly depends on the Co concentration and pH level in the fabrication process. The optimal pH level and Co concentration for the Fe-Co nanoparticles were found to be 7 and 35 at%, respectively. A quite high saturation magnetization of 228 emu/g has been achieved for the Fe-Co nanoparticles.

  5. Alternative energy input: Mechanochemical, microwave and ultrasound-assisted organic synthesis

    EPA Science Inventory

    Microwave, ultrasound, sunlight and mechanochemical mixing can be used to augment conventional laboratory techniques. By applying these alternative means of activation, a number of chemical transformations have been achieved thereby improving many existing protocols with superi...

  6. Urchin-like CdS/ZrO2 nanocomposite prepared by microwave-assisted hydrothermal combined with ion-exchange and its multimode photocatalytic activity

    NASA Astrophysics Data System (ADS)

    Li, Li; Wang, Lili; Zhang, Wenzhi; Zhang, Xiuli; Chen, Xi; Dong, Xue

    2014-12-01

    A series of urchin-like CdS/ZrO2 nanocomposites with different mole ratios of Cd/Zr were prepared by a two-step method combining the microwave-assisted hydrothermal and ion exchange methods. The products were characterized by X-ray diffraction, ultraviolet-visible diffuse reflectance spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscopy, and N2 adsorption-desorption measurements. The results of the study revealed that the CdS/ZrO2 nanocomposites had mixed phases of tetragonal ZrO2 and hexagonal CdS. Moreover, the samples prepared by the microwave-assisted hydrothermal method possessed the urchin-like structure with a surface composed of protrude-like nanoparticles in large quantities. The absorption in the visible region changed slightly with increasing mole ratio of Cd/Zr. Moreover, compared to the nanocomposites prepared by the conventional heating, the nanocomposites prepared by the microwave-assisted hydrothermal synthesis showed significantly different Brunauer-Emmett-Teller values, and the urchin-like CdS/ZrO2 structures were obtained. The photocatalytic degradation of methyl orange under ultraviolet (UV) light irradiation indicated that the photocatalytic activity of the CdS/ZrO2 nanocomposite with CdS/ZrO2 molar ratio of 30 % was higher than those of CdS, ZrO2, and other different ratios of CdS/ZrO2 nanocomposites. Moreover, under UV light, visible light, and microwave-assisted multimode photocatalytic degradation, the urchin-like CdS/ZrO2 nanocomposites significantly affected the photodegradation of various dyes. To understand the possible reaction mechanism of the photocatalysis by the CdS/ZrO2 nanocomposites, a series of controlled experiments were performed, and the stability and reusability of the CdS/ZrO2 nanocomposites were further investigated by the photocatalytic reaction.

  7. Dietary sorbitol and mannitol: food content and distinct absorption patterns between healthy individuals and patients with irritable bowel syndrome.

    PubMed

    Yao, C K; Tan, H-L; van Langenberg, D R; Barrett, J S; Rose, R; Liels, K; Gibson, P R; Muir, J G

    2014-04-01

    Sorbitol and mannitol are naturally-occurring polyol isomers. Although poor absorption and induction of gastrointestinal symptoms by sorbitol are known, the properties of mannitol are poorly described. We aimed to expand data on food composition of these polyols, and to compare their absorptive capacities and symptom induction in patients with irritable bowel syndrome (IBS) and healthy individuals. Food samples were analysed for sorbitol and mannitol content. The degree of absorption measured by breath hydrogen production and gastrointestinal symptoms (visual analogue scales) was evaluated in a randomised, double-blinded, placebo-controlled study in 21 healthy and 20 IBS subjects after challenges with 10 g of sorbitol, mannitol or glucose. Certain fruits and sugar-free gum contained sorbitol, whereas mannitol content was higher in certain vegetables. Similar proportions of patients with IBS (40%) and healthy subjects (33%) completely absorbed sorbitol, although more so with IBS absorbed mannitol (80% versus 43%; P = 0.02). Breath hydrogen production was similar in both groups after lactulose but was reduced in patients with IBS after both polyols. No difference in mean (SEM) hydrogen production was found in healthy controls after sorbitol [area-under-the-curve: 2766 (591) ppm 4 h(-1) ] or mannitol [2062 (468) ppm 4 h(-1) ] but, in patients with IBS, this was greater after sorbitol [1136 (204) ppm 4 h(-1) ] than mannitol [404 (154) ppm 4 h(-1) ; P = 0.002]. Overall gastrointestinal symptoms increased significantly after both polyols in patients with IBS only, although they were independent of malabsorption of either of the polyols. Increased and discordant absorption of mannitol and sorbitol occurs in patients with IBS compared to that in healthy controls. Polyols induced gastrointestinal symptoms in patients with IBS independently of their absorptive patterns, suggesting that the dietary restriction of polyols may be efficacious. © 2013 The British Dietetic Association Ltd.

  8. Advancement of green process through microwave-assisted extraction of bioactive metabolites from Arthrospira Platensis and bioactivity evaluation.

    PubMed

    Esquivel-Hernández, Diego A; Rodríguez-Rodríguez, José; Rostro-Alanis, Magdalena; Cuéllar-Bermúdez, Sara P; Mancera-Andrade, Elena I; Núñez-Echevarría, Jade E; García-Pérez, J Saúl; Chandra, Rashmi; Parra-Saldívar, Roberto

    2017-01-01

    Bioactivity and functional properties of cyanobacterial extract mostly depends on process of extraction, temperature and solvent used (polar or non-polar). To evaluate these parameters a design of experiment (DOE; using a 2 k design) was performed with Arthrospira platensis. Extraction process was optimized through microwave-assisted extraction considering solvent ratio, temperature and time of extraction with polar (PS) and non-polar (NPS). Maximum extract yield obtained was 4.32±0.25% and 5.26±0.11% (w/w) respectively for PS and NPS. Maximum content of bioactive metabolites in PS extracts were thiamine (846.57±14.12μg/g), riboflavin (101.09±1.63μg/g), C-phycocyanin (2.28±0.10μg/g) and A-phycocyanin (4.11±0.03μg/g), while for NPS extracts were α-tocopherol (37.86±0.78μg/g), β-carotene (123.64±1.45μg/g) and 19.44±0.21mg/g of fatty acids. A. platensis PS extracts showed high antimicrobial activity and PS extracts had antioxidant activity of 0.79±0.12μmolTE/g for FRAP assay, while for NPS extracts 1.03±0.08μmol α-TE/g for FRAP assay. Copyright © 2016. Published by Elsevier Ltd.

  9. Rapid microwave-assisted preparation of binary and ternary transition metal sulfide compounds

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

    Butala, Megan M.; Perez, Minue A.; Arnon, Shiri

    Transition metal chalcogenides are of interest for energy applications, including energy generation in photoelectrochemical cells and as electrodes for next-generation electrochemical energy storage. Synthetic routes for such chalcogenides typically involve extended heating at elevated temperatures for multiple weeks. We demonstrate here the feasibility of rapidly preparing select sulfide compounds in a matter of minutes, rather than weeks, using microwave-assisted heating in domestic microwaves. We report the preparations of phase pure FeS2, CoS2, and solid solutions thereof from the elements with only 40 min of heating. Conventional furnace and rapid microwave preparations of CuTi2S4 both result in a majority of themore » targeted phase, even with the significantly shorter heating time of 40 min for microwave methods relative to 12 days using a conventional furnace. The preparations we describe for these compounds can be extended to related structures and chemistries and thus enable rapid screening of the properties and performance of various compositions of interest for electronic, optical, and electrochemical applications.« less

  10. Microwave-assisted extraction of silkworm pupal oil and evaluation of its fatty acid composition, physicochemical properties and antioxidant activities.

    PubMed

    Hu, Bin; Li, Cheng; Zhang, Zhiqing; Zhao, Qing; Zhu, Yadong; Su, Zhao; Chen, Yizi

    2017-09-15

    Microwave-assisted extraction (MAE) of oil from silkworm pupae was firstly performed in the present research. The response surface methodology was applied to optimize the parameters for MAE. The yield of oil by MAE was 30.16% under optimal conditions of a mixed solvent consisting of ethanol and n-hexane (1:1, v/v), microwave power (360W), liquid to solid ratio (7.5/1mL/g), microwave time (29min). Moreover, oil extracted by MAE was quantitatively (yield) and qualitatively (fatty acid profile) similar to those obtained using Soxhlet extraction (SE), but oil extracted by MAE exhibited favourable physicochemical properties and oxidation stability. Additionally, oil extracted by MAE had a higher content of total phenolic, and it showed stronger antioxidant activities. Scanning electron microscopy revealed that microwave technique efficiently promoted the release of oil by breaking down the cell structure of silkworm pupae. Therefore, MAE can be an effective method for the silkworm pupal oil extraction. Copyright © 2017 Elsevier Ltd. All rights reserved.

  11. Microwave-assisted Stille-coupling of steroidal substrates.

    PubMed

    Skoda-Földes, Rita; Pfeiffer, Péter; Horváth, Judit; Tuba, Zoltán; Kollár, László

    2002-07-01

    Steroidal dienes were synthesised by Stille-coupling of the corresponding alkenyl iodides with vinyltributyltin under microwave irradiation in a domestic microwave oven in drastically reduced reaction times. Rate acceleration was observed also in the one-pot Stille-coupling-Diels-Alder reaction of 17-iodo-5alpha-androst-16-ene. Stereoselectivity of cycloaddition was slightly improved with diethyl maleate as the dienophile, compared to that achieved with thermal heating.

  12. Rapid synthesis of flower shaped Cu{sub 2}ZnSnS{sub 4} nanoparticles by microwave irradiation for solar cell application

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

    Ansari, Mohd Zubair, E-mail: mhd.zubair1@gmail.com; Khare, Neeraj

    Single phase Cu{sub 2}ZnSnS{sub 4} (CZTS) nanoparticles have been synthesized by the microwave-assisted solution method in a one step process. Structural, morphological and optical characterizations of the CZTS nanoparticles have been carried out. X-ray diffraction confirms the single phase formation of CZTS nanoparticles with kesterite structure. SEM confirms the homogenous distribution of CZTS nanoparticles flower like assemblies. High resolution TEM image confirms the good crystallinity of the CZTS nanoparticles with the average grain size ~20 nm. The CZTS nanoparticles have strong optical absorption in the visible region with direct band gap as ~1.6 eV which is optimal for photovoltaic application.

  13. Self-excitation of microwave oscillations in plasma-assisted slow-wave oscillators by an electron beam with a movable focus

    NASA Astrophysics Data System (ADS)

    Bliokh, Yu. P.; Nusinovich, G. S.; Shkvarunets, A. G.; Carmel, Y.

    2004-10-01

    Plasma-assisted slow-wave oscillators (pasotrons) operate without external magnetic fields, which makes these devices quite compact and lightweight. Beam focusing in pasotrons is provided by ions, which appear in the device due to the impact ionization of a neutral gas by beam electrons. Typically, the ionization time is on the order of the rise time of the beam current. This means that, during the rise of the current, beam focusing by ions becomes stronger. Correspondingly, a beam of electrons, which was initially diverging radially due to the self-electric field, starts to be focused by ions, and this focus moves towards the gun as the ion density increases. This feature makes the self-excitation of electromagnetic (em) oscillations in pasotrons quite different from practically all other microwave sources where em oscillations are excited by a stationary electron beam. The process of self-excitation of em oscillations has been studied both theoretically and experimentally. It is shown that in pasotrons, during the beam current rise the amount of current entering the interaction space and the beam coupling to the em field vary. As a result, the self-excitation can proceed faster than in conventional microwave sources with similar operating parameters such as the operating frequency, cavity quality-factor and the beam current and voltage.

  14. Metal-assisted and microwave accelerated-evaporative crystallization: Application to lysozyme protein

    NASA Astrophysics Data System (ADS)

    Mauge-Lewis, Kevin

    In response to the growing need for new crystallization techniques that afford for rapid processing times along with control over crystal size and distribution, the Aslan Research Group has recently demonstrated the use of Metal-Assisted and Microwave-Accelerated Evaporative Crystallization MA-MAEC technique in conjunction with metal nanoparticles and nanostructures for the crystallization of amino acids and organic small molecules. In this study, we have employed the newly developed MA-MAEC technique to the accelerated crystallization of chicken egg-white lysozyme on circular crystallization platforms in order to demonstrate the proof-of-principle application of the method for protein crystallization. The circular crystallization platforms are constructed in-house from poly (methyl methacrylate) (PMMA) and silver nanoparticle films (SNFs), indium tin oxide (ITO) and iron nano-columns. In this study, we prove the MA-MAEC method to be a more effective technique in the rapid crystallization of macromolecules in comparison to other conventional methods. Furthermore, we demonstrate the use of the novel iCrystal system, which incorporates the use of continuous, low wattage heating to facilitate the rapid crystallization of the lysozyme while still retaining excellent crystal quality. With the incorporation of the iCrystal system, we observe crystallization times that are even shorter than those produced by the MA-MAEC technique using a conventional microwave oven in addition to significantly improved crystal quality.

  15. HIGHLY DIASTEREOSELECTIVE MICHAEL REACTION UNDER SOLVENT-FREE CONDITIONS USING MICROWAVES: CONJUGATE ADDITION OF FLAVANONE TO ITS CHALCONE PRECURSOR

    EPA Science Inventory

    Microwave-assisted reaction of 2'-hydroxychalcones in the presence of DBU resulted in the formation of hitherto unknown dimers by conjugate addition of the intermediate cyclic ketone to the starting enone.

  16. AN EXPEDITIOUS SOLVENT-FREE ROUTE TO IONIC LIQUIDS USING MICROWAVES

    EPA Science Inventory

    A microwave-assisted preparation of a series of ambient temperature ionic liquids, 1-alkyl-3-methyl imidazolium (IMIM) halides, that proceeds via efficient raction of 1-methyl imidazole with alkylhalides/terminal dihalides under solvent-free conditions, is described.

  17. CARBON NANOTUBES IN MICROWAVE ENVIRONMENT-IGNITION AND RECONSTRUCTION

    EPA Science Inventory

    The unusual property of single-walled carbon nanotubes (SWNT), multi-wall (MWNT) nanotubes and Buckminsterfullerene (C-60) is observed upon exposure to microwave-assisted ignition. Carbon nanotubes known for a range of mechanical and electronic properties because of their unique...

  18. Fiber-optic control and thermometry of single-cell thermosensation logic.

    PubMed

    Fedotov, I V; Safronov, N A; Ermakova, Yu G; Matlashov, M E; Sidorov-Biryukov, D A; Fedotov, A B; Belousov, V V; Zheltikov, A M

    2015-11-13

    Thermal activation of transient receptor potential (TRP) cation channels is one of the most striking examples of temperature-controlled processes in cell biology. As the evidence indicating the fundamental role of such processes in thermosensation builds at a fast pace, adequately accurate tools that would allow heat receptor logic behind thermosensation to be examined on a single-cell level are in great demand. Here, we demonstrate a specifically designed fiber-optic probe that enables thermal activation with simultaneous online thermometry of individual cells expressing genetically encoded TRP channels. This probe integrates a fiber-optic tract for the delivery of laser light with a two-wire microwave transmission line. A diamond microcrystal fixed on the fiber tip is heated by laser radiation transmitted through the fiber, providing a local heating of a cell culture, enabling a well-controlled TRP-assisted thermal activation of cells. Online local temperature measurements are performed by using the temperature-dependent frequency shift of optically detected magnetic resonance, induced by coupling the microwave field, delivered by the microwave transmission line, to nitrogen--vacancy centers in the diamond microcrystal. Activation of TRP channels is verified by using genetically encoded fluorescence indicators, visualizing an increase in the calcium flow through activated TRP channels.

  19. Deproteinated palm kernel cake-derived oligosaccharides: A preliminary study

    NASA Astrophysics Data System (ADS)

    Fan, Suet Pin; Chia, Chin Hua; Fang, Zhen; Zakaria, Sarani; Chee, Kah Leong

    2014-09-01

    Preliminary study on microwave-assisted hydrolysis of deproteinated palm kernel cake (DPKC) to produce oligosaccharides using succinic acid was performed. Three important factors, i.e., temperature, acid concentration and reaction time, were selected to carry out the hydrolysis processes. Results showed that the highest yield of DPKC-derived oligosaccharides can be obtained at a parameter 170 °C, 0.2 N SA and 20 min of reaction time.

  20. Optimization and Performance parameters for adsorption of Cr6+ by microwave assisted carbon from Sterculia foetida shells

    NASA Astrophysics Data System (ADS)

    Gnanasundaram, N.; Loganathan, M.; Singh, A.

    2017-06-01

    Modeling of adsorption of Cr6+ on to activated carbon prepared from Sterculia foetida dried seed shells under different drying techniques namely sun, oven, and microwave drying (450W, 600W, 900W power). Optimization of process parameters such as pH, adsorbent dosage (g/ml), temperature (°C), contact time (min) were evaluated using Central Composite Rotatable Design (CCRD) of Response Surface Methodology (RSM). For batch adsorption studies at pH 3, adsorbent dosage of 1.5 g/ml, temperature 35°C and contact time 90 min were found to be optimum for the system under consideration and Microwave Activated Carbonized Sterculia foetida (MACSF) at 450W was found to be best suited for the adsorption of Cr+6 ions. The system was found to follow Langmuir type monolayer adsorption for the given operational parameters. SEM analysis was used to study the surface morphology of the carbon samples and the effect of pretreatment on carbonization.

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