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Sample records for microwave assisted tandem

  1. Microwave-assisted extraction and large-volume injection gas chromatography tandem mass spectrometry determination of multiresidue pesticides in edible seaweed.

    Science.gov (United States)

    García-Rodríguez, D; Carro, A M; Cela, R; Lorenzo, R A

    2010-09-01

    A microwave-assisted extraction method followed by clean-up with solid-phase extraction (SPE) combined with large-volume injection gas chromatography-tandem mass spectrometry (LVI-GC-MS/MS) for the analysis of 17 pesticides in wild and aquaculture edible seaweeds has been developed. An experimental central composite design was employed to evaluate the effects of the main variables potentially affecting the extraction (temperature, time, and solvent volume) and to optimize the process. The most effective microwave extraction conditions were achieved at 125 °C and 12 min with 24 mL of hexane/ethyl acetate (80:20). SPE clean-up of the extracts with graphitized carbon and Florisil, optimized by means of the experimental design, proved to be efficient in the removal of matrix interferences. The analytical recoveries were close to 100% for all the analytes, with relative standard deviations lower than 13%. The limits of detection ranged from 0.3 to 23.1 pg g(-1) and the limits of quantification were between 2.3 and 76.9 pg g(-1), far below the maximum residue levels established by the European Union for pesticides in seaweed. The results obtained prove the suitability of the microwave-assisted extraction for the routine analysis of pesticides in aquaculture and wild seaweed samples.

  2. [Simultaneous determination of six organophosphorous flame retardants in textiles by gas chromatography-tandem mass spectrometry combined with microwave assisted extraction].

    Science.gov (United States)

    Wang, Chengyun; Li, Lixia; Xie, Tangtang; Zhang, Weiya; Liu, Caiming; Zhu, Naiqing

    2011-08-01

    An effective method was established for the simultaneous determination of six banned organophosphorous flame retardants in textiles by gas chromatography-tandem mass spectrometry (GC-MS/MS) combined with microwave assisted extraction (MAE). By investigating the extraction efficiency of 12 different extraction solvents for the target analytes, the optimal conditions were that the sample was extracted by microwave assisted extraction using acetone as the solvent at 76 degrees C for 30 min. Then the extract was analyzed by GC-MS/MS in multiple reaction monitoring (MRM) mode, and the concentration of each analyte was calibrated by external standard method. The linear ranges of tris-(1-aziridinyl) phosphine oxide (TEPA), tris-(2-chloroethyl) phosphate (TCEP), tris-(1,3-dichloropropyl) phosphate (TDCP), bis-(2,3-dibromopropyl) phosphate (DDBPP), tri-o-cresyl phosphate (TOCP) and tris-(2,3-dibromopropyl) phosphate (TRIS) were 9.17 - 366.80, 0.95 - 75.98, 1.04 - 83.20, 41.60 - 832.00, 3.80 - 75.90, and 40.48 - 809.60 microg/L, respectively, the correlation coefficients were not less than 0.997 5, while the limits of quantification (LOQ) (S/N = 10) were 3.0, 0.2, 0.3, 25.0, 2.5 and 29.0 microg/kg, respectively. The spiked recoveries varied from 82.62% to 96.88% with the relative standard deviations of 3.80% to 8.79%. The proposed method was successfully applied to the determination of organophosphorous flame retardants in eight commercial textiles. The experimental results demonstrated that the method developed is simple, rapid, sensitive and accurate, which could satisfy the demand of the analysis of banned organophosphorous flame retardants in textiles.

  3. Microwave-assisted extraction and determination of cyanuric acid residue in pet food samples by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Han, Chao; Zhou, Yongfang; Xia, Biqi; Zhu, Zhenou; Liu, Cuiping; Shen, Yan

    2011-02-01

    Cyanuric acid (CYA) is attracting more attention due to its potential toxicity. In the present work, microwave-assisted extraction method in combination with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was proposed for the determination of CYA in pet food samples. Among different solvents, diethylamine-acetonitrile-water mixture (1:5:4, v/v) was found to be the best one as the extractant due to the strong polarity of CYA in the pet food. An internal standard, (13) C(3) -labeled CYA, was used in the extractions. The separation was performed on a MERCK ZIC HILIC column (150 mm × 2.1 mm id, 5 μm) with gradient elution of 20 mM ammonium acetate solution-acetonitrile. CYA was well retained (Rt = 5.10 min) and eluted with good peak shape. The method could respond linearly with CYA at concentrations from 1.0 to 50 ng/mL with a quantification limit of 0.25 mg/kg. The intra- and inter-day precision was less than 4.0% and the recovery of the assay was in the range of 90.4-108.1%. In the analysis of practical spiked pet food samples, the new method yielded satisfactory results. Due to its simplicity and accuracy the straightforward method is particularly suitable for routine CYA detection. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Microwave-assisted extraction and determination of citrus red 2 dye in oranges and orange juice by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Han, Chao; Liu, Bin; Zhu, Zhenou; Huang, Fuzhen; Chen, Xiangzhun; Shen, Yan

    2012-12-01

    A fast, simple, low cost, and high-throughput method has been developed for the determination of citrus red 2 dye in orange and orange juice samples. The procedure is based on microwave-assisted extraction followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. The method was optimized, and the analyte was efficiently extracted from the samples in 30 min using hexane/acetone (v/v, 3 : 1). The method was validated and showed good linearity and selectivity. The limits of quantification (LOQs) were 5 μg/kg (sample size of 2 g) for both orange and orange juice samples. The average recoveries, measured at 3 concentration levels (5, 10, and 20 μg/kg), were in the range 77.5% to 87.6% for the compound tested with relative standard deviations below 7.3%. The proposed method is rapid, accurate, and could be utilized for the routine analysis of citrus red 2 dye in orange and orange juice samples.

  5. Facile Synthesis of 3-Substituted Isoquinolines Derivatives via Microwave-assisted Tandem Three-component Coupling Cyclization

    Institute of Scientific and Technical Information of China (English)

    林龙; 吴琼友; 黄绍维; 杨光富

    2012-01-01

    A novel three-component reaction of o-bromobenzaldehyde, terminal alkynes and tert-butyl amine has been established, which proceeded smoothly to give 3-substituted isoquinolines in good yields in the presence of palladium/copper catalysts under microwave irradiation.

  6. Microwave-assisted Chemical Transformations

    Science.gov (United States)

    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...

  7. Dual ultrasonic-assisted dispersive liquid-liquid microextraction coupled with microwave-assisted derivatization for simultaneous determination of 20(S)-protopanaxadiol and 20(S)-protopanaxatriol by ultra high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Zhao, Xian-En; Lv, Tao; Zhu, Shuyun; Qu, Fei; Chen, Guang; He, Yongrui; Wei, Na; Li, Guoliang; Xia, Lian; Sun, Zhiwei; Zhang, Shijuan; You, Jinmao; Liu, Shu; Liu, Zhiqiang; Sun, Jing; Liu, Shuying

    2016-03-11

    This paper, for the first time, reported a speedy hyphenated technique of low toxic dual ultrasonic-assisted dispersive liquid-liquid microextraction (dual-UADLLME) coupled with microwave-assisted derivatization (MAD) for the simultaneous determination of 20(S)-protopanaxadiol (PPD) and 20(S)-protopanaxatriol (PPT). The developed method was based on ultra high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) detection using multiple-reaction monitoring (MRM) mode. A mass spectrometry sensitizing reagent, 4'-carboxy-substituted rosamine (CSR) with high reaction activity and ionization efficiency was synthesized and firstly used as derivatization reagent. Parameters of dual-UADLLME, MAD and UHPLC-MS/MS conditions were all optimized in detail. Low toxic brominated solvents were used as extractant instead of traditional chlorinated solvents. Satisfactory linearity, recovery, repeatability, accuracy and precision, absence of matrix effect and extremely low limits of detection (LODs, 0.010 and 0.015ng/mL for PPD and PPT, respectively) were achieved. The main advantages were rapid, sensitive and environmentally friendly, and exhibited high selectivity, accuracy and good matrix effect results. The proposed method was successfully applied to pharmacokinetics of PPD and PPT in rat plasma.

  8. In-gel microwave-assisted acid hydrolysis of proteins combined with liquid chromatography tandem mass spectrometry for mapping protein sequences.

    Science.gov (United States)

    Sun, Difei; Wang, Nan; Li, Liang

    2014-01-07

    We report an enabling method for mapping the protein sequence with high sequence coverage. This method combines the high separation power of gel electrophoresis for protein separation with the high sequence coverage capability of microwave-assisted acid hydrolysis (MAAH) mass spectrometry (MS). In-gel MAAH using 25% trifluoroacetic acid was developed and optimized for degrading the gel-separated protein into small peptides suitable for tandem MS sequencing. For bovine serum albumin (BSA) (∼67 kDa), with 4 μg of protein loading onto a gel for separation, followed by excising the protein gel band for in-gel MAAH and then injecting ∼2 μg of the resultant peptides into a liquid chromatography quadrupole time-of-flight mass spectrometer for analysis, 689 ± 54 (n = 3) unique peptides were identified with a protein sequence coverage of 99 ± 1%. Both the number of peptides detected and sequence coverage decreased as the sample amount decreased, mainly due to background interference: 316 ± 59 peptides and 94 ± 3% coverage for 2 μg loading, 136 ± 19 and 76 ± 5% for 1 μg loading, and 30 ± 2 and 32 ± 2% for 0.5 μg loading. To demonstrate the general applicability of the method, 10 gel bands from gel electrophoresis of an albumin-depleted human plasma sample were excised for in-gel MAAH LC-MS analysis. In total, 19 relatively high abundance proteins with molecular weights ranging from ∼8 to ∼160 kD could be mapped with coverage of 100% for six proteins (MW 8759 to 68 425 Da), 96-98% for five proteins (MW 11 458 to 36 431 Da), 92% for three proteins (MW 15 971 to 36 431 Da), 80-87% for four proteins (MW 42 287 to 162 134 Da), and 56% for one protein (MW 51 358 Da). Finally, to demonstrate the applicability of the method for more detailed analysis of complex protein mixtures, two-dimensional (2D) gel electrophoresis was combined with in-gel MAAH, affinity purification, and LC-MS/MS to characterize six bovine alpha-S1-casein phosphoprotein

  9. Rapid analytical method for the determination of pesticide residues in sunflower seeds based on focused microwave-assisted Soxhlet extraction prior to gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Prados-Rosales, R C; Luque García, J L; Luque de Castro, M D

    2003-04-18

    A rapid analytical method for determination of organochlorine pesticide residues in sunflower seeds based on focused microwave-assisted Soxhlet extraction has been developed. The main factors affecting the extraction efficiency--namely microwave power, irradiation time, volume of extractant and number of cycles--were optimized by a two-level factorial fractional design. After extraction, a liquid-liquid extraction and a clean-up step including the use of Florisil macrocolumns were required prior to injection of the extracts into the chromatograph in order to isolate the pesticide residues from the lipid fraction of the original extract. The MS-MS ion preparation mode was selected due to the high sensitivity and selectivity it provides. Seed samples were used collected near a crop subjected to aerial pesticide application. Residues of hexachlorocyclohexane isomers and endosulfan were found in the seeds although they were not subjected to pesticide application, thus showing the spray-drift contamination. The validation of the proposed approach was carried out by comparison with the ISO 659-1988 reference extraction method obtaining similar, or even better efficiencies by the proposed approach.

  10. Microwave Assisted Drug Delivery

    DEFF Research Database (Denmark)

    Jónasson, Sævar Þór; Zhurbenko, Vitaliy; Johansen, Tom Keinicke

    2014-01-01

    In this work, the microwave radiation is adopted for remote activation of pharmaceutical drug capsules inside the human body in order to release drugs at a pre-determined time and location. An array of controllable transmitting sources is used to produce a constructive interference at a certain...... focus point inside the body, where the drugs are then released from the specially designed capsules. An experimental setup for microwave activation has been developed and tested on a body phantom that emulates the human torso. A design of sensitive receiving structures for integration with a drug...

  11. Microwave Assisted Drug Delivery

    DEFF Research Database (Denmark)

    Jónasson, Sævar Þór; Zhurbenko, Vitaliy; Johansen, Tom Keinicke

    2014-01-01

    In this work, the microwave radiation is adopted for remote activation of pharmaceutical drug capsules inside the human body in order to release drugs at a pre-determined time and location. An array of controllable transmitting sources is used to produce a constructive interference at a certain...... focus point inside the body, where the drugs are then released from the specially designed capsules. An experimental setup for microwave activation has been developed and tested on a body phantom that emulates the human torso. A design of sensitive receiving structures for integration with a drug...

  12. Multi-residue determination of micropollutants in Phragmites australis from constructed wetlands using microwave assisted extraction and ultra-high-performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Petrie, Bruce; Smith, Benjamin D; Youdan, Jane; Barden, Ruth; Kasprzyk-Hordern, Barbara

    2017-03-22

    In constructed wetlands micropollutants can be removed from water by phytoremediation. However, micropollutant uptake and metabolism by plants here is poorly understood due to the lack of good analytical approaches. Reported herein is the first methodology developed and validated for the multi-residue determination of 81 micropollutants (pharmaceuticals, personal care products and illicit drugs) in the emergent macrophyte Phragmites australis. The method involved extraction by microwave accelerated extraction (MAE), clean-up using off-line solid phase extraction and analysis by ultra-high-performance liquid chromatography tandem mass spectrometry. Development of the MAE method found the influence of studied variables on micropollutant recovery to be: extraction temperature > sample mass > solvent composition. Validation of the developed extraction protocol revealed method recoveries were in the range 80-120% for the majority of micropollutants. Method quantitation limits (MQLs) were generally <5 ng g(-1) dry weight demonstrating the sensitivity of the methodology. Application of the method to P. australis from a constructed wetland used to treat trickling filter effluent found 17 micropollutants above their MQL, up to concentrations of 200 ng g(-1). Other than uptake, the presence of several metabolites (carbamazepine 10,11 epoxide, desvenlafaxine, 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine, N-desmethyltramadol and norketamine) indicated metabolism within the plant may also occur. This new analytical methodology will enable a process mass balance of the constructed wetland to be attained for the first time, and thus help understand the role of phytoremediation in micropollutant removal by such systems.

  13. Trace determination of antibacterial pharmaceuticals in fishes by microwave-assisted extraction and solid-phase purification combined with dispersive liquid-liquid microextraction followed by ultra-high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Huang, Peiting; Zhao, Pan; Dai, Xinpeng; Hou, Xiaohong; Zhao, Longshan; Liang, Ning

    2016-02-01

    A novel pretreatment method involving microwave-assisted extraction and solid-phase purification combined with dispersive liquid-liquid microextraction (MAE-SPP-DLLME) followed by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was established for the simultaneous determination of six antibacterial pharmaceuticals including metronidazole, tinidazole, chloramphenicol, thiamphenicol, malachite green and crystal violet. The conditions of MAE were optimized using an orthogonal design and the optimal conditions were found to be 8mL for acetonitrile, 50°C for 5min. Then, neutral alumina column was employed in the solid-phase purification. Finally, the critical parameters affecting DLLME, including selection of extraction and dispersive solvent, adjustment of pH, salt concentration, extraction time, were investigated by single factor study. Under optimum conditions, good linearities (r>0.9991) and satisfied recoveries (Recoveries>87.0%, relative standard deviation (RSD)extraction followed by purification. The established method was sensitive, rapid, accurate and employable to simultaneously determine target analytes in farmed fish, river fish and marine fish.

  14. A high-throughput method based on microwave-assisted extraction and liquid chromatography-tandem mass spectrometry for simultaneous analysis of amphetamines, ketamine, opiates, and their metabolites in hair.

    Science.gov (United States)

    Chang, Yuan-Jhe; Chao, Mu-Rong; Chen, Su-Chin; Chen, Chih-Hong; Chang, Yan-Zin

    2014-04-01

    A total sample-preparation and analysis time of 50 min is required for the high-throughput method of hair analysis proposed in this paper. The method is applicable to analysis of drugs commonly used in Asia, and their metabolites--methamphetamine (MA), amphetamine (AMP), methylenedioxymethamphetamine (MDMA), methylenedioxyamphetamine (MDA), ketamine (K), norketamine (NK), dehydronorketamine (DHNK), 6-acetylmorphine (6-AM), morphine (MOR), and codeine (COD). Cut and weighed hair (10 mg) was incubated for 3 min with methanol-trifluoroacetic acid (TFA) during microwave-assisted extraction (MAE) at 700 W. The incubation solution was evaporated, the residue was reconstituted in deionized water-methanol, 99:1 (v/v), and 20 μL was injected on to a core-shell column (50 × 4.6 mm, 2.6 μm particle size) for liquid chromatographic-tandem mass spectrometric (LC-MS-MS) analysis. Gradient elution separation was performed in 8 min at a flow rate of 1 mL min(-1). No signal interfering with any of the analytes was found in fourteen blank hair samples from different sources. The limits of detection and quantification were 0.5 pg mg(-1) and 2.0 pg mg(-1), respectively, for MA, AMP, MDMA, MDA, K, NK, and DHNK, and 2.0 pg mg(-1) and 5.0 pg mg(-1), respectively, for 6-AM, MOR and COD. The linear range was between the LOQ and 1000 pg mg(-1), and the correlation coefficients were all greater than 0.999. Investigation of matrix effects revealed that all the analytes were suppressed by less than 20% and the standard deviation (SD) was always less than 7%. Recovery was always greater than 90% and the SD for each compound was less than 6%. Precision and accuracy for each analyte were within 15%. Eight authentic hair specimens from known drug abusers were successfully analyzed. Compared with traditional overnight incubation methods, the rapid 3-min extraction time achieved similar or greater extraction yields. Sample preparation by MAE was a reliable procedure for extraction of the

  15. Microwave-Assisted Olefin Metathesis

    Science.gov (United States)

    Nicks, François; Borguet, Yannick; Sauvage, Xavier; Bicchielli, Dario; Delfosse, Sébastien; Delaude, Lionel; Demonceau, Albert

    Since the first reports on the use of microwave irradiation to accelerate organic chemical transformations, a plethora of papers have been published in this field. In most examples, microwave heating has been shown to dramatically reduce reaction times, increase product yields, and enhance product purity by reducing unwanted side reactions compared to conventional heating methods. The present contribution aims at illustrating the advantages of this technology in olefin metathesis and, when data are available, at comparing microwave-heated and conventionally heated experiments

  16. Microwave assisted template synthesis of silver nanoparticles

    Indian Academy of Sciences (India)

    K J Sreeram; M Nidhin; B U Nair

    2008-12-01

    Easier, less time consuming, green processes, which yield silver nanoparticles of uniform size, shape and morphology are of interest. Various methods for synthesis, such as conventional temperature assisted process, controlled reaction at elevated temperatures, and microwave assisted process have been evaluated for the kind of silver nanoparticles synthesized. Starch has been employed as a template and reducing agent. Electron microscopy, photon correlation spectroscopy and surface plasmon resonance have been employed to characterize the silver nanoparticles synthesized. Compared to conventional methods, microwave assisted synthesis was faster and provided particles with an average particle size of 12 nm. Further, the starch functions as template, preventing the aggregation of silver nanoparticles.

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

    Science.gov (United States)

    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.

  18. Microwave-Assisted Transesterification of Macroalgae

    Directory of Open Access Journals (Sweden)

    Angel Sanchez

    2012-03-01

    Full Text Available Nowadays microwave radiation is being researched to produce biodiesel from different raw materials due to the many advantages that this technology presents compared to traditional transesterification, such as shorter reaction times and less amount of heat energy to obtain biodiesel. The aim of this research was to explore the possibility of carrying out the microwave-assisted transesterification of macroalgae and compare the results with the traditional transesterification. For that reason, some experiences were conducted using sunflower oil and macroalgae as raw material. Based on the obtained results, the best conditions for microwave-assisted transesterification reaction were macroalgae to methanol ratio of 1:15 (wt/vol, sodium hydroxide concentration of 2 wt % and reaction time of 3 min.

  19. Design of experiment approach for the optimization of polybrominated diphenyl ethers determination in fine airborne particulate matter by microwave-assisted extraction and gas chromatography coupled to tandem mass spectrometry.

    Science.gov (United States)

    Beser, Maria Isabel; Beltrán, Joaquim; Yusà, Vicent

    2014-01-03

    A sensitive and selective procedure for the determination of 12 polybrominated diphenyl ethers (BDE-28, BDE-49, BDE-47, BDE-66, BDE-100, BDE-119, BDE-99, BDE-155, BDE-154, BDE-153, BDE-139 and BDE-183) in airbone particulate matter (PM2.5) at trace level has been developed. The proposed method includes extraction PM2.5-bound PBDEs by microwave-assisted extraction (MAE) followed by gel permeation chromatography (GPC) clean-up and determination by GC-MS/MS using a programmed temperature vaporizer (PTV) in large volume injection (LVI) mode to introduce the sample to the chromatographic system. A design of experiment (DoE) approach was used for the optimization of large volume injection and microwave-assisted extraction parameters to improve these techniques efficiency. Other conditions of the method were studied: GC-MS/MS parameters, extraction solvent and matrix effect. The limit of quantification ranged from 0.063pgm(-3) to 0.210pgm(-3) when air volumes of 723m(3) were collected. Recoveries ranged from 80% to 106%. The method was successfully applied to eight real samples collected from a residential area of the monitoring network of the Region of Valencia Government (Spain) during April-August 2012. BDE-47 and BDE-99 were quantified in six and five samples respectively. The concentrations were ranged from 0.063 to 0.112pgm(-3) for BDE-47, and from 0.107 to 0.212pgm(-3) for BDE-99.

  20. Multiwalled carbon nanotubes as a solid-phase extraction adsorbent for the determination of three barbiturates in pork by ion trap gas chromatography-tandem mass spectrometry (GC/MS/MS) following microwave assisted derivatization

    Energy Technology Data Exchange (ETDEWEB)

    Zhao Haixiang [College of Science, China Agricultural University, Beijing 100094 (China); Inspection Technology and Equipment Institute, Chinese Academy of Inspection and Quarantine, Beijing 100025 (China); Department of Basic Agricultural Science, Hebei North College, Zhangjiakou Hebei 075131 (China); Wang Liping [College of Science, China Agricultural University, Beijing 100094 (China); Qiu Yueming [Inspection Technology and Equipment Institute, Chinese Academy of Inspection and Quarantine, Beijing 100025 (China); Zhou Zhiqiang [College of Science, China Agricultural University, Beijing 100094 (China)]. E-mail: zqzhou@cau.edu.cn; Zhong Weike [Inspection Technology and Equipment Institute, Chinese Academy of Inspection and Quarantine, Beijing 100025 (China); Li Xiang [Inspection Technology and Equipment Institute, Chinese Academy of Inspection and Quarantine, Beijing 100025 (China)

    2007-03-14

    A new method was developed for the rapid screening and confirmation analysis of barbital, amobarbital and phenobarbital residues in pork by gas chromatography-tandem mass spectrometry (GC/MS/MS) with ion trap MSD. The residual barbiturates in pork were extracted by ultrasonic extraction, cleaned up on a multiwalled carbon nanotubes (MWCNTs) packed solid phase extraction (SPE) cartridge and applied acetone-ethyl acetate (3:7, v/v) mixture as eluting solvent and derivatized with CH{sub 3}I under microwave irradiation. The methylated barbiturates were separated on a TR-5MS capillary column and detected with an ion trap mass detector. Electron impact ion source (EI) operating MS/MS mode was adopted for identification and external standard method was employed for quantification. One precursor ion m/z 169 was selected for analysis of barbital and amobarbital and m/z 232 was selected for phenobarbital. The product ions were obtained under 1.0 V excitation voltage. Good linearities (linear coefficient R > 0.99) were obtained at the range of 0.5-50 {mu}g kg{sup -1}. Limit of detection (LOD) of barbital was 0.2 {mu}g kg{sup -1} and that of amobarbital and phenobarbital were both 0.1 {mu}g kg{sup -1} (S/N {>=} 3). Limit of quatification (LOQ) was 0.5 {mu}g kg{sup -1} for three barbiturates (S/N {>=} 10). Satisfying recoveries ranging from 75% to 96% of the three barbiturates spiked in pork were obtained, with relative standard deviations (R.S.D.) in the range of 2.1-7.8%.

  1. Piroxicam loaded alginate beads obtained by prilling/microwave tandem technique: morphology and drug release.

    Science.gov (United States)

    Aquino, Rita P; Auriemma, Giulia; d'Amore, Matteo; D'Ursi, Anna Maria; Mencherini, Teresa; Del Gaudio, Pasquale

    2012-07-01

    This paper presents a tandem technique, based on the combination of prilling and microwave (MW) assisted treatments, to produce biodegradable alginate carriers of piroxicam with different drug controlled release behaviours. Results showed that alginate/piroxicam beads demonstrated high encapsulation efficiency and very narrow dimensional distribution. Beads dried by MW retained shape and size distribution of the hydrated particles while drying rate was strongly increased compared to convective drying processes. Moreover, different MW irradiation regimes promoted interactions between the drug and alginate matrix, affected drug polymorphism as well as inner and surface matrix structure leading to different piroxicam release profiles. High level MW irradiation led to beads with highly porous and swellable matrix able to release piroxicam in few minutes in the intestine while convective drying produced gastro-resistant beads that exhibit sustained piroxicam release (total release in 5.5h) in intestinal environment. On these results the tandem technique prilling/MW irradiation appears to be promising to obtain alginate carrier with tailored NSAIDs release depending on drug characteristics and MW irradiation.

  2. Application and research advancement on the microwave-assisted extraction

    Institute of Scientific and Technical Information of China (English)

    WANG Xin; ZHENG Xianzhe

    2007-01-01

    This paper summarized application and research advancement of the microwave-assisted extraction in the agriculture,food industry, environmental analytical chemistry, traditional Chinese medicine industry, and so on. The microwave-assisted extraction was manifested to be a simple device, wide area of application, high extraction efficiency, good reproducibility and low consumption of agent and time as well as low environmental pollution. At present, industrialization question of the microwave-assisted extraction technology has been attached importance, which will impel the microwave-assisted extraction technology to more development in the future.

  3. Multi-residue analysis of 30 currently used pesticides in fine airborne particulate matter (PM 2.5) by microwave-assisted extraction and liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Coscollà, Clara; Yusà, Vicent; Beser, Ma Isabel; Pastor, Agustin

    2009-12-18

    A confirmatory and rapid procedure has been developed for the determination of 30 currently used pesticides (CUP) in fine airborne particulate matter (PM 2.5) at trace level. The proposed method includes extraction of PM 2.5-bound pesticides by microwave-assisted extraction (MAE) followed by a direct injection into LC-MS/MS. The main parameters affecting the MAE extraction (time, temperature and volume of solvent) were optimised using statistical design of experiments (DoE). The matrix effect was also evaluated. Recoveries ranged from 72 to 109% and the limit of quantification (LoQ) was 32.5 pg m(-3) for chlorpyrifos, 13.5 pg m(-3) for fenhexamid, imazalil and prochloraz, and 6.5 pg m(-3) for the rest of pesticides, when air volumes of 760 m(3) were collected. The method was applied to 54 samples collected from three stations of the atmospheric monitoring network of the Regional Valencia Government (Spain) during April-July 2009. Nineteen out of 30 pesticides investigated were found in at least one sample: omethoate, carbendazim, acetamiprid, thiabendazole, malathion, flusilazole, metalaxyl, azoxystrobin, iprovalicarb, myclobutanil, tebuconazole, triflumizole, cyprodinil, tebufenpyrad, buprofezin, pyriproxyfen, hexythiazox, flufenoxuron and fenazaquin. The measured concentrations ranged from 6.5 to 1208 pg m(-3). To our knowledge, 11 of the pesticides detected have been reported for the first time in ambient air.

  4. Microwave-assisted synthesis of bismuth oxide

    Directory of Open Access Journals (Sweden)

    Eva Bartonickova

    2007-12-01

    Full Text Available Single phase and ultrafine bismuth oxide was synthesized via microwave-assisted hydrothermal synthesis. The effect of reaction parameters (temperature/pressure and pH on the product phase composition and morphology was discussed. The transformation of bismuth hydroxide into bismuth oxide was controlled by pH value and it was accelerated by time and temperature. The phase composition of reaction products was strongly dependent on pH value. The amorphous products were obtained at acidic pH conditions and the crystalline single phase product α-Bi2O3 phase was obtained at pH ≥12. The particle size was reduced from micrometric to nanometric size in the presence of a chelating agent. The bismuth hydroxides into bismuth oxides transformation mechanism, consisting in polycondensation ofBi–OH bounds to Bi–O–Bi bridges and crystallization of Bi2O3, was proposed.

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

    DEFF Research Database (Denmark)

    Yin, Chungen

    2012-01-01

    Production of 2nd-generation biofuels from biomass residues and waste feedstock is gaining great concerns worldwide. Pyrolysis, a thermochemical conversion process involving rapid heating of feedstock under oxygen-absent condition to moderate temperature and rapid quenching of intermediate products......, is an attractive way for bio-oil production. Various efforts have been made to improve pyrolysis process towards higher yield and quality of liquid biofuels and better energy efficiency. Microwave-assisted pyrolysis is one of the promising attempts, mainly due to efficient heating of feedstock by ‘‘microwave...... dielectric heating’’ effects. This paper presents a state-of-the-art review of microwave-assisted pyrolysis of biomass. First, conventional fast pyrolysis and microwave dielectric heating is briefly introduced. Then microwave-assisted pyrolysis process is thoroughly discussed stepwise from biomass...

  6. Microwave assisted centrifuge and related methods

    Science.gov (United States)

    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. Microwave-Assisted Rapid Enzymatic Synthesis of Nucleic Acids.

    Science.gov (United States)

    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.

  8. Microwave-assisted extraction kinetics of terpenes from caraway seeds

    NARCIS (Netherlands)

    Chemat, S.; Ait-Amar, H.; Lagha, A.; Esveld, D.C.

    2005-01-01

    The process conditions during the extraction of carvone and limonene from caraway seed (Carum carvi L.) with microwave-assisted extraction have been studied with respect to microwave power, radiation dose and extraction time in order to obtain the secondary metabolites selectively. Using classical s

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

    Science.gov (United States)

    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…

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

    Science.gov (United States)

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

    2017-03-01

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

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

    Science.gov (United States)

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

    2017-06-01

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

  12. Microwave-assisted extraction of polysaccharides from solanum nigrum

    Institute of Scientific and Technical Information of China (English)

    CHEN Xiao-qing; LIU-qin; JIANG xin-yu; ZENG fan

    2005-01-01

    The microwave-assisted method was used to extract polysaccharides from solanum nigrum. The optimum experimental parameters, mechanism of the extraction and the effect of microwave-assisted extraction process on the structures of polysaccharides were investigated. The extract was analyzed by the modified phenol-sulfuric acid method at 490 nm. The optimum experimental parameters were obtained by orthogonal experiments as follows: extraction time 15 min, microwave radiation power 455 W and the process ratio of materials mass to solvent volume 1∶20. The results show that compared with the conventional reflux extraction, the microwave-assisted extraction has a higher yield in shorter time, with no effect on the finally obtained polysaccharides as seen from the FT-IR spectra. The scanning electron microscopy images reveal that the mechanism of the extraction is related to the structural changes of the plant cells in different extracting conditions.

  13. Microwave-assisted synthesis of photochromic fulgides

    Indian Academy of Sciences (India)

    Sivasankaran Nithyanandan; Chinnusamy Saravanan; Sengodan Senthil; Palaninathan Kannan

    2010-03-01

    The oxazole and indole based heterocyclic photochromic fulgides were synthesized from their corresponding fulgenic acid derivatives by clay catalysed microwave irradiation methodology. Improved yields of fulgides were observed by the microwave irradiation method as compared other chemical methods employed so far. The proportions of clay (montmorillonite KSF) and isopropenyl acetate play a key role in increasing the yields of fulgides.

  14. Atmospheric Pressure Microwave Assisted Heterogeneous Catalytic Reactions

    Directory of Open Access Journals (Sweden)

    Farid Chemat

    2007-07-01

    Full Text Available The purpose of the study was to investigate microwave selective heatingphenomena and their impact on heterogeneous chemical reactions. We also present a toolwhich will help microwave chemists to answer to such questions as “My reaction yields90% after 7 days at reflux; is it possible to obtain the same yield after a few minutes undermicrowaves?” and to have an approximation of their reactions when conducted undermicrowaves with different heterogeneous procedures. This model predicting reactionkinetics and yields under microwave heating is based on the Arrhenius equation, inagreement with experimental data and procedures.

  15. Microwave assisted wet oxidation of p-nitrophenol

    Institute of Scientific and Technical Information of China (English)

    BO; Longli; CHEN; Shuo; QUAN; Xie; LIU; Xitao; ZHAO; Huimin

    2005-01-01

    Aqueous solution of p-nitrophenol (PNP) was treated continuously by microwave assisted wet oxidation while flowing through a granular activated carbon (GAC) fixed bed. PNP was pre-adsorbed onto GAC prior to being put into the reactor so as to prevent PNP adsorption on GAC during microwave irradiation. PNP solutions with different initial concentration (218.6 mg/L and 1200 mg/L) were treated under conditions of microwave power 500 W, liquid flow 6.4 mL/min and air flow 40 mL/min or 60 mL/min. The results indicated that the removal of PNP was higher than 90% and more than 65% PNP was mineralized. Phenol, nitrobenzene, hydroquinone and benzoquinone occurred as course products during the operation process, which were degraded further. The biodegradability of the outflow was improved greatly by microwave assisted wet oxidation.

  16. Microwave-assisted rapid characterization of lipase selectivities.

    Science.gov (United States)

    Bradoo, Sapna; Rathi, Pooja; Saxena, R K; Gupta, Rani

    2002-04-18

    A rapid screening procedure for characterization of lipase selectivities using microwaves was developed. The rate of reaction of various commercial lipases (porcine pancreas, Mucor miehei, Candida rugosa, Pseudomonas cepacia) as well as lipases from laboratory isolates-Bacillus stearothermophilus and Burkholderia cepacia RGP-10 for triolein hydrolysis was 7- to 12-fold higher in a microwave oven as compared to that by pH stat. The esterification of sucrose/methanol and ascorbic acid with different fatty acids was also achieved within 30 s in a microwave using porcine pancreas, B. stearothermophilus SB-1 and B. cepacia RGP-10 lipases. The relative rates and selectivity of the lipases both for hydrolytic and synthesis reactions remains unaltered. However, the rate of reaction was dynamically enhanced when exposed to microwaves. Microwave-assisted enzyme catalysis can become an attractive procedure for rapid characterization of large number of enzyme samples and substrates, which otherwise is a cumbersome and time-consuming exercise.

  17. MICROWAVE-ASSISTED SURFACE MODIFICATION OF CALCIUM BICARBONATE

    Institute of Scientific and Technical Information of China (English)

    Jing Ye; Xiaofei Zhang

    2004-01-01

    Surface modification of calcium bicarbonate powder with isopropyl triisostearoyl titanate (TTS) by microwave-assisted heating was studied in the present work. The features of microwave treated powder show obvious superiority to those of powder samples treated by traditional surface modification method and of untreated calcium bicarbonate - in suspension turbidity, suction potential, contact angle with water, and mechanical properties of their composites with PVC resin.

  18. Microwave assisted synthesis of 6-Substituted aminopurine analogs in water

    OpenAIRE

    Qu, Guirong; Han,Suhui; Zhang,Zhiguang; Geng,Mingwei; Xue, Feng

    2006-01-01

    Microwave assisted amination of 6-chloropurine derivatives with various amines in water resulted in a "green chemistry" protocol for the preparation of 6-substituted aminopurine analogs in very good yields. Using a simply modified microwave oven with the refluxing apparatus, the amination of the 6-chloro in the purine structure occurred smoothly. 19 known and 16 unknown 6-substituted aminopurine analogs were prepared through nucleophilic aromatic substitution with simple filtration or column ...

  19. Microwave assisted extraction of mangiferin from Curcuma amada

    OpenAIRE

    PADMAPRIYA K.; Dutta, Abhishek; Chaudhuri, Surabhi; Debjani DUTTA

    2011-01-01

    Mangiferin present in Curcuma amada was extracted with the help of microwave assisted extraction (MAE). The extraction solvent used was ethanol, which is eco-friendly and reduced the risk of environmental hazard. The mangiferin content was found to increase until 500 W, but decreased as the microwave power was increased further. A similar threshold was also obtained for microwave irradiation time. Following a mathematical analysis, an optimal mangiferin yield of 41 μg/mL was obtained from an ...

  20. Microwave-assisted hydrothermal synthesis of lead zirconate fine powders

    Directory of Open Access Journals (Sweden)

    Apinpus Rujiwatra

    2011-01-01

    Full Text Available A rapid synthesis of lead zirconate fine powders by microwave-assisted hydrothermal technique is reported. The influences of type of lead precursor, concentration of potassium hydroxide mineraliser, applied microwave power and irradiation time are described. The synthesised powders were characterised by powder X-ray diffraction, field emission scanning electron microscopy, energy-dispersive X-ray spectroscopic microanalysis and light scattering technique. The merits of the microwave application in reducing reaction time and improving particle mono-dispersion and size uniformity as well as the drawbacks, viz. low purity of the desired phase and increasing demand of mineraliser, are discussed in relation to conventional heating method.

  1. Microwave Assisted Synthesis of Biorelevant Benzazoles.

    Science.gov (United States)

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

    2016-10-25

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

  2. 微波辅助萃取-液相色谱-串联质谱法测定植物源产品中的阿维菌素B1a残留量%Determination of Avermectin B1a Residues in Plant-originated Foodstuffs by Microwave Assisted Extraction-Liquid Chromatography Tandem Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    蒋宏; 胡贝贞; 宋伟华

    2012-01-01

    建立了植物源产品茶叶、粮谷、中药材中阿维菌素B1a残留量的液相色谱-串联质谱(LC-MS/MS)测定方法.样品用丙酮-二氯甲烷(体积比1∶1)微波辅助提取,提取液经石墨化炭黑/氨基(Carb/NH2)固相萃取小柱净化.采用Hypersil Gold C18色谱柱(150mm×2.1 mm,Sμ m),乙腈-2.5 mmol/L乙酸铵水溶液为流动相,以电喷雾电离正离子(ESI+)、多反应监测模式(MRM)定性、定量测定阿维菌素Bla,采用基质标准曲线外标法定量.在5~100 μg/L范围内,阿维菌素Bla的峰面积与质量浓度呈线性关系,相关系数大于0.998,方法的检出限(S/N>3)为5μg/kg,定量限(S/N>10)为10μg/kg.取有代表性的绿茶、小麦、丹参阴性样品进行加标回收试验,在10,50 μg/kg加标水平下,回收率为75%~87%,相对标准偏差为4.04%~6.38%(n=5).该法提取效果好、净化较彻底,灵敏度满足国内外限量标准的要求,适合复杂基质植物源产品中阿维菌素B1a残留量的测定.%A microwave assisted extraction—liquid chromatography—tandem mass spectrometry method for the determiantion of avermectin Bla residues in tea, cereals and Chinese herbal medicine was developed. The sample was extracted by microwave assisted extraction with acetone-dichloromethane(volume ratio was 1 : 1) as solvent, the extract was cleaned up by Carb/NH2 SPE column. The separation was performed on a Hypersil Gold C18 column(150 mm × 2.1 mm,5 μm) and with the gradient elution of acetonitrile and water (containing 2.S mmol/L ammonium acetate). Avermectin Bla was determined in the mode of electrospry positive ionization (ESI+) and multiple reaction monitoring(MRM). The quantification was carried out by matrix-matched external standard curve, the calibration curves showed good linearity in the concentration range of 5-100 μg/L and the correlation coefficient was more than 0.998. The limit of detection(S/N > 3) was 5 μg/kg and the limit of quantification {S/N > 10

  3. Microwave-assisted preparation of naphthenic acid esters

    Directory of Open Access Journals (Sweden)

    VERA CIRIN-NOVTA

    2006-12-01

    Full Text Available The synthesis of esters of natural petroleum acids of the naphthenic type assisted with microwave irradiation under the conditions of acid catalysis was carried out with various alcohols: methanol, ethanol, n-butanol and tert-butyl alcohol. Microwave dielectric heating of the reaction mixture in an unmodified microwave oven with activation of the naphthenic acids with sulfuric and p-toluenesulfonic acid afforded the esters of the naphthenic acids. Depending on the catalyst and the steric and nucleophilic properties of the alcohols, the yield of naphthenic esters ranged from 31.25 % to 88.90 %. As a consequence of microwave dielectric heating, the esterification time was reduced from 6–10 h to 5 min.

  4. 气相色谱-串联质谱法测定涂布纸中邻苯二甲酸酯类增塑剂%Simultaneous Determination of Phthalate Plasticizers in Coated Papers by Gas Chromatography-tandem Mass Spectrometry Coupled with Microwave-assisted Extraction

    Institute of Scientific and Technical Information of China (English)

    王成云; 徐嵘; 杨左军; 吴透明; 谢堂堂; 褚乃清

    2013-01-01

    以丙酮为萃取溶剂,采用微波辅助萃取技术提取涂布纸中的邻苯二甲酸酯类增塑剂,提取产物进行气相色谱-串联质谱法(GC-MS)测定,从而建立了一种同时测定涂布纸中多种邻苯二甲酸酯类增塑剂的快速检测方法.该方法的精密度(RSD)均小于14%,加标平均回收率为83.6% ~104.1%.在信噪比为10(S/N=10)的条件下,DINP、DIDP和DMPP的定量下限分别为0.2、0.2、0.1 mg/kg,其余各组分的定量下限均小于0.05 mg/kg.采用该方法对市售涂布纸进行测定,结果在部分涂布纸中检出多种邻苯二甲酸酯类增塑剂.%Phthalate plasticizers in coated papers were microwave-assisted extracted using acetone as the extraction solvent, and then were analyzed by gas chromatography-tandem mass spectrometry(GC-MS). Therefore, an effective method was established to determine simultaneously the contents of phthalate plasticizers in coated papers. The relative standard deviation (RSD) of the proposed method was less than 14% while the average spike recoveries varied from 83.6% to 104.1%. The quantification limits (S/N = 10) were 0.2, 0.2 and 0.1 mg/ kg for DINP, DIDP and DMPP, respectively. The limits of quantification (S/N = 10) were all less than 0.05 mg/kg for other phthalate plasticizers. The proposed method was successfully applied to the determination of phthalate plasticizers in coated papers and the results showed that various phthalate plasticizers existed in some commercial coated papers.

  5. Microwave assisted extraction of phenolic compounds from four different spices.

    Science.gov (United States)

    Gallo, Monica; Ferracane, Rosalia; Graziani, Giulia; Ritieni, Alberto; Fogliano, Vincenzo

    2010-09-09

    Spices and herbs are known not only for their taste, aroma and flavour, but also for their medical properties and value. Both spices and herbs have been used for centuries in traditional medical systems to cure various kinds of illnesses such as common cold, diabetes, cough and cancers. The aim of this work was the comparison between two different extractive techniques in order to get qualitative and quantitative data regarding bioactive compounds of four different spices (Cinnamomum zeylanicum, Coriandrum sativum, Cuminum cyminum, Crocus sativus). The plants were extracted employing ultrasonication and microwave-assisted extractions. The efficiency of extraction of bioactive compounds obtained with the microwave extraction process was in general about four times higher than that resulting from sonication extraction. The various extracts obtained were analyzed for their antioxidant activity using ABTS, DPPH and FRAP assays and for their total polyphenolic content. It can be concluded that microwave-assisted extractions provide significant advantages in terms of extraction efficiency and time savings.

  6. Microwave-assisted Weak Acid Hydrolysis of Proteins

    Directory of Open Access Journals (Sweden)

    Miyeong Seo

    2012-06-01

    Full Text Available Myoglobin was hydrolyzed by microwave-assisted weak acid hydrolysis with 2% formic acid at 37 oC, 50 oC, and100 oC for 1 h. The most effective hydrolysis was observed at 100 oC. Hydrolysis products were investigated using matrixassistedlaser desorption/ionization time-of-flight mass spectrometry. Most cleavages predominantly occurred at the C-termini ofaspartyl residues. For comparison, weak acid hydrolysis was also performed in boiling water for 20, 40, 60, and 120 min. A 60-min weak acid hydrolysis in boiling water yielded similar results as a 60-min microwave-assisted weak acid hydrolysis at100 oC. These results strongly suggest that microwave irradiation has no notable enhancement effect on acid hydrolysis of proteinsand that temperature is the major factor that determines the effectiveness of weak acid hydrolysis.

  7. Dynamic Microwave-assisted Extraction of Flavonoids from Radix Scutellariae

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Dynamic microwave-assisted extraction(DMAE) of flavonoids from Radix Scutellarie was described in this article. A TM010 microwave resonant cavity was used as the energy coupler. Several parameters of DMAE, including concentration, flow rate, volume of the extraction solvent, and irradiation power, were optimized. The extraction was performed under the optimum conditions for the extraction of total flavonoids. The total flavonoids were determined by UV-Vis spectrophotometry. The main bioactive components, including baicalin, baicalein, and wogonin, were determined by HPLC. The extraction yields of the flavonoids obtained by DMAE were compared with those obtained by pressurized microwave assisted extraction( PMAE), ultrasonic extraction ( UE ), soxhlet extraction ( SE ), and reflux extraction( RE), and these results indicate that DMAE is a good alternative method for the extraction of flavonoids from Radix Scutellarie.

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

    Science.gov (United States)

    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...

  9. Efficient Microwave-Assisted Synthesis of 5-Deazaflavine Derivatives

    Directory of Open Access Journals (Sweden)

    Justo Cobo

    2010-10-01

    Full Text Available A series of pyrimido[4,5-b]quinolines  (5-deazaflavines, were synthesized by microwave assisted intramolecular cyclization. The N4-substituted-2,4-diamino-6-chloro-pyrimidine-5-carbaldehydes, were prepared by selective monoamination of 2-amino-4,6-dichloropyrimidine-5-carbaldehyde with aliphatic and aromatic amines.

  10. Microwave Assisted Healing of Thermally Mendable Composites

    Directory of Open Access Journals (Sweden)

    Edward D. Sosa

    2015-01-01

    Full Text Available Polymer matrix composites offer high specific strength; however, their potential weight savings have been limited by the concern of damage tolerance. If microcracking and similar incurred damage could be autonomously sealed, composite structures could be built thinner and lighter while still addressing damage tolerance, thus achieving the weight savings they promise. Various self-healing mechanisms have been proposed to this end. Herein, a method of thermally reversible polymerization is investigated. To date, thermally activated repair of composites have been accomplished typically through resistive heating, which has certain inherent complexities. An alternate heating method, via microwave exposure of carbon nanotubes incorporated throughout a thermal reversible polymer matrix, is demonstrated. Carbon nanotube-doped composites exhibit enhanced microwave absorption over an undoped control sample. Furthermore, it is shown that these composites can be heated locally by a focused microwave source. The particular composite formulation and layup studied could be uniformly heated to the targeted healing temperature of 100°C in as little as 20 seconds, followed by a healing time on the scale of minutes with total time depending upon the extent of damage.

  11. Microwave-Assisted Preparation of High Entropy Alloys

    Directory of Open Access Journals (Sweden)

    Paolo Veronesi

    2015-10-01

    Full Text Available Microwaves at the ISM (Industrial, Scientific and Medical, reserved internationally frequency of 2450 or 5800 MHz have been used to prepare FeCoNiCuAl, FeCrNiTiAl and FeCoCrNiAl2.5 high entropy alloys by direct heating of pressed mixtures of metal powders. The aim of this work is to explore a new microwave-assisted near-net-shape technology, using a powder metallurgy approach for the preparation of high entropy alloys, able to overcome the limits of current melting technologies (defects formation or solid state ones (time demanding. High entropy alloy compositions have been selected so as to comprise at least one ferromagnetic element and one highly reactive couple, like Ni-Al, Ti-Al, Co-Al or Fe-Al. Results show that direct microwave heating of the powder precursors occurs, and further heating generation is favored by the ignition of exothermal reactions in the load. Microwaves have been applied both for the ignition and sustaining of such reactions, showing that by the proposed technique, it is possible to control the cooling rate of the newly-synthesized high entropy alloys. Results showed also that microwave heating in predominant magnetic field regions of the microwave applicator is more effective at controlling the cooling rate. The herein proposed microwave-assisted powder metallurgy approach is suitable to retain the shape of the load imparted during forming by uniaxial pressing. The homogeneity of the prepared high entropy alloys in all cases was good, without the dendritic segregation typical of arc melting, even if some partially-unreacted powders were detected in the samples.

  12. Microwave-Assisted Drying for the Conservation of Honeybee Pollen

    Directory of Open Access Journals (Sweden)

    Angelo Canale

    2016-05-01

    Full Text Available 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.

  13. Monodisperse Silver Nanoparticles Synthesized by a Microwave-Assisted Method

    Institute of Scientific and Technical Information of China (English)

    ZHU Shao-Peng; TANG Shao-Chun; MENG Xiang-Kang

    2009-01-01

    Silver nanoparticles with an average size of about 2Onto are synthesized in a colloidal solution with the aid of microwave irradiation. Neither additional reductant nor stabilizer is required in this microwave-assisted method.The color of the colloidal solution is found to be dark green, different from the characteristic yellow of silver colloidal solutions. The silver nanoparticles in the colloidal solution have a narrow size distribution and large yield quantity. UV-visible absorption spectroscopy analysis reveals that the as-synthesized monodisperse silver nanoparticles have exceptional optical properties. Raman spectroscopy measurements demonstrate that these silver nanoparticles exhibit a notable surface-enhanced Raman scattering ability.

  14. The influence of microwave irradiation on rocks for microwave-assisted underground excavation

    Directory of Open Access Journals (Sweden)

    Ferri Hassani

    2016-02-01

    Full Text Available Demand is growing for explosive-free rock breakage systems for civil and mining engineering, and space industry applications. This paper highlights the work being undertaken in the Geomechanics Laboratory of McGill University to make a real application of microwave-assisted mechanical rock breakage to full-face tunneling machines and drilling. Comprehensive laboratory tests investigated the effect of microwave radiation on temperature profiles and strength reduction in hard rocks (norite, granite, and basalt for a range of exposure times and microwave power levels. The heating rate on the surface of the rock specimens linearly decreased with distance between the sample and the microwave antenna, regardless of microwave power level and exposure time. Tensile and uniaxial compressive strengths were reduced with increasing exposure time and power level. Scanning electron micrographs (SEMs highlighted fracture development in treated basalt. It was concluded that the microwave power level has a strong positive influence on the amount of heat damage induced to the rock surface. Numerical simulations of electric field intensity and wave propagation conducted with COMSOL Multiphysics® software generated temperature profiles that were in close agreement with experimental results.

  15. Study on microwave-assisted extraction of coal

    Institute of Scientific and Technical Information of China (English)

    CHEN Hong; LU Jun-qing; GE Ling-mei; Li Jian-wei

    2007-01-01

    The effect of different factors on coal extraction yield-temperature,solvent,coal type and irradiation time were investigated for different China coals under microwave-assisted extraction(MAE).The results show that the optimum temperature for ethanol,acetone and THF are 393,373 and 373 K respectively and the extraction yield of THF is higher than that of other two solvents under MAE.Extraction with several single organic solvents were conducted for the 5 typical China coals-Shenfu,Tongchuan,Panzhihua,Yitai and Huating coal under microwave-assisted extraction and Soxhlet extraction.Resuits indicat that extraction yield of ethylenediamine,ethanol,acetone,tetrahydrofuran under MAE are are higher than that of Soxhlet extraction and MAE required less time.Tonqchuan coal extracts of ethanol and acetone which were extracted by MAE and Soxhlet extraction were analyzed by GC/MS.

  16. 微波辅助萃取/高效液相色谱串联质谱法对山银花中活性成分含量的测定%Determination of the Active Components in Flos Lonicerae by Microwave Assistant Extraction Combined with High Performance Liquid Chromatography- Tandem Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    宋伟峰; 陶玲; 钟鸣

    2012-01-01

    建立了微波辅助萃取/高效液相色谱串联质谱法( MAE/HPLC - MS/MS)同时测定山银花中10种活性成分含量的方法.山银花药材采用MAE萃取,萃取溶剂为乙醇-水(7∶3),固液比1∶30,萃取温度70℃,萃取时间 10 min.采用HPLC - MS/MS测定萃取液中活性成分的含量,色谱柱采用Agilent Poroshell 120 SB-C18( 100 mm × 2.1 mm,2.7 μm),以0.5%甲酸-乙腈为流动相进行梯度洗脱,负离子多重反应离子监测模式检测.在优化条件下,10种成分的定量分析在10 min内完成.结果表明,10种活性成分的线性范围为0.05~ 500 mg/L,相关系数(r)不低于0.9969,检出限和定量下限分别在69~4413 μg/kg和231 ~ 14709μg/kg范围,回收率为94%~105%.采用该方法检测6个不同产地的山银花样品,10种活性成分的含量在3.98 ~ 14 356.31 mg/kg范围.该方法快速、准确,可有效地用于山银花药材的质量控制.%A method of microwave assistant extraction (MAE) combined with high performance liquid chromatography -tandem mass spectrometry( HPLC - MS/MS)was developed for the determination of 10 active components in Flos Lonicerae. The Flos Lonicerae samples were extracted by MAE, using ethanol -H2O(7 : 3) as solvent with a solid - liquid ratio of 1 : 30 at a temperature of 70℃. The extracts were separated on an Agilent Poroshell 120 SB-C18(100 mm×2. 1 mm, 2.7 μm) column by gradient elution of 0. 5% formic acid - acetonitrile. A triple quadrupole MS operating in multiple-reaction monitoring( MRM) mode with negative ion was used for the quantitative analysis of 10 active components. Under the optimized conditions, 10 constituents in Flos Lonicerae were analyzed com-pletely within 10 min. The linear ranges of 10 active components were in the range of 0. 05 - 500 mg/L, with correlation coefficients no less than 0. 996 9. The limits of detection and limits of quanti-tation were in the ranges of 69 -4 413 μg/kg and 231 - 14 709 μg/kg, respectively. The

  17. 微波辅助萃取-气相色谱-串联质谱法同时测定纺织品中6种有机磷阻燃剂%Simultaneous determination of six organophosphorous flame retardants in textiles by gas chromatography-tandem mass spectrometry combined with microwave assisted extraction

    Institute of Scientific and Technical Information of China (English)

    王成云; 李丽霞; 谢堂堂; 张伟亚; 刘彩明; 褚乃清

    2011-01-01

    An effective method was established for the simultaneous determination of six banned organophosphorous flame retardants in textiles by gas chromatography-tandem mass spectrometry (GC-MS/MS) combined with microwave assisted extraction (MAE). By investigating the extraction efficiency of 12 different extraction solvents for the target analytes, the optimal conditions were that the sample was extracted by microwave assisted extraction using acetone as the solvent at 76 ℃ for 30 min. Then the extract was analyzed by GC-MS/MS in multiple reaction monitoring (MRM) mode, and the concentration of each analyte was calibrated by external standard method. The linear ranges of tris-( 1-aziridinyl) phosphine oxide (TEPA), tris-( 2-chloroethyl) phosphate ( TCEP ), tris-( 1, 3-dichloropropyl) phosphate (TDCP), bis-(2,3-dibromopropyl) phosphate (DDBPP), tri-o-cresyl phosphate (TOCP) and tris-( 2,3-dibromopropyl) phosphate (TEIS) were 9. 17 -366.80, 0.95 -75.98, 1.04 -83.20, 41.60-832.00, 3.80 -75.90, and 40.48 -809.60 μg/L, respectively, the correlation coefficients were not less than 0. 997 5 , while the limits of quantification ( LOQ) (S/N = 10) were 3.0, 0.2, 0.3, 25.0, 2.5 and 29.0 μg/kg, respectively. The spiked recoveries varied from 82. 62% to 96. 88% with the relative standard deviations of 3. 80% to 8. 79%. The proposedmethod was successfully applied to the determination of organophosphorous flame retardants in eight commercial textiles. The experimental results demonstrated that the method developed is simple, rapid, sensitive and accurate, which could satisfy the demand of the analysis of banned organophosphorous flame retardants in textiles.%建立了微波辅助萃取-气相色谱-串联质谱(MAE-GC-MS/MS)同时测定纺织品中6种禁用有机磷阻燃剂的分析方法.通过考察12种不同萃取溶剂对目标分析物的萃取效率,确定了以丙酮为萃取溶剂,在76℃下萃取30min的萃取条件.在多反应监测(MRM)模式下采用GC-MS/MS检测

  18. Determination of Pt from coke samples by ICP-MS after microwave assisted digestion and microwave assisted cloud point extraction

    Energy Technology Data Exchange (ETDEWEB)

    Niemela, M.; Huttunen, S.M.; Gornostayev, S.S.; Peramaki, P. [University of Oulu, Oulu (Finland). Dept. of Chemistry

    2009-09-15

    Platinum in coke samples was determined by inductively coupled plasma mass spectrometry (ICP-MS) after microwave-assisted sample digestion and temperature controlled microwave assisted cloud point extraction (MW-CPE). Interferences due to hafnium were successfully eliminated using MW-CPE with 2-MBT prior to the determination of platinum by ICP-MS. The validity of the method was studied by spike recovery tests and by analyzing certified reference material (BCR-723 street dust). The results obtained for platinum in the BCR-723 were generally in good agreement with the certified values. Furthermore, the preliminary platinum results obtained for coke sample by ICP-MS after MW-CPE were compared to those obtained by a reference method (NiS-Fire Assay preconcentration/Te coprecipitation and ICP-MS determination).

  19. TANDEM

    Data.gov (United States)

    Federal Laboratory Consortium — The Tandem Van de Graaff facility provides researchers with beams of more than 40 different types of ions - atoms that have been stripped of their electrons. One of...

  20. Optimization of microwave assisted extraction of pectin from orange peel.

    Science.gov (United States)

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

    2013-09-12

    In this study, microwave-assisted extraction was applied for pectin extraction from the dried orange peel and Box-Behnken response surface design was used to study and optimize the effects of processing variables (microwave power, irradiation time, pH and solid-liquid ratio) on the yield of pectin. The amount of pectin extracted increased with increasing microwave power, while it reduces as the time, pH and solid-liquid ratio increased. From the results, second order polynomial model was developed and it adequately explained the data variation and significantly represented the actual relationship between independent variables and the response. An optimization study using Derringer's desired function methodology was performed and optimal conditions based on both individual and combinations of all independent variables (microwave power of 422W, irradiation time of 169 s, pH of 1.4 and solid-liquid ratio of 1:16.9 g/ml) were determined with maximum pectin yield of 19.24%, which was confirmed through validation experiments.

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

    Science.gov (United States)

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

    2012-04-01

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

  2. Microwave Assisted Extraction of Phenolic Compounds from Four Different Spices

    Directory of Open Access Journals (Sweden)

    Alberto Ritieni

    2010-09-01

    Full Text Available Spices and herbs are known not only for their taste, aroma and flavour, but also for their medical properties and value. Both spices and herbs have been used for centuries in traditional medical systems to cure various kinds of illnesses such as common cold, diabetes, cough and cancers. The aim of this work was the comparison between two different extractive techniques in order to get qualitative and quantitative data regarding bioactive compounds of four different spices (Cinnamomum zeylanicum, Coriandrum sativum, Cuminum cyminum, Crocus sativus. The plants were extracted employing ultrasonication and microwave-assisted extractions. The efficiency of extraction of bioactive compounds obtained with the microwave extraction process was in general about four times higher than that resulting from sonication extraction. The various extracts obtained were analyzed for their antioxidant activity using ABTS, DPPH and FRAP assays and for their total polyphenolic content. It can be concluded that microwave-assisted extractions provide significant advantages in terms of extraction efficiency and time savings.

  3. Vacuum-assisted microwave drying characteristics of green bell pepper

    Directory of Open Access Journals (Sweden)

    Vivek Kumar

    2017-04-01

    Full Text Available Chopped green bell pepper pieces were blanched (95 °C, 5 min and chemically pretreated (1% potassium metabisulphite solution, 25 min at room temperature before drying in hot air dryer (HAD at various temperature ranges (60 – 80 °C. Three vacuum levels (200, 400, 600 mm Hg and microwave power levels (100, 200, 300 W were also used to dry green bell pepper samples in a vacuum assisted microwave (VAM (2.45 GHz, 0.8 kW dryer. VAM drying methods offered a maximum reduction by four to five times in drying time as compared to that in HAD. The logarithmic model was found to have the best fit based on high R2 and small values of reduced χ2 and RMSE.  VAM method has higher values for effective moisture diffusivity (Deff and lower values for activation energy (Ea, in comparison to the HAD method. 

  4. Fast microwave-assisted pyrolysis of microalgae using microwave absorbent and HZSM-5 catalyst.

    Science.gov (United States)

    Borges, Fernanda Cabral; Xie, Qinglong; Min, Min; Muniz, Luis Antônio Rezende; Farenzena, Marcelo; Trierweiler, Jorge Otávio; Chen, Paul; Ruan, Roger

    2014-08-01

    Fast microwave-assisted pyrolysis (fMAP) in the presence of a microwave absorbent (SiC) and catalyst (HZSM-5) was tested on a Chlorella sp. strain and on a Nannochloropsis strain. The liquid products were characterized, and the effects of temperature and catalyst:biomass ratio were analyzed. For Chlorella sp., a temperature of 550 °C, with no catalyst were the optimal conditions, resulting in a maximum bio-oil yield of 57 wt.%. For Nannochloropsis, a temperature of 500 °C, with 0.5 of catalyst ratio were shown to be the optimal condition, resulting in a maximum bio-oil yield of 59 wt.%. These results show that the use of microwave absorbents in fMAP increased bio-oil yields and quality, and it is a promising technology to improve the commercial application and economic outlook of microwave pyrolysis technology. Additionally, the use of a different catalyst needs to be considered to improve the bio-oil characteristics.

  5. Negative Feedback Effect of Microwave Irradiation in the Microwave-assisted Hydrothermal Synthesis of Bi2S3 Nanorods

    Institute of Scientific and Technical Information of China (English)

    TAO,Xiu-Cheng(陶秀成); SHAO,Ming-Wang(邵名望)

    2002-01-01

    The microwave-assisted hydrothermal synthesis of Bi2S3 nanorods was reported. The result showed that microwave irradiation can help to produce Bi2S3 nanorods in very short time.There is a negative feedback effect which increases the degree of crystallinity in the reaction.

  6. Microwave-Assisted Extraction of Brewers' Spent Grain Arabinoxylans

    OpenAIRE

    Rocha, M. A. M.; Saraiva, J.; Coimbra,M. A.

    2011-01-01

    Brewers´ spent grain (BSG) is a by-product from beer industry that can be exploited as a source of arabinoxylo-oligosaccharides (AXOS) with prebiotic activity. In this study, microwave-assisted extractions were performed during 2 min at 140-210°Cin order to evaluate the feasibility of this extraction technology for quantitative extraction of the arabinoxylans (AX) or AXOS from BSG. The AX yield increasedwith the increase of the temperature in the range used. The best condition...

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

    Science.gov (United States)

    Kerst, M; Andersson, J T

    2001-08-01

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

  8. Microwave-assisted Extraction of Rutin and Quercetin from Flos Sophorae

    Institute of Scientific and Technical Information of China (English)

    LI Min-jing; YOU Jing-yan; YAO Shuang; DING Lan; LIU Zhong-ying; ZHANG Han-qi

    2004-01-01

    Three microwave-assisted extraction(MAE) procedures were studied. The first procedure was household microwave oven dynamic extraction(HMODE). The second procedure was special microwave oven bath extraction(SMOBE). The third procedure was microwave resonant cavity dynamic extraction(MRCDE). The results obtained by the three microwave-assisted extraction procedures were compared with those obtained by using traditional Soxhlet extraction. The results indicate that the MAE not only took a shorter time, but also simplified the procedure, and made the extraction a higher yield. At the same time the results obtained by the three MAE procedures were also compared with each other.

  9. Magnetic gold nanotriangles by microwave-assisted polyol synthesis

    Science.gov (United States)

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

    2015-08-01

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

  10. Rapid synthesis of tantalum oxide dielectric films by microwave microwave-assisted atmospheric chemical vapor deposition

    Energy Technology Data Exchange (ETDEWEB)

    Ndiege, Nicholas [School of Chemical Sciences, University of Illinois at Urbana-Champaign, 600 South Mathews Avenue, Urbana, IL 61801 (United States)], E-mail: ndiege@uiuc.edu; Subramanian, Vaidyanathan [School of Chemical Sciences, University of Illinois at Urbana-Champaign, 600 South Mathews Avenue, Urbana, IL 61801 (United States)], E-mail: ravisv@unr.edu; Shannon, Mark A. [Mechanical Science and Engineering, University of Illinois at Urbana-Champaign, 1206 West Green street, Urbana, IL 61801 (United States)], E-mail: mshannon@uiuc.edu; Masel, Richard I. [School of Chemical Sciences, University of Illinois at Urbana-Champaign, 600 South Mathews Avenue, Urbana, IL 61801 (United States)], E-mail: r-masel@uiuc.edu

    2008-10-01

    Microwave-assisted chemical vapor deposition has been used to generate high quality, high-k dielectric films on silicon at high deposition rates with film thicknesses varying from 50 nm to 110 {mu}m using inexpensive equipment. Characterization of the post deposition products was performed by scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, Auger electron spectroscopy and Raman spectroscopy. Film growth was determined to occur via rapid formation and accumulation of tantalum oxide clusters from tantalum (v) ethoxide (Ta(OC{sub 2}H{sub 5}){sub 5}) vapor on the deposition surface.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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…

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

    Science.gov (United States)

    Worzakowska, Marta

    2015-06-08

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

  14. Microwave assisted synthesis and biological activity of novel coumarinyltriazolothiadiazoles

    Directory of Open Access Journals (Sweden)

    Kumar P

    2010-01-01

    Full Text Available A series of new 3-(4-methylcoumarinyl-7-oxymethyl-6-substitutedphenyl-5,6-dihydro-s-triazolo (3,4-b(1,3,4-thiadiazoles 2(a-j have been synthesized by reacting 5-(4-methyl coumarinyl-7-oxymethyl-4-amino-3-mercapto(4H-1,2,4-triazole with various aromatic aldehydes by microwave assisted organic synthesis. The structure of the compounds 2 (a-j has been confirmed by IR, 1 H NMR and mass spectral data. All the compounds were screened for antimicrobial and antioxidant activity. Among the compounds tested, compounds 2d (4-dimethyl amino phenyl derivative and 2h (3,4-dimethoxy phenyl derivative showed better antimicrobial and antioxidant activity than rest of the compounds in the series.

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

    Energy Technology Data Exchange (ETDEWEB)

    Carpenter, Gopal; Sen, Ravindra; Gupta, Nitish, E-mail: nitish.nidhi75@gmail.com [Department of Applied Chemistry, Shri G. S. Institute of Technology and Science, Indore Madhyapradesh (India); Malviya, Nitin [Department of Applied Physics, Shri G. S. Institute of Technology and Science, Indore Madhyapradesh (India)

    2015-08-28

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

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

    OpenAIRE

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

    2014-01-01

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

  17. Microwave-assisted magnetization reversal using transient precession of magnetization in permalloy hexagons

    Science.gov (United States)

    Okano, Genki; Nozaki, Yukio

    2016-06-01

    Microwave-assisted magnetization reversal utilizing a transient precession of magnetization was demonstrated in a permalloy hexagon by applying a 25-ns-wide microwave field and a 500-ps-wide pulsed field with a tunable delay to the microwave field. The switching field in a combination of these two fields becomes smaller than that in only the microwave field, and this additional reduction in switching field oscillates relative to the delay time. From the comparison with the results of micromagnetic simulations, we found that the oscillatory behavior is attributed to the beats in transient precession that occurs in the early stage of microwave-field-induced magnetization excitation.

  18. Microwave Assisted Hot Air Convective Dehydration of Fish Slice: Drying Characteristics, Energy Aspects and Colour Assessment

    Directory of Open Access Journals (Sweden)

    Mohd Rozainee Taib

    2011-01-01

    Full Text Available Dried fish is commonly produced by convective hot air drying. Microwave technology was presented in this paper to improve both process and product quality. Catfish (order Siluriformes slices were dehydrated in a microwave assisted hot air convective dehydration (MWHA system to investigate the effects of microwave power and hot air temperature on drying time, dehydration behaviour, energy consumption and colour of dried fish. Three different microwave power outputs namely medium (373 W, medium low (217 W and low (91 W combined with convective hot air temperature of 40°C, 70°C and 130°C accordingly were employed in the drying experiments. Results show that microwave accelerates drying time up to 120 folds faster compared to drying with hot air convective alone. It was also noted that increasing the hot air temperature was not as significant as increasing the microwave power in reducing the drying time. Experiments show that drying time was reduced about 75 % when an increase of microwave power from low (91 W to medium mode (373 W combining with convective hot air. However, drying with microwave alone required longer drying time. Energy consumption analysis shows that microwave assisted drying process requires less energy usage. Drying fish with microwave assisted hot air dehydration treatment make the colour brighter, shifting towards red and yellow.

  19. Microwave-assisted extraction of lignin from triticale straw: optimization and microwave effects.

    Science.gov (United States)

    Monteil-Rivera, Fanny; Huang, Guang Hai; Paquet, Louise; Deschamps, Stéphane; Beaulieu, Chantale; Hawari, Jalal

    2012-01-01

    Presently lignin is used as fuel but recent interests in biomaterials encourage the use of this polymer as a renewable feedstock in manufacturing. The present study was undertaken to explore the potential applicability of microwaves to isolate lignin from agricultural residues. A central composite design (CCD) was used to optimize the processing conditions for the microwave (MW)-assisted extraction of lignin from triticale straw. Maximal lignin yield (91%) was found when using 92% EtOH, 0.64 N H(2)SO(4), and 148 °C. The yield and chemical structure of MW-extracted lignin were compared to those of lignin extracted with conventional heating. Under similar conditions, MW irradiation led to higher lignin yields, lignins of lower sugar content, and lignins of smaller molecular weights. Except for these differences the lignins resulting from both types of heating exhibited comparable chemical structures. The present findings should provide a clean source of lignin for potential testing in manufacturing of biomaterials. Crown Copyright © 2011. Published by Elsevier Ltd. All rights reserved.

  20. A REVIEW ON: A SIGNIFICANCE OF MICROWAVE ASSIST TECHNIQUE IN GREEN CHEMISTRY

    Directory of Open Access Journals (Sweden)

    Manoj S. Charde

    2012-05-01

    Full Text Available Microwave Assisted Synthesis is rapidly becoming the method of choice in modern synthesis and discovery chemistry laboratories. Microwave-assisted synthesis improves both throughput and turn-around time for chemists by offering the benefits of drastically reduced reaction times, increased yields, and purer products. In this type of synthesis we applying microwave irradiation to chemical reactions. The fundamental mechanism of microwave heating involves agitation of polar molecules or ions that oscillate under the effect of an oscillating electric or magnetic field. In the presence of an oscillating field, particles try to orient themselves or be in phase with the field. Only materials that absorb microwave radiation are relevant to microwave chemistry. These materials can be categorized according to the three main mechanisms of heating, namely. Dipolar polarization, Conduction mechanism, Interfacial polarization. Microwave chemistry apparatus are classified: Single-mode apparatus and Multi-mode apparatus. Although occasionally known by such acronyms as 'MEC' (Microwave-Enhanced Chemistry or ‘MORE’ synthesis (Microwave-organic Reaction Enhancement, these acronyms have had little acceptance outside a small number of groups. The ability to combine microwave technology with in-situ reaction monitoring as an analytical tools will offer opportunities for chemists to optimize the reaction conditions. Different compounds convert microwave radiation to heat by different amounts. This selectivity allows some parts of the object being heated to heat more quickly or more slowly than others (particularly the reaction vessel.

  1. Microwave assisted organic modification and surface functionalization of Phyllosilicates

    CSIR Research Space (South Africa)

    Kesavan Pillai, Sreejarani

    2012-11-01

    Full Text Available Organically modified phyllosilicates (montmorillonite and palygorskite) using Arquad 2HT-75 surfactant were effectively synthesized utilizing a microwave irradiation technique. The microwave method was successfully used also for the surface...

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

    Science.gov (United States)

    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.

  3. Sugarcane Bagasse Pyrolysis in a Carbon Dioxide Atmosphere with Conventional and Microwave-Assisted Heating

    OpenAIRE

    Lin, Bo-Jhih; Chen, Wei-Hsin

    2015-01-01

    Pyrolysis is an important thermochemical method to convert biomass into bio-oil. In this study, the pyrolysis of sugarcane bagasse in a CO2 atmosphere under conventional and microwave-assisted heating is investigated to achieve CO2 utilization. In the microwave pyrolysis, charcoal is used as the microwave absorber to aid in pyrolysis reactions. The results indicate that the yields of pyrolysis products are greatly influenced by the heating modes. In the conventional heating, the prime product...

  4. Sugarcane bagasse pyrolysis in a carbon dioxide atmosphere with conventional and microwave-assisted heating

    OpenAIRE

    Bo-Jhih eLin; Wei-Hsin eChen

    2015-01-01

    Pyrolysis is an important thermochemical method to convert biomass into bio-oil. In this study, the pyrolysis of sugarcane bagasse in a CO2 atmosphere under conventional and microwave-assisted heating is investigated to achieve CO2 utilization. In the microwave pyrolysis, charcoal is used as the microwave absorber to aid in pyrolysis reactions. The results indicate that the yields of pyrolysis products are greatly influenced by the heating modes. In the conventional heating, the prime product...

  5. Microwave Assisted Synthesis and Characterization of Perovskite Oxides

    OpenAIRE

    Prado-Gonjal, Jesus; Schmidt, Rainer; Moran, Emilio

    2014-01-01

    The use of microwave irradiation is a promising alternative heat source for the synthesis of inorganic materials such as perovskite oxides. The method offers massive energy and time savings as compared to the traditional ceramic method. In this work we review the basic principles of the microwave heating mechanism based on interactions between dipoles in the material and the electromagnetic microwave. Furthermore, we comment on and classify all different sub-types of microwave synthesis such ...

  6. Microwave assisted flow synthesis: Coupling of electromagnetic and hydrodynamic phenomena

    NARCIS (Netherlands)

    Patil, N.G.; Benaskar, F.; Meuldijk, J.; Hulshof, L.A.; Hessel, V.; Schouten, J.C.; Esveld, D.C.; Rebrov, E.V.

    2014-01-01

    This article describes the results of a modeling study performed to understand the microwave heating process in continuous-flow reactors. It demonstrates the influence of liquid velocity profiles on temperature and microwave energy dissipation in a microwave integrated milli reactor-heat exchanger.

  7. A convenient microwave-assisted synthesis of cinchona alkaloid-derived ligands

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    An efficient synthesis of cinchona alkaloid-derived ligands based on solvent-free microwave-assisted reaction was described. The coupling of 1,4-dichlorophthalazine or 3,6-dichloropyridazine with quinine, cinchonine or cinchonidine provide bis- or mono-cinchona alkaloid-derived ligands in moderate to good yields (52-89%) within 15 rain under optimum microwave conditions.

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

    Science.gov (United States)

    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...

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

    Science.gov (United States)

    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…

  10. Ionic liquid-based ultrasonic/microwave-assisted extraction combined with UPLC-MS-MS for the determination of tannins in Galla chinensis.

    Science.gov (United States)

    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.

  11. Conventional wet impregnation versus microwave-assisted synthesis of SnO2/CNT composites

    CSIR Research Space (South Africa)

    Motshekga, S

    2011-03-01

    Full Text Available Carbon nanotubes decorated with SnO2 nanoparticles were prepared by conventional and microwave-assisted wet impregnation. The composites were thoroughly characterized by X-ray diffraction, Raman spectroscopy, BET-surface area measurement, Scanning...

  12. Comparative study on conventional, ultrasonication and microwave assisted extraction of γ-oryzanol from rice bran

    National Research Council Canada - National Science Library

    Kumar, Pramod; Yadav, Devbrat; Kumar, Pradyuman; Panesar, Paramjeet Singh; Bunkar, Durga Shankar; Mishra, Diwaker; Chopra, H K

    2016-01-01

    In present study, conventional, ultrasonic and microwave assisted extraction methods were compared with the aim of optimizing best fitting solvent and method, solvent concentration and digestion time for high yield of γ...

  13. An easy two-step microwave assisted synthesis of SnO2/CNT hybrids

    CSIR Research Space (South Africa)

    Motshekga, SC

    2011-11-01

    Full Text Available -ray diffraction, Raman spectroscopy, high resolution transmission electron microscopy, BET surface area analysis and DC conductivity measurement. The results showed that the microwave assisted synthesis is a very efficient method in producing CNTs that are heavily...

  14. Surface modification of titanium hydride with epoxy resin via microwave-assisted ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Ning, Rong [College of Materials Science and Engineering, Hunan University, Changsha 410082 (China); Chen, Ding, E-mail: ma97chen@hotmail.com [College of Materials Science and Engineering, Hunan University, Changsha 410082 (China); Zhang, Qianxia [College of Materials Science and Engineering, Hunan University, Changsha 410082 (China); Bian, Zhibing; Dai, Haixiong; Zhang, Chi [Jiangsu Jinling Special Paint Co., Ltd., Yangzhou 225212 (China)

    2014-10-15

    Highlights: • TiH{sub 2} was modified with epoxy resin by microwave-assisted ball milling. • The epoxy ring was opened under the coupling effect of microwave and ball milling. • Microwave-assisted ball milling improved the compatibility of TiH{sub 2} with epoxy. - Abstract: Surface modification of titanium hydride with epoxy resin was carried out via microwave-assisted ball milling and the products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), thermo-gravimetry (TG) and Fourier transform infrared spectroscopy (FT-IR). A sedimentation test was performed to investigate the compatibility of the modified nano titanium hydride with the epoxy resin. The results show that the epoxy resin molecules were grafted on the surface of nano titanium hydride particles during the microwave-assisted ball milling process, which led to the improvement of compatibility between the nanoparticles and epoxy resin. According to the FT-IR, the grafting site was likely to be located around the epoxy group due to the fact that the epoxy ring was opened. However, compared with microwave-assisted ball milling, the conventional ball milling could not realize the surface modification, indicating that the coupling effect of mechanical force and microwave played a key role during the process.

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

    OpenAIRE

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

    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, ...

  16. Microwave-Assisted Hydrothermal Synthesis of Cellulose/Hydroxyapatite Nanocomposites

    Directory of Open Access Journals (Sweden)

    Lian-Hua Fu

    2016-09-01

    Full Text Available In this paper, we report a facile, rapid, and green strategy for the synthesis of cellulose/hydroxyapatite (HA nanocomposites using an inorganic phosphorus source (sodium dihydrogen phosphate dihydrate (NaH2PO4·2H2O, or organic phosphorus sources (adenosine 5′-triphosphate disodium salt (ATP, creatine phosphate disodium salt tetrahydrate (CP, or D-fructose 1,6-bisphosphate trisodium salt octahydrate (FBP through the microwave-assisted hydrothermal method. The effects of the phosphorus sources, heating time, and heating temperature on the phase, size, and morphology of the products were systematically investigated. The experimental results revealed that the phosphate sources played a critical role on the phase, size, and morphology of the minerals in the nanocomposites. For example, the pure HA was obtained by using NaH2PO4·2H2O as phosphorus source, while all the ATP, CP, and FBP led to the byproduct, calcite. The HA nanostructures with various morphologies (including nanorods, pseudo-cubic, pseudo-spherical, and nano-spherical particles were obtained by varying the phosphorus sources or adjusting the reaction parameters. In addition, this strategy is surfactant-free, avoiding the post-treatment procedure and cost for the surfactant removal from the product. We believe that this work can be a guidance for the green synthesis of cellulose/HA nanocomposites in the future.

  17. Suitability of microwave-assisted extraction coupled with solid-phase extraction for organophosphorus pesticide determination in olive oil.

    Science.gov (United States)

    Fuentes, Edwar; Báez, María E; Quiñones, Adalí

    2008-10-17

    A systematic study of the microwave-assisted extraction coupled to solid-phase extraction of nine organophosphorus pesticides (dimethoate, diazinon, pirimiphos methyl, parathion methyl, malathion, fenthion, chlorpyriphos, methidathion and azinphos methyl) from olive oil is described. The method is based on microwave-assisted liquid-liquid extraction with partition of organophosphorus pesticides between an acetonitrile-dichloromethane mixture and oil. Cleanup of extracts was performed with ENVI-Carb solid-phase extraction cartridge using dichloromethane as the elution solvent. The determination of pesticides in the final extracts was carried out by gas chromatography-flame photometric detection and gas chromatography-tandem mass spectrometry, using a triple quadrupole mass analyzer, for confirmative purposes. The study and optimization of the method was achieved through experimental design where recovery of compounds using acetonitrile for partition ranged from 62 to 99%. By adding dichloromethane to the extracting solution, the recoveries of more hydrophobic compounds were significantly increased. Under optimized conditions recoveries of pesticides from oil were equal to or higher than 73%, except for fenthion and chlorpyriphos at concentrations higher than 0.06microgg(-1) and diazinon at 0.03microgg(-1), with RSDs equal to or lower than 11% and quantification limits ranging from 0.007 to 0.020microgg(-1). The proposed method was applied to residue determination of the selected pesticides in commercial olive and avocado oil produced in Chile.

  18. Microwave-assisted shingled magnetic recording simulations on an exchange-coupled composite medium

    Science.gov (United States)

    Tanaka, T.; Kashiwagi, S.; Kanai, Y.; Matsuyama, K.

    2016-10-01

    The potential of microwave-assisted magnetic recording combined with the shingled recording scheme has been studied by simulating read/write processes on exchange-coupled composite media focusing on recording characteristics in the cross-track direction. Microwave fields enhance writability, especially at the track edge, resulting in lower noise and higher signal-to-noise ratio (SNR), which enables higher track density in the shingled recording scheme. Read/write simulations of microwave-assisted shingled recording achieve 1.4 Mtracks/in. while retaining high SNR. Further increases in SNR and track density will require either a narrower reader or track edge noise reduction.

  19. Microwave-Assisted Routes for the Synthesis of Complex Functional Oxides

    Directory of Open Access Journals (Sweden)

    Jesús Prado-Gonjal

    2015-05-01

    Full Text Available The synthesis of complex functional inorganic materials, such as oxides, can be successfully performed by using microwave irradiation as the source of heat. To achieve this, different routes and set-ups can be used: microwave-assisted synthesis may proceed in the solid state or in solution, aqueous or not, and the set ups may be as simple and accessible as domestic oven or quite sophisticated laboratory equipment. An obvious advantage of this innovative methodology is the considerable reduction in time—minutes rather than hours or days—and, as a consequence, energy saving. No less important is the fact that the particle growth is inhibited and the broad variety of different microwave or microwave-assisted synthesis techniques opens up opportunities for the preparation of inorganic nanoparticles and nanostructures. In this work, various microwave synthesis techniques have been employed: solid-state microwaves, single-mode microwaves using a TE10p cavity and microwave-assisted hydrothermal synthesis. Relevant examples are presented and discussed.

  20. Semi-automated microwave assisted solid-phase peptide synthesis

    DEFF Research Database (Denmark)

    Pedersen, Søren Ljungberg

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

  1. Microwave-assisted extraction in toxicological screening of skeletal tissues.

    Science.gov (United States)

    Desrosiers, Nathalie A; Betit, Caroline C; Watterson, James H

    2009-07-01

    The use of microwave-assisted extraction (MAE) in screening of decomposed bone tissue for model drugs of abuse is described. Rats received 50 mg/kg (i.p.) pentobarbital (n=2), 75 mg/kg (i.p.) ketamine (n=2) or 16 mg/kg (i.p.) diazepam (n=1), or remained drug-free (control). Drug-positive animals were euthanized within 20 min of drug administration. Animal remains were allowed to decompose in a secure outdoor environment to the point of complete skeletonization. Bones (tibiae, femora, vertebrae, ribs, pelvi, humeri and scapulae) were collected and pooled (according to drug) in order to minimize effects due to inter-bone differences in drug distribution. Bones were crushed and cleaned of marrow and residual soft tissue in alkaline solution or phosphate buffer with ultrasonication. Cleaned bones were then ground and underwent MAE in phosphate buffer (pH 6), methanol or a methanol:water mixture (1:1, v/v) at atmospheric pressure in a domestic microwave oven, or passive extraction in methanol. Bone extracts (control and drug-exposed) containing methanol were evaporated to dryness before reconstitution in phosphate buffer (pH 6) and subsequent analysis by ELISA, while bone extracts containing only phosphate buffer were assayed directly by the same ELISA protocol. Measured absorbance values were expressed as the decrease in absorbance, measured as a percentage, relative to the corresponding drug-free control bone extract. The semi-quantitative nature of the ELISA assay allowed examination of the effects of extraction solvent and bone sample mass on the assay response for each drug examined, and subsequent comparison to assays of extracts obtained through passive methanolic extraction of various bone tissues. Overall, the time required for maximal extraction varied with extraction solvent and bone mass for each drug investigated, with significant extraction occurring with all solvent systems examined. MAE may represent a substantially faster extraction system than passive

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

    Science.gov (United States)

    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

  3. Non-polar Solvent Microwave-Assisted Extraction of Volatile Constituents from Dried Zingiber Officinale Rosc.

    Institute of Scientific and Technical Information of China (English)

    YU Yong; WANG Zi-Ming; WANG Yu-Tang; LI Tie-Chun; CHENG Jian-Hua; LIU Zhong-Ying; ZHANG Han-Qi

    2007-01-01

    A new method, non-polar solvent microwave-assisted extraction (NPSMAE), was applied to the extraction of essential oil from Zingiber officinale Rosc. in closed-vessel system. By adding microwave absorption mediumcarbonyl iron powders (CIP) into extraction system, the essential oil was extracted by the non-polar solvent (ether)which can be heated by CIP. The constituents of essential oil obtained by NPSMAE were comparable with those obtained by hydrodistillation (HD) by GC-MS analysis, which indicates that NPSMAE is a feasible way to extract essential oil from dried plant materials. The NPSMAE took much less extraction time (5 min) than HD (180 min),and its extraction efficiency was much higher than that of conventional polar solvent microwave-assisted extraction (PSMAE) and mixed solvent microwave-assisted extraction (MSMAE). It can be a good alternative for the extraction of volatile constituents from dried plant samples.

  4. Microwave-assisted synthesis of graphene–Ni composites with enhanced microwave absorption properties in Ku-band

    Energy Technology Data Exchange (ETDEWEB)

    Zhu, Zetao [College of Materials Science and Technology, Nanjing University of Aeronautics and Astronautics, 210016 Nanjing (China); Sun, Xin [Science and Technology on Electromagnetic Scattering Laboratory, 100854 Beijing (China); Li, Guoxian [Shenyang National Laboratory for Materials Science Institute of Metal Research, Chinese Academy of Sciences, 110016 Shenyang (China); Xue, Hairong; Guo, Hu; Fan, Xiaoli; Pan, Xuchen [College of Materials Science and Technology, Nanjing University of Aeronautics and Astronautics, 210016 Nanjing (China); He, Jianping, E-mail: jianph@nuaa.edu.cn [College of Materials Science and Technology, Nanjing University of Aeronautics and Astronautics, 210016 Nanjing (China)

    2015-03-01

    Recently, graphene has been applied as a new microwave absorber because of its high dielectric loss and low density. Nevertheless, the high dielectric constant of pristine graphene has caused unbalanced electromagnetic parameters and results in a bad impedance matching characteristic. In this study, we report a facile microwave-assisted heating approach to produce reduced graphene oxide–nickel (RGO–Ni) composites. The phase and morphology of as-synthesized RGO–Ni composites are characterized by XRD, Raman, FESEM and TEM. The results show that Ni nanoparticles with a diameter around 20 nm are grown densely and uniformly on the RGO sheets. In addition, enhanced microwave absorption properties in Ku-band of RGO–Ni composites is mainly due to the synergistic effect of dielectric loss and magnetic loss and the dramatically electron polarizations caused by the formation of large conductive network. The minimum reflection loss of RGO–Ni-2 composite with the thickness of 2 mm can reaches −42 dB at 17.6 GHz. The RGO–Ni composite is an attractive candidate for the new type of high performance microwave absorbing material. - Highlights: • Ni nanoparticles are grown densely and uniformly on the RGO sheets via microwave-assisted heating approach. • Ni resistance effect is proposed to explain the mechanism to decrease the permittivity with the rising combination of Ni and RGO. • The microwave absorption properties in Ku-band of RGO–Ni composites are effectively enhanced. • The mechanism to improve the microwave absorption properties is discussed.

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

    KAUST Repository

    Patole, Shashikant P.

    2015-10-21

    It is common for as-prepared carbon nanotube (CNT) and graphene samples to contain remnants of the transition metals used to catalyze their growth; contamination may also leave other trace elemental impurities in the samples. Although a full quantification of impurities in as-prepared samples of carbon nanostructures is difficult, particularly when trace elements are intercalated or encapsulated within a protective layer of graphitic carbon, reliable information is essential for reasons such as quantifying the adulteration of physico-chemical properties of the materials and for evaluating environmental issues. Here, we introduce a microwave-based fusion method to degrade single- and double-walled CNTs and graphene nanoplatelets into a fusion flux thereby thoroughly leaching all metallic impurities. Subsequent dissolution of the fusion product in diluted hydrochloric and nitric acid allowed us to identify their trace elemental impurities using inductively coupled plasma optical emission spectrometry. Comparisons of the results from the proposed microwave-assisted fusion method against those of a more classical microwave-assisted acid digestion approach suggest complementarity between the two that ultimately could lead to a more reliable and less costly determination of trace elemental impurities in carbon nanostructured materials. Graphical abstract A method for the complete digestion of carbon nanostructures has been demonstrated. Photographs (on the left side) show zirconium crucibles containing SWCNTs with flux of Na2CO3 and K2CO3, before and after microwave fusion; (on the right side) the appearance of the final solutions containing dissolved samples, from microwave-assisted fusion and microwave-assisted acid digestion. These solutions were used for determining the trace elemental impurities by ICP‒OES.

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

    Science.gov (United States)

    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.

  7. Microwave assisted apatite coating deposition on Ti6Al4V implants.

    Science.gov (United States)

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

    2013-10-01

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

  8. Microwave-assisted rock breaking modelling and application

    CSIR Research Space (South Africa)

    Monchusi, B

    2012-10-01

    Full Text Available As part of the ongoing development of novel mining methods, the CSIR has developed alternative methods to break rocks. In this case, we show the application of microwave energy to break narrow tabular ore bodies....

  9. short communication microwave assisted oxidative coupling of thiols ...

    African Journals Online (AJOL)

    Preferred Customer

    minimal amount of solvent under microwave irradiation. ... [7-8] and also the industrial applications of disulfides in the vulcanization of rubbers and ..... Holbrook, D.L. Handbook of Petroleum Refining Processes, Meyers, R.A. (Ed.), McGraw.

  10. Microwave-assisted additive free synthesis of nanocrystalline zinc oxide

    OpenAIRE

    Bhatte, Kushal D.; Tambade, Pawan; Fujita, Shin-ichiro; Arai, Masahiko; Bhalchandra M. Bhanage

    2010-01-01

    An additive free synthesis of nanocrystalline zinc oxide using microwave technique is reported. Current methodology is faster, cleaner and cost effective compared with conventional method for the synthesis of zinc oxide nanocrystalline materials. The structure and morphology of nanocrystalline zinc oxide was investigated by TEM, XRD, EDAX, UV-Vis spectroscopy. The results demonstrate that microwave heating can produce polygonal zinc oxide within a short span of time.

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

    Science.gov (United States)

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

    2016-10-01

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

  12. Comparison of Microwave-Assisted and Hydrodistillation Methods for Extraction of Essential Oil from Achillea millefolium

    Directory of Open Access Journals (Sweden)

    S. Mollasalehi

    2013-08-01

    Full Text Available Microwave-assisted hydrodistillation (MAHD method has been compared with hydrodistillation (HD conventional technique for extraction of essential oil from Achillea millefolium. Microwave-assisted hydrodistillation were examined at three levels of microwave powers (300, 500, and 700 W. Obtained results show that MAHD offers important advantages over HD in terms of energy savings and extraction time (20 min against 2.5 h. Also, the essential oils were analyzed by GC-MS. The amount of oxygenated compounds and monoterpene, such as 1,8 -Cineole, Lavandulyl acetate,Caryophylla-dien, Aromadendrene were increased in the microwave method. All these results suggest that MAHD represents an excellent alternative method for extraction of essential oils from plant materials.

  13. Microwave assisted synthesis of 2-pyridone and 2-pyridone based compounds

    Directory of Open Access Journals (Sweden)

    Mijin Dušan Ž.

    2014-01-01

    Full Text Available 2-Pyridones are important heterocyclic compounds that are widely used in medical chemistry, and their various derivatives have significant biological and medical applications. In this paper, the synthesis of 2-pyridones as well as 2-pyridone based compounds such as 2-quinolones using microwave assisted organic chemistry is reviewed. The review is divided in three parts. In the first part, microwave synthesis of 2-pyridones according to the type of condensation is discussed. In the second part, microwave assisted synthesis of 2-quionolones is listed. At the end of the review several examples of microwave synthesis of other 2-pyridone based compounds (ring fused N-substituted 2-pyridones are given. [Projekat Ministarstva nauke Republike Srbije, br. 172013

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

    Science.gov (United States)

    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.

  15. Microwave-assisted Ionothermal Synthesis and Characteriza- tion of Zeolitic Imidazolate Framework-8

    Institute of Scientific and Technical Information of China (English)

    杨丽莎; 卢惠民

    2012-01-01

    The zeolitic imidazolate framework-8 (ZIF-8) was successfully synthesized using ionic liquids as struc- ture-directing agent under microwave irradiation. Ionic liquids are green solvents with low vapour pressure and good thermal stability. They are appropriate templates for microporous materials and ideal microwave absorbers. The microwave-assisted ionothermal synthesis applied in this paper was expected to be a promising method for the preparation of microporous materials. Results showed that the as-synthesized samples (300---500 nm in diameter) could be synthesized in a short time (60 min) and possessed regular morphology, stable structure and high thermal stability (up to 720 ~C in argon atmosphere). Nitrogen adsorption-desorption test illustrated that samples produced by microwave heating had a higher surface area. Carbon dioxide adsorption test indicated that the samples synthe- sized by microwave heating had better carbon dioxide adsorption ability than those by conventional heating.

  16. RAPID SOLVENT-FREE MICROWAVE ASSISTED SYNTHESIS OF SOME N’-BENZYLIDENE SALICYLIC ACID HYDRAZIDES

    Directory of Open Access Journals (Sweden)

    Tutuk Budiati

    2012-06-01

    Full Text Available Condensation reaction has been carried out for the synthesis of some N'-benzylidene-2-hydroxybenzohydrazides using microwave assisted solvent-free method. The structures of all the products obtained in the present work are supported by spectral and analytical data (UV, IR, and 1H-NMR spectroscopy. The desired hydrazides are in 62-80% yields under microwave irradiation. The reaction was completed in 8-10 min.

  17. Experimental and modeling studies on microwave-assisted extraction of mangiferin from Curcuma amada

    OpenAIRE

    Kullu, Jeke; Dutta, Abhishek; Constales, Denis; Chaudhuri, Surabhi; Debjani DUTTA

    2013-01-01

    Mangiferin, a bioactive compound having potent nutraceutical, strong antioxidant and pharmacological significance has been extracted using microwave-assisted extraction (MAE) technique from Curcuma amada, commonly known as mango ginger. The extraction solvent ethanol is eco-friendly, nontoxic and reduces the risk of environmental hazards. The influence of several independent variables such as microwave power, ethanol concentration, extraction (irradiation) time and pre-leaching time has been ...

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

    Science.gov (United States)

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

    1996-05-01

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

  19. Fast, microwave-assisted synthesis of monodisperse HfO{sub 2} nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Roo, Jonathan De; Keukeleere, Katrien De; Feys, Jonas; Lommens, Petra [Ghent University, Sol-Gel Centre for Research on Inorganic Powders and Thin Films Synthesis (SCRiPTS) (Belgium); Hens, Zeger [Ghent University, Physics and Chemistry of Nanostructures (PCN) (Belgium); Driessche, Isabel Van, E-mail: Isabel.VanDriessche@ugent.be [Ghent University, Sol-Gel Centre for Research on Inorganic Powders and Thin Films Synthesis (SCRiPTS) (Belgium)

    2013-07-15

    A conventional solvothermal synthesis was compared to a microwave-assisted method for the synthesis of HfO{sub 2} nanoparticles. In a microwave, the reaction could be completed in 3 h, compared to 3 days in an autoclave. In the microwave synthesis, the ensemble of particles was found to have a better size dispersion and a smaller average size (4 nm). The reaction mechanism was investigated and proof for an ether elimination process was provided. Post-synthetic modification with dopamine or dodecanoic acid permitted the suspension of the synthesized particles in both polar and apolar solvents, which is an advantage for further processing.

  20. Low temperature microwave-assisted vs conventional pyrolysis of various biomass feedstocks

    Institute of Scientific and Technical Information of China (English)

    Peter Shuttleworth; Vitaliy Budarin; Mark Gronnow; James H. Clark; Rafael Luque

    2012-01-01

    A comparison between conventional pyrolysis and a novel developed low-temperature microwave-assisted pyrolysis methodology has been performed for the valorisation of a range of biomass feedstocks including waste residues.Microwave pyrolysis was found to efficiently deliver comparable evolution of bio-gases in the system as compared with conventional pyrolysis at significantly reduced temperatures (120-180 ℃ vs 250-400 ℃).The gas obtained from microwave-assistet pyrolysis was found to contain CO2,CH4 and CO as major components as well as other related chemicals (e.g.acids,aldehydes,alkanes) which were obtained in different proportions depending on the selected feedstock.

  1. Process Parameter Study on Microwave-assisted Foam-mat Drying Properties of Corn Soaking Water

    Institute of Scientific and Technical Information of China (English)

    Zheng Xian-zhe

    2016-01-01

    In order to study the microwave-assisted foam-mat drying properties of corn soaking water and optimize process parameters, a quadratic regression orthogonal rotary method was used to analyze the influence of microwave power, material weight, material thickness and drying time on moisture content (dry basis), color value and protein content. Results showed that the primary and secondary sequence of parameters with regard to moisture content (d. b.) was drying time, microwave power, material weight and material thickness; the primary and secondary sequence of parameters with regard to color value was material weight, drying time, microwave power and material thickness; the primary and secondary sequence of parameters with regard to protein content was drying time, material weight, microwave power and material thickness. Optimum conditions were obtained as microwave power of 560 W, material weight of 46.88 g, material thickness of 6.20 mm and drying time of 8.01 min. The results might provide the theoretical basis and technical support for the microwave-assisted foam-mat drying of corn soaking water to produce yeast protein power.

  2. Sugarcane bagasse pyrolysis in a carbon dioxide atmosphere with conventional and microwave-assisted heating

    Directory of Open Access Journals (Sweden)

    Bo-Jhih eLin

    2015-02-01

    Full Text Available Pyrolysis is an important thermochemical method to convert biomass into bio-oil. In this study, the pyrolysis of sugarcane bagasse in a CO2 atmosphere under conventional and microwave-assisted heating is investigated to achieve CO2 utilization. In the microwave pyrolysis, charcoal is used as the microwave absorber to aid in pyrolysis reactions. The results indicate that the yields of pyrolysis products are greatly influenced by the heating modes. In the conventional heating, the prime product is bio-oil and its yield is in the range of 51-54 wt%, whereas biochar is the major product in microwave-assisted heating and its yield ranges from 61 to 84 wt%. Two different absorber blending ratios of 0.1 and 0.3 are considered in the microwave pyrolysis. The solid yield decreases when the absorber blending ratio decreases from 0.3 to 0.1, while the gas and liquid yields increase. This is attributed to more energy consumed for bagasse pyrolysis at the lower blending ratio. Hydrogen is produced under the microwave pyrolysis and its concentration is between 2 and 12 vol%. This arises from the fact that the secondary cracking of vapors and the secondary decomposition of biochar in an environment with microwave irradiation is easier than those with conventional heating.

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

    Science.gov (United States)

    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.

  4. Microwave Assisted Alkali Pretreatment of Rice Straw for Enhancing Enzymatic Digestibility

    Directory of Open Access Journals (Sweden)

    Renu Singh

    2014-01-01

    Full Text Available Rapid industrialization, increasing energy demand, and climate change are the conditions that forced the researchers to develop a clean, efficient, renewable, and sustainable source of energy which has a potential to replace fossil fuels. Ethanol is one of the attractive and suitable renewable energy resources. In present study, effectiveness of microwave pretreatment in combination with sodium hydroxide (NaOH for increasing enzymatic hydrolysis of rice straw has been investigated and under optimum conditions obtained a maximum reducing sugar (1334.79 µg/mL through microwave assisted NaOH pretreatment. Chemical composition analysis and scanning electron microscope (SEM images showed that the removal of lignin, hemicellulose, and silicon content is more in microwave assisted NaOH pretreatment than the blank sample. X-ray diffraction (XRD analysis revealed that the crystallinity index of rice straw treated with microwave assisted alkali (54.55% is significantly high as compared to the blank (49.07%. Hence, the present study proves that microwave assisted alkali pretreatment can effectively enhance enzymatic digestibility of rice straw and it is feasible to convert rice straw for bioethanol production.

  5. Microwave assisted dehulling of black gram (Vigna mungo L).

    Science.gov (United States)

    Joyner, J Jerish; Yadav, B K

    2015-04-01

    This article summarises the results of the investigation of application of microwave exposure on the dehulling characteristics of the black gram and the properties of the dehulled grains. Black gram was exposed to 3 microwave power levels, viz., 450, 630 and 810 W for 7 different exposure, ranging from 60 to 150 s at an interval of 15 s with a view to determine the suitable combination of dosage in order to get the maximum yield with little change in colour. Related changes in properties were also studied. It was observed that the surface temperature of the grain increased with the increase in microwave power level from 450 to 810 W as well as exposure time from 60 to 150 s in the range from 58 to 123 °C while the dehulling time reduced from 445 to 170 s. The dehulling yield increased with increasing microwave dosage in the beginning and reached to the maximum value followed by decreasing trend. The colour of the dehulled grain changed slowly up to a microwave dosage of 972 J/g after that it changed vividly darker than the control. The dehulling and dhal yields and colour change were polynomial functions of microwave dosage. The highest yield of 73.7 % was achieved at about 972 J/g with a little change in colour (CIELAB ΔE* value of 2.58). The corresponding dehulling time, cooking time and losses during dehulling were respectively 185 s, 10 min and 15.1 % as compared to 492 s, 20 min and 31.5 % for control respectively. It is concluded that a dosage of about 972 J/g was the best for the black gram dehulling at a rate of 630 W or higher power level.

  6. Synthesis of benzamides by microwave assisted ring opening of less reactive dimethylaminobenzylidene oxazolone

    Directory of Open Access Journals (Sweden)

    Saurabh C. Khadse

    2017-02-01

    Full Text Available This paper presents the synthesis of some benzamide compounds (B1–B10 by microwave-assisted ring opening of 4-(4-dimethylaminobenzylidene-2-phenyl-5-oxazolone (AZ4. By conventional synthesis involving heating, it was found difficult to obtain ring-opened products, probably due to poor tendency of the carbonyl carbon (C5 of AZ4 to undergo nucleophilic attack by mono/or disubstituted anilines. Microwave assisted reactions were easy to perform, have reduced the reaction time and produced good yields.

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

    Science.gov (United States)

    Shukla, Himanshu S; Pratap, Amit

    2017-09-01

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

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

    Science.gov (United States)

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

    2012-11-27

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

  9. Microwave-assisted synthesis of transition metal phosphide

    Science.gov (United States)

    Viswanathan, Tito

    2014-12-30

    A method of synthesizing transition metal phosphide. In one embodiment, the method has the steps of preparing a transition metal lignosulfonate, mixing the transition metal lignosulfonate with phosphoric acid to form a mixture, and subjecting the mixture to a microwave radiation for a duration of time effective to obtain a transition metal phosphide.

  10. Microwave-Assisted Hydantoins Synthesis on Solid Support

    Science.gov (United States)

    Coursindel, Thibault; Martinez, Jean; Parrot, Isabelle

    2010-01-01

    In this laboratory activity, students are introduced to a three-step synthesis of hydantoin (imidazolidine-2,4-dione), a moiety that is found in many biologically active compounds. Using a microwave oven and solid-support technology, this synthetic experiment is designed for masters-degree candidates working in organic chemistry or upper-level…

  11. Microwave-Assisted Synthesis of Nanomaterials and Nanocomposites

    Science.gov (United States)

    The aqueous preparation of nanoparticles using vitamins B1 and B2, and vitamin C which can function both as reducing and capping agents prompted us accomplished the bulk syntheses of Ag and Fe nanorods using polyethylene glycol (PEG) under microwave (MW) irradiation conditions; t...

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

    Directory of Open Access Journals (Sweden)

    Trinath Biswal

    2010-10-01

    Full Text Available Trinath Biswal, Ramakanta Samal, Prafulla K SahooDepartment of Chemistry, Utkal University, Vani Vihar, Bhubaneswar 751004, IndiaAbstract: The polymerization of acrylonitrile (AN is efficiently, easily, and quickly achieved in the presence of trans-[Co(IIIen2Cl2]Cl complex in a domestic microwave (MW oven. MW irradiation notably promoted the polymerization reaction; this phenomenon is ascribed to the acceleration of the initiator, ammonium persulfate (APS, decomposition by microwave irradiation in the presence of [Co(IIIen2Cl2]Cl. The conversion of monomer to the polymer was mostly excellent in gram scale. Irradiation at low power and time produced more homogeneous polymers with high molecular weight and low polydispersity when compared with the polymer formed by a conventional heating method. The interaction of reacting components was monitored by UV-visible spectrometer. The average molecular weight was derived by gel permeation chromatography (GPC, viscosity methods, and sound velocity by ultrasonic interferometer. The uniform and reduced molecular size was characterized by transmission electron microscopy, the diameter of polyacrylonitrile nanoparticles (PAN being in the range 50–115 nm and 40–230 nm in microwave and conventional heating methods respectively. The surface morphology of PAN prepared by MW irradiation was characterized by scanning electron microscope (SEM. From the kinetic results, the rate of polymerization (Rp was expressed as Rp = [AN]0.63 [APS]0.57 [complex (I].0.88Keywords: microwave, complex catalyst, nanoparticle, kinetics

  13. Microwave-assisted reactions in heterocyclic compounds with applications in medicinal and supramolecular chemistry.

    Science.gov (United States)

    de la Hoz, Antonio; Díaz-Ortiz, Angel; Moreno, Andrés; Sanchéz-Migallón, Ana; Prieto, Pilar; Carrillo, José Ramón; Vázquez, Ester; Gómez, M Victoria; Herrero, M Antonia

    2007-12-01

    Microwave irradiation has been successfully applied in organic chemistry. Spectacular accelerations, higher yields under milder reaction conditions and higher product purities have all been reported. Indeed, a number of authors have described success in reactions that do not occur under conventional heating and modifications in selectivity (chemo-, regio- and stereoselectivity) have even been reported. Recent advances in microwave-assisted combinatorial chemistry include high-speed solid-phase and polymer-supported organic synthesis, rapid parallel synthesis of compound libraries, and library generation by automated sequential microwave irradiation. In addition, new instrumentation for high-throughput microwave-assisted synthesis continues to be developed at a steady pace. The impressive speed combined with the unmatched control over reaction parameters justifies the growing interest in this application of microwave heating. In this review we highlight our recent advances in this area, with a particular emphasis on cycloaddition reactions of heterocyclic compounds both with and without supports, applications in supramolecular chemistry and the reproducibility and scalability of organic reactions involving the use of microwave irradiation techniques.

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

    Science.gov (United States)

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

    2007-07-16

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

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

    Science.gov (United States)

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

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

    2016-09-01

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

  18. Microwave-assisted grinding of metallurgical coke; Molienda asistida con microondas de un coque metalurgico

    Energy Technology Data Exchange (ETDEWEB)

    Ruisanchez, E.; Juarez-Perez, E. J.; Arenillas, A.; Bermudez, J. M.; Menendez, J. A.

    2014-10-01

    Metallurgical cokes are composed of graphitic carbon (s2p2) and different inorganic compounds with very different capacities to absorb microwave radiation. Moreover, due to the electric conductivity shown by the metallurgical cokes, microwave radiation produces electric arcs or microplasmas, which gives rise to hot spots. Therefore, when these cokes are irradiated with microwaves some parts of the particle experiment a rapid heating, while some others do not heat at all. As a result of the different expansion and stress caused by thermal the shock, small cracks and micro-fissures are produced in the particle. The weakening of the coke particles, and therefore an improvement of its grind ability, is produced. This paper studies the microwave-assisted grinding of metallurgical coke and evaluates the grinding improvement and energy saving. (Author)

  19. Microwave assisted synthesis and optimization of Aegle marmelos-g-poly(acrylamide): release kinetics studies.

    Science.gov (United States)

    Setia, A; Kumar, R

    2014-04-01

    Microwave assisted grafting of poly(acrylamide) on to Aegle marmelos gum was carried out employing 3-factor 3-level full factorial design. Microwave power, microwave exposure time and concentration of gum were selected as independent variable and grafting efficiency was taken as dependent variable. A. marmelos-g-poly(acrylamide) was characterized by FTIR, DSC, X-ray diffraction and scanning electron microscopy. Microwave power, microwave exposure time had synergistic effect on grafting efficiency where as concentration of the gum did not contributed much to grafting efficiency. Batch having microwave power - 80%, microwave exposure time -120 s and concentration of A. marmelos gum - 2% was selected as the optimized formulation. Comparative release behaviour of diclofenac sodium from the matrix tablets of A. marmelos gum and A. marmelos-g-polyacrylamide was evaluated. The results of kinetic studies revealed that the graft copolymer matrix, marketed tablets and polymer matrix tablets of A. marmelos gum released the drug by zero order kinetics and with n value greater than 1, indicating that the mechanism for release as super case II transport i.e. dominated by the erosion and swelling of the polymer.

  20. Microwave-Assisted Radiosynthesis of [18F]Fluorinated Fatty Acid Analogs

    Science.gov (United States)

    Belanger, Anthony P.; Pandey, Mukesh K.; DeGrado, Timothy R.

    2010-01-01

    Microwave reactors remain largely underutilized in the field of PET chemistry. This is particularly unfortunate since microwave synthesis elegantly addresses two of the most critical issues of PET radiochemistry with short-lived radionuclides: reaction rate and side-product formation. In this study we investigate the efficiency of synthesis of terminally [18F]fluorinated fatty acid analogs using a commercial microwave reactor in comparison with conventional heating. Methods The labeling precursors were methyl esters of terminally substituted alkyl bromides and iodides. Duration and temperatures of the [18F]fluorination reaction were varied. Chemical and radiochemical purities, and radiochemical yields were investigated for conventional (CH) and microwave-assisted (MW) radiosyntheses. Results The results demonstrate that microwave heating enhanced [18F]fluoride incorporation to >95% (up to 55% improvement), while reducing reaction times to 2 min (~10-fold reduction) or temperatures to 55–60°C (20°C reduction). Overall decay-corrected radiochemical yields of purified [18F]fluoro fatty acids were higher (MW=49.0 ± 4.5%, CH=23.6 ± 3.5%, p<0.05) with microwave heating and side-products were notably fewer. Conclusion For routine synthesis of [18F]fluoro fatty acid analogs, microwave heating is faster, milder, cleaner, less variable and higher yielding than conventional heating and therefore the preferred reaction method. PMID:21492792

  1. Microwave-assisted degradation of acid orange using a conjugated polymer, polyaniline, as catalyst

    Directory of Open Access Journals (Sweden)

    Ufana Riaz

    2014-01-01

    Full Text Available Microwave-assisted photocatalytic degradation of dyes is one of the emerging technologies for waste water remediation. Microwave effectively accelerates photocatalytic degradation, when microwave electrodeless lamp (MEL substitutes traditional UV lamp as light source. This setup can be extremely simplified if MEL and photocatalyst can be replaced by a catalyst which can work under microwave irradiation in the absence of any light source. The present work reports for the first time degradation of acid orange 7 (AO under microwave irradiation using polyaniline (PANI as catalyst in the absence of any UV lamp as light source. The degradation/decolourization was carried out in neutral acidic and basic media and was monitored spectrophotometrically to evaluate the ability of microwave irradiation to degrade AO. Microwave irradiation showed excellent performance as it completely decolourizes AO dye solution in 10 min. With the advantages of low cost and rapid processing, this novel catalyst is expected to gain promising application in the treatment of various dyestuff wastewaters on a large scale.

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

    Science.gov (United States)

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

    2015-06-01

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

  3. Microwave-assisted brazing of alumina ceramics for electron tube applications

    Indian Academy of Sciences (India)

    2016-04-01

    Alumina was joined with alumina using microwave-assisted and conventional brazing methods at 960$^{\\circ}$C for 15 min using TiCuSil (68.8Ag–26.7Cu–4.5Ti in wt.%) as the brazing alloy. The brazed joints were characterizedby X-ray diffraction, scanning electron microscopy, energy dispersive X-ray analysis, Vickers microhardness evaluation, brazing strength measurement and helium leak test. X-ray diffraction analysis confirmed the formationof Ti-based compounds at the substrate-filler alloy interfaces of the microwave and conventionally brazed joints. The elemental compositions at the joint cross-section were determined by energy dispersive X-ray analysis. Vickers microhardness measurement indicated reliable joint performance for the microwave-assisted brazed joints during actual application in an electron tube. Brazing strength measurement and helium leak test provided the evidence forgood alumina-alumina joint formation.

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

    Science.gov (United States)

    Abano, Ernest Ekow

    2016-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Ernest Ekow Abano

    2016-01-01

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

  6. Microwave-assisted addition of azomethines to isatoic anhydride

    Indian Academy of Sciences (India)

    E Dominic Jacob; Lopez Mathew; Baby Thomas

    2007-01-01

    Diels-Alder addition of azomethines to isatoic anhydride in a solvent-free and eco-friendly condition is investigated using a microwave oven. The product is exclusively 2,3-diaryl-2,3-dihydroquinazolin-4(1H)-ones 4a-d. HOMO-LUMO energy of the iminoketene and the dienophiles were calculated using semi-empirical AM1 calculations.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

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

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

    Science.gov (United States)

    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...

  10. Microwave-assisted one-pot synthesis of benzothiazole and benzoxazole libraries as analgesic agents

    Indian Academy of Sciences (India)

    C Praveen; A Nandakumar; P Dheenkumar; D Muralidharan; P T Perumal

    2012-05-01

    Microwave-assisted synthesis of benzothiazole and benzoxazole libraries via PIFA promoted cyclocondensation of 2-aminothiophenols/2-aminophenols with aldehydes under one-pot condition in good to excellent yields was achieved. Twenty compounds have been investigated for their analgesic activity and showed moderate to good activity.

  11. Solvent-free microwave-assisted synthesis of oxadiazoles containing imidazole moiety

    Indian Academy of Sciences (India)

    Priya V Frank; K S Girish; Balakrishna Kalluraya

    2007-01-01

    Microwave-assisted as well as conventional synthesis of 5-substituted-2-(2-methyl-4-nitro-1-imidazomethyl)-1,3,4-oxadiazoles containing the nitroimidazole moiety is carried out and their antibacterial, antifungal and anti-inflammatory activity is reported.

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

    Science.gov (United States)

    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...

  13. Microwave-assisted solid-phase Ugi four-component condensations

    DEFF Research Database (Denmark)

    Nielsen, John

    1999-01-01

    An 18-member library was constructed from 2 isocyanides, 3 aldehydes and 3 carboxylic acids via microwave-assisted solid-phase Ugi reactions on TentaGel S RAM. Products of high purity were obtained in moderate to excellent yields after reaction times of 5 minutes or less (irradiation at 60W). (C...

  14. Microwave-assisted synthesis of geopolymers from fluidised bed gasifier bottom ash

    CSIR Research Space (South Africa)

    Oboirien, BO

    2013-09-01

    Full Text Available -1 International Conference of Coal Science and Technology, State College, Pennysylvania, USA, 29 September- 3 October 2013 Microwave-assisted synthesis of geopolymers from fluidised bed gasifier bottom ash B.O. Oboirien1, B.C. North1 and E. R. Sadiku2...

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

    Science.gov (United States)

    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...

  16. Microwave assisted air drying of osmotically treated pineapple with variable power programmes

    CSIR Research Space (South Africa)

    Botha, GE

    2012-01-01

    Full Text Available Variable power programmes for microwave assisted air drying of pineapple were studied. The pineapple pieces were pre-treated by osmotic dehydration in a 55º Brix sucrose solution at 40ºC for 90 minutes. Variable power output programmes were designed...

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

    Science.gov (United States)

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

    2011-02-07

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

  18. Microwave-assisted fast and efficient synthesis of some crown ethers

    Institute of Scientific and Technical Information of China (English)

    Ahmad Ziafati; Hossein Eshghi; Omolbanin Sabzevari

    2009-01-01

    13-Crown-4, 16-crown-5, dibenzo-12-crown-4 and dibenzo-14-crown-4 were synthesized by a one-pot microwave-assisted procedure in good yields. Irradiation of diols and dichlorides in the presence of sodium hydroxide in DMSO gave title crown ethers presumably within a template effect.

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

    DEFF Research Database (Denmark)

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

    2014-01-01

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

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

    Science.gov (United States)

    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 NOx, 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 NOx 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.

  1. Heat-Modeling of Microwave Assisted Epoxidation of Palm Acid Oil

    Directory of Open Access Journals (Sweden)

    N. Saifuddin

    2011-01-01

    Full Text Available Problem statement: While microwave chemistry could well be the most convenient, rapid and energy-saving way to initiate a chemical reaction, the issues of thermal versus microwave specific effect remain unaddressed. Approach: A three-dimensional Finite Element Model (FEM was developed to predict temperature profile during the enzymatic epoxidation of palm acid oil using microwave heating. Three-dimensional partial differential equations are formulated for the electromagnetic field and heat and mass transfer processes. The temperature profile of the FEM generated from the commercial software (ANSYS Emag was verified using experimental data from microwave oven heated samples containing palm acid oil and reactants in cylindrical bottles and has compared favorably with real time data. An Infra Red thermometer was used to measure temperature of the reactants during the real time experiment to ensure less contact with the reaction vessel. Results: Apart from ascertaining the temperature profile of the epoxidation process in the cylindrical bottle, the heat-modeling of this reaction can predict the Energy required during the reaction and provide insights to non-thermal microwave effects. It has shown the possibility of Microwave Non-Thermal Effects and Microwave Selectivity in Substrate Specificity. The energy used by the microwave irradiated reaction is by far much lesser than the energy used in conventional heating. This study has also improved the epoxidation process of Palm Acid Oil by incorporating enzyme as a catalyst and using microwave heating. Epoxidation can be done rapidly and at a lower level of activation energy of 27.767 kJ mol−1. It is a green process with increased efficiency as it reduced a typically 5-hour reaction to less than an hour. Conclusion: In this study, a quantitative view of a microwave assisted process of enzymatic epoxidation has been established. We have successfully developed and experimentally

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

    Science.gov (United States)

    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.

  3. Optimization and comparison of ultrasound/microwave assisted extraction (UMAE) and ultrasonic assisted extraction (UAE) of lycopene from tomatoes.

    Science.gov (United States)

    Lianfu, Zhang; Zelong, Liu

    2008-07-01

    The extracting technology including ultrasonic and microwave assisted extraction (UMAE) and ultrasonic assisted extraction (UAE) of lycopene from tomato paste were optimized and compared. The results showed that the optimal conditions for UMAE were 98 W microwave power together with 40 KHz ultrasonic processing, the ratio of solvents to tomato paste was 10.6:1 (V/W) and the extracting time should be 367 s; as for UAE, the extracting temperature was 86.4 degrees C, the ratio of the solvents to tomato paste was 8.0:1 (V/W) and the extracting time should be 29.1 min, while the percentage of lycopene yield was 97.4% and 89.4% for UMAE and UAE, respectively. These results implied that UMAE was far more efficient extracting method than UAE.

  4. A study of pressureless microwave sintering, microwave-assisted hot press sintering and conventional hot pressing on properties of aluminium/alumina nanocomposite

    Energy Technology Data Exchange (ETDEWEB)

    Abedinzadeh, Reza; Safavi, Seyed Mohsen; Karimzadeh, Fathallah [Isfahan University, Isfahan (Iran, Islamic Republic of)

    2016-05-15

    Bulk Al/4wt-%Al{sub 2}O{sub 3} nanocomposites were prepared by consolidating nanocomposite powders using pressureless microwave sintering, microwave-assisted hot press sintering and conventional hot pressing techniques. Microstructural observations revealed that the microwave-assisted hot press sintering at different sintering temperatures of 400.deg.C and 500.deg.C resulted in more densification and smaller grain size for Al/Al{sub 2}O{sub 3} nanocomposite as compared with the conventional hot pressing. Moreover, the application of pressure in microwave sintering process led to more densification and grain growth. Mechanical properties resulting from microhardness and nanoindentation tests were also compared between three-method processed samples. It was found that the microwave-assisted hot-pressed sample exhibited higher hardness and elastic modulus in comparison with microwave-sintered and conventional hot-pressed samples. The improvement in the mechanical properties can be ascribed to lower porosity of microwave-assisted hot-pressed sample.

  5. Enhancement of flame development by microwave-assisted spark ignition in constant volume combustion chamber

    KAUST Repository

    Wolk, Benjamin

    2013-07-01

    The enhancement of laminar flame development using microwave-assisted spark ignition has been investigated for methane-air mixtures at a range of initial pressures and equivalence ratios in a 1.45. l constant volume combustion chamber. Microwave enhancement was evaluated on the basis of several parameters including flame development time (FDT) (time for 0-10% of total net heat release), flame rise time (FRT) (time for 10-90% of total net heat release), total net heat release, flame kernel growth rate, flame kernel size, and ignitability limit extension. Compared to a capacitive discharge spark, microwave-assisted spark ignition extended the lean and rich ignition limits at all pressures investigated (1.08-7.22. bar). The addition of microwaves to a capacitive discharge spark reduced FDT and increased the flame kernel size for all equivalence ratios tested and resulted in increases in the spatial flame speed for sufficiently lean flames. Flame enhancement is believed to be caused by (1) a non-thermal chemical kinetic enhancement from energy deposition to free electrons in the flame front and (2) induced flame wrinkling from excitation of flame (plasma) instability. The enhancement of flame development by microwaves diminishes as the initial pressure of the mixture increases, with negligible flame enhancement observed above 3. bar. © 2013 The Combustion Institute.

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

    Directory of Open Access Journals (Sweden)

    Yang Song

    2011-08-01

    Full Text Available 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.

  7. Highly efficient isocyanate-free microwave-assisted synthesis of [6]-oligourea

    KAUST Repository

    Qaroush, Abdussalam K.

    2013-01-01

    A new eco-friendly, isocyanate-free, energy-saving method for the production of [6]-oligourea, utilizing a green carbonylating agent, viz. propylene carbonate, is reported. It comprises an organocatalyzed, microwave-assisted, solvent-free synthesis. Two modes of microwave-assisted synthesis, viz. dynamic and fixed energy modes, were applied. Upon optimization, the dynamic mode gave 79% yields of [6]-oligourea. On the other hand, almost quantitative yields were obtained using the fixed mode, within 20 min, at 10 W and with the same catalyst loading. Combination of both organocatalysis and microwave energy input appears to be a key issue for the efficiency of the reaction, with the fixed energy mode being best suited. It should be noted that all data reported are reproducible (due to the homogeneous microwave technology used by CEM Discover S-Class of microwave reactors). To the best of our knowledge, this is the best eco-friendly synthetic approach for the preparation of the title oligomers. It paves the way for using more of the biorenewable and sustainable chemicals as a feedstock for the production of polyureas. The oligomer produced was analyzed by EA, ATR-FTIR, XRD, 1H and 13CNMR. Furthermore, thermal properties of the resulting [6]-oligourea were analyzed using TGA and DSC. © The Royal Society of Chemistry 2013.

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

    Science.gov (United States)

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

    2014-07-17

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

  9. Fatty Acid Characteristics of Isochrysis galbana Lipids Extracted Using a Microwave-Assisted Method

    Directory of Open Access Journals (Sweden)

    Cherng-Yuan Lin

    2015-02-01

    Full Text Available Lipids were extracted from Isochrysis galbana using a microwave-assisted method accompanied by various types of organic solvents. The effects of organic solvent type and microwave input energy on the fatty acid characteristics of the extracted lipids and their biodiesel product were investigated. Variations in the characteristics of the lipids extracted using a combination of n-hexane and iso-propanol solvents in both emulsion and direct mixtures were also compared. The experimental results showed that greater quantities of Isochrysis galbana lipids, and fatty acid methyl esters transesterified from those lipids, were extracted when using microwave irradiation with an organic solvent mixture of n-hexane and isopropanol in a 2:1 volumetric ratio than when using either n-hexane or isopropanol as the sole solvent. A greater quantity of Isochrysis galbana lipids was extracted when an emulsion of isopropanol solvent evenly dispersed in the continuous phase of n-hexane solvent was used than when a direct mixture of the two solvents was used. In addition, the quantity of lipids extracted from the dried Isochrysis galbana powder with the assistance of microwave irradiation was 9.08 wt% greater than when using traditional Soxhlet extraction without microwave irradiation.

  10. Microwave assisted click chemistry on a conductive polymer film

    DEFF Research Database (Denmark)

    Daugaard, Anders Egede; Hansen, Thomas S.; Larsen, Niels Bent

    2011-01-01

    Microwave (MW) irradiation has been used to accelerate the functionalization of an azide functional poly(3,4-ethylenedioxythiophene) film by click chemistry. The absorption of MW energy by the conductive polymer has been exploited for localized activation of the reaction on the polymer surface....... The method has been applied for anchoring of the chelating agent nitrilotriacetic acid (NTA) on the conductive polymer. The chelating linkage ability of NTA on the surface was investigated through a sandwich ELISA study confirming the selective bonding of a histidine tagged protein....

  11. Microwave and blanch-assisted drying of white yam (Dioscorea rotundata).

    Science.gov (United States)

    Abano, Ernest Ekow; Amoah, Robert Sarpong

    2015-11-01

    The effect of microwave and blanch pretreatments on the drying kinetics and quality of white yam (Dioscorea rotundata) was investigated. Yam cubes destined for hot air drying at temperatures 70-90°C were predried in a domestic microwave or blanched in hot water for 1-5 min. Microwave pretreatment time had a positive significant effect on drying rate but both pretreatments had a negative influence on the ascorbic acid content and the nonenzymatic browning. The optimum drying conditions were a microwave pretreatment time of 5 min and a temperature of 70°C and a blanching time of 1 min at a temperature of 80°C. Among the models fitted, the Midilli et al. and the Page models gave the best fits for yam cubes predried with microwave and blanch, respectively. The effective moisture diffusivity for microwave-assisted drying increased from 1.05 × 10(-8 )m(2 )s(-1) to 2.00 × 10(-8) m(2 )s(-1) while the hot water blanched samples decreased from 1.53 × 10(-8) to 8.81 × 10(-9 )m(2 )s(-1) with time. The study demonstrates that microwave-assisted drying could be used to enhance heat and mass transfer processes to produce better quality dried yam products.

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

    Energy Technology Data Exchange (ETDEWEB)

    Xiaodi Huang; J.Y. Hwang

    2007-04-18

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

  13. Microwave-Assisted Solid Phase Organic Synthesis.Application to Indole Library Construction

    Institute of Scientific and Technical Information of China (English)

    DAI Wei-Min; SUN Li-Ping; GUO Dian-Shun; HUANG Xiang-Hong

    2004-01-01

    Microwave-assisted organic synthesis (MAOS) has attained increasing popularity due to recent advancement in the instrumentation of microwave technology. Now, MAOS can be performed under controlled temperature and pressure to yield reproducible results. For combinatorial chemistry,the dramatically increased reaction rate under microwave irradiation at high temperature provides an ideal solution to those sluggish reactions, in particular the combinatorial reactions carried out on solid supports. In this presentation, we describe our results on microwave-assisted solid-phase organic synthesis (MASPOS) applied to the construction of indole libraries such as 5. Compounds 4 were synthesized on the Rink amide resins using IRORI MicroKanTM reactors encoded with a radio-frequency (Rf) tag. The resin-bound terminal alkynes 2, prepared via the amide bond, were cross-coupled with the nitroaryl triflate under the conditions adopted from the solution reactions developed by us1,2. The nitro group of 3 was then reduced and sulfonylated to give 4. Ring closure reactions within 4 with Cu(OAc)2 were examined initially in refluxing DCE for 24 h, but no indole product was detected after cleavage from the resin. Therefore, the same reactions were carried out under microwave irradiation at 200 ℃ for 10 min on a Personal Chemistry Emrys Creator, the desired indoles 5 were obtained in 60-95% overall yields calculated from 1 and in >90% purities in most cases3. It is necessary to mention that the IRORI microreactors cannot tolerate the high temperature and the resin-bound 4 must be transferred to the reaction vials for the microwave-assisted ring closure reactions. A traceless synthesis of an indole library via MASPOS will be discussed as well.4

  14. Polyol synthesis of nanosized Pt/C electrocatalysts assisted by pulse microwave activation

    Energy Technology Data Exchange (ETDEWEB)

    Lebegue, E.; Baranton, S.; Coutanceau, C. [Laboratoire de Catalyse en Chimie Organique (LACCO), UMR 6503 CNRS, Universite de Poitiers, 40 av recteur Pineau, F-86000 Poitiers (France)

    2011-02-01

    A polyol process assisted by pulse microwave activation was used to prepare efficient Pt/C electrocatalysts for PEMFC applications with reducing cost. Catalysts from pulsed microwave method were compared with a catalyst issued from a classical method, in terms of active surface area, platinum loading and activity towards the oxygen reduction reaction. A design of experiments (DOE derived from the Taguchi method) has been implemented to optimize experimental parameters only related to pulse microwave activation, the intrinsic synthesis parameters (concentration of platinum salt, platinum/carbon weight ratio and pH) being kept constant. Controlled parameters were duration of microwave pulse, maximum temperature and total duration of the synthesis. Considered responses were catalyst active surface area and the Pt/C loading. An optimized configuration of synthesis parameter was proposed. The confirmation experiment revealed a trend in agreement with that expected. Three catalysts (two from pulsed microwave synthesis method and one prepared by the classical method) were characterized by transmission electron microscopy, cyclic voltammetry and CO stripping. Catalysts from pulsed microwave method display higher characteristics than the one prepared by the classical method. The Pt/C catalyst from the confirmation experiment displays the highest catalytic activity toward oxygen reduction reaction. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

    Preda, Silviu, E-mail: predas01@yahoo.co.uk [Institute of Physical Chemistry “Ilie Murgulescu”, 202 Splaiul Independentei, 060021 Bucharest (Romania); Rutar, Melita [Jožef Stefan Institute, Jamova cesta 39, SI-1000 Ljubljana (Slovenia); Jožef Stefan International Postgraduate School, Jamova cesta 39, SI-1000 Ljubljana (Slovenia); Umek, Polona [Jožef Stefan Institute, Jamova cesta 39, SI-1000 Ljubljana (Slovenia); Zaharescu, Maria [Institute of Physical Chemistry “Ilie Murgulescu”, 202 Splaiul Independentei, 060021 Bucharest (Romania)

    2015-11-15

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

  16. Microwave assisted solvent free synthesis of 1,3-diphenylpropenones

    Directory of Open Access Journals (Sweden)

    Sarma Jadab C

    2011-02-01

    Full Text Available Abstract Background 1,3-Diphenylpropenones (chalcones are well known for their diverse array of bioactivities. Hydroxyl group substituted chalcones are the main precursor in the synthesis of flavonoids. Till date various methods have been developed for the synthesis of these very interesting molecules. Continuing our efforts for the development of simple, eco-friendly and cost-effective methodologies, we report here a solvent free condensation of aryl ketones and aldehydes using iodine impregnated alumina under microwave activation. This new protocol has been applied to a variety of substituted aryl carbonyls with excellent yield of substituted 1,3-diphenylpropenones. Results Differently substituted chalcones were synthesized using iodine impregnated neutral alumina as catalyst in 79-95% yield in less than 2 minutes time under microwave activation without using any solvent. The reaction was studied under different catalytic conditions and it was found that molecular iodine supported over neutral alumina gives the best yield. The otherwise difficult single step condensation of hydroxy substituted aryl carbonyls is an attractive feature of this protocol to obtain polyhydroxychalcones in excellent yields. In order to find out the general applicability of this new endeavor it was successfully applied for the synthesis of 15 different chalcones including highly bioactive prenylated hydroxychalcone xanthohumol. Conclusion A new, simple and solvent free method was developed for the synthesis of substituted chalcones in environmentally benign way. The mild reaction conditions, easy work-up, clean reaction profiles render this approach as an interesting alternative to the existing methods.

  17. Microwave assisted antibacterial chitosan-silver nanocomposite films.

    Science.gov (United States)

    Raghavendra, Gownolla Malegowd; Jung, Jeyoung; Kim, Dowan; Seo, Jongchul

    2016-03-01

    In the current approach, antibacterial chitosan-silver nanocomposite films were fabricated through microwave irradiation. During the process, by utilizing chitosan as reducing agent, silver nanoparticles were synthesized within 11 min by microwave irradiation. Further, films were fabricated within 90 min. It involved an energy consumption of just 0.146 kWh to synthesize silver nanoparticles. This is many times less than the energy consumed during conventional methods. The silver nanoparticles were examined through UV-vis spectrum and transmission electron microscopy (TEM). The fabricated films were characterized by using scanning electron microscopy coupled with an energy dispersive spectrometer (SEM-EDS), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), and contact angle (CA) measurements. The films exhibited antibacterial properties against both Gram-negative micro-organisms (Escherichia coli; E. coli) and Gram-positive micro-organisms (Staphylococcus aureus; S. aureus). In overall, the procedure adopted for fabricating these antibacterial films is environmental friendly, time-saving and energy-saving.

  18. A novel microwave synthesis of calcium hydroxyapatite. Optimisation and investigation of a microwave assisted reaction route

    CERN Document Server

    Zawahreh, Y

    2001-01-01

    Hydroxyapatite is a bioactive calcium phosphate used in non-load bearing applications, such as space-filling in maxillofacial reconstruction. As a coating, hydroxyapatite is used on load-bearing orthopaedic metal prostheses to improve fixation and/or biocompatibility. Conventional synthesis processes for the production of hydroxyapatite are time-consuming and labour-intensive. Microwave irradiation was investigated as a means to enhance the synthesis reaction using calcium hydroxide (Ca(OH) sub 2) and orthophosphoric acid (H sub 3 PO sub 4) as reactants. An initial set of reactions indicated the feasibility of the microwave synthesis route. Optimisation reactions were then performed followed by investigation sets of reactions. Parameters such as microwave power, irradiation time, and reactant concentrations were varied. Using 0.5M Ca(OH) sub 2 and 0.3M H sub 3 PO sub 4 , a phase-pure hydroxyapatite powder with a stoichiometric molar Ca/P ratio of 1.67 was produced in 60 seconds at 450W and 2.45GHz. The microw...

  19. Microwave Assisted Hydrolysis of Holocellulose Catalyzed with Sulfonated Char Derived from Lignin-Rich Residue

    Directory of Open Access Journals (Sweden)

    Kui Wang

    2015-01-01

    Full Text Available A microwave assisted green process has been developed for production of sugars through liquefying holocellulose catalyzed with sulfonated char derived from the lignin-rich residue produced during pretreatment of lignocellulose. Various reaction parameters including the hydrolysis temperature, hydrolysis time, catalyst content, and the ratio of water to feedstock were evaluated. The maximum sugars yield of 82.6% (based on the dry mass of holocellulose was obtained under the optimum reaction conditions. The sulfonated char showed superior catalytic performance to that of dilute sulfuric acid in converting holocellulose into sugars under microwave irradiation.

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

    Energy Technology Data Exchange (ETDEWEB)

    Vaidhyanathan, B.; Balaji, K.; Rao, K.J. [Indian Inst. of Science, Bangalore (India). Solid State and Structural Chemistry Unit

    1998-11-01

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

  1. Efficient microwave-assisted synthesis of 5-hydroxymethylfurfural from concentrated aqueous fructose

    DEFF Research Database (Denmark)

    Søndergaard Hansen, Thomas; Woodley, John; Riisager, Anders

    2009-01-01

    Studies on the HCl-catalysed microwave-assisted dehydration of highly concentrated aqueous fructose (27 wt %) to 5-hydroxymethylfurfural (HMF) revealed a significant increase in the fructose conversion rate over the conventional heated systems. Water, being the most benign solvent and therefore...... ideal for green and sustainable chemistry, normally is a poor solvent for the dehydration process resulting in low HMF selectivities and yields. However, reaction at 200 °C with microwave irradiation with a short reaction time of only 1 s resulted in good HMF selectivity of 63% and fructose conversion...

  2. Microwave assisted bi-functional activation of -bromo-tert-alcohols

    Indian Academy of Sciences (India)

    Nandini Kannan; Manjunatha Javagal Rangaswamy; Bettadaiah Bheemanakere Kemapaiah

    2015-08-01

    Microwave-assisted dehydration-oxidation of -bromo-tert-alcohols to afford 2,3-unsaturated ketones in good yield is reported. The reaction of substrates with DMSO in 1:1 ratio (w/v) is promoted by ZnS in a solvent-free condition. A concurrent bi-functional activation of trans-vicinal bromo- and hydroxyl groups with ZnS is elucidated. This is a new observation under microwave and applies to -bromo-tert-alcohols derived from 1,4-disubstitued-1-cyclohexenes. It is very useful in the synthesis of 2,3-unsaturated ketones derived from monoterpenes which are valuable flavour compounds.

  3. Microwave-assisted synthesis of α-aryl malonates: Key intermediates for the

    Directory of Open Access Journals (Sweden)

    Mohamed A. Ibrahim

    2016-11-01

    Full Text Available We disclose a new microwave-assisted protocol for the effective α-arylation of diethyl malonate. The coupling of aryl halides with diethyl malonate proceeds smoothly in short reaction time in the presence of a catalytic amount of Cu(OTf2, 2-picolinic acid and Cs2CO3 in toluene using microwave irradiation. The resulting α-aryl malonates are then used as key intermediates for synthesis of variety of heterocyclic compounds, including benzodiazepines, isoquinolines and pyrrolopyridine scaffolds.

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

    Science.gov (United States)

    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.

  5. Microwave-assisted Extraction and GC-MS Analysis of Zanthoxylum Oil from Zanthoxylum bungeanum

    Directory of Open Access Journals (Sweden)

    Xiaoguang Wang

    2015-03-01

    Full Text Available The conditions for microwave-assisted extracting oil from Zanthoxylum bungeanum seeds were studied and its chemical composition was analyzed by GC-MS. The effects of extract medium, microwave power, time and ratio of liquid to solid on extraction yield of Zanthoxylum bungeanum oil were investigated, using an orthogonal array design. The experimental results showed that using petroleum ether as extract medium, microwave power 350 w, solid-to-solvent ratio 1:5 (g/mL, 60 sec, can obtained 7.85% of Zanthoxylum bungeanum oil. Thirty-three substances in Zanthoxylum bungeanum oil were authenticated by GC-MS, of which 33 were identified for the first time and its chemical composition was analyzed. Accounting for 97.82% of the total volatile compounds.

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

    Science.gov (United States)

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

    2017-02-10

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

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

    Science.gov (United States)

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

    2017-02-01

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

  8. Microwave assisted-semi bionic extraction of lignan compounds from Fructus Forsythiae by orthogonal design

    Institute of Scientific and Technical Information of China (English)

    TU Qiu-yun; ZHOU Chun-shan; TANG Jian-ping

    2008-01-01

    Microwave assisted-semi bionic extraction (MASBE) process for lignans from Fructus Forsythiae was studied. The influences of solvent pH value, microwave power, dosage of solvent and irradiation time were investigated. Optimum extracting parameters were determined by orthogonal experiments as follows: pH value of solvent at first extraction is 5.5-6.0, that at the second extraction is 7-8; microwave power is 700 W; mass ratio of Fructus Forsythiae to water is 1:12; irradiation time is 10 min, and extracting times is two. Under these optimal conditions, the yield of lignans reaches 0.364%. Compared with the conventionalextraction methods, the MASBE process has the advantages of high extraction rate, high extraction selectivity.

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

    Science.gov (United States)

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

    2014-09-09

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

  10. Green synthesis of silver nanoparticles using extract of Parkia speciosa Hassk pods assisted by microwave irradiation

    Directory of Open Access Journals (Sweden)

    Is Fatimah

    2016-11-01

    Full Text Available This paper reports an investigation of the microwave-assisted synthesis of silver nanoparticles (Ag NPs using extract of stinky bean (Parkia speciosa Hassk pods (BP. The formation of Ag NPs was identified by instrumental analysis consists of UV–vis spectrophotometry, Fourier-transform infrared (FTIR spectrophotometry, scanning electron microscopy (SEM, transmission electron microscopy (TEM and particle size analysis. Furthermore, Ag NPs were used as antibacterial agents against Escherichia coli, Staphylococcus aureus, and Pseudomonas aeruginosa. The results indicate rapid formation of Ag NPs during microwave irradiation with similar properties to those obtained through the aging method. In general, the use of microwave irradiation yields larger particles, and it is affected by volume ratio of the extract to the AgNO3 solution. The prepared materials demonstrated antibacterial activity.

  11. Microwave-Assisted Chemical Functionalization of Single-Walled Carbon Nanotubes with Organic Peroxides

    Institute of Scientific and Technical Information of China (English)

    WAN Li; WANG Xianbao; LI Shaoqing; LI Qin; TIAN Rong; LI Mingjian; CHENG Jing

    2009-01-01

    Microwave-assisted chemical functionalization of single-walled carbon nanotubes, with undecyl groups de-composed from lauroyl peroxides was reported. This rapid efficient procedure reduced the reaction time to 10 min, and obtained the products with higher functionalized degree than that by the conventional refluxing method. The in-fluence of different reaction time and microwave power on the functionalized degree has been explored by using FT-IR, TGA and Raman analyses. The results show that longer treatment time will lead to partial defunctionaliza-tion, and higher microwave power (higher than 900 W) can reduce the functionalized degree by removing some ini-tially-attached functional groups. Dispersion stability images and HRTEM images show that the resulting SWNT has enhanced dispersivity in organic solvents compared to the pristine nanotubes.

  12. Application of microwave-assisted micro-solid-phase extraction for determination of parabens in human ovarian cancer tissues.

    Science.gov (United States)

    Sajid, Muhammad; Basheer, Chanbasha; Narasimhan, Kothandaraman; Choolani, Mahesh; Lee, Hian Kee

    2015-09-01

    Parabens (alkyl esters of p-hydroxybenzoic acid) are widely used as preservatives in food, cosmetics and pharmaceutical products. However, weak estrogenicity of some parabens has been reported in several studies, which provided the impetus for this work. Here, a simple and efficient analytical method for quantifying parabens in cancer tissues has been developed. This technique involves the simultaneous use of microwave-assisted solvent extraction (MASE) and micro-solid phase extraction (μ-SPE), in tandem with high performance liquid chromatography (HPLC/UV) analysis for the determination of parabens. The pollutants studied included four parabens (methyl, ethyl, propyl and butyl parabens). Optimization of the experimental parameters for MASE and μ-SPE was performed. Good relative standard deviation (%RSD) ranged from 0.09 to 2.81% and high enrichment factors (27-314) were obtained. Coefficients of determination (r(2)) up to 0.9962 were obtained across a concentration range of 5.0-200ngg(-1). The method detection limits for parabens ranged from 0.005 to 0.0244ngg(-1). The procedure was initially tested on prawn samples to demonstrate its feasibility on a complex biological matrix. Preliminary studies on human ovarian cancer (OC) tissues showed presence of parabens. Higher levels of parabens were detected in malignant ovarian tumor tissues compared to benign tumor tissue samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Effect of Sulfation on Zirconia-Pillared Montmorillonite to the Catalytic Activity in Microwave-Assisted Citronellal Conversion

    Directory of Open Access Journals (Sweden)

    Is Fatimah

    2014-01-01

    Full Text Available Preparation of sulfated zirconia-pillared montmorillonite was carried out in two steps; zirconia pillarization and sulfation to zirconia-pillared montmorillonite. The prepared materials were characterized by using X-ray diffraction (XRD, measurement of the specific surface area, total pore volume and pore size distribution by the N2 adsorption method, scanning electron microscopy-energy dispersive X-ray (SEM-EDX, and surface acidity determination by using pyridine adsorption-FTIR analysis. The activity of the materials as catalysts was evaluated for a microwave-assisted conversion of citronellal. The results showed that the prepared materials had a physicochemical character that promoted high catalytic activity to convert citronellal. From varied Zr content and study of the effect of sulfation on the activity, it was found that Zr content and sulfation increase the surface acidity of the material as shown by the higher total conversion and tendency to produce menthol as a product of the tandem cyclization-hydrogenation mechanism.

  14. Microwave assisted acid and alkali pretreatment of Miscanthus biomass for biorefineries

    Directory of Open Access Journals (Sweden)

    Zongyuan Zhu

    2015-10-01

    Full Text Available Miscanthus is a major bioenergy crop in Europe and a potential feedstock for second generation biofuels. Thermochemical pretreatment is a significant step in the process of converting lignocellulosic biomass into fermentable sugars. In this work, microwave energy was applied to facilitate NaOH and H2SO4 pretreatments of Miscanthus. This was carried out at 180 ℃ in a monomode microwave cavity at 300 W. Our results show that H2SO4 pretreatment contributes to the breakdown of hemicelluloses and cellulose, leading to a high glucose yield. The maximum sugar yield from available carbohydrates during pretreatment is 75.3% (0.2 M H2SO4 20 Min, and glucose yield is 46.7% under these conditions. NaOH and water pretreatments tend to break down only hemicellulose in preference to cellulose, contributing to high xylose yield. Compared to conventional heating NaOH/H2SO4 pretreatment, 12 times higher sugar yield was obtained by using microwave assisted pretreatment within half the time. NaOH pretreatments lead to a significantly enhanced digestibility of the residue, because the effective removal of lignin and hemicellulose makes cellulose fibres more accessible to cellulases. Morphological study of biomass shows that the tightly packed fibres in the Miscanthus were dismantled and exposed under NaOH condition. We studied sugar degradation under microwave assisted H2SO4 conditions. The results shows that 6-8% biomass was converted into levulinic acid (LA during pretreatment, showing the possibility of using microwave technology to produce LA from biomass. The outcome of this work shows great potential for using microwave in the thermo-chemical pretreatment for biomass and also selective production of LA from biomass.

  15. Negative Feedback Effect of Microwave Irradiation in the Microwave—assisted Hydrothermal Synthesis of Bi2S3 Nanorods

    Institute of Scientific and Technical Information of China (English)

    陶秀成; 邵名望

    2002-01-01

    The microwave-assisted hydrothermal synthesis of Bi2S3 nanorods was reported.The result showed that microwave irradiation can help to produce Bi2S3 nanorods in very short time.There is a negative feedback effcet which increases the degree of crystallinity in the reaction.

  16. Efficient three-wave mixing in a three-level atomic medium with an assisting microwave driven field

    Institute of Scientific and Technical Information of China (English)

    Li Jia-Hua; Luo Jin-Ming; Yang Wen-Xing; Zhan Zhi-Ming

    2006-01-01

    The potential for nonlinear conversion between two laser pulses in a three-level V-type medium with assistance of an auxiliary microwave resonant radiation is studied. The results show that microwave driven field can lead to the parametric generation of a new laser pulse with high conversion efficiency when a weak pump laser pulse is applied.

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

    Science.gov (United States)

    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.

  18. SINTESIS PATI JAGUNG TERFOSFORILASI MELALUI TEKNIK GELOMBANG MIKRO [Microwave-Assisted Synthesis of Phosphorylated Corn Starch

    Directory of Open Access Journals (Sweden)

    Atep Dian Supardan*

    2014-06-01

    Full Text Available Phosphorylated starch is a type of modified starches which is mostly imported. Commonly, starch to be modified must contain more than 25% of amylose. This study aimed to synthesize phosphorylated starch and evaluate its potency as a heavy metal adsorbent. Corn starch was subjected to phosphorylation through microwave-assisted reaction with a mixture of sodium dihydrogen orthophosphate and disodium hydrogen phosphate. The experiment was designed to optimize the pH, microwave radiation power, and phosphorylation time. The results showed that the maximum phosphate subtitution degree was obtained at pH of 6, microwave radiation of 500 W, and a reaction time of 10 minutes. The degree of subtitution ranged from 0.567 to 0.787. The physicochemical properties of the product i.e. swelling capacity, solubility, water binding capacity, and paste clarity were significantly different than that of the unmodified corn starch. The infrared spectrum showed a high peak absorption at the wavelength of 1651 cm-1, indicating hydrogen bond formation of phosphoric group-water- phosphoric group. In the fingerprint area, there were two new absorption peaks at 1200 and 990 cm-1, which were assigned for the P=O and C-O-P vibrations, respectively. The phosphorylated corn starch adsorbed methylene blue up to 73.3% and mercury up to 73.6%, suggesting the prospect of the microwave-assisted synthetic phosphorylated corn starch as an effective adsorbent for heavy metals.

  19. Microwave-assisted extraction of anthocyanin from Chinese bayberry and its effects on anthocyanin stability

    Directory of Open Access Journals (Sweden)

    Wenkai DUAN

    2015-09-01

    Full Text Available AbstractAnthocyanins are present in high concentrations in Chinese bayberry, Myrica rubra Sieb. & Zucc. Herein, a microwave-assisted extraction was used to extract the anthocyanins from Chinese bayberry. The HPLC chromatogram of the extracts showed that the anthocyanin components were slightly hydrolysed during the extraction process. Further experiments confirmed that microwave irradiation slightly hydrolysed cyanidin-3-O-glucoside to cyanidin, but did not significantly influence the antioxidant activity of the extracts. Optimized extraction conditions for total anthocyanin content were a solid-to-liquid ratio, extraction temperature, and extraction time of 1:50, 80 °C, and 15 min, respectively. Under these conditions, the anthocyanin content was 2.95 ± 0.08 mg·g−1, and the antioxidant activity yield was 279.96 ± 0.1 μmol.·g−1 Trolox equivalent on a dry weight basis. These results indicated that microwave-assisted extraction was a highly efficient extraction method with reduced processing time. However, under some extraction conditions it could damage the anthocyanins. These results provide an important guide for the application of microwave extraction.

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

    Science.gov (United States)

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

    2015-06-05

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

  1. Response surface optimization of microwave-assisted extraction for HPLC-fluorescence determination of puerarin and daidz

    Institute of Scientific and Technical Information of China (English)

    Ying-Kun Liu; E Yan; Han-Ying Zhan; Zhi-Qi Zhang

    2011-01-01

    Microwave-assisted extraction was optimized with response surface methodology for HPLC-fluorescence determination of puerarin and daidzein in Radix Puerariae thomsonii.The optimized extraction procedure was achieved by soaking the sample with 70% methanol

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

    Science.gov (United States)

    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.

  3. Application of ionic liquids in the microwave-assisted extraction of proanthocyanidins from Larix gmelini bark.

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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

  5. Application of ionic liquids in the microwave-assisted extraction of pectin from lemon peels.

    Science.gov (United States)

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

    2012-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Huang Guolin

    2012-01-01

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

  7. Microwave-Assisted Synthesis of Alginate-Stabilized Gold Nanoparticles

    Directory of Open Access Journals (Sweden)

    Foliatini Foliatini

    2014-12-01

    Full Text Available An efficient and rapid method for preparation of Au nanoparticles (Au-NP has been developed by direct microwave irradiation of metal precursor and alginate mixed solution in a single step. Here, alginate molecules act as both the reducing and stabilizing agents of Au-NP. The obtained nanoparticles were characterized by ultraviolet-visible (UV-Vis spectroscopy, particle size analyzer, fourier transform infrared spectroscopy, and transmission electron microscopy. The nanoparticles have a spherical form and perfectly capped with alginate when using alginate and chloro auric acid (HAuCl4 precursor in the concentration range of 0.50 to 0.75% (w/v and 0.40 mM, respectively. The use of a lower concentration of alginate and/or higher concentration of HAuCl4 caused agglomeration to occur, thereby resulting in a bigger size of Au-NP and red shifting of surface plasmon resonance (SPR peak to a higher wavelength.

  8. Microwave-Assisted Synthesis of Boron-Modified TiO2 Nanocrystals

    OpenAIRE

    Claudia Carlucci; Barbara Federica Scremin; Teresa Sibillano; Cinzia Giannini; Emanuela Filippo; Patrizia Perulli; Agostina Lina Capodilupo; Giuseppina Anna Corrente; Giuseppe Ciccarella

    2014-01-01

    An efficient microwave-assisted synthesis of TiO2:(B) nanorods, using titanium tetraisopropoxide (TTIP), benzyl alcohol as the solvent, together with boric acid and oleic acid as the additive reagents, has been developed. Chemical modification of TTIP by oleic acid was demonstrated as a rational strategy to tune the shape of TiO2 nanocrystals toward nanorod formation. The differently-shaped TiO2:(B) nanocrystals were characterized in detail by transmission electron microscopy (TEM), inductive...

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

    Science.gov (United States)

    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%...

  10. Rapid, Microwave-Assisted Organic Synthesis of Selective V600EBRAF Inhibitors for Preclinical Cancer Research

    Science.gov (United States)

    Buck, Jason R.; Saleh, Sam; Uddin, Md. Imam; Manning, H. Charles

    2012-01-01

    We report a dramatically improved total synthesis of two highly selective V600EBRAF inhibitors, PLX4720 and PLX4032, that leverages microwave-assisted organic synthesis (MAOS). Compared with previously reported approaches, our novel MAOS method significantly reduces overall reaction time without compromising yield. In addition to providing a gram-scale route to these compounds for preclinical oncology research, we anticipate this approach could accelerate the synthesis of azaindoles in high-throughput, library-based formats. PMID:23180892

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

    OpenAIRE

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

    2013-01-01

    This paper describes a portable microwave assisted extraction apparatus (PMAE) for extraction of bioactive compounds especially essential oils and aromas directly in a crop or in a forest. The developed procedure, based on the concept of green analytical chemistry, is appropriate to obtain direct in-field information about the level of essential oils in natural samples and to illustrate green chemical lesson and research. The efficiency of this experiment was validated for the extraction of e...

  12. Nordihydroguaiaretic acid recovery from Larrea tridentata by microwave-assisted extraction

    OpenAIRE

    Martins, Sílvia; Mussatto, Solange I.; Aguilar, Cristóbal N.; Garza-Rodriguez, I.; Teixeira, J.A.

    2010-01-01

    Nordihydroguaiaretic acid (NDGA) is a powerful antioxidant with biological activities of great interest in several health areas, including antiviral, cancer chemopreventive, and antitumorgenic. Little information is available on extraction methods of NDGA from Larrea tridentata. Hence, the aim of this study was to develop a rapid and effective microwave-assisted extraction (MAE) method for NDGA recovery from Larrea tridentata leaves, and to compare the results ob...

  13. Microwave-irradiation-assisted hybrid chemical approach for titanium dioxide nanoparticle synthesis: microbial and cytotoxicological evaluation.

    Science.gov (United States)

    Ranjan, Shivendu; Dasgupta, Nandita; Rajendran, Bhavapriya; Avadhani, Ganesh S; Ramalingam, Chidambaram; Kumar, Ashutosh

    2016-06-01

    Titanium dioxide nanoparticles (TNPs) are widely used in the pharmaceutical and cosmetics industries. It is used for protection against UV exposure due to its light-scattering properties and high refractive index. Though TNPs are increasingly used, the synthesis of TNPs is tedious and time consuming; therefore, in the present study, microwave-assisted hybrid chemical approach was used for TNP synthesis. In the present study, we demonstrated that TNPs can be synthesized only in 2.5 h; however, the commonly used chemical approach using muffle furnace takes 5 h. The activity of TNP depends on the synthetic protocol; therefore, the present study also determined the effect of microwave-assisted hybrid chemical approach synthetic protocol on microbial and cytotoxicity. The results showed that TNP has the best antibacterial activity in decreasing order from Escherichia coli, Bacillus subtilis, and Staphylococcus aureus. The IC50 values of TNP for HCT116 and A549 were found to be 6.43 and 6.04 ppm, respectively. Cell death was also confirmed from trypan blue exclusion assay and membrane integrity loss was observed. Therefore, the study determines that the microwave-assisted hybrid chemical approach is time-saving; hence, this technique can be upgraded from lab scale to industrial scale via pilot plant scale. Moreover, it is necessary to find the mechanism of action at the molecular level to establish the reason for greater bacterial and cytotoxicological toxicity. Graphical abstract A graphical representation of TNP synthesis.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

  17. Microwave-assisted extraction at atmospheric pressure coupled to different clean-up methods for the determination of organophosphorus pesticides in olive and avocado oil.

    Science.gov (United States)

    Fuentes, Edwar; Báez, María E; Díaz, Juan

    2009-12-18

    An effective extraction method was devised for the determination of organophosphorus pesticides (OPPs) in olive and avocado oil samples, using atmospheric pressure microwave-assisted liquid-liquid extraction (APMAE) and solid-phase extraction or low-temperature precipitation as clean-up step. A simple glass system equipped with an air-cooled condenser was designed as an extraction vessel. The pesticides were partitioned between acetonitrile and oil solution in hexane. Analytical determinations were carried out by gas chromatography-flame photometric detection and gas chromatography-tandem mass spectrometry, using a triple quadrupole mass analyzer, for confirmation purposes. Several factors influencing the extraction efficiency were investigated and optimized through fractional factorial design and Doehlert design. Under optimal conditions the recovery of pesticides from oil at 0.025 microg g(-1) ranged from 71% to 103%, except for fenthion in avocado oil, with RSDs avocado oils produced in Chile. Detectable residues of different OPPs were observed in 85% of samples.

  18. Microwave assisted hydrolysis of aluminium metal and preparation of high surface area Al2O3 powder

    Indian Academy of Sciences (India)

    A K Sivadasan; I Packia Selvam; Sankara Narayanan Potty

    2010-12-01

    Phase pure boehmite particles were prepared by microwave assisted hydrolysis of aluminium sheets. These particles were calcined in air to produce Al2O3 particles with specific surface area of ∼210 m2/g. The alumina particles were characterized by studying X-ray diffraction, transmission electron microscopy and Fourier transform infrared spectroscopy. For comparison, the aluminium hydroxide particles were also prepared by normal hydrolysis of aluminium metal. Normal hydrolysis yielded a mixture of boehmite and bayerite particles whereas microwave assisted hydrolysis produced phase pure boehmite particles. The importance of using microwave radiation for the hydrolysis of aluminium metal is also manifested in a shorter reaction time.

  19. Factors Affecting Delignification of Oil Palm Empty Fruit Bunch by Microwave-assisted Dilute Acid/Alkali Pretreatment

    Directory of Open Access Journals (Sweden)

    Junaid Akhtar

    2014-11-01

    Full Text Available Microwave-assisted dilute acid/alkali pretreatment is an efficient and rapid method of removing lignin and hemicellulose, however, the optimized parameters for the maximum efficiency have to date not been presented in the literature. The purpose of this study was to determine those conditions by examining the effects of three factors: microwave power, temperature, and time on delignification in microwave-assisted dilute acid/alkali pretreatment. For the control condition of conventional pretreatment (CP, empty fruit bunches (EFBs were soaked in 2.5 M NaOH for two hours in the autoclave. In the experimental condition, EFB were first soaked in dilute sulfuric acid with conventional autoclave heating, which removed 90% of their hemicellulose. The acid-treated EFBs were then soaked in 2.5 M NaOH solution and microwaved at different conditions: microwave power (700 - 100 watts, time (60 - 90 min, and temperature (80 -110 °C. The amount of acid-insoluble lignin was determined by Klason method. Microwave-Alkali (Mw-A pretreatment was modeled until it attained maximum delignification. More than twice the rate of delignification that is, 71.9% was attained with microwave-assisted alkali/acid pretreatment of 900 W microwave power at 110 °C for 80 min compared to 34.6% with conventional pretreatment.

  20. Microwave-assisted steam distillation for simple determination of polychlorinated biphenyls and organochlorine pesticides in sediments.

    Science.gov (United States)

    Numata, Masahiko; Yarita, Takashi; Aoyagi, Yoshie; Takatsu, Akiko

    2003-03-15

    A novel sample extraction technique for polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) analysis using microwave-heating device is developed. In this study, microwave-assisted extraction (MAE) and steam distillation techniques were combined. Desorption of the anatytes from solid matrixes was accelerated with water vapor which was generated by microwave irradiation. A sample holder in a commercial microwave extraction cell kept the sample from direct contact with the organic solvent for analytes trapping during the treatment process. Therefore, relatively clean extracts were obtained with small amount of solvents. Without any cleanup steps, the obtained extract could be analyzed with gas chromatograph/mass spectrometers (GC/MS). Six PCB congeners (PCB15, 28, 70, 101, 180, 194, 209) and three OCPs (gamma-HCH, 4,4'-DDE, 4,4'-DDD) in two marine sediment samples (a sediment collected from a bay of Kyusyu Island, Japan, and a certified reference material NIST SRM1944) were analyzed by using this microwave-assisted steam distillation (MASD) technique and another extraction method (exhaustive steam distillation, MAE, and Soxhlet extraction); and comparisons of the results are shown in this report. Although recovery yields of highly chlorinated biphenyls (PCB180, 194, 209) and relatively polar OCPs (gamma-HCH, 4,4'-DDD) were low (30-60%) compared with other analytes (PCB15, 28, 70, 101, 4,4'-DDE; recovery, 80-100%), use of isotope labeled internal standards for the MASD technique gave comparable results with the values obtained by other extraction methods and the certified values in the samples.

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

    Science.gov (United States)

    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.

  2. Experimentos didáticos envolvendo radiação microondas Microwave-assisted experiments for undergraduate courses

    Directory of Open Access Journals (Sweden)

    Fabiana Rosini

    2004-12-01

    Full Text Available Theoretical and practical aspects of the use of microwave-assisted strategies in chemistry are introduced for students using simple and safe experiments employing a domestic oven. Three procedures are proposed for evaluating the distribution of microwave radiation inside the microwave oven cavity: (1 variation of the volume of marshmallows; (2 drying of filter paper wetted with Co(II solution, and (3 variation of water temperature, after microwave-assisted heating. These experiments establish the position with the highest incidence of microwave radiation in the oven cavity, which was chosen for the synthesis of salicylic acid acetate. This synthesis was performed in 5 min of heating and the yield was around 85%. All experiments can be carried out in a 4 h lab-session using low-cost instrumentation.

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

    Science.gov (United States)

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

    2015-04-24

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

  4. Solution-phase microwave-assisted synthesis of unsubstituted and modified alpha-quinque- and sexithiophenes.

    Science.gov (United States)

    Melucci, M; Barbarella, G; Zambianchi, M; Di Pietro, P; Bongini, A

    2004-07-09

    The facile synthesis of poorly soluble unsubstituted and modified alpha-quinque- and sexithiophenes under microwave irradiation in the liquid phase is described. The use of microwave irradiation allowed these compounds to be prepared in a few minutes and at high yields by means of the Suzuki cross-coupling reaction. Unsubstituted sexithiophene was obtained in 10 min via the one-pot borylation/Suzuki reaction, purified according to a very simple procedure, and isolated in 84% yield. The efficient synthesis of two new methylated quinque- and sexithiophenes displaying liquid crystalline properties is reported. A new microwave-assisted methodology for the conversion of aldehyde-terminated quinque- and sexithiophenes into the corresponding cyano derivatives is also described. The use of microwaves was extended to the Sonogashira coupling reaction and found to be very effective in the preparation of a quinquethiophene containing acetylenic spacers. The electronic and optical characterization of this compound is reported and discussed in relation to that of unsubstituted quinquethiophene.

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

    Science.gov (United States)

    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.

  6. Microwave-Assisted Decarboxylation of Sodium Oleate and Renewable Hydrocarbon Fuel Production

    Institute of Scientific and Technical Information of China (English)

    Wang Yunpu; Liu Yuhuan; Ruan Rongsheng; Wen Pingwei; Wan Yiqin; Zhang Jinsheng

    2013-01-01

    The carboxyl terminal of sodium oleate has a stronger polarity than that of oleic acid;this terminal is more likely to be dipole polarized and ionically conductive in a microwave ifeld. Sodium oleate was used as the model compound to study the decarboxylation of oleic acid leading to hydrocarbon formation via microwave-assisted pyrolysis technology. The pyrolysis gas, liquid, and solid products were precisely analyzed to deduce the mechanism for decarboxylation of sodium oleate. Microwave energy was able to selectively heat the carboxyl terminal of sodium oleate. During decarboxylation, the double bond in the long hydrocarbon chain formed a p-πconjugated system with the carbanion intermediate. The resulting p-πconjugated system was more stable and beneifcial to the pyrolysis reaction (decarboxylation, terminal allylation, isomeriza-tion, and aromatization). The physical properties of pyrolysis liquid were generally similar to those of diesel fuel, thereby demonstrating the possible use of microwaves for controlling the decarboxylation of sodium oleate in order to manufacture renewable hydrocarbon fuels.

  7. Optimization of microwave-assisted extraction of polyphenols from Myrtus communis L. leaves.

    Science.gov (United States)

    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 (pMyrtus 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Huan, E-mail: huanzhou@cczu.edu.cn [Institute of Biomedical Engineering and Health Sciences, Changzhou University, Changzhou, Jiangsu 213164 (China); Kong, Shiqin [Institute of Biomedical Engineering and Health Sciences, Changzhou University, Changzhou, Jiangsu 213164 (China); School of Materials Science and Engineering, Changzhou University, Changzhou, Jiangsu 213164 (China); Pan, Yan; Zhang, Zhiguo [Institute of Biomedical Engineering and Health Sciences, Changzhou University, Changzhou, Jiangsu 213164 (China); Deng, Linhong, E-mail: dlh@cczu.edu.cn [Institute of Biomedical Engineering and Health Sciences, Changzhou University, Changzhou, Jiangsu 213164 (China)

    2015-11-01

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

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

    Science.gov (United States)

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

    2013-04-07

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

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

    Directory of Open Access Journals (Sweden)

    Le Pham Tan Quoc

    2016-06-01

    Full Text Available Background. The aim of this study was to determine the best extraction conditions for total phenolic con- tent (TPC and antioxidant capacity (AC of Polygonum multiflorum Thunb. root using microwave-assisted extraction (MAE. Material and methods. The raw material used was Polygonum multiflorum Thunb. root powder. Five fac- tors 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. Results. 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 mi- crowaving 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. Conclusion. These factors significantly affected TPC and AC. We can use acetone as a solvent with micro- wave-assisted extraction to achieve the best result.

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

    Directory of Open Access Journals (Sweden)

    Hemanth Mohandas

    2013-01-01

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

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

    Science.gov (United States)

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

    2016-11-14

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

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

    Science.gov (United States)

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

    2016-01-01

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

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

    Science.gov (United States)

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

    2014-03-01

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

  15. The Microwave-Assisted Green Synthesis of TiC Powders

    Directory of Open Access Journals (Sweden)

    Hui Wang

    2016-11-01

    Full Text Available 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.

  16. Development of microwave-assisted drying methods for sample preparation for dried spot micro-X-ray fluorescence analysis.

    Science.gov (United States)

    Link, Dirk D; Kingston, H M; Havrilla, George J; Colletti, Lisa P

    2002-03-01

    Although dried spot micro X-ray fluorescence (MXRF) is an effective analytical technique for trace elemental analysis, the sample preparation procedures currently used suffer from a number of drawbacks. These drawbacks include relatively long preparation times, lack of control of the sample preparation environment, and possibility of loss of volatile analytes during the drying process. Microwave-assisted drying offers several advantages for dried spot preparation, including control of the environment and minimized volatility because of the differences between microwave heating and conventional heating. A microwave-assisted drying technique has been evaluated for use in preparing dried spots for trace analysis. Two apparatus designs for microwave drying were constructed and tested using multielement standard solutions, a standard reference material, and a "real-world" semiconductor cleaning solution. Following microwave-assisted drying of these aqueous samples, the residues were redissolved and analyzed by ICPMS. Effective recovery was obtained using the microwave drying methods, demonstrating that the microwave drying apparatus and methods described here may be more efficient alternatives for dried spot sample preparation.

  17. Rapid Microwave-Assisted Copper-Catalyzed Nitration of Aromatic Halides with Nitrite Salts

    Energy Technology Data Exchange (ETDEWEB)

    Paik, Seung Uk; Jung, Myoung Geun [Keimyung University, Daegu (Korea, Republic of)

    2012-02-15

    A rapid and efficient copper-catalyzed nitration of aryl halides has been established under microwave irradiation. The catalytic systems were found to be the most effective with 4-substituted aryl iodides leading to nearly complete conversions. Nitration of aromatic compounds is one of the important industrial processes as underlying intermediates in the manufacture of a wide range of chemicals such as dyes, pharmaceuticals, agrochemicals and explosives. General methods for the nitration of aromatic compounds utilize strongly acidic conditions employing nitric acid or a mixture of nitric and sulfuric acids, sometimes leading to problems with poor regioselectivity, overnitration, oxidized byproducts and excess acid waste in many cases of functionalized aromatic compounds. Several other nitrating agents or methods avoiding harsh reaction conditions have been explored using metal nitrates, nitrite salts, and ionic liquid-mediated or microwave-assisted nitrations. Recently, copper or palladium compounds have been successfully used as efficient catalysts for the arylation of amines with aryl halides under mild conditions.

  18. Microwave Assisted Synthesis, Modification With Platinum And Photocatalytical Properties of TiO2 Nanofibers

    Directory of Open Access Journals (Sweden)

    Reinis DRUNKA

    2016-05-01

    Full Text Available In the present work formation of active TiO2 nanoparticles in microwave synthesis and their modification with platinum were studied. Anatase nanopowder and 10 M KOH solution were used as raw materials. Microwave assisted synthesis method permited to obtain TiO2 nanofibres and nanowires with a diameter of 10 nm and a specific surface area in the range of 70 – 150 m2/g. In order to modify TiO2 nanofibers with platinum it was stirred in H2PtCl6 solution under UV irradiation. Photocatalytic activity was determined by degradation of the methylene blue (MB solution under UV and visible light irradiation. The obtained samples showed higher photocatalytic activity with respect to pure TiO2 nanofibers. The doped TiO2 nanofibers were appropriate for degradation of harmful organic compounds as well as for hydrogen production by water splitting.

  19. Microwave-assisted synthesis and characterization of ZnO-nanorod arrays

    Institute of Scientific and Technical Information of China (English)

    ZHU Jian-yu; ZHANG Jing-xia; ZHOU Hui-fen; QIN Wen-qing; CHAI Li-yuan; HU Yue-hua

    2009-01-01

    High density ZnO-nanorod arrays (rod length 1.59 μm) were successfully synthesized via a microwave-assisted solution-phase method using zinc chloride and ammonia solution as reactants.The influence of concentration of ammonia solution,work power,and microwave irradiation time on the morphology and size of final products was carefully investigated.The crystal structure,chemical composition and morphologies of final products were characterized using X-ray powder diffraction (XRD),scanning electron microscopy (SEM) and photoluminescence (PL).The as-synthesized ZnO is composed of single crystalline and possesses three photoluminescence emissions centered at 400,469 and 534.5 nm,respectively.

  20. Microwave-assisted synthesis of narcis-like zinc oxide nanostructures

    Energy Technology Data Exchange (ETDEWEB)

    Kajbafvala, Amir, E-mail: akajbaf@ncsu.ed [Department of Materials Science and Engineering, North Carolina State University, 911 Partners Way, Raleigh, NC 27695-7907 (United States); Department of Materials Science and Engineering, Center of Excellence for Production of Advanced Materials, Sharif University of Technology, P.O. Box 11365-9466, Tehran (Iran, Islamic Republic of); Zanganeh, Saeid [Department of Electrical and Computer Engineering, University of Connecticut, 371 Fairfield Way, U-2157 Storrs, CT 06269-2157 (United States); Kajbafvala, Ehsan; Zargar, H.R.; Bayati, M.R. [Department of Metallurgy and Materials Engineering, Iran University of Science and Technology, P.O. Box 16845-161, Tehran (Iran, Islamic Republic of); Sadrnezhaad, S.K., E-mail: sadrnezh@sharif.ed [Department of Materials Science and Engineering, Center of Excellence for Production of Advanced Materials, Sharif University of Technology, P.O. Box 11365-9466, Tehran (Iran, Islamic Republic of)

    2010-05-14

    Through a fast, simple, low cost, surfactant-free and convenient microwave-assisted route, narcis-like ZnO nanostructures (10-15 nm size) with flower diameters in the range of 1-2.5 {mu}m were synthesized. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy and room temperature photoluminescence (PL) measurements were used to characterize the produced ZnO nanostructures. The principle raw materials - ammonium hydroxide (NH{sub 4}OH) and zinc acetate dihydrate [Zn(CH{sub 3}COO){sub 2}.2H{sub 2}O] - were both inexpensive. The method was fast, simple and surfactant-free capable of producing larger quantities of zinc oxide nanostructures. Formation mechanism of narcis ZnO nanostructures has been studied due to the self-assembly of small form ZnO clusters in microwave treated precursor.

  1. Microwave-assisted extraction of Shenfu coal and its macromolecule structure

    Institute of Scientific and Technical Information of China (English)

    CHEN Hong; LI Jian-wei; LEI Zhao; GE Ling-mei

    2009-01-01

    Coals consist of some molecules trapped within an organic matrix from which some organic compounds can be extracted by solvents. The Soxhlet technique has been widely used for extracting organic compounds. Microwave heating methods may be successfully applied in the field of coal science. Acetone extraction yields and the chemical composition of the extract were inves-tigated using a typical Chinese coal, Shenfu coal, with microwave-assisted extraction. The acetone extract and residue were ana-lyzed by GC/MS and carbon-13 nuclear magnetic resonance spectroscopy respectively. The carbon spectra were converted into several numerical parameters, fa, Ha, Xb, which indicate the difference in macromolecular structure between Shenfu coal and its residue. Furthermore, a hybrid genetic algorithm was employed using these parameters to approximate a coal macromolecule by assembling the structural fragments or functional groups into a large and complicated structure.

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

    Directory of Open Access Journals (Sweden)

    Loredana Salerno

    2014-01-01

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

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

    Science.gov (United States)

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

    2016-11-01

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

  4. New Approaches for Effective Microwave Assisted Extraction of Caffeine and Catechins from Green Tea

    Directory of Open Access Journals (Sweden)

    Gönül SERDAR

    2016-01-01

    Full Text Available This study was designed to develop an effective microwave assisted extraction (MAE method for extraction of caffeine and catechins from green tea samples. A series of solvents (water, ethanol:water mixture or citric acid:water mixture were used for extraction of green tea samples (fresh, frozen or dried collected in three collection periods (first, second and third collection periods. Tea samples were extracted using water in a close microwave system under the certain extraction conditions. Extraction was carried out under a controlled 600 W microwave power at 80 oC temperature for 4 min irradiation time. Alternative to water, an ethanol-water mixture (1:1 or a citric acid-water (1:1 mixture was used as extracting solvent under the same conditions. After MAE crude aqueous extract was partitioned first with chloroform to separate caffeine then ethyl acetate for catechins.  Both caffeine and catechin extraction was quite successful with microwave assisted system employing only 4 minutes treatment. The highest caffeine yield was obtained in the second collection period using frozen green tea samples and ethanol-water as extracting solvent. The yield of catechin extracts was between 0.84-3.96% depending on the solvent system used for extraction. Ethanol-water mixture seems to be appropriate for effective extraction in the basis of extract yields. However, HPLC results showed that individual catechin content of each extraction is more important criteria for the evaluation of most effective extraction medium rather than the mass of the extract.  Using citric acid as extracting solvent in MAE seem to be more fruitful providing 100% catechin mixture with the highest EGCG content. 

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

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Dandan [Key Laboratory of Processing and Testing Technology of Glass and Functional Ceramics of Shandong Province, Qilu University of Technology, Jinan 250353 (China); Du, Yi, E-mail: duyi234@126.com [Key Laboratory of Processing and Testing Technology of Glass and Functional Ceramics of Shandong Province, Qilu University of Technology, Jinan 250353 (China); Tian, Xiuying, E-mail: xiuyingt@yahoo.com [Department of Chemistry and Materials Science, Hunan Institute of Humanities Science and Technology, Loudi 417000 (China); Li, Zhongfu; Chen, Zhongtao; Zhu, Chaofeng [Key Laboratory of Processing and Testing Technology of Glass and Functional Ceramics of Shandong Province, Qilu University of Technology, Jinan 250353 (China)

    2014-12-15

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

  6. Improvement of rate capability of spinel lithium titanate anodes using microwave-assisted zinc nanocoating

    Energy Technology Data Exchange (ETDEWEB)

    Hsieh, Chien-Te, E-mail: cthsieh@saturn.yzu.edu.tw [Department of Chemical Engineering and Materials Science, Yuan Ze Fuel Cell Center, Yuan Ze University, Taoyuan 320, Taiwan (China); Chang, Bi-Sheng; Lin, Jia-Yi; Juang, Ruey-Shin [Department of Chemical Engineering and Materials Science, Yuan Ze Fuel Cell Center, Yuan Ze University, Taoyuan 320, Taiwan (China)

    2012-02-05

    Highlights: Black-Right-Pointing-Pointer Microwave-assisted Zn layers onto Li{sub 4}Ti{sub 5}O{sub 12} crystals serves as superior anode materials. Black-Right-Pointing-Pointer Microwave heating is capable of depositing Zn layers over the surface of spinel Li{sub 4}Ti{sub 5}O{sub 12} within 6 min. Black-Right-Pointing-Pointer The thickness of Zn layer is an increasing function of zinc nitrate concentration. Black-Right-Pointing-Pointer The deposition of Zn coating shows a positive effect on the rate-capability improvement of anodes. - Abstract: In this study, the deposition of microwave-assisted Zn layers onto spinel lithium titanate (Li{sub 4}Ti{sub 5}O{sub 12}) crystals as superior anode materials for Li-ion batteries has been investigated. Microwave heating is capable of rapidly depositing Zn layers over the surface of spinel Li{sub 4}Ti{sub 5}O{sub 12} within 6 min. The thickness of Zn layer (i.e., 1-10 nm) is an increasing function of zinc nitrate concentration under the microwave irradiation. The charge-discharge curve of Zn-Li{sub 4}Ti{sub 5}O{sub 12} anode still maintains the plateau at 1.5 V, contributing to the major portion in the overall specific capacity. The presence of Zn coating significantly facilitates the capacity retention (78.1% at 10 C/0.2 C) of the composite anodes with high Coulombic efficiency (>99.9%), indicating an excellent reversibility of insertion/de-insertion of Li ions. This can be ascribed to the fact that well-dispersed Zn layer offers an electronic pathway over the Li{sub 4}Ti{sub 5}O{sub 12} powder, thus imparting electronic conduction and reducing cell polarization. Accordingly, the deposition of Zn coating, prepared by the rapid microwave heating, shows a positive effect on the rate-capability improvement of Li{sub 4}Ti{sub 5}O{sub 12} anodes.

  7. Optimization of microwave-assisted enzymatic extraction of polysaccharides from the fruit of Schisandra chinensis Baill.

    Science.gov (United States)

    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.

  8. Microwave-assisted one-pot synthesis of polycyclic 4-quinolone derivatives

    OpenAIRE

    2015-01-01

    A microwave-assisted solvent-free one-pot method to afford 1,2,3,4-tetrahydroacridines-9-one derivatives was developed, with shorter reaction time and from easily available starting materials compared to the known methods. Fil: Muscia, Gisela Celeste. Universidad de Buenos Aires. Facultad de Farmacia y Bioquímica. Departamento de Química Orgánica; Argentina; Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Houssay; Argentina; Fil: Carnev...

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

    Science.gov (United States)

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

    2013-02-01

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

  10. Microwave-assisted synthesis of new aryliminothiazolylidene-2-thiazolidin-4-ones and their azarhodacyanines analogues

    Directory of Open Access Journals (Sweden)

    Souad Kasmi-Mir

    2014-07-01

    Full Text Available We here report an efficient microwave-assisted protocol for the synthesis of new arylimino-thiazolylidene-2-thiazolidin-4-ones 6 and their azarhodacyanines derivatives 7 with quantitative yield from 2'-(methylthio-4'-oxo-3H,4'H-[2,5-bithiazolylidene]-3'-ium tosylates 5 and 2-arylimino-5-(thiazol-2(3H-ylidene thiazolidin-4-ones 6, respectively, using as starting material the 4-thiazoline-2-thiones 1 and 3-methyl-2-thioxo-1,3-thiazolidin-4-one 3. The transformation of the tosylate salts 5 into their arylimino derivatives 6 has not been reported to date.

  11. Microwave assisted synthesis of CdS nanoparticles and their size evolution

    Energy Technology Data Exchange (ETDEWEB)

    Lopez, I. A.; Vazquez, A.; Gomez, I., E-mail: idaliagomezmx@yahoo.com.mx [Universidad Autonoma de Nuevo Leon, Facultad de Ciencias Quimicas, Laboratorio de Materiales I, Av. Universidad, Cd. Universitaria, 66451 San Nicolas de los Garza, Nuevo Leon (Mexico)

    2013-05-01

    The study of the size evolution of CdS nanoparticles in aqueous dispersion is presented in this paper. The sodium citrate was employed as stabilizer of CdS nanoparticles synthesized by microwave assisted synthesis. Analysis of this study was carried out by UV-Vis spectrophotometry, by comparison of the band gap energy using theoretical and empirical models. Results obtained show that the synthesis conditions produce CdS nanoparticles with diameters below of 6 nm, which remains stabilized by at least 14 days. These characteristics were confirmed by transmission electron microscopy. The X-ray diffraction pattern confirms cubic phase of the CdS nanoparticles. (Author)

  12. Microwave-assisted one step synthesis of 8-arylmethyl-9H-purin-6-amines

    OpenAIRE

    2008-01-01

    Molecular chaperone heat shock protein 90 (Hsp90) is an important target in cancer and neurodegenerative diseases, and has rapidly become the focus of several drug discovery efforts. Among small molecule Hsp90 inhibitors with clinical applicability are derivatives of 8-arylmethyl-9H-purin-6-amine class. Here we report the use of microwave-assisted chemistry for the successful one-pot delivery of 8-arylmethyl-9H-purin-6-amines. We discuss the applicability as well as the limitations of this me...

  13. Microwave-assisted one step synthesis of 8-arylmethyl-9H-purin-6-amines.

    Science.gov (United States)

    Tao, Hui; Kang, Yanlong; Taldone, Tony; Chiosis, Gabriela

    2009-01-15

    Molecular chaperone heat shock protein 90 (Hsp90) is an important target in cancer and neurodegenerative diseases, and has rapidly become the focus of several drug discovery efforts. Among small molecule Hsp90 inhibitors with clinical applicability are derivatives of 8-arylmethyl-9H-purin-6-amine class. Here we report the use of microwave-assisted chemistry for the successful one-pot delivery of 8-arylmethyl-9H-purin-6-amines. We discuss the applicability as well as the limitations of this method towards the creation of a large chemical diversity in the 8-arylmethyl-9H-purin-6-amine series.

  14. Microwave-assisted Synthesis of Hierarchical ZnO Nanostructures and Their Photocatalytic Properties

    Directory of Open Access Journals (Sweden)

    Ou Ming

    2016-01-01

    Full Text Available Hierarchical ZnO nanostructures were fabricated via a rapid and facile microwave-assisted route with different zinc salts as reactants. The obtained hierarchical ZnO nanostructures have good crystallinity and high purity. Moreover, it was found that various zinc salts have an obvious effect on the morphologies and microstructures of the final products. Additionally, the photocatalytic activity of the obtained ZnO samples under visible-light irradiation was also evaluated by degradation of Rhodamine B (RhB.

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

    Science.gov (United States)

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

    2013-11-08

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

  16. Parameters Affecting the Microwave-Assisted Polyol Synthesis of Silver Nanorods

    OpenAIRE

    Srichandana Nandikonda; Davis, Edward W.

    2011-01-01

    The effects of salt chemistry and concentration on the morphology and yield of silver nanorods produced by the microwave-assisted polyol synthesis are reported. Compared to NaCl, iron and copper salts reduced nanorod yield and length and increased diameter. This is in stark contrast to expectations based on the slower traditional polyol process. The role of the cation was further explored using MgCl2 and MnCl2 which showed different concentration dependent effects on nanorod diameter. In addi...

  17. Heterogeneous Phase Microwave-Assisted Reactions under CO2 or CO Pressure

    Directory of Open Access Journals (Sweden)

    Emanuela Calcio Gaudino

    2016-02-01

    Full Text Available The present review deals with the recent achievements and impressive potential applications of microwave (MW heating to promote heterogeneous reactions under gas pressure. The high versatility of the latest generation of professional reactors combines extreme reaction conditions with safer and more efficient protocols. The double aims of this survey are to provide a panoramic snapshot of MW-assisted organic reactions with gaseous reagents, in particular CO and CO2, and outline future applications. Stubborn and time-consuming carbonylation-like heterogeneous reactions, which have not yet been studied under dielectric heating, may well find an outstanding ally in the present protocol.

  18. Efficient synthesis of a fluorescent tripod detection system for pesticides by microwave-assisted click chemistry.

    Science.gov (United States)

    Mallard-Favier, Isabelle; Blach, Philippe; Cazier, Francine; Delattre, François

    2009-01-26

    A new tripod molecule containing an aromatic core bearing three peracetylated cyclodextrins was synthesized via a microwave-assisted Huisgen 1,3-dipolar cycloaddition and was studied by fluorescence spectroscopy. The photoluminescent properties of complexation phenomena with different pesticides were evaluated in acetonitrile. Fluorescence titrations have been performed to calculate binding constants, sensitivity factors, and limit of detection of the resulting complexes. 2D NMR experiments confirmed the inclusion of pesticide in the hydrophobic cavity of the macrocycle and validated the supramolecular association responsible for the quenching of the fluorescence.

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

    Science.gov (United States)

    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.

  20. Gain-assisted superluminal microwave pulse propagation via four-wave mixing in superconducting phase quantum circuits

    CERN Document Server

    Sabegh, Z Amini; Maleki, M A; Mahmoudi, M

    2015-01-01

    We study the propagation and amplification of a microwave field in a four-level cascade quantum system which is realized in a superconducting phase quantum circuit. It is shown that by increasing the microwave pump tones feeding the system, the normal dispersion switches to the anomalous and the gain-assisted superluminal microwave propagation is obtained in this system. Moreover, it is demonstrated that the stimulated microwave field is generated via four-wave mixing without any inversion population in the energy levels of the system (amplification without inversion) and the group velocity of the generated pulse can be controlled by the external oscillating magnetic fluxes. We also show that in some special set of parameters, the absorption-free superluminal generated microwave propagation is obtained in superconducting phase quantum circuit system.

  1. The effect of microwave-assisted for photo-catalytic reaction in aqueous nano TiO2 particles dispersions.

    Science.gov (United States)

    Chae, Jeong-Seok; Chung, Minchul; Ahn, Ho-Geun; Jung, Sang-Chul

    2010-05-01

    In this study, the photo-catalytic degradation of methylene blue in TiO2 particles-dispersed aqueous solution was carried out by irradiating microwave and UV light simultaneously. The results of photocatalytic degradation of methylene blue showed that the decomposition rate increased with the microwave intensity, UV intensity, TiO2 particle dosages and the circulating fluid velocity. From the result of microwave-assisted photo-catalytic degradation of methylene blue, decomposition rate were shown gradually increased according to the increase of pH. The photo-catalytic degradation rate constant obtained under simultaneous irradiation of microwave and UV light case was about 1.5 times higher than irradiation of UV light only case. This result suggests that there is a synergy effect when the constituent techniques are applied together and that the additional irradiation of microwave can play a very important role in photo-catalysis of organic water pollutants.

  2. Pd(OAc)2/DPPF-catalysed microwave-assisted cyanide-free synthesis of aryl nitriles

    Indian Academy of Sciences (India)

    Dinesh N Sawant; Bhalchandra M Bhanage

    2014-03-01

    This study reports microwave-assisted cyanide-free synthesis of aryl nitriles from aryl halides using palladium acetate/1,1-bis(diphenylphosphino)ferrocene as a new catalyst system. Reported protocol is a rapid, cyanide-free, single step reaction, wherein formamide acts as a solvent as well as a source of cyanide. The use of microwave increases the rate of reaction substantially and it was observed that aryl nitriles can be synthesised in 50 min of microwave irradiation compared to conventional thermal heating protocol which requires 48 h.

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

    Directory of Open Access Journals (Sweden)

    Ning Liu

    2015-05-01

    Full Text Available 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.

  4. Microwave assisted extraction of biodiesel feedstock from the seeds of invasive chinese tallow tree.

    Science.gov (United States)

    Boldor, Dorin; Kanitkar, Akanksha; Terigar, Beatrice G; Leonardi, Claudia; Lima, Marybeth; Breitenbeck, Gary A

    2010-05-15

    Chinese tallow tree (TT) seeds are a rich source of lipids and have the potential to be a biodiesel feedstock, but currently, its invasive nature does not favor large scale cultivation. Being a nonfood material, they have many advantages over conventional crops that are used for biodiesel production. The purpose of this study was to determine optimal oil extraction parameters in a batch-type and laboratory scale continuous-flow microwave system to obtain maximum oil recovery from whole TT seeds using ethanol as the extracting solvent. For the batch system, extractions were carried out for different time-temperature combinations ranging from 60 to 120 degrees C for up to 20 min. The batch system was modified for continuous extractions, which were carried out at 50, 60, and 73 degrees C and maintained for various residence times of up to 20 min. Control runs were performed under similar extraction conditions and the results compared well, especially when accounting for extremely short extraction times (minutes vs hours). Maximum yields of 35.32% and 32.51% (by weight of dry mass) were obtained for the continuous and batch process, respectively. The major advantage of microwave assisted solvent extraction is the reduced time of extraction required to obtain total recoverable lipids, with corresponding reduction in energy consumption costs per unit of lipid extracted. This study indicates that microwave extraction using ethanol as a solvent can be used as a viable alternative to conventional lipid extraction techniques for TT seeds.

  5. Short Time and Low Temperature Reaction between Metal Oxides through Microwave-Assisted Hydrothermal Method

    Directory of Open Access Journals (Sweden)

    S. M. V. Novais

    2016-01-01

    Full Text Available This work demonstrates the possibility of synthesis of cadmium tungstate at low temperatures using oxide precursors. Cadmium tungstate (CdWO4 scintillator was produced via microwave-assisted hydrothermal reaction using the precursors CdO and WO3. The methodology was based on microwave radiation for heating, which is remarkably faster than the solid-state route or conventional hydrothermal procedure. CdWO4 monoclinic (wolframite structure was successfully obtained at 120°C for synthesis times as short as 20 min. This route does not require the use of templates or surfactants and yields self-assembled nanorods with size of around 24 ± 9 nm width and 260 ± 47 nm length. The growth mechanism for the formation of CdWO4 involves microwave-induced dissociation of the reagents and solvation of Cd2+ and WO42- ions, which are free to move and start the nucleation process. The luminescence properties of the produced nanoparticles were investigated, presenting a broad emission band at around 500 nm, which is comparable to that observed for samples produced using other chemical routes. This result highlights the great potential of the proposed method as a low-cost and time saving process to fabricate luminescent oxide nanoparticles.

  6. Synthesis of wurtzite ZnS nanoparticles using the microwave assisted solvothermal method

    Energy Technology Data Exchange (ETDEWEB)

    La Porta, Felipe A., E-mail: felipe_laporta@yahoo.com.br [Instituto de Química, UNESP, PO Box 355, 14801-970 Araraquara, SP (Brazil); Department of Analytical and Physical Chemistry, Univ. Jaume I, Castelló de la Plana 12071 (Spain); Ferrer, Mateus M.; Santana, Yuri V.B. de; Raubach, Cristiane W. [Departamento de Química, UFSCar, PO Box 676, 13565-905 São Carlos, SP (Brazil); Longo, Valéria M. [Instituto de Química, UNESP, PO Box 355, 14801-970 Araraquara, SP (Brazil); Sambrano, Júlio R. [Laboratório de Simulação Molecular, UNESP, PO Box 473, 17033-360 Bauru, SP (Brazil); Longo, Elson [Instituto de Química, UNESP, PO Box 355, 14801-970 Araraquara, SP (Brazil); Andrés, Juan [Department of Analytical and Physical Chemistry, Univ. Jaume I, Castelló de la Plana 12071 (Spain); Li, Máximo S. [Departamento de Física, USP, PO Box 369, 13560-970 São Carlos, São Paulo (Brazil); Varela, José A. [Instituto de Química, UNESP, PO Box 355, 14801-970 Araraquara, SP (Brazil)

    2013-04-15

    Highlights: ► This work details the efficiency of microwave solvothermal synthesis in obtaining ZnS nanocrystals. ► The structure, surface chemical composition and optical properties were investigated as function of the precursor. ► According to the different precursors used, the PL behavior of ZnS causes a red shift which enables the design of LEDs with different colors. ► Photoluminescence is one more interesting property for technological applications this material. -- Abstract: In this article, we report the development of an efficient and rapid microwave assisted solvothermal (MAS) method to prepare wurtzite ZnS nanoparticles at 413 K using different precursors. The materials obtained were analyzed by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (MET) ultraviolet–visible (UV–vis) and photoluminescence (PL) measurements. The structure, surface chemical composition and optical properties were investigated as a function of the precursor. In addition, effects as well as merits of microwave heating on the processing and characteristics of ZnS nanoparticles obtained are reported. The possible formation mechanism and optical properties of these nanoparticles were also reported.

  7. Microwave assisted extraction of pectin from waste Citrullus lanatus fruit rinds.

    Science.gov (United States)

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

    2014-01-30

    In this present study, microwave-assisted extraction (MAE) was applied to extraction of pectin from waste Citrullus Lanatus fruit rinds. Extraction parameters which are employed in this study are microwave power (160-480 W), irradiation time (60-180s), pH (1-2) and solid-liquid ratio (1:10-1: 30 g/ml) and they were optimized using a four factor three levels Box-Behnken response surface design (BBD) coupled with desirability function methodology. The results showed that, all the process variables have significant effect on the extraction yield of pectin. Optimum MAE conditions for the highest pectin yield from waste C. Lanatus fruit rinds (25.79%) were obtained with microwave power of 477 W, irradiation time of 128 s, pH of 1.52, solid-liquid ratio of 1:20.3g/ml respectively. Validation experiment results were well agreed with predicted value. Copyright © 2013 Elsevier Ltd. All rights reserved.

  8. Microwave-Assisted Synthesis of Chitosan/Polyvinyl Alcohol Silver Nanoparticles Gel for Wound Dressing Applications

    Directory of Open Access Journals (Sweden)

    Nguyen Thi Hiep

    2016-01-01

    Full Text Available The purpose of this study was to fabricate chitosan/poly(vinyl alcohol/Ag nanoparticles (CPA gels with microwave-assistance for skin applications. Microwave irradiation was employed to reduce silver ions to silver nanoparticles and to crosslink chitosan (CS with polyvinyl alcohol (PVA. The presence of silver nanoparticles in CPA gels matrix was examined using UV-Vis spectroscopy, transmission electron microscopy, and X-ray diffraction. The interaction of CS and PVA was analysed by Fourier transform infrared spectroscopy. The release of silver ions was determined by atomic absorption spectrometry. The antimicrobial properties of CPA gels against P. aeruginosa and S. aureus were investigated using agar diffusion method. Finally, the biocompatibility and wound-healing ability of the gels were studied using fibroblast cells (in vitro and mice models (in vivo. In conclusion, the results showed that CPA gels were successfully fabricated using microwave irradiation method. These gels can be applied to heal an open wound thanks to their antibacterial activity and biocompatibility.

  9. [Investigation on low power microwave irradiation-assisted enzymatic esterification in organic solvent by fluorescence spectroscopy].

    Science.gov (United States)

    Min, Rui; Fang, Yun; Xia, Yong-Mei

    2009-02-01

    The authors studied the fluorescence change of immobilized lipase from Rhizomucor miehei in the microwave assisted enzymatic esterification of caprylic acid and butanol in organic medium by investigating the fluorescence spectra in solvent or aqueous buffer after incubating the lipase with the solvent, caprylic acid and butanol under microwave irradiation, respectively. A comparison was made with the conventional heated enzymatic esterification in the solvents. Both of the heating modes, the microwave irradiation and conventional heating, can enhance the fluorescence intensity without shifting the emission wavelength of the lipase. In the circumstance that the irradiation can accelerate the esterification, the irradiation can enhance the exposure of the lipase protein molecules in the aqueous environment after incubating the lipase with solvents or the substrates. The effect of the reaction mixture on the fluorescence intensity was dominated by the solvents. The trend of the plot of log P versus the initial reaction rate was similar to that of log P versus fluorescence intensity of lipase in aqueous buffer after esterification; but was different from that of log P versus fluorescence intensity of lipase in organic medium.

  10. Optimization of microwave assisted extraction of pectin from sour orange peel and its physicochemical properties.

    Science.gov (United States)

    Hosseini, Seyed Saeid; Khodaiyan, Faramarz; Yarmand, Mohammad Saeid

    2016-04-20

    Microwave assisted extraction technique was used to extract pectin from sour orange peel. Box-Behnken design was used to study the effect of irradiation time, microwave power and pH on the yield and degree of esterification (DE) of pectin. The results showed that the optimum conditions for the highest yield of pectin (29.1%) were obtained at pH of 1.50, microwave power of 700W, and irradiation time of 3min. DE values of pectin ranged from 1.7% to 37.5%, indicating that the obtained pectin was low in methoxyl. Under optimal conditions, the galacturonic acid content and emulsifying activity were 71.0±0.8% and 40.7%, respectively. In addition, the emulsion stability value ranged from 72.1% to 83.4%. Viscosity measurement revealed that the solutions of pectin at low concentrations showed nearly Newtonian flow behavior, and as the concentration increased, pseudoplastic flow became dominant.

  11. Effect of Microwave-Assisted Extraction on the Phenolic Compounds and Antioxidant Capacity of Blackthorn Flowers.

    Science.gov (United States)

    Lovrić, Vanja; Putnik, Predrag; Kovačević, Danijela Bursać; Jukić, Marijana; Dragović-Uzelac, Verica

    2017-06-01

    This research was undertaken to investigate the influence of extraction parameters during microwave-assisted extraction on total phenolic content, total flavonoids, total hydroxycinnamic acids and total flavonols of blackthorn flowers as well as to evaluate the antioxidant capacity by two different methods (2,2-diphenyl-1-picrylhydrazyl free radical scavenging capacity and ferric reducing antioxidant power assays). The investigated extraction parameters were: solvent type and volume fraction of alcohol in solvent (50 and 70% aqueous solutions of ethanol and methanol), extraction time (5, 15 and 25 min) and extraction temperature (40, 50 and 60 °C) controlled by microwave power of 100, 200 and 300 W. Multivariate analysis of variance (MANOVA) was used to evaluate the differences at a 95% confidence level (p≤0.05). The obtained results show that aqueous solution of ethanol was more appropriate solvent for extraction of phenolic compounds (total flavonoids, total hydroxycinnamic acids and total flavonols) than aqueous solution of methanol. The amount of phenolic compounds was higher in 70% aqueous solution of ethanol or methanol, while higher antioxidant capacity was observed in 50% aqueous solution of methanol. Higher temperature of extraction improved the amount of phenolic compounds and also antioxidant capacity determined by 2,2-diphenyl-1-picrylhydrazyl free radical scavenging capacity assay. Extensive duration of extraction (15- to 25-minute interval) has a significant effect only on the increase of total phenolic content, while specific phenolic compound content and antioxidant capacity were the highest when microwave extraction time of 5 min was applied.

  12. Pectin from Opuntia ficus indica: Optimization of microwave-assisted extraction and preliminary characterization.

    Science.gov (United States)

    Lefsih, Khalef; Giacomazza, Daniela; Dahmoune, Farid; Mangione, Maria Rosalia; Bulone, Donatella; San Biagio, Pier Luigi; Passantino, Rosa; Costa, Maria Assunta; Guarrasi, Valeria; Madani, Khodir

    2017-04-15

    Optimization of microwave-assisted extraction (MAE) of water-soluble pectin (WSP) from Opuntia ficus indica cladodes was performed using Response Surface Methodology. The effect of extraction time (X1), microwave power (X2), pH (X3) and solid-to-liquid ratio (X4) on the extraction yield was examined. The optimum conditions of MAE were as follows: X1=2.15min; X2=517W; X3=2.26 and X4=2g/30.6mL. The maximum obtained yield of pectin extraction was 12.57%. Total carbohydrate content of WSP is about 95.5% including 34.4% of Galacturonic acid. Pectin-related proteins represent only the 0.66% of WSP mass. HPSEC and light scattering analyses reveal that WSP is mostly constituted of high molecular pectin and FTIR measurements show that the microwave treatment does not alter the chemical structure of WSP, in which Galacturonic acid content and yield are 34.4% and 4.33%, respectively. Overall, application of MAE can give rise to high quality pectin.

  13. Self-assembly of nanostructures obtained in a microwave-assisted oxidative polymerization of aniline

    Directory of Open Access Journals (Sweden)

    M. R. Gizdavic-Nikolaidis

    2014-10-01

    Full Text Available For the first time, microwave assisted aniline oxidative polymerization is performed in the presence of acetic acid (CH3COOH and ammonium hydroxide (NH4OH at different microwave power levels. The reaction system is kept at constant temperature of 24±1°C. The products are investigated by Fourier Transform Infrared Spectroscopy (FTIR, Raman, solid-state Nuclear Magnetic Resonance (NMR and Electron Paramagnetic Resonance (EPR spectroscopies. EPR signals in polyaniline (PANI originate from the polarons formed upon protonation and doping by acid. The microwave radiation causes an increase in the spin concentration which is slightly more evident for 8 W than for 93 W. The morphology is investigated by using scanning electron microscopy (SEM. SEM micrographs revealed the formation of nanorods (in the presence of CH3COOH and nanospheres (in the presence of NH4OH. FTIR, Raman and solid-state NMR spectroscopies indicate the presence of PANI and aniline oligomers. X-ray Diffraction (XRD measurements showed the presence of well-ordered structures.

  14. Assisted Tandem Catalysis : Metathesis Followed by Asymmetric Hydrogenation from a Single Ruthenium Source

    NARCIS (Netherlands)

    Renom-Carrasco, Marc; Gajewski, Piotr; Pignataro, Luca; de Vries, Johannes G.; Piarulli, Umberto; Gennari, Cesare; Lefort, Laurent

    2015-01-01

    Here we report the first example of a tandem metathesis-asymmetric hydrogenation protocol where the prochiral olefin generated by metathesis is hydrogenated with high enantioselectivity by an in situ formed chiral ruthenium catalyst. We show that either the ruthenium metathesis catalysts or the ruth

  15. Physicochemical characterization of microwave assisted synthesis of silver nanoparticles using Aloe Vera (Aloe barbadensis)

    Science.gov (United States)

    Kuponiyi, Abiola John

    Biosynthesis of silver nanoparticles (AgNP) using different biological extracts is gaining recognition for its numerous applications in different disciplines. Although different approaches (physical and chemical) have been used for the synthesis of AgNP, the green chemistry method is most preferable because of its high efficacy, cost effectiveness, and environmental benignity. Aloe Vera (AV) contains chemical compounds (anthraquinones) that are known to possess antibacterial, antivirus and anticancer properties and the extract is a good chemical reduction agent for AgNP. Hence, it was hypothesized that a microwave assisted synthesis will produce highly concentrated, homogeneous, stable and biologically active AgNP. Thus, the main objective of the study was to evaluate the effect of microwave assisted synthesis of AgNP, the effect of pulse laser treatment on size reduction of a microwave synthesized AgNP, and the physicochemical characterization of AgNP synthesized with Aloe Vera water and ethanol extract. The experiment was conducted in two phases. Phase 1 was first conducted to optimize the experimental variables, thus establishing the optimum variables to apply in the second phase. The experiment in Phase 1 was conducted using three-factor factorial experimental design comprised of the following factors: 1) Extraction Solvent, 2) Heating Methods, 3) pH; and their corresponding levels were water and ethanol, conventional and microwave, pH (7, 8, 10 and 12), respectively. All synthesis was conducted at constant temperature of 80°C. Phase II experimental treatments were Laser ablation (0, 5, and 10 min) and Storage time (Week 1, 2 & 3). The Phase I of the results showed that increased AgNP concentrations were significantly (p 0.05) impact the particle size distribution. Hence, the Zeta potential of the particles has values typically ranging between +100 mV to -100 mV, hence indicative of colloidal stability matrix. Furthermore, the Polydispersity indexes of Week 1

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

    Energy Technology Data Exchange (ETDEWEB)

    Wang Ziming, E-mail: wangziming@jlu.edu.cn [College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012 (China); College of Environment and Resources, Jilin University, 2699 Qianjin Street, Changchun 130012 (China); Zhao Xin; Xu Xu; Wu Lijie; Su Rui; Zhao Yajing; Jiang Chengfei; Zhang Hanqi [College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012 (China); Ma Qiang [Chinese Academy of Inspection and Quarantine, Beijing 100123 (China); Lu Chunmei [College of Technology Center, Jilin Entry-Exit Inspection and Quarantine Bureau, Changchun 130062 (China); Dong Deming [College of Environment and Resources, Jilin University, 2699 Qianjin Street, Changchun 130012 (China)

    2013-01-14

    Highlights: Black-Right-Pointing-Pointer An absorbing microwave {mu}-SPE device packed with activated carbon was used. Black-Right-Pointing-Pointer Absorbing microwave {mu}-SPE device was made and used to enrich the analytes. Black-Right-Pointing-Pointer Absorbing microwave {mu}-SPE device was made and used to heat samples directly. Black-Right-Pointing-Pointer MAE-{mu}-SPE was applied to the extraction of OPPs with non-polar solvent only. - Abstract: A single-step extraction-cleanup method, including microwave-assisted extraction (MAE) and micro-solid-phase extraction ({mu}-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 {mu}-SPE device, was prepared by packing activated carbon with microporous polypropylene membrane envelope, and used as not only the sorbent in {mu}-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 {mu}-SPE devices were added in the microwave extraction vessel, the extraction was carried out under 400 W irradiation power at 60 Degree-Sign C for 10 min. The extracts obtained by MAE-{mu}-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%.

  17. A simultaneous, direct microwave/ultrasound-assisted digestion procedure for the determination of total Kjeldahl nitrogen.

    Science.gov (United States)

    Domini, Claudia; Vidal, Lorena; Cravotto, Giancarlo; Canals, Antonio

    2009-04-01

    Simultaneous direct irradiation with microwaves and ultrasound was used to determine total Kjeldahl nitrogen. The method involves chemical digestion in two steps, mineralization with sulfuric acid and oxidation with H(2)O(2). The most influential variables for the microwave/ultrasound (MW/US)-assisted digestion were optimized using tryptophan as the model substance. The optimum conditions were: H(2)SO(4) volume, 10 mL; H(2)O(2) volume, 5 mL; weight of sample, 0.05 g; MW power, 500 W; US power, 50 W; digestion time, 7 min (i.e., 5 min mineralization and 2 min oxidation). A modification of the classical Kjeldahl (Hach) method and an US-assisted digestion method were used for comparison. The latter was also optimized; the optimum conditions were: H(2)SO(4) volume, 10 mL; H(2)O(2) volume, 5 mL; sonication time with H(2)SO(4), 15 min; sonication time with H(2)O(2),10 min; US power, 50 W; weight of sample, 0.05 g. Five pure amino acids and two certified reference materials (NIST standard reference materials 1547 (peach leaves), and soil, NCS DC 73322) were analyzed to assess the accuracy of our new MW/US-assisted digestion method, that was successfully applied to five real samples. The significant reduction in digestion time (being 30 min and 25 min for classical Kjeldahl and US-assisted digestion methods, respectively) and consumption of reagents show that simultaneous and direct MW/US irradiation is a powerful and promising tool for low-pressure digestion of solid and liquid samples.

  18. MICROWAVE ASSISTED HYDRODISTILLATION UNTUK EKSTRAKSI MINYAK ATSIRI DARI KULIT JERUK BALI SEBAGAI LILIN AROMATERAPI

    Directory of Open Access Journals (Sweden)

    Megawati -

    2015-07-01

    Full Text Available Ekstraksi minyak atsiri kulit jeruk bali dilakukan menggunakan metode Microwave Assisted Hydrodistillation dengan variasi daya (800, 600, 450, 300, dan 100 W dan massa bahan (150, 125, 100, 75,dan 50 g. Ektraksi dengan variasi daya dilakukan pada massa 150 g dan didapat daya optimum yaitu 600 W, sedangkan ekstraksi dengan variasi massa bahan dilakukan pada daya 600 W. Minyak atsiri yang diperoleh dianalisis densitas, kelarutan dalam alkohol 95% dan senyawa kimia minyak atsiri kulit jeruk bali menggunakan Gas Chromatography-Mass Spectrometry (GC-MS dan minyak atsiri kulit jeruk bali yang didapat diaplikasikan untuk lilin aromaterapi. Hasil penelitian menunjukkan semakin besar daya yang digunakan maka volum minyak yang dihasilkan semakin besar dan waktu ekstraksinya lebih cepat. Variasi massa bahan menunjukkan semakin besar massa bahan massa bahan yang digunakan maka volum minyak yang dihasilkan semakin besar. Densitas minyak atsiri kulit jeruk bali hasil penelitian yaitu 0,810 g/mL, larut pada alkohol 95% dengan perbandingan minyak-alkohol 1:6 dan terdapat tiga komponen senyawa kimia penyusun minyak atsiri kulit jeruk bali yaitu limonen (93,99%, β-pinene (3,20%, dan germakren-D (2,82%. Minyak atsiri kulit jeruk bali hasil ekstraksi yang diperoleh dapat diaplikasikan untuk lilin aromaterapi. Kata kunci: Kulit jeruk bali, lilin aromaterapi, microwave assisted hydrodistillation, minyak atsiri. Essential oils extracted from pomelo peel was performed using Microwave Assisted Hydrodistillation with variations of microwave oven power (800, 600, 450, 300, and 100 W and material mass (150, 125, 100, 75, and 50 g. The extraction with power variation was conducted with 150 g of material and the optimum extraction power was obtained at 600 W. Therefore material mass variation was conducted with microwave oven power of 600 W. The essential oils produced were analyzed for its density, solubility in alcohol of 95% v/v, and chemical composition. The chemical

  19. Microwave-assisted methyl esters synthesis of Kapok (Ceiba pentandra seed oil: parametric and optimization study

    Directory of Open Access Journals (Sweden)

    Awais Bokhari

    2015-09-01

    Full Text Available The depleting fossil fuel reserves and increasing environmental concerns have continued to stimulate research into biodiesel as a green fuel alternative produced from renewable resources. In this study, Kapok (Ceiba pentandra oil methyl ester was produced by using microwave-assisted technique. The optimum operating conditions for the microwave-assisted transesterification of Kapok seed oil including temperature, catalyst loading, methanol to oil molar ratio, and irradiation time were investigated by using Response Surface Methodology (RSM based on Central Composite Design (CCD. A maximum conversion of 98.9 % was obtained under optimum conditions of 57.09 °C reaction temperature, 2.15 wt% catalyst (KOH loading, oil to methanol molar ratio of 1:9.85, and reaction time of 3.29 min. Fourier Transform Infra-Red (FT-IR spectroscopy was performed to verify the conversion of the fatty acid into methyl esters. The properties of Kapok oil methyl ester produced under the optimum conditions were characterized and found in agreement with the international ASTM D 6751 and EN 14214 standards.

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

    Science.gov (United States)

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

    2008-10-01

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

  1. Evaluation of hemocompatibility and in vitro immersion on microwave-assisted hydroxyapatite–alumina nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Radha, G. [National Centre for Nanoscience and Nanotechnology, University of Madras, Guindy campus, Chennai - 600025 (India); Balakumar, S., E-mail: balasuga@yahoo.com [National Centre for Nanoscience and Nanotechnology, University of Madras, Guindy campus, Chennai - 600025 (India); Venkatesan, Balaji; Vellaichamy, Elangovan [Department of Biochemistry, University of Madras, Guindy campus, Chennai - 600025 (India)

    2015-05-01

    This study reports the microwave-assisted synthesis and characterization of nHAp (nano-hydroxyapatite)–alumina composites. The crystalline phase and interaction of alumina with nHAp was analyzed using X-ray diffraction (XRD) and Raman microscopy analysis, respectively. High resolution transmission electron microscopy (HRTEM) micrographs exhibit morphological changes of nHAp composites with increasing alumina concentrations. Microhardness studies reveal the enhanced mechanical strength of nHAp10 and nHAp20 nanocomposites than pure nHAp. In vitro bioactivity of the nanocomposites was studied by immersing samples in simulated body fluid (Hank's solution) for 21 days. The surface of biomineralized samples were analyzed using field emission scanning electron microscopy (FESEM) and energy dispersive X-ray spectroscopy (EDX). Hemolytic assay revealed acceptable compatibility for varying concentrations of all the samples. Cell proliferation assay was systematically investigated for 1 day and 3 days on Saos-2 osteoblast-like cell lines and it was found that nHAp nanocomposites improved the proliferation. - Highlights: • The microwave-assisted hydroxyapatite (nHAp)–alumina nanocomposites were prepared. • Structural and interaction between nHAp and alumina have been explored. • Increased alumina concentration enhanced mechanical strength of the nHAp. • Trace elements from SBF, incorporated on nHAp–alumina nanocomposite surface, were characterized by FESEM and EDX techniques. • Hemocompatibility of the samples were evaluated and the results are in accordance with ASTM standards.

  2. Ionic Liquid-Based Microwave-Assisted Extraction of Flavonoids from Bauhinia championii (Benth. Benth.

    Directory of Open Access Journals (Sweden)

    Wei Xu

    2012-12-01

    Full Text Available An ionic liquids (IL-based microwave-assisted approach for extraction and determination of flavonoids from Bauhinia championii (Benth. Benth. was proposed for the first time. Several ILs with different cations and anions and the microwave-assisted extraction (MAE conditions, including sample particle size, extraction time and liquid-solid ratio, were investigated. Two M 1-butyl-3-methylimidazolium bromide ([bmim] Br solution with 0.80 M HCl was selected as the optimal solvent. Meanwhile the optimized conditions a ratio of liquid to material of 30:1, and the extraction for 10 min at 70 °C. Compared with conventional heat-reflux extraction (CHRE and the regular MAE, IL-MAE exhibited a higher extraction yield and shorter extraction time (from 1.5 h to 10 min. The optimized extraction samples were analysed by LC-MS/MS. IL extracts of Bauhinia championii (Benth.Benth consisted mainly of flavonoids, among which myricetin, quercetin and kaempferol, β-sitosterol, triacontane and hexacontane were identified. The study indicated that IL-MAE was an efficient and rapid method with simple sample preparation. LC-MS/MS was also used to determine the chemical composition of the ethyl acetate/MAE extract of Bauhinia championii (Benth. Benth, and it maybe become a rapid method to determine the composition of new plant extracts.

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

    Science.gov (United States)

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

    2013-06-19

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

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

    Science.gov (United States)

    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.

  5. Efficient synthesis of sulfonamide derivatives on solid supports catalyzed using solvent-free and microwave-assisted methods

    Directory of Open Access Journals (Sweden)

    Argelia Camargo-Ordoñez

    2011-01-01

    Full Text Available In this work we report the synthesis of sulfonamide derivatives using a conventional procedure and with solid supports, such as silica gel, florisil, alumina, 4Å molecular sieves, montmorillonite KSF, and montmorillonite K10 using solvent-free and microwave-assisted methods. Our results show that solid supports have a catalytic activity in the formation of sulfonamide derivatives. We found that florisil, montmorillonite KSF, and K10 could be used as inexpensive alternative catalysts that are easily separated from the reaction media. Additionally, solvent-free and microwave-assisted methods were more efficient in reducing reaction time and in increasing yield.

  6. Efficient synthesis of sulfonamide derivatives on solid supports catalyzed using solvent-free and microwave-assisted methods

    Energy Technology Data Exchange (ETDEWEB)

    Camargo-Ordonez, Argelia; Moreno-Reyes, Christian; Olazaran-Santibanez, Fabian; Martinez-Hernandez, Sheila; Bocanegra-Garcia, Virgilio; Rivera, Gildardo [Universidad Autonoma de Tamaulipas, Reynosa (Mexico). Dep. de Farmacia y Quimica Medicinal

    2011-07-01

    In this work we report the synthesis of sulfonamide derivatives using a conventional procedure and with solid supports, such as silica gel, florisil, alumina, 4A molecular sieves, montmorillonite KSF, and montmorillonite K10 using solvent-free and microwave-assisted methods. Our results show that solid supports have a catalytic activity in the formation of sulfonamide derivatives. We found that florisil, montmorillonite KSF, and K10 could be used as inexpensive alternative catalysts that are easily separated from the reaction media. Additionally, solvent-free and microwave-assisted methods were more efficient in reducing reaction time and in increasing yield. (author)

  7. Microwave assisted synthesis of fluorene-based copolymers with different conjugate degreed quinoxaline segments from reactive polymer

    Energy Technology Data Exchange (ETDEWEB)

    Li, Jixin; Song, Xiaohui; Feng, Ying [School of Petrochemical Engineering, Shenyang University of Technology, 30 Guanghua Street, Liaoyang 111003 (China); Wang, Zhiming, E-mail: wangzm2011@yahoo.com.cn [School of Petrochemical Engineering, Shenyang University of Technology, 30 Guanghua Street, Liaoyang 111003 (China); State Key Laboratory of Supramolecular Structure and Materials, Jilin University, 2699 Qianjin Avenue, Changchun 130012 (China); Zhang, Xiaojuan [School of Petrochemical Engineering, Shenyang University of Technology, 30 Guanghua Street, Liaoyang 111003 (China); Shen, Fangzhong; Lu, Ping [State Key Laboratory of Supramolecular Structure and Materials, Jilin University, 2699 Qianjin Avenue, Changchun 130012 (China)

    2013-10-31

    In this work, we prepared three fluorene-based copolymers with different conjugate degreed quinoxaline segments from one reactive polymer by microwave assisted method. The obtained quinoxaline-based copolymers exhibited different bright color emissions, high photoluminescence quantum, low electron affinity and electron injection barrier. This approach not only simplified the steps of similar-structure polymers, but also avoided the monomer solubility problem. - Highlights: • Quinoxaline-based copolymers were prepared in microwave-assisted synthesis. • Polymer-synthesis containing different acceptors was simplified from reactive polymer. • Multi-functions were tuned by controlling reactive monomer structures.

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

    Science.gov (United States)

    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.

  9. Fast preparation of LiFePO4 nanoparticles for lithium batteries by microwave-assisted hydrothermal method.

    Science.gov (United States)

    Yang, Gang; Ji, Hongmei; Liu, Haidong; Huo, Kaifu; Fu, Jijiang; Chu, Paul K

    2010-02-01

    Nanomaterial for lithium batteries can decrease mechanical strain upon lithium intercalation/ deintercalation from lattice, and lead to high rate capability. The currently available microwave technology permits the development and implantation of a temperature-controlled microwave-assisted hydrothermal synthesis (TCMH) of nano-sized cathode material for lithium batteries. Unlike in previous reported traditional hydrothermal synthesis of cathode material LiFePO4, the pure phase of LiFePO4 can be simply and rapidly synthesized for 5 minutes in water under hydrothermal treatment with microwave irradiation. The homogeneous effects induced by microwave irradiation could create a uniform seeding condition. The colloid precursor Li3PO4 plays the key role to be the nucleation center for the new phase while the formation energy for LiFePO4 would be decreased during the following microwave irradiation. The as-prepared pristine LiFePO4 without carbon coating are characterized by X-ray diffraction, Raman, scanning and transmission electron microscopy, and tested as the cathode in lithium batteries. The particle sizes of pristine LiFePO4 are dependent on hydrothermal and microwave-assisted hydrothermal condition and the electrochemical performance are relatively determined.

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

    Science.gov (United States)

    Nad, Shreya; Gu, Yajun; Asmussen, Jes

    2015-07-01

    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 efficiencies (η(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.

  11. Fast microwave-assisted extraction of rotenone for its quantification in seeds of yam bean (Pachyrhizus sp.).

    Science.gov (United States)

    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.

  12. Effect of deposition parameters on the structural properties of ZnO nanopowders prepared by microwave-assisted hydrothermal synthesis.

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Zhenxing [School of Chemistry and Materials Science, Huaibei Normal University, Huaibei 235000 (China); Wang, Guangjian, E-mail: wgj2260@chnu.edu.cn [School of Chemistry and Materials Science, Huaibei Normal University, Huaibei 235000 (China); Guo, Yajie; Kang, Fangfang; Huang, Yanhong; Bo, Dongsheng [School of Chemistry and Materials Science, Huaibei Normal University, Huaibei 235000 (China)

    2012-12-15

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

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

    Science.gov (United States)

    Lieu, Thanh; Yusup, Suzana; Moniruzzaman, Muhammad

    2016-07-01

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

  15. Oyster and Pyramidella Shells as Heterogeneous Catalysts for the Microwave-Assisted Biodiesel Production from Jatropha curcas Oil

    Directory of Open Access Journals (Sweden)

    Achanai Buasri

    2015-01-01

    Full Text Available Microwave-assisted biodiesel production via transesterification of Jatropha curcas oil with methanol using solid oxide catalyst derived from waste shells of oyster and Pyramidella was studied. The shells were calcined at 900°C for 2 h and calcium oxide (CaO catalyst characterizations were carried out by X-ray diffraction (XRD, X-ray fluorescence (XRF, scanning electron microscope (SEM, and the Brunauer-Emmett-Teller (BET surface area measurements. The effects of reaction variables such as reaction time, microwave power, methanol/oil molar ratio, and catalyst loading on the yield of biodiesel were investigated. Reusability of waste shell catalyst was also examined. The results indicated that the economic and environmentally friendly catalysts derived from oyster and Pyramidella shells showed good reusability and had high potential to be used as biodiesel production catalysts under microwave-assisted transesterification of Jatropha curcas oil with methanol.

  16. Enhanced photocatalytic degradation of methylene blue by ZnO-reduced graphene oxide composite synthesized via microwave-assisted reaction

    Energy Technology Data Exchange (ETDEWEB)

    Lv Tian [Engineering Research Center for Nanophotonics and Advanced Instrument, Ministry of Education, Department of Physics, East China Normal University, Shanghai, 200062 (China); Pan Likun, E-mail: lkpan@phy.ecnu.edu.cn [Engineering Research Center for Nanophotonics and Advanced Instrument, Ministry of Education, Department of Physics, East China Normal University, Shanghai, 200062 (China); Liu Xinjuan; Lu Ting; Zhu Guang; Sun Zhuo [Engineering Research Center for Nanophotonics and Advanced Instrument, Ministry of Education, Department of Physics, East China Normal University, Shanghai, 200062 (China)

    2011-10-13

    Highlights: > ZnO-reduced graphene oxide composite is synthesized via microwave assisted reaction. > The method allows a facile, safe and rapid reaction in aqueous media. > A high dye degradation efficiency is achieved under UV light irradiation. - Abstract: A quick and facile microwave-assisted reaction is used to synthesize ZnO-reduced graphene oxide (RGO) hybrid composites by reducing graphite oxide dispersion with zinc nitrate using a microwave synthesis system. Their photocatalytic performance in degradation of methylene blue is investigated and the results show that the RGO plays an important role in the enhancement of photocatalytic performance and the ZnO-RGO composite with 1.1 wt. % RGO achieves a maximum degradation efficiency of 88% in a neutral solution under UV light irradiation for 260 min as compared with pure ZnO (68%) due to the increased light absorption, the reduced charge recombination with the introduction of RGO.

  17. Affinity labeling coupled with matrix assistant laser desorption tandem time of flight mass spectrometry for quantitative proteomies research

    Institute of Scientific and Technical Information of China (English)

    MENG Qingfang; ZHANG Yangjun; CAI Yun; QIAN Xiaohong

    2007-01-01

    A relative quantitative method for differential proteomics by cleavable isotope-coded atTmity tag (cICAT)and matrix-assisted laser desorption/ionization tandem time-of-flight mass spectrometry (MALDI-TOF-MS) was estab-lished. The accuracy and reproducibility of the method were evaluated by bovine serum albumin (BSA) digest as having a relative standard deviation of less than 30% and good reproducibility. The dynamic range was als0 evaluated by analyzing two mixtures of several standard proteins with dif-ferent concentration. The experimental results showed that in the dynamic range of 1:30, the quantitation error of the method was less than 30%. Although the quantitation error becomes very large when used beyond this range, it does not affect the derivation of information on the differential proteins. All the work provides an alternative method for differential proteomics analysis in biological samples from different origins.

  18. Microwave-assisted Fenton-like decolorization of methyl orange solution using chromium compounds

    Institute of Scientific and Technical Information of China (English)

    LIU Zuo-hua; TAO Chang-yuan; DU Jun; SUN Da-gui; LI Bai-zhan

    2008-01-01

    Azo dyes discharged in the environment are persistent organic pollutants (POPs), which are very difficult to remove. We developed a microwave-assisted Fenton-like process to degrade methyl orange (MO), an azo dye, with hydrogen peroxide (H2O2) catalyzed by chromium compounds coexisting with MO in the solution. Comparison between the Cr(III)-H2O2 and Cr(VI)-H2O2 systems shows that Cr(VI) has a stronger and more stable catalytical activity than Cr(III), and Cr(III) is more susceptible to a change in the acidity or alkalinity of the reaction system. With a Cr(VI) concentration of 10 mmol L-1 or a Cr(III) concentration of 12 mmol L-1 in the solution under the microwave irradiation of a power larger than 300 W for 3 min, 10 mmol L-1 H2O2 can degrade more than 95% of 1 000 mg L-1 methyl orange; when the microwave power is increased to 700 W, the same amount of H2O2 can degrade all methyl orange in the solution with the same amount of Cr(VI) catalyst. Ultraviolet-visible spectrography indicates the cleavage of the azo bond in methyl orange after treatment, suggesting the potential of this Fenton-like process to degrade azo dye POPs. Reusing waste chromium compounds coexisting with dyestuff in wastewater to catalyze the degradation of azo dyes could be a cost-effective technique for azo dyes and chromate manufacturers and/or users to treat their wastewater and prevent POPs from endangering the environment. This is of particular importance to controlling the water quality of the Three Gorges Reservoir.

  19. Rapid synthesis of tin oxide nanostructures by microwave-assisted thermal oxidation for sensor applications

    Science.gov (United States)

    Phadungdhitidhada, S.; Ruankham, P.; Gardchareon, A.; Wongratanaphisan, D.; Choopun, S.

    2017-09-01

    In the present work nanostructures of tin oxides were synthesized by a microwave-assisted thermal oxidation. Tin precursor powder was loaded into a cylindrical quartz tube and further radiated in a microwave oven. The as-synthesized products were characterized by scanning electron microscope, transmission electron microscope, and x-ray diffractometer. The results showed that two different morphologies of SnO2 microwires (MWs) and nanoparticles (NPs) were obtained in one minute of microwave radiation under atmospheric ambient. A few tens of the SnO2 MWs with the length of 10-50 µm were found. Some parts of the MWs were decorated with the SnO2 NPs. However, most of the products were SnO2 NPs with the diameter ranging from 30-200 nm. Preparation under loosely closed system lead to mixed phase SnO-SnO2 NPs with diameter of 30-200 nm. The single-phase of SnO2 could be obtained by mixing the Sn precursor powders with CuO2. The products were mostly found to be SnO2 nanowires (NWs) and MWs. The diameter of SnO2 NWs was less than 50 nm. The SnO2 NPs, MWs, and NWs were in the cassiterite rutile structure phase. The SnO NPs was in the tetragonal structure phase. The growth direction of the SnO2 NWs was observed in (1 1 0) and (2 2 1) direction. The ethanol sensor performance of these tin oxide nanostructures showed that the SnO-SnO2 NPs exhibited extremely high sensitivity. Invited talk at 5th Thailand International Nanotechnology Conference (Nano Thailand-2016), 27-29 November 2016, Nakhon Ratchasima, Thailand.

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

    Science.gov (United States)

    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. Au-controlled enhancement of photoluminescence of NiS nanostructures synthesized via a microwave-assisted hydrothermal technique

    CSIR Research Space (South Africa)

    Linganiso, EC

    2014-11-01

    Full Text Available Nickel sulphide (NiS) nanostructures decorated with gold (Au) nanoparticles (NPs) were synthesized via a microwave-assisted hydrothermal technique. Binary phase NiS (a and ß) crystalline nanostructures, bare, and decorated with Au NPs were obtained...

  2. Effect of the Solvent on the Microstructure of Bi2Te3 Obtained Solvothermal Microwave-assisted Synthesis

    Directory of Open Access Journals (Sweden)

    R.A. Lyubushkin

    2014-04-01

    Full Text Available In the present work, nanoparticles and nanowires have been prepared by solvothermal microwave-assisted synthesis using isopropyl alcohol, dimethylformamide (DMF and 1,4-dioxane respectively as the solvents. The microstructures of the synthesized powders have been characterized and the relationship with the solvent has been investigated.

  3. Microwave-assisted modulated synthesis of zirconium-based metal–organic framework (Zr-MOF) for hydrogen storage applications

    CSIR Research Space (South Africa)

    Ren, Jianwei

    2014-05-01

    Full Text Available Zirconium-based metal–organic framework (Zr-MOF) was synthesized using a microwave-assisted modulated method in a short reaction time of 5 min. The Zr-MOF material was highly crystalline with well-defined octahedral shaped crystals, and it exhibited...

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

    Science.gov (United States)

    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…

  5. Empirical modeling of drying kinetics and microwave assisted extraction of bioactive compounds from Adathoda vasica

    Directory of Open Access Journals (Sweden)

    Prithvi Simha

    2016-03-01

    Full Text Available To highlight the shortcomings in conventional methods of extraction, this study investigates the efficacy of Microwave Assisted Extraction (MAE toward bioactive compound recovery from pharmaceutically-significant medicinal plants, Adathoda vasica and Cymbopogon citratus. Initially, the microwave (MW drying behavior of the plant leaves was investigated at different sample loadings, MW power and drying time. Kinetics was analyzed through empirical modeling of drying data against 10 conventional thin-layer drying equations that were further improvised through the incorporation of Arrhenius, exponential and linear-type expressions. 81 semi-empirical Midilli equations were derived and subjected to non-linear regression to arrive at the characteristic drying equations. Bioactive compounds recovery from the leaves was examined under various parameters through a comparative approach that studied MAE against Soxhlet extraction. MAE of A. vasica reported similar yields although drastic reduction in extraction time (210 s as against the average time of 10 h in the Soxhlet apparatus. Extract yield for MAE of C. citratus was higher than the conventional process with optimal parameters determined to be 20 g sample load, 1:20 sample/solvent ratio, extraction time of 150 s and 300 W output power. Scanning Electron Microscopy and Fourier Transform Infrared Spectroscopy were performed to depict changes in internal leaf morphology.

  6. Microwave assisted leaching and electrochemical recovery of copper from printed circuit boards of computer waste

    Science.gov (United States)

    Ivǎnuş, R. C.; ǎnuş, D., IV; Cǎlmuc, F.

    2010-06-01

    Due to the rapid technological progress, the replacement of electronic equipment is very often necessary, leading to huge amounts that end up as waste. In addition, waste electrical and electronic equipment (WEEE) contains metals of high commercial value and others that are supposed to be hazardous for the environment. Consequently, WEEE could be considered as a significant source for recovery of nonferrous metals. Among these wastes, computers appear to be distinctive, as far as further exploitation is concerned. The most ″useful″ parts of the computers are the printed circuit boards that contain many metals of interest. A study on microwave assisted electronic scrap (printed circuit boards of computer waste - PCBs) leaching was carried out with a microwave hydrothermal reactor. The leaching was conducted with thick slurries (50-100 g/L). The leaching media is a mixed solution of CuCl2 and NaCl. Preliminary electrolysis from leaching solution has investigated the feasibility of electrodeposition of copper. The results were discussed and compared with the conventional leaching method and demonstrated the potential for selective extraction of copper from PCBs.

  7. Solvent-free, microwave-assisted synthesis of thiophene oligomers via Suzuki coupling.

    Science.gov (United States)

    Melucci, Manuela; Barbarella, Giovanna; Sotgiu, Giovanna

    2002-12-13

    The purpose of this study was to obtain a rapid, efficient, and environmentally friendly methodology for the synthesis of highly pure thiophene oligomers. The solvent-free, microwave-assisted coupling of thienyl boronic acids and esters with thienyl bromides, using aluminum oxide as the solid support, allowed us to rapidly check the reaction trends on changing times, temperature, catalyst, and base and easily optimize the experimental conditions to obtain the targeted product in fair amounts. This procedure offers a novel, general, and very rapid route to the preparation of soluble thiophene oligomers. Thus, for example, quaterthiophene was obtained in 6 min by reaction of 2-bromo-2,2'-bithiophene with bis(pinacolato)diboron (isolated yield 65%), whereas quinquethiophene was obtained in 11 min by reaction of dibromoterthiophene with thienylboronic acid (isolated yield 74%). The synthesis of new chiral 2,2'-bithiophenes is reported. The detailed analysis of the byproducts of some reactions allowed us to elucidate a few aspects of reaction mechanisms. While the use of microwaves proved to be very convenient for the coupling between conventional thienyl moieties, the same was not true for the coupling of thienyl rings to thienyl-S,S-dioxide moieties. Indeed, in this case, the targeted product was obtained in low yields because of the competitive, accelerated, Diels-Alder reaction that affords a variety of condensation products.

  8. Microwave assisted extraction for trace element analysis of plant materials by ICP-AES

    Energy Technology Data Exchange (ETDEWEB)

    Borkowska-Burnecka, J. [Wroclaw Univ. (Poland). Inst. Chemii

    2000-11-01

    Application of microwave assisted extraction for the decomposition and dissolution of plant samples for trace metal determination by ICP-AES was examined. Dried onion, leaves of spinach beet and three reference materials CTA-OTL-1, CTA-VTL-2 and CL-1 were analyzed. Water, EDTA and hydrochloric acid (0.01, 0.10 and 1.0 M, respectively) were used as leaching solutions. The extraction efficiency was investigated by comparison of the results with those obtained after microwave wet digestion. HCl was found to be very suitable for quantitative extraction of B, Ba, Cd, Cu, Mn, Ni, Pb, Sr and Zn from the samples. For reference materials, the measured concentrations are well consistent with the certified values. The use of EDTA led to a complete extraction of B, Cd, Ni, Pb, Sr and Zn. Water was found to be a good leaching solution for boron. For extraction with HCl and EDTA, the RSD values for the concentrations measured were below 8% for most of the elements. (orig.)

  9. Microwave-assisted extraction of active pharmaceutical ingredient from solid dosage forms.

    Science.gov (United States)

    Hoang, T H; Sharma, R; Susanto, D; Di Maso, M; Kwong, E

    2007-07-13

    The microwave assisted extraction (MAE) technique has been evaluated for the extraction of active pharmaceutical ingredients (API) from various solid dosage forms. Using immediate release tablets of Compound A as a model, optimization of the extraction method with regards to extraction solvent composition, extraction time and temperature was briefly discussed. Complete recovery of Compound A was achieved when samples were extracted using acetonitrile as the extraction solvent under microwave heating at a constant cell temperature of 50 degrees C for 5 min. The optimized MAE method was applied for content uniformity (single tablet extraction) and potency (multiple tablets extraction) assays of release and stability samples of two products of Compound A (5 and 25mg dose strength) stored at various conditions. To further demonstrate the applicability of MAE, the instrumental extraction conditions (50 degrees C for 5 min) were adopted for the extraction of montelukast sodium (Singulair) from various solid dosage forms using methanol-water (75:25, v/v) as the extraction solvent. The MAE procedure demonstrated an extraction efficiency of 97.4-101.9% label claim with the greatest RSD at 1.4%. The results compare favorably with 97.6-102.3% label claim with the greatest RSD at 2.9% obtained with validated mechanical extraction procedures. The system is affordable, user-friendly and simple to operate and troubleshoot. Rapid extraction process (7 min/run) along with high throughput capacity (up to 23 samples simultaneously) would lead to reduced cycle time and thus increased productivity.

  10. Microwave assisted leaching and electrochemical recovery of copper from printed circuit boards of computer waste

    Directory of Open Access Journals (Sweden)

    Ivănuş R.C.

    2010-06-01

    Full Text Available Due to the rapid technological progress, the replacement of electronic equipment is very often necessary, leading to huge amounts that end up as waste. In addition, waste electrical and electronic equipment (WEEE contains metals of high commercial value and others that are supposed to be hazardous for the environment. Consequently, WEEE could be considered as a significant source for recovery of nonferrous metals. Among these wastes, computers appear to be distinctive, as far as further exploitation is concerned. The most ″useful″ parts of the computers are the printed circuit boards that contain many metals of interest. A study on microwave assisted electronic scrap (printed circuit boards of computer waste – PCBs leaching was carried out with a microwave hydrothermal reactor. The leaching was conducted with thick slurries (50-100 g/L. The leaching media is a mixed solution of CuCl2 and NaCl. Preliminary electrolysis from leaching solution has investigated the feasibility of electrodeposition of copper. The results were discussed and compared with the conventional leaching method and demonstrated the potential for selective extraction of copper from PCBs.

  11. Phytochemical analysis of Myrtus communis plant: Conventional versus microwave assisted-extraction procedures.

    Science.gov (United States)

    Bouaoudia-Madi, Nadia; Boulekbache-Makhlouf, Lila; Kadri, Nabil; Dahmoune, Farid; Remini, Hocine; Dairi, Sofiane; Oukhmanou-Bensidhoum, Sonia; Madani, Khodir

    2017-06-10

    Background Myrtle (Myrtus communis L) may constitute an interesting dietary source of health protective compounds. Microwave-assisted extraction (MAE) of total phenolic compounds (TPC) from myrtle leaf, stems, pericarp, and seeds was studied and the results were compared with those of the conventional method extraction (CME) in terms of extraction time. Methods Extraction yield/efficiency and antioxidant activity were measured using radical scavenging assay (DPPH•) and reducing power. Results The results show that the MAE was higher in terms of saving energy, extraction time (62 s) and extraction efficiency of bioactive compound compared to CME (2 h). Leaf presented the optimum content of total phenols (250 mg GAE.g-1 DW) and flavonoids (13.65 mg GAE.g-1 DW). However, the anthocyanin content was most important in pericarp extract (176.50±2.17 mg Cyd-3-glu g-1 DW). The antioxidant activity was important in all parts, mainly in leaves. The results indicated that appropriate microwave treatment could be an efficient process to phenolic compounds recovery and thus, better the antioxidant activity of myrtle extract. Conclusions Principal component analysis (PCA) applied to the experimental data shows that the distribution of the myrtle phenolic compounds depended on their plant part localization as well as the extraction method.

  12. Microwave-assisted extraction and mild saponification for determination of organochlorine pesticides in oyster samples.

    Science.gov (United States)

    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.

  13. Microwave-Assisted Extraction Studies of Target Analyte Artemisinin from Dried Leaves of Artemisia annua L.

    Directory of Open Access Journals (Sweden)

    Himanshu Misra

    2013-01-01

    Full Text Available Artemisia annua L. (Asteraceae is an annual herb native of Asia. This plant has been used for many centuries in traditional Chinese medicine for the treatment of fever and malaria. Conventional methods for the extraction of artemisinin from A. annua including solvent extraction, Soxhlet extraction, and heat reflux extraction are characterized by long extraction times and the consumption of large volume of solvents. A simple, rapid, and precise microwave-assisted extraction process was optimized for fast sample preparation for the faster quantitative determination of artemisinin, potential new generation antimalarial drug, from dried leaves of Artemisia annua L. A simple experiment was designed for the optimization of the appropriate solvent under same extraction conditions. The selected appropriate solvent was then standardized for various different extraction variables. The major parameters studied showed effects on extraction efficiency including processing time, strength of microwave, moisture content, volume and nature of the solvent. The most favorable conditions were obtained by using plant material of 25 mesh (particle size extracted with acetone for 120 seconds at 160 W (i.e., 20% of total power. Quantitative analysis was performed using thin-layer chromatography coupled with a densitometer (TLC densitometry. The results showed that MAE can be used as an efficient and rapid method for the extraction of the active components from plants.

  14. Microwave Assisted Synthesis of Ferrite Nanoparticles: Effect of Reaction Temperature on Particle Size and Magnetic Properties.

    Science.gov (United States)

    Kalyani, S; Sangeetha, J; Philip, John

    2015-08-01

    The preparation of ferrite magnetic nanoparticles of different particle sizes by controlling the reaction temperature using microwave assisted synthesis is reported. The iron oxide nanoparticles synthesized at two different temperatures viz., 45 and 85 °C were characterized using techniques such as X-ray diffraction (XRD), small angle X-ray scattering (SAXS), vibrating sample magnetometry (VSM), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and Fourier transform infrared spectroscopy (FTIR). The average size of iron oxide nanoparticles synthesized at 45 and 85 °C is found to be 10 and 13.8 nm, respectively, and the nanoparticles exhibited superparamagantic behavior at room temperature. The saturation magnetization values of nanoparticles synthesized at 45 and 85 °C were found to be 67 and 72 emu/g, respectively. The increase in particle size and saturation magnetization values with increase in incubation temperature is attributed to a decrease in supersaturation at elevated temperature. The Curie temperature was found to be 561 and 566 0C for the iron oxide nanoparticles synthesized at 45 and 85 °C, respectively. The FTIR spectrum of the iron oxide nanoparticles synthesized at different temperatures exhibited the characteristic peaks that corresponded to the stretching of bonds between octahedral and tetrahedral metal ions to oxide ions. Our results showed that the ferrite nanoparticle size can be varied by controlling the reaction temperature inside a microwave reactor.

  15. Microwave-assisted extraction of jujube polysaccharide: Optimization, purification and functional characterization.

    Science.gov (United States)

    Rostami, Hosein; Gharibzahedi, Seyed Mohammad Taghi

    2016-06-05

    The operational parameters involved in microwave-assisted extraction (MAE) of jujube polysaccharide including microwave power, water to raw material ratio and extraction temperature and time were optimized by RSM. MAE at 400W, 75°C, 60 min, using 30 g water/g powdered jujube was the best condition for maximum yield (9.02%) of polysaccharide. Two novel water-soluble polysaccharides (JCP-1 and JCP-2) with average molecular weights of 9.1×10(4)-1.5×10(5)Da in term of the symmetrical narrow peaks were identified using the analytical purification procedures. The JCP-1 and JCP-2 mainly composed of glucose, arabinose, galactose and rhamnose in molar ratios of 1.4:2.1:4.2:0.9 and 1.2:1.8:4.1:1.1, respectively. The use of 1.5% JCP-1 led to a high emulsifying stability (95.5%) in a model oil-in-water type emulsion with a reduced surface tension (44.1 mN/m) and droplet size (1.32 μm), and an increased apparent viscosity (0.13 Pas) during 21-day cold storage. The antioxidant activities were increased in dose-dependent manners (25-200 μg/mL).

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

    Science.gov (United States)

    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.

  17. Microwave-assisted Syntheses and Crystal Structures of Benzimidazole Thiazolinone Derivatives

    Institute of Scientific and Technical Information of China (English)

    HU Jun; WANG Peng; WANG Ji-Kui; XU Yan-Hua

    2012-01-01

    A rapid and efficient microwave-assisted synthesis method for the preparation of 3-(lH-benzo[d]imidazol-2-yl)-2-substituted phenyl thiazolidin-4-one (4a, 4b) was described. The structures of 4a and 4b were determined by elemental analyses, IR, 1H NMR and X-ray diffraction. In the crystals of compounds 4a and 4b, the imidazole ring and two benzene rings are planar. Interestingly, the dihedral angle between two benzene rings is 71.5° in 4a, while it is almost perpendicular in 4b due to the different benzene substituents. Meanwhile, the thiazolidinone ring is planar in 4a while slightly distorted with an r.m.s deviation of 0.1494(2) A in 4b. The hydrogen bonding interactions observed link the molecules to form a dimeric unit, which may be effective in the stabilization of the structure.

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

    Science.gov (United States)

    Yuan, Yuan; Macquarrie, Duncan

    2015-09-20

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

  19. Microwave-assisted synthesis of WS2 nanowires through tetrathiotungstate precursors

    Directory of Open Access Journals (Sweden)

    Pravas Kumar Panigrahi and Amita Pathak

    2008-01-01

    Full Text Available Tungsten disulfide (WS2 nanowires have been synthesized through a microwave-assisted chemical route that uses tungstic acid, elemental sulfur and monoethanolamine as starting reagents for obtaining a precursor solution of tetrathiotungstate ions. Acidification of the precursor solution yields amorphous precipitates, which lead to the formation of nanowires of WS2 with thickness of about 5–10 nm when heated at 750 °C under argon atmosphere for 1.5 h. Phase and the microstructure of the prepared powders have been investigated through x-ray powder diffraction and high-resolution transmission electron microscopy, respectively. Optical absorption of the WS2 powders reveals a red shift of the exciton bands compared to bulk WS2.

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

    Science.gov (United States)

    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.

  1. Microwave assisted extraction process of betalain from dragon fruit and its antioxidant activities

    Directory of Open Access Journals (Sweden)

    K. Thirugnanasambandham

    2017-01-01

    Full Text Available The aim of this research was to optimize the operating parameters in microwave assisted extraction process (MIE such as temperature, mass of the sample, extraction time on the betalain content from dragon fruit peel using response surface methodology (RSM. Three factors three levels Box-Behnken response surface design (BBD was used for optimization and mathematical model development. Significant quadratic polynomial model was obtained (R2 = 0.9892 for betalain content with high coefficient determination value and numerical optimization was employed to achieve optimum conditions which was found to be; temperature of 35 °C, mass of the sample of 20 g, and treatment time of 8 min. Under these conditions, 9 mg/L of betalain content was obtained and it was validated using experimental values.

  2. Microwave-Assisted Synthesis of Alumina Nanoparticles Using Some Plants Extracts

    Directory of Open Access Journals (Sweden)

    Meisam Hasanpoor

    2017-01-01

    Full Text Available In present study we used five green plants for microwave assisted synthesis of Alumina nanoparticles from Aluminum nitrate. Structural characterization was studied using x-ray diffraction that showed semi- crystalline and possibly, amorphous structure. Fourier infrared spectroscopy was used to determine Al-O bond and functional groups responsible for synthesis of nanoparticles. FTIR confirmed existence of Al-O band and bio-functional groups, originated from plant extract. Morphology and size of nanoparticles were investigated using scanning electron microscopy, transmission electron microscopy and atomic force microscopy techniques. It was observed that nanoparticles have near-spherical shape. Average size of clusters of nanoparticles varied with different routes from of 60 nm to 300 nm. AFM images showed that Individual nanoparticles were less than 10 nm.

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

    Science.gov (United States)

    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.

  4. Antioxidant/antiradical properties of microwave-assisted extracts of three wild edible mushrooms.

    Science.gov (United States)

    Özyürek, Mustafa; Bener, Mustafa; Güçlü, Kubilay; Apak, Reşat

    2014-08-15

    A microwave-assisted extraction (MAE) process for polyphenols from three wild edible mushrooms was studied. The optimal extraction conditions were found to be methanol concentration of 80%, extraction temperature of 80 °C, and extraction time of 5 min. Different antioxidant assays (i.e., total antioxidant capacity (TAC) and total phenolic content (TPC)) were utilized to evaluate the antioxidant capacity of the methanolic extracts of Terfezia boudieri Chatin, Boletus edulis, and Lactarius volemus. The reactive species scavenging activities of these extracts were also investigated in vitro. High contents of phenolic and flavonoid compounds may be the major contributors to the observed high antioxidant activities of these extracts. B. edulis showed the higher TAC and TPC; highest inhibitory effect on DPPH and on other studied reactive oxygen species (ROS). MAE showed obvious advantages of high extraction efficiency with lower solvent consumption in terms of high antioxidant capacity/activity of extracts achieved within the shortest time.

  5. Thermal analysis on the process of microwave-assisted biodiesel production.

    Science.gov (United States)

    Wu, Li; Zhu, Huacheng; Huang, Kama

    2013-04-01

    The aim of this work was firstly to do a precise thermal analysis of microwave assisted production of biodiesel. In this paper, the effective permittivity of biodiesel synthesis was updated with two methods: a traditional method and a bivariate function of temperature and concentration of one component, then the thermal analysis of the reaction process were accomplished with multi-physics calculation. The results show that there exists large distinction in temperature between these two simulation results calculated by the two methods. The two hot spots locate in the opposite side and their temperature's difference is up to 9°C when the reaction is just carried out for 18s. But the temperature risings and distributions calculated by the new method are closer to the measured results. The thermal analysis based on the new method will be helpful for the industrial design of biodiesel production.

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

    Directory of Open Access Journals (Sweden)

    Silvia Tabasso

    2016-03-01

    Full Text Available 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. Microwave-Assisted γ-Valerolactone Production for Biomass Lignin Extraction: A Cascade Protocol.

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

  9. Photonic-assisted microwave frequency measurement system based on a silicon ORR

    Science.gov (United States)

    Jiang, Jianfei; Shao, Haifeng; Li, Xia; Li, Yan; Dai, Tingge; Wang, Gencheng; Yang, Jianyi; Jiang, Xiaoqing; Yu, Hui

    2017-01-01

    A photonic-assisted instantaneous microwave frequency measurement (IFM) system is demonstrated with add-drop optical ring resonators (ORRs) on silicon-on-insulator (SOI) platform. By launching a double-sideband suppressed carrier modulated optical signal into the ring, a monotonous amplitude comparison function (ACF) irrespective of the amplitudes of both optical and RF signals is established to translate the RF frequency to the power ratio between the through and drop ports of the ring. Two experiments have been set up with two rings which have different Q values. Two 25 μm radius ORRs with Q values of 3974 and 25833 are used to offer different measurement ranges and accuracies. In the experiments the ORR with low Q value has a large measurement range of 0.5-35 GHz, and the other one with high Q value exhibits a high accuracy of 0.1 GHz in the frequency range of 0.1-5 GHz.

  10. Ultrasound-assisted microwave preparation of Ag-doped CdS nanoparticles.

    Science.gov (United States)

    Ma, Jun; Tai, Guo'an; Guo, Wanlin

    2010-03-01

    Ag-doped CdS nanoparticles were synthesized by an ultrasound-assisted microwave synthesis method. The X-ray diffraction patterns reveal a structural evolution from cubic to hexagonal with increasing molar ratios of Ag(+)/Cd(2+) from 0% to 5%. It shows that the Ag-doped hexagonal CdS nanoparticles are polycrystal. The X-ray photoelectron spectroscopy of the CdS nanoparticles doping with 5% Ag(+) shows that the doped Ag in CdS is metallic. Simultaneously, the characteristic Raman peaks of the CdS nanoparticles enhance with increasing Ag(+) concentrations. The photocatalytic activity of different Ag-doped samples show a reasonable change due to different ratios of Ag which doped into CdS. Copyright 2009 Elsevier B.V. All rights reserved.

  11. Microwave-assisted hydrothermal synthesis and gas sensitivity of nanostructured SnO2

    Institute of Scientific and Technical Information of China (English)

    Liying Man; Jun Zhang; Jieqiang wang; Hongyan Xu; Bingqiang Cao

    2013-01-01

    Precursors for nanostructured SnO2 were synthesized via a microwave-assisted hydrothermal method under different conditions,using SnCl2·2H2O,urea and citric acid as reactants.After calcination of the precursors at 700 ℃ for 2 h.nanostructured SnO2 with different morphologies were obtained,and were then characterized using X-ray powder diffraction (XRD),and field-emission scanning electron microscopy (FESEM).The results show that synthesis temperature and time play an important role in the formation of the 3D hierarchical morphology of the nanostructured SnO2.Gas sensing experiments demonstrate that the synthesized SnO2 materials,especially those with a 3D network structure,exhibit superb sensitivity to alcohol vapors at 240 ℃.

  12. Microwave assisted synthesis of zinc stannate nanocubes for dye sensitized solar cell application

    Science.gov (United States)

    Jayabal, P.; Sasirekha, V.; Mayandi, J.; Ramakrishnan, V.

    2014-11-01

    The ternary complex oxide Zn2SnO4 (ZS) has become more essential because of its photonic energy conversion, tremendous stability and higher electron mobility compared to the binary counterparts. The ZS nanocubes were prepared by simple microwave assisted route. The cubic spinel structured ZS was confirmed by X-ray diffraction (XRD) and micro-Raman techniques. Scanning electron micrograph revealed the formation of nanocubes with size of ∼90 nm. The Dye Sensitized Solar Cells (DSSCs) were fabricated using the synthesized ZS as photoanode and low cost organic dyes such as Rose Bengal (RB), Eosin Yellow (EY) and Fluorescein sodium salt (FY) as sensitizers to study their light conversion efficiencies. The DSSCs exhibited power conversion efficiency (PCE) of 0.64%, 0.05% and 0.02% for RB, EY and FY sensitized films, respectively.

  13. Microwave assisted synthesis and solid-state characterization of lithocholyl amides of isomeric aminopyridines.

    Science.gov (United States)

    Ahonen, Kari V; Lahtinen, Manu K; Valkonen, Arto M; Dracínský, Martin; Kolehmainen, Erkki T

    2011-02-01

    Microwave (MW) assisted synthesis and solid state structural characterizations of novel lithocholyl amides of 2-, 3-, and 4-aminopyridine are reported. It is shown that the MW technique is a proper method in the preparation of N-lithocholyl amides of isomeric aminopyridines. It offers many advantages compared to conventional heating. The molecular and crystal structures as well as the polymorphic and hydrated forms of prepared conjugates with their thermodynamic stabilities have been characterized by means of high resolution liquid- and solid-state NMR spectroscopy, single crystal and powder X-ray diffraction, and thermogravimetric analysis. Owing to the many biological functions of bile acids and amino substituted nitrogen heterocycles, knowledge of the crystal packing of these novel conjugates may have relevance for potential pharmaceutical applications.

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

    Science.gov (United States)

    Sari, Fitri Nur Indah; Ting, Jyh-Ming

    2015-11-01

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

  15. Microwave plasma assisted chemical vapor deposition of ultra-nanocrystalline diamond films

    Science.gov (United States)

    Huang, Wen-Shin

    Microwave plasma assisted ultra-nanocrystalline diamond film deposition was investigated using hydrogen deficient, carbon containing argon plasma chemistries with MSU-developed microwave plasma reactors. Ultra-nanocrystalline diamond film deposition on mechanically scratched silicon wafers was experimentally explored over the following input variables: (1) pressure: 60--240Torr, (2) total gas flow rate: 101--642 sccm, (3) input microwave power 732--1518W, (4) substrate temperature: 500°C--770°C, (5) deposition time: 2--48 hours, and (6) N2 impurities 5--2500 ppm. H2 concentrations were less than 9%, while CH 4 concentration was 0.17--1.85%. It was desired to grow films uniformly over 3″ diameter substrates and to minimize the grain size. Large, uniform, intense, and greenish-white discharges were sustained in contact with three inch silicon substrates over a 60--240 Torr pressure regime. At a given operating pressure, film uniformity was controlled by adjusting substrate holder geometry, substrate position, input microwave power, gas chemistries, and total gas flow rates. Film ultra-nanocrystallinity and smoothness required high purity deposition conditions. Uniform ultra-nanocrystalline films were synthesized in low leak-rate system with crystal sizes ranging from 3--30 nm. Films with 11--50 nm RMS roughness and respective thickness values of 1--23 mum were synthesized over 3″ wafers under a wide range of different deposition conditions. Film RMS roughness 7 nm was synthesized with thickness of 430 nm. Film uniformities of almost 100% were achieved over three inch silicon wafers. UV Raman and XRD characterization results indicated the presence of diamond in the synthesized films. Optical Emission Spectroscopy measurements showed that the discharge gas temperature was in excess of 2000 K. The synthesized films are uniformly smooth and the as grown ultra-nanocrystalline diamond can be used for a high frequency SAW device substrate material. IR measurements

  16. Mg-doped hydroxyapatite nanoplates for biomedical applications: A surfactant assisted microwave synthesis and spectroscopic investigations

    Energy Technology Data Exchange (ETDEWEB)

    Mishra, Vijay Kumar [Department of Physics, Faculty of Science, Banaras Hindu University, Varanasi 221005 (India); Bhattacharjee, Birendra Nath; Parkash, Om [Department of Ceramic Engineering, Indian Institute of Technology, Banaras Hindu University, Varanasi 221005 (India); Kumar, Devendra, E-mail: devendra.cer@iitbhu.ac.in [Department of Ceramic Engineering, Indian Institute of Technology, Banaras Hindu University, Varanasi 221005 (India); Rai, Shyam Bahadur, E-mail: sbrai49@yahoo.co.in [Department of Physics, Faculty of Science, Banaras Hindu University, Varanasi 221005 (India)

    2014-11-25

    Highlights: • Microwave irradiation technique: employed for the synthesis of Mg-HAp nanoplates. • Surfactant (EDTA) assisted synthesis of Mg-HAp. • FT-IR and Raman analysis of functional groups of Mg-HAp. - Abstract: Nanoplates of Mg doped hydroxyapatite (Mg-HAp) were derived successfully and rapidly via microwave irradiation technique. Hydroxyapatite (HAp) is the hard tissues and main inorganic component in mammals. Different nanostructures of HAp exist in different parts of human bone but nanorods are very common due to its intrinsic nature to grow in rode-like structure under physiological as well as under applied ambient conditions in laboratory. On the addition of Mg at very low level (0.06 mol%) in pure HAp results the formation of 2-D plate-like nanostructures rather than rod-like which is the matter of interest. In this attempt our efforts have been focused on the study of effect of Mg incorporation on structural and spectroscopic properties of HAp prepared via microwave irradiation technique. This technique is preferred due to several advantages viz. very fast as well as homogeneous heating, time/energy saving and eco-friendliness. The calcium nitrate tetrahydrate (Ca(NO{sub 3}){sub 2}⋅4H{sub 2}O)) as a source of calcium, magnesium nitrate hexahydrate (Mg(NO{sub 3}){sub 2}⋅6H{sub 2}O) as a source of magnesium, disodium hydrogen phosphate dihydrate (NaH{sub 2}PO{sub 4}⋅2H{sub 2}O) as a source of phosphorous and sodium ethylene diamine tetra acetate (NaEDTA) as a surfactant were used as starting reagents. Sodium hydroxide (NaOH) pellets were employed to adjust the pH value of final solution. The solution of fixed pH value was kept into the microwave oven generating waves of frequency 2.45 GHz (water absorption frequency) and power 750 W for 8 min. The precipitate thus obtained was washed, centrifuged and then dried at 100 °C for 2 h. Dried powder was then calcined at 700 °C for 2 h. The bright white powder thus obtained was characterized

  17. Advanced retorting, microwave assisted thermal sterilization (MATS), and pressure assisted thermal sterilization (PATS) to process meat products.

    Science.gov (United States)

    Barbosa-Cánovas, Gustavo V; Medina-Meza, Ilce; Candoğan, Kezban; Bermúdez-Aguirre, Daniela

    2014-11-01

    Conventional thermal processes have been very reliable in offering safe sterilized meat products, but some of those products are of questionable overall quality. Flavor, aroma, and texture, among other attributes, are significantly affected during such processes. To improve those quality attributes, alternative approaches to sterilizing meat and meat products have been explored in the last few years. Most of the new strategies for sterilizing meat products rely on using thermal approaches, but in a more efficient way than in conventional methods. Some of these emerging technologies have proven to be reliable and have been formally approved by regulatory agencies such as the FDA. Additional work needs to be done in order for these technologies to be fully adopted by the food industry and to optimize their use. Some of these emerging technologies for sterilizing meat include pressure assisted thermal sterilization (PATS), microwaves, and advanced retorting. This review deals with fundamental and applied aspects of these new and very promising approaches to sterilization of meat products. Copyright © 2014 Elsevier Ltd. All rights reserved.

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Huan, E-mail: Huan.Zhou@rockets.utoledo.edu [Department of Mechanical, Industrial and Manufacturing Engineering, The University of Toledo, Toledo, OH 43606 (United States); Agarwal, Anand K.; Goel, Vijay K. [Department of Bioengineering, The University of Toledo, Toledo, OH 43606 (United States); Bhaduri, Sarit B. [Department of Mechanical, Industrial and Manufacturing Engineering, The University of Toledo, Toledo, OH 43606 (United States); Division of Dentistry, The University of Toledo, Toledo, OH 43606 (United States)

    2013-10-15

    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. - Highlights: • A microwave assisted system for bone cement manufacturing • A solution to exothermicity problem of acid–base reaction based bone cement

  20. Microwave-assisted synthesis and characterization of bimetallic PtRu alloy nanoparticles supported on carbon nanotubes

    Energy Technology Data Exchange (ETDEWEB)

    Rahsepar, Mansour, E-mail: rahsepar@shirazu.ac.ir [Department of Materials Science and Engineering, School of Engineering, Shiraz University, Zand Boulevard, Shiraz, 7134851154 (Iran, Islamic Republic of); Kim, Hasuck, E-mail: hasuckim@snu.ac.kr [Department of Chemistry, Seoul National University, 599 Gwanak-ro, Gwanak-gu, Seoul, 151-747 (Korea, Republic of); Department of Energy Systems Engineering, Daegu Gyeongbuk Institute of Science & Technology, Daegu, 711-873 (Korea, Republic of)

    2015-11-15

    Multiwalled carbon nanotube (MWCNT) supported PtRu nanoparticles were synthesized by using a microwave-assisted improved impregnation technique. X-ray diffraction, transmission electron microscopy and X-ray photo electron spectroscopy were used to characterize the prepared PtRu/MWCNT nanoparticles. The PtRu nanoparticles with a satisfactory dispersion were formed on the external surface of MWCNTs. The CO stripping experiment was performed to evaluate the poisoning resistance of the prepared PtRu/MWCNT nanoparticles. Results of electrochemical measurements indicate that the prepared PtRu/MWCNTs shows an enhanced performance toward CO poisoning. The results of characterization revealed that microwave-assisted improved impregnation technique have a high yield of alloy phase formation and could be effectively used as a simple, quick and efficient technique for preparation of bimetallic PtRu/MWCNT nanoparticles. - Highlights: • Highly dispersed PtRu/MWCNTs were formed without use of any stabilizing agent. • Microwave irradiation enhances the uniform dispersion of the PtRu nanoparticles. • Microwave-assisted improved impregnation have a high yield of alloy phase formation. • The prepared PtRu/MWCNTs shows an enhanced performance toward CO poisoning.

  1. Preparation of novel biodegradable pHEMA hydrogel for a tissue engineering scaffold by microwave-assisted polymerization

    Institute of Scientific and Technical Information of China (English)

    Li Zhang; Gen-Jian Zheng; Ya-Tong Guo; Lan Zhou; Jie Du; Hong He

    2014-01-01

    Objective:To prepare a novel biodegradable poly(2-hydroxyethylmethacrilate)(pHEMA) hydrogel as tissue engineering scaffold.Methods:The pHEMA hydrogel was synthesized by microwave-assisted polymerization using2-hydroxyethyl methacrylate(HEMA) as the raw material, potassium persulfate as the initiator, andPCLX as the cross-linking additive.The hydrogels was characterized withFTIR andNMR spectroscopy.The physical and chemical properties of the prepared hydrogel were evaluated, and its degradation performance was tested.The cytotoxicity of the optimum composite hydrogel was measured by anMTT assay to confirm the feasibility of its use in tissue engineering.Results:The optimum conditions under which the hydrogel was prepared by microwave-assisted polymerization are as follows:1.5 g cross-linking additive,0.3 g initiator, reaction temperature of80℃, and microwave power of800W.Degradation studies showed good degradation profiles with75% in17 days.Additionally, the hydrogels did not elicit any cytotoxic response inin vitro cytotoxic assays.Conclusion:A biodegradable pHEMA hydrogel was successfully prepared by microwave-assisted polymerization, as confirmed from FTIR andNMR results.The hydrogel shows promising applications in tissue engineering, and its healing ability and biocompatibility will be evaluated in detail in the future.

  2. Antioxidative Peptides Derived from Enzyme Hydrolysis of Bone Collagen after Microwave Assisted Acid Pre-Treatment and Nitrogen Protection

    Directory of Open Access Journals (Sweden)

    Jin Sun

    2010-11-01

    Full Text Available 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.

  3. Covalent immobilization of Candida antarctica lipase B on nanopolystyrene and its application to microwave-assisted esterification

    Institute of Scientific and Technical Information of China (English)

    Attaullah Bukhari; Ani Idris; Madiha Atta; Teo Chee Loong

    2014-01-01

    Nanopolystyrene was used as a solid support for the covalent immobilization of Candida antarctica lipase B (CalB) using the photoreactive reagent 1-fluoro-2-nitro-4-azido benzene (FNAB) as a cou-pling reagent. The obtained derivative was then used as a biocatalyst in a microwave assisted ester-ification experiment. Factors such as contact time, pH, and enzyme concentration were investigated during immobilization. The hydrolytic activity, thermal, and operational stability of immobi-lized-CalB were determined. The maximum immobilized yield (218 µg/mg support) obtained at pH 6.8 exhibited optimum hydrolytic activity (4.42 × 103 mU p-nitrophenol/min). The thermal stability of CalB improved significantly when it was immobilized at pH 10, however, the immobilized yield was very low (93.6 µg/mg support). The immobilized-CalB prepared at pH 6.8 and pH 10 retained 50%of its initial activity after incubation periods of 14 and 16 h, respectively, at 60 °C. The opera-tional stability was investigated for the microwave assisted esterification of oleic acid with metha-nol. Immobilized-CalB retained 50% of its initial activity after 15 batch cycles in the micro-wave-assisted esterification. The esterification time was notably reduced under microwave irradia-tion. The combined use of a biocatalyst and microwave heating is thus an alternative total green synthesis process.

  4. Microwave assisted synthesis of polyacrylamide grafted starch (St-g-PAM) and its applicability as flocculant for water treatment.

    Science.gov (United States)

    Mishra, Sumit; Mukul, Ankita; Sen, Gautam; Jha, Usha

    2011-01-01

    Polyacrylamide grafted starch (St-g-PAM) was made by a novel method of synthesis, involving combination of microwave radiation and a chemical free radical initiator (ceric ammonium nitrate) to initiate grafting reaction. This method (microwave assisted synthesis) is quick, highly reliable, reproducible and yields high quality product as compared to the conventional method (which uses a chemical free radical initiator alone to initiate the grafting reaction).The St-g-PAM grades synthesized were characterized by various physicochemical techniques. Further, its application as flocculant for wastewater treatment was investigated.

  5. Optimization of Microwave-Assisted Extraction Conditions for Five Major Bioactive Compounds from Flos Sophorae Immaturus (Cultivars of Sophora japonica L. Using Response Surface Methodology

    Directory of Open Access Journals (Sweden)

    Jin-Liang Liu

    2016-03-01

    Full Text Available Microwave-assisted extraction was applied to extract rutin; quercetin; genistein; kaempferol; and isorhamnetin from Flos Sophorae Immaturus. Six independent variables; namely; solvent type; particle size; extraction frequency; liquid-to-solid ratio; microwave power; and extraction time were examined. Response surface methodology using a central composite design was employed to optimize experimental conditions (liquid-to-solid ratio; microwave power; and extraction time based on the results of single factor tests to extract the five major components in Flos Sophorae Immaturus. Experimental data were fitted to a second-order polynomial equation using multiple regression analysis. Data were also analyzed using appropriate statistical methods. Optimal extraction conditions were as follows: extraction solvent; 100% methanol; particle size; 100 mesh; extraction frequency; 1; liquid-to-solid ratio; 50:1; microwave power; 287 W; and extraction time; 80 s. A rapid and sensitive ultra-high performance liquid chromatography method coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (EIS-Q-TOF MS/MS was developed and validated for the simultaneous determination of rutin; quercetin; genistein; kaempferol; and isorhamnetin in Flos Sophorae Immaturus. Chromatographic separation was accomplished on a Kinetex C18 column (100 mm × 2.1 mm; 2.6 μm at 40 °C within 5 min. The mobile phase consisted of 0.1% aqueous formic acid and acetonitrile (71:29; v/v. Isocratic elution was carried out at a flow rate of 0.35 mL/min. The constituents of Flos Sophorae Immaturus were simultaneously identified by EIS-Q-TOF MS/MS in multiple reaction monitoring mode. During quantitative analysis; all of the calibration curves showed good linear relationships (R2 > 0.999 within the tested ranges; and mean recoveries ranged from 96.0216% to 101.0601%. The precision determined through intra- and inter-day studies showed an RSD% of <2.833%. These

  6. Microwave-assisted synthesis of bismuth oxybromochloride nanoflakes for visible light photodegradation of pollutants

    Energy Technology Data Exchange (ETDEWEB)

    Bijanzad, Keyvan; Tadjarodi, Azadeh; Moghaddasi Khiavi, Mohammad [Research Laboratory of Inorganic Materials Synthesis, Department of Chemistry, Iran University of Science and Technology, Narmak, Tehran 16846-13114 (Iran, Islamic Republic of); Akhavan, Omid, E-mail: oakhavan@sharif.ir [Department of Physics, Sharif University of Technology, P.O. Box 11155-9161, Tehran (Iran, Islamic Republic of); Institute for Nanoscience and Nanotechnology, Sharif University of Technology, P.O. Box 14588-89694, Tehran (Iran, Islamic Republic of)

    2015-10-15

    BiOBr{sub x}Cl{sub 1−x} (0microwave-assisted synthesis method. The X-ray diffraction (XRD) studies confirmed the formation of pure crystalline phase of BiOBr{sub x}Cl{sub 1−x}. The UV–visible diffuse reflectance and photoluminescence (PL) spectroscopies revealed the indirect band gap of ~2.82 eV for the bismuth oxybromochloride nanoflakes. Visible light-assisted photocatalytic studies showed that the degradation efficiency of the as-prepared BiOBr{sub x}Cl{sub 1−x} for (100 mL of 10 mg L{sup −1}) Rhodamine B (RhB), Natural Red 4 (N-Red) dye solutions was 98.14% and for the colorless organic pentachlorophenol (PCP) solution was 91.09% over 150 min. The possible mechanisms involved in the visible light photodegradation of the pollutants by BiOBr{sub x}Cl{sub 1−x} photocatalyst were also discussed.

  7. Optimized microwave-assisted extraction of 6-gingerol from Zingiber officinale Roscoeand evaluation of antioxidant activity in vitro

    Directory of Open Access Journals (Sweden)

    Wei Liu

    2014-06-01

    Full Text Available Background. 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. Material and methods. 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. Results. The optimum extraction conditions were as follows: microwave power 528 W, ratio of liquid to solid 26 mL g1, extraction time 31s 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. Conclusion. 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

  8. Development of microwave-assisted acid hydrolysis of proteins using a commercial microwave reactor and its combination with LC-MS for protein full-sequence analysis.

    Science.gov (United States)

    Chen, Lu; Wang, Nan; Li, Liang

    2014-11-01

    Microwave-assisted acid hydrolysis (MAAH) can be used to degrade a protein non-specifically into many peptides with overlapping sequences which can be identified by mass spectrometry (MS) to produce a sequence map that covers the full sequence of a protein. The success of this method for protein sequence analysis depends on the proper control of the MAAH process, which is currently done using a household microwave oven. However, to meet the regulatory or good laboratory practice (GLP) requirement in a clinical or pharmaceutical laboratory, using a commercial microwave device is often required. In this paper, we report a method of performing MAAH using a CEM Discover single-mode microwave reactor. It is shown that, using an optimized protocol for MAAH, reproducible results comparable to those obtained using a household microwave oven can be generated using the commercial reactor. To illustrate the potential applications of MAAH MS for characterizing clinically relevant proteins, this method was applied, for the first time, to map the amino acid sequences of normal and sickle-cell human hemoglobin as well as bovine hemoglobin. Full sequence coverage was readily achieved from 294 and 266 unique peptides matched to the alpha and beta subunits of normal hemoglobin, respectively, 334 and 265 unique peptides matched to the alpha and beta submit units of sickle-cell hemoglobin, and 377 and 224 unique peptides matched to the alpha and beta subunits of bovine hemoglobin. This method opens the possibility for any laboratory to use a commercial laboratory equipment to perform MAAH MS for protein full-sequence analysis.

  9. Microwave assisted transformation of N,N-diphenylamine as precursors of organic light emitting diodes (OLED)

    Energy Technology Data Exchange (ETDEWEB)

    Jefri,; Wahyuningrum, Deana, E-mail: deana@chem.itb.ac.id [Organic Chemistry Research Division, Department of Chemistry, Faculty of Mathematics and Natural Sciences, Institut Teknologi Bandung, Jalan Ganesha 10, Bandung 40132 (Indonesia)

    2015-09-30

    In this research, study on the transformation of N,N-diphenylamine (DPA) using iodine (I2) utilizing solid state Microwave Assisted Organic Synthesis (MAOS) method has been carried out. The reaction was performed by variations of three parameters namely the mole of reagents, the amount and type of solid support (alumina/Al2O3), and the reaction conditions. Experimental results showed that neutral-alumina was a better solid support than basic-alumina. The optimum temperature for the reaction was approximately at 125-133 °C with reaction time of 15 minutes and microwave reactor power at 500-600 W. The separation of the yellowish green product solution with preparative Thin Layer Chromatography (TLC) method using n-hexane:ethyl acetate = 4:1 (v/v) as eluent yielded two fractions (I and II) and both fractions can undergo fluorescence under 365 nm UV light. Based on the LC chromatogram with methanol:water = 95:5 (v/v) as eluent and its corresponding mass spectra (ESI+), fraction I contained three compounds, which were tetracarbazole A, triphenylamine, and impurities in the form of plasticizer such as bis(2-ethylhexyl) phthalate. Fraction II also contained three compounds, which were tetracarbazole C, tetraphenylhydrazine, and plasticizer such as bis(2-ethylhexyl) phthalate. Both FT-IR (KBr disks) and NMR (500 MHz, CDCl{sub 3}) spectra of fraction I and II confirmed the aromatic amine groups in those compounds. The observed fluorescence colors of fraction I and II were violet and violet-blue, respectively. Based on their structures and fluorescence characters, the compounds in fraction I and II have the potential to be used as Organic Light Emitting Diode (OLED) compound precursors.

  10. Bit patterned media with composite structure for microwave assisted magnetic recording

    Science.gov (United States)

    Eibagi, Nasim

    Patterned magnetic nano-structures are under extensive research due to their interesting emergent physics and promising applications in high-density magnetic data storage, through magnetic logic to bio-magnetic functionality. Bit-patterned media is an example of such structures which is a leading candidate to reach magnetic densities which cannot be achieved by conventional magnetic media. Patterned arrays of complex heterostructures such as exchange-coupled composites are studied in this thesis as a potential for next generation of magnetic recording media. Exchange-coupled composites have shown new functionality and performance advantages in magnetic recording and bit patterned media provide unique capability to implement such architectures. Due to unique resonant properties of such structures, their possible application in spin transfer torque memory and microwave assisted switching is also studied. This dissertation is divided into seven chapters. The first chapter covers the history of magnetic recording, the need to increase magnetic storage density, and the challenges in the field. The second chapter introduces basic concepts of magnetism. The third chapter explains the fabrication methods for thin films and various lithographic techniques that were used to pattern the devices under study for this thesis. The fourth chapter introduces the exchanged coupled system with the structure of [Co/Pd] / Fe / [Co/Pd], where the thickness of Fe is varied, and presents the magnetic properties of such structures using conventional magnetometers. The fifth chapter goes beyond what is learned in the fourth chapter and utilizes polarized neutron reflectometry to study the vertical exchange coupling and reversal mechanism in patterned structures with such structure. The sixth chapter explores the dynamic properties of the patterned samples, and their reversal mechanism under microwave field. The final chapter summarizes the results and describes the prospects for future

  11. Characterization and antibacterial properties of stable silver substituted hydroxyapatite nanoparticles synthesized through surfactant assisted microwave process

    Energy Technology Data Exchange (ETDEWEB)

    Iqbal, Nida [Medical Implant Technology Group (MEDITEG), Faculty of Bioscience and Medical Engineering, Universiti Teknologi Malaysia, 81310 Skudai, Johor Darul Takzim (Malaysia); Abdul Kadir, Mohammed Rafiq, E-mail: rafiq@biomedical.utm.my [Medical Implant Technology Group (MEDITEG), Faculty of Bioscience and Medical Engineering, Universiti Teknologi Malaysia, 81310 Skudai, Johor Darul Takzim (Malaysia); Nik Malek, Nik Ahmad Nazim [Faculty of Bioscience and Medical Engineering (FBME), Universiti Teknologi Malaysia, 81310 Skudai, Johor Darul Takzim (Malaysia); Mahmood, Nasrul Humaimi Bin [Medical Implant Technology Group (MEDITEG), Faculty of Bioscience and Medical Engineering, Universiti Teknologi Malaysia, 81310 Skudai, Johor Darul Takzim (Malaysia); Murali, Malliga Raman; Kamarul, T. [Tissue Engineering Group, NOCERAL, Department of Orthopaedic Surgery, Faculty of Medicine, University of Malaya, 50603 Kuala Lumpur (Malaysia)

    2013-09-01

    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 for 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.

  12. Microwave assisted transformation of N,N-diphenylamine as precursors of organic light emitting diodes (OLED)

    Science.gov (United States)

    Jefri, Wahyuningrum, Deana

    2015-09-01

    In this research, study on the transformation of N,N-diphenylamine (DPA) using iodine (I2) utilizing solid state Microwave Assisted Organic Synthesis (MAOS) method has been carried out. The reaction was performed by variations of three parameters namely the mole of reagents, the amount and type of solid support (alumina/Al2O3), and the reaction conditions. Experimental results showed that neutral-alumina was a better solid support than basic-alumina. The optimum temperature for the reaction was approximately at 125-133 °C with reaction time of 15 minutes and microwave reactor power at 500-600 W. The separation of the yellowish green product solution with preparative Thin Layer Chromatography (TLC) method using n-hexane:ethyl acetate = 4:1 (v/v) as eluent yielded two fractions (I and II) and both fractions can undergo fluorescence under 365 nm UV light. Based on the LC chromatogram with methanol:water = 95:5 (v/v) as eluent and its corresponding mass spectra (ESI+), fraction I contained three compounds, which were tetracarbazole A, triphenylamine, and impurities in the form of plasticizer such as bis(2-ethylhexyl) phthalate. Fraction II also contained three compounds, which were tetracarbazole C, tetraphenylhydrazine, and plasticizer such as bis(2-ethylhexyl) phthalate. Both FT-IR (KBr disks) and NMR (500 MHz, CDCl3) spectra of fraction I and II confirmed the aromatic amine groups in those compounds. The observed fluorescence colors of fraction I and II were violet and violet-blue, respectively. Based on their structures and fluorescence characters, the compounds in fraction I and II have the potential to be used as Organic Light Emitting Diode (OLED) compound precursors.

  13. Thrust Stand Measurements of the Microwave Assisted Discharge Inductive Plasma Accelerator

    Science.gov (United States)

    Hallock, Ashley K.; Polzin, Kurt A.; Emsellem, Gregory D.

    2011-01-01

    Pulsed inductive plasma thrusters [1-3] are spacecraft propulsion devices in which electrical energy is capacitively stored and then discharged through an inductive coil. This type of pulsed thruster is electrodeless, with a time-varying current in the coil interacting with a plasma covering the face of the coil to induce a plasma current. Propellant is accelerated and expelled at a high exhaust velocity (O(10-100 km/s)) by the Lorentz body force arising from the interaction of the magnetic field and the induced plasma current. While this class of thruster mitigates the life-limiting issues associated with electrode erosion, pulsed inductive plasma thrusters require high pulse energies to inductively ionize propellant. The Microwave Assisted Dis- charge Inductive Plasma Accelerator (MAD-IPA), shown in Fig. 1, is a pulsed inductive plasma thruster that addressees this issue by partially ionizing propellant inside a conical inductive coil before the main current pulse via an electron cyclotron resonance (ECR) discharge. The ECR plasma is produced using microwaves and a static magnetic field from a set of permanent magnets arranged to create a thin resonance region along the inner surface of the coil, restricting plasma formation, and in turn current sheet formation, to a region where the magnetic coupling between the plasma and the theta-pinch coil is high. The use of a conical theta-pinch coil also serves to provide neutral propellant containment and plasma plume focusing that is improved relative to the more common planar geometry of the Pulsed Inductive Thruster (PIT) [1, 2]. In this paper, we describe thrust stand measurements performed to characterize the performance (specific impulse, thrust efficiency) of the MAD-IPA thruster. Impulse data are obtained at various pulse energies, mass flow rates and inductive coil geometries. Dependencies on these experimental parameters are discussed in the context of the current sheet formation and electromagnetic plasma

  14. Comparison of microwave-assisted hydrodistillation withthe traditional hydrodistillation method in the extractionof essential oils from Thymus vulgaris L.

    Science.gov (United States)

    Golmakani, Mohammad-Taghi; Rezaei, Karamatollah

    2008-08-15

    Microwave-assisted hydrodistillation (MAHD) is an advanced hydrodistillation (HD) technique utilizing a microwave oven in the extraction process. MAHD of essential oils from the aerial parts (tops) of Thymus vulgaris L. (common thyme) was studied and the results were compared with those of the conventional HD in terms of extraction time, extraction yield/efficiency, chemical composition, quality of the essential oils and cost of the operation. MAHD was superior in terms of saving energy and extraction time (75min, compared to 4h in HD). Scanning electron microscopy (SEM) of thyme leaves undergone HD and MAHD provided evidences as to a sudden rupture of essential oil glands with MAHD. Gas chromatography-mass spectrometry analysis of the extracted essential oils indicated that the use of microwave irradiation did not adversely influence the composition of the essential oils. MAHD was found to be a green technology. Copyright © 2008 Elsevier Ltd. All rights reserved.

  15. Synthesis of Nano Crystalline MgAl2O4Spinel Powder by Microwave Assisted Combustion%Synthesis of Nano Crystalline MgAl2O4 Spinel Powder by Microwave Assisted Combustion

    Institute of Scientific and Technical Information of China (English)

    Leila Torkian; Mostafa M Amini; Zohreh Bahrami

    2011-01-01

    Stoichiometric MgAl2O4 spinel nanoparticles were synthesized by microwave assisted combustion reaction from aluminium nitrate nanohydrate (Al(NO3)3.9H2O) and Sol-Gel prepared magnesium hydroxide (Mg(OH)2) in the presence of urea ((NH2)2CO) as a fuel, in about 20 min of irradiation. X-ray diffraction (XRD) studies reveal that microwave assisted combustion synthesis route yields single-phase spinel nanoparticles with larger crystalline size (around 75 nm) than other conventional heating methods. Scanning electronic microscope (SEM) images show nanoparticles with spherical shape and homogenous morphology. The surface area measurements (SBET) show crystals with 2.11 m2/g and 0.0033 mL/g pore volume.

  16. Microwave Assisted Bioethanol Production from Sago Starch by Co-Culturing of Ragi Tapai and Saccharomyces Cerevisiae

    Directory of Open Access Journals (Sweden)

    N. Saifuddin

    2011-01-01

    Full Text Available Problem statement: Environmental issues such as global warming and recent events throughout the world, including the shortage of petroleum crude oil, the sharp increase in the cost of oil and the political instability of some crude oil producing countries, have demonstrated the vulnerability of the present sources for liquid fuel. These situations have created great demand for ethanol from fermentation process as green fuel. A main challenge in producing the ethanol is the production cost. A rapid and economical single step fermentation process for reliable production of bioethanol was studied by co-culturing commercialized ragi tapai with Saccharomyces cerevisae using raw sago starch. Approach: Enzymatic hydrolysis of sago starch by various amylolytic enzymes was investigated to reveal the potential coupling mechanism of Microwave Irradiation-Enzyme Coupling Catalysis (MIECC. Results: It was shown that enzymatic hydrolysis of starch using typical enzymes may successfully be carried out at microwave condition. The MIECC resulted in increasing initial reaction rate by about 2 times. The results testify on specific activation of enzymes by microwaves and prove the existence of non-thermal effect in microwave assisted reactions. Low power microwave irradiation (80W does not increase the temperature beyond 40°C and hence denaturation of the enzyme is avoided. The maximum ethanol fermentation efficiency was achieved (97.7% of the theoretical value using 100 g L-1 sago starch concentration. The microwave assisted process improved the yield of ethanol by 45.5% compared to the non-microwave process. Among the other advantages of co-culturing of ragi tapai with S. cerevisiae is the enhancement of ethanol production and prevention of the inhibitory effect of reducing sugars on amylolytic activity and the reaction could be completed within 32±1 h. Conclusion: The present study have demonstrated the ability of using cheaply and readily ragi tapai for

  17. Total synthesis of human urotension-Ⅱ by microwave-assisted solid phase method

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Human urotension-Ⅱ was synthesized efficiently on Wang resin under microwave irradiation using Fmoc/tBu orthogonal protection strategy. Disulphide bridge was formed on solid phase with the irradiation of microwave, then the whole peptide was cleaved from the resin. The purity of crude peptide cyclized under microwave irradiation was higher than that under room temperature.

  18. Stabilized γ-BIMNVOX solid electrolyte: Ethylene glycol–citrate sol–gel synthesis, microwave-assisted calcination, and structural and electrical characterization

    Energy Technology Data Exchange (ETDEWEB)

    Al-Areqi, Niyazi A.S., E-mail: niyazi.alareqi@gmail.com [Department of Chemistry, Faculty of Applied Science, Taiz University, Taiz, Republic of Yemen (Yemen); Beg, Saba [Department of Chemistry, Aligarh Muslim University, Aligarh 202002 (India); Al-Alas, Ahlam [Department of Chemistry, Faculty of Applied Science, Taiz University, Taiz, Republic of Yemen (Yemen); Hafeez, Shehla [Department of Chemistry, Aligarh Muslim University, Aligarh 202002 (India)

    2013-12-25

    Highlights: •γ-BIMNVOX was synthesized by ethylene glycol–citrate sol–gel route. •γ-BIMNVOX crystallizes by 25-min microwave-assisted calcination. •Smaller particle sizes for microwave calcined BIMNVOX samples. •Best oxide-ion performance for microwave calcined BIMNVOX samples. -- Abstract: Samples of γ-BIMNVOX (Bi{sub 2}V{sub 1−x}Mn{sub x}O{sub 5.5−x/2}; 0.13 ⩽ x ⩽ 0.20) system were synthesized by an ethylene glycol–citrate sol–gel route. The resulting xerogels were then calcined by the microwave heating using a modified domestic microwave oven operated at 2.45 GHz. Microwave-assisted calcination samples in comparison with other conventionally calcined samples were characterized in terms of phase crystallization, stabilization and particle size using simultaneous thermogravimetric–differential thermal analysis (TG–DTA), X-ray powder diffraction (XRPD) and scanning electron microscopy (SEM). The AC impedance spectroscopy was employed for electrical characterization. It was found that the microwave-assisted calcination route successfully produces better crystalline stabilized γ-BIMNVOX samples with appreciably small average particle sizes after only 25 min of microwave heating. The electrical properties of microwave calcined γ-BIMNVOX system make it an advanced low-temperature solid electrolyte suitable for use in oxide-ion based electrochemical applications.

  19. Deep Eutectic Solvent-Based Microwave-Assisted Method for Extraction of Hydrophilic and Hydrophobic Components from Radix Salviae miltiorrhizae

    Directory of Open Access Journals (Sweden)

    Jue Chen

    2016-10-01

    Full Text Available Deep eutectic solvents (DESs have attracted significant attention as a promising green media. In this work, twenty-five kinds of benign choline chloride-based DESs with microwave-assisted methods were applied to quickly extract active components from Radix Salviae miltiorrhizae. The extraction factors, including temperature, time, power of microwave, and solid/liquid ratio, were investigated systematically by response surface methodology. The hydrophilic and hydrophobic ingredients were extracted simultaneously under the optimized conditions: 20 vol% of water in choline chloride/1,2-propanediol (1:1, molar ratio as solvent, microwave power of 800 W, temperature at 70 °C, time at 11.11 min, and solid/liquid ratio of 0.007 g·mL−1. The extraction yield was comparable to, or even better than, conventional methods with organic solvents. The microstructure alteration of samples before and after extraction was also investigated. The method validation was tested as the linearity of analytes (r2 > 0.9997 over two orders of magnitude, precision (intra-day relative standard deviation (RSD < 2.49 and inter-day RSD < 2.96, and accuracy (recoveries ranging from 95.04% to 99.93%. The proposed DESs combined with the microwave-assisted method provided a prominent advantage for fast and efficient extraction of active components, and DESs could be extended as solvents to extract and analyze complex environmental and pharmaceutical samples.

  20. Microwave blanching and drying characteristics of Centella asiatica (L.) urban leaves using tray and heat pump-assisted dehumidified drying.

    Science.gov (United States)

    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.

  1. Microwave-assisted chemical reduction routes for direct synthesis of (fct) L1 phase of Fe-Pt.

    Science.gov (United States)

    Acharya, Smita; Singh, Kamal

    2011-01-01

    Microwave-assisted chemical reduction route has been explored for the direct synthesis of fct L1(0) - phase of Fe-Pt nanoparticles in the present work. Effects of microwave power and irradiation time on the growth process are systematically studied. Using this facile and high yield technique we could tune particle size from 7 to 17 nm. Prepared Fe-Pt NPs exhibited ordered face centered tetragonal (fct) L1(0) phase without any post-synthesis treatment. The particle size and magnetic properties of the prepared Fe-Pt were found to be very sensitive to the microwave irradiation power, while influence of exposure time was insignificant. The hysteresis measurements were performed at 300 K to study magnetic properties of the synthesized Fe-Pt as a function of crystallite size. Coercivity and saturation magnetization were observed to be decreasing with diminishing particle size. The microwave-assisted route is found to be a simple technique for direct synthesis of metal alloys and may prove to be a potential tool of high density data storage materials such as Fe-Pt.

  2. Microwave Assisted Synthesis of Some Bioactive 1,8-Naphthyridinyl Heterocycles and Development of New Synthetic Methodologies in Organic Synthesis

    Institute of Scientific and Technical Information of China (English)

    K. Mogilaiah

    2005-01-01

    @@ 1Introduction Organic synthesis is a powerful discipline, which forms the basis for numerous other areas of research in chemistry and chemical biology. Organic chemists and chemical research in general are under great demand to develop environmentally benign technologies for the synthesis of well-defined precursors and target molecules.It is at this juncture that the microwave assisted technique comes into the picture.Microwave assisted organic reactions have blossomed into an important tool with a variety of applications,particularly after the development of Microwave-induced Organic Reaction Enhancement (MORE) chemistry techniques[1-3]. These techniques require open vessels with little or no solvents and are free of the risk of explosion. MORE chemistry reactions are extremely fast, cleaner than conventional reactions and lead to higher atom economy. Because of short time requirement, ease of workability and eco-friendliness, microwaves provide an alternative green approach to environmentally unacceptable procedures using toxic and expensive reagents. Recently, the use of inorganic solid supports as catalysts[4] have been developed for solvent-free reactions resulting in higher selectivity, milder conditions and easy handling. Clay catalyzed organic reactions are gaining importance owing to their inexpensive nature and special catalytic attributes in heterogeneous reactions[5].

  3. Recent Trends in the Microwave-Assisted Synthesis of Metal Oxide Nanoparticles Supported on Carbon Nanotubes and Their Applications

    Directory of Open Access Journals (Sweden)

    Sarah C. Motshekga

    2012-01-01

    Full Text Available The study of coating carbon nanotubes with metal/oxides nanoparticles is now becoming a promising and challenging area of research. To optimize the use of carbon nanotubes in various applications, it is necessary to attach functional groups or other nanostructures to their surface. The combination of the distinctive properties of carbon nanotubes and metal/oxides is expected to be applied in field emission displays, nanoelectronic devices, novel catalysts, and polymer or ceramic reinforcement. The synthesis of these composites is still largely based on conventional techniques, such as wet impregnation followed by chemical reduction of the metal nanoparticle precursors. These techniques based on thermal heating can be time consuming and often lack control of particle size and morphology. Hence, there is interest in microwave technology recently, where using microwaves represents an alternative way of power input into chemical reactions through dielectric heating. This paper covers the synthesis and applications of carbon-nanotube-coated metal/oxides nanoparticles prepared by a microwave-assisted method. The reviewed studies show that the microwave-assisted synthesis of the composites allows processes to be completed within a shorter reaction time with uniform and well-dispersed nanoparticle formation.

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

    Science.gov (United States)

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

    2017-06-01

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

  5. Study on chromatographic fingerprint of sarcandra glabra (Thunb.) by microwave-assisted extraction coupled to HPLC/DAD

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    Microwave-assisted extraction(MAE)was used for extraction of effective components of sarcandra glabra(Thunb.),and then chromatographic fingerprint of sarcandra glabra(Thunb.)was studied by high performance liquid chromatography/diode array detector(HPLC/DAD).The conditions of MAE were optimized by an orthogonal experiment,and then the authentication and validation of the chromatographic fingerprint were conducted.Nine peaks were identified as common peaks in the fingerprint chromatograms,and isofraxidin was...

  6. An efficient, microwave-assisted, one-pot synthesis of novel 5,6,7,8-tetrahydroquinoline-3-carbonitriles

    Directory of Open Access Journals (Sweden)

    VIRESH H. SHAH

    2011-06-01

    Full Text Available An efficient, microwave-assisted synthesis of novel 2-alkoxy-5,6,7,8--tetrahydroquinoline-3-carbonitriles, which have not hitherto been reported, via reactions of cyclohexanone and arylidene malononitriles in the corresponding alcohols in presence of sodium is described. All the newly synthesized compounds were characterized by the IR, 1H-NMR, 13C-NMR and mass spectrescopic techniques and by elemental analyses. The newly synthesized compounds were evaluated for their antibacterial and antifungal activities.

  7. Microwave-assisted modulated synthesis of zirconium-based metal-organic framework (Zr-MOF) for hydrogen storage applications

    Energy Technology Data Exchange (ETDEWEB)

    Ren, Jianwei; Segakweng, Tshiamo; Langmi, Henrietta W.; Musyoka, Nicholas M.; North, Brian C.; Mathe, Mkhulu [Council for Scientific and Industrial Research (CSIR), Pretoria (South Africa). HySA Infrastructure Centre of Competence, Materials Science and Manufacturing; Bessarabov, Dmitri [North-West Univ. (NWU), Potchefstroom (South Africa). HySA Infrastructure Centre of Competence

    2014-05-15

    Zirconium-based metal-organic framework (Zr-MOF) was synthesized using a microwave-assisted modulated method in a short reaction time of 5 min. The Zr-MOF material was highly crystalline with well-defined octahedral shaped crystals, and it exhibited comparable hydrogen storage capacity to Zr-MOF of similar specific surface area synthesized using conventional methods with much longer synthesis time. (orig.)

  8. Ionic liquid-based microwave-assisted extraction of rutin from Chinese medicinal plants.

    Science.gov (United States)

    Zeng, Huan; Wang, Yuzhi; Kong, Jinhuan; Nie, Chan; Yuan, Ya

    2010-12-15

    An ionic liquid-based microwave-assisted extraction (ILMAE) method has been developed for the effective extraction of rutin from Chinese medicinal plants including Saururus chinensis (Lour.) Bail. (S. chinensis) and Flos Sophorae. A series of 1-butyl-3-methylimidazolium ionic liquids with different anions were investigated. The results indicated that the characteristics of anions have remarkable effects on the extraction efficiency of rutin and among the investigated ionic liquids, 1-butyl-3-methylimidazolium bromide ([bmim]Br) aqueous solution was the best. In addition, the ILMAE procedures for the two kinds of medicinal herbs were also optimized by means of a series of single factor experiments and an L(9) (3(4)) orthogonal design. Compared with the optimal ionic liquid-based heating extraction (ILHE), marinated extraction (ILME), ultrasonic-assisted extraction (ILUAE), the optimized approach of ILMAE gained higher extraction efficiency which is 4.879 mg/g in S. chinensis with RSD 1.33% and 171.82 mg/g in Flos Sophorae with RSD 1.47% within the shortest extraction time. Reversed phase high performance liquid chromatography (RP-HPLC) with ultraviolet detection was employed for the analysis of rutin in Chinese medicinal plants. Under the optimum conditions, the average recoveries of rutin from S. chinensis and Flos Sophorae were 101.23% and 99.62% with RSD lower than 3%, respectively. The developed approach is linear at concentrations from 42 to 252 mg L(-1) of rutin solution, with the regression coefficient (r) at 0.99917. Moreover, the extraction mechanism of ILMAE and the microstructures and chemical structures of the two researched samples before and after extraction were also investigated. With the help of LC-MS, it was future demonstrated that the two researched herbs do contain active ingredient of rutin and ionic liquids would not influence the structure of rutin.

  9. Microwave-assisted acid and base hydrolysis of intact proteins containing disulfide bonds for protein sequence analysis by mass spectrometry.

    Science.gov (United States)

    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.

  10. Analysis of parameter and interaction between parameter of the microwave assisted transesterification process of coconut oil using response surface methodology

    Science.gov (United States)

    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.

  11. A rapid fractionation method for heavy metals in soil by continuous-flow sequential extraction assisted by focused microwaves.

    Science.gov (United States)

    Nakazato, Tetsuya; Akasaka, Mikio; Tao, Hiroaki

    2006-11-01

    A microwave-assisted continuous-flow sequential extraction system was developed for rapid fractionation analysis of heavy metals in soil. Insertion of pressure-adjusted air between the extractants provided stable flows of the extractants without mutual mixing and back-pressure influence of a column packed with soil, thereby facilitating reliable continuous-flow extractions. In addition, use of pure water as a pumping solvent removed metal contamination because of direct contact between corrosive extractants and the pump containing metallic materials. Focused microwave irradiation to the soil accelerated the selective extractions of the acid-soluble and reducible fractions of heavy metals in soil in the first and second steps of the sequential extraction conditions, as defined by the Commission of the European Bureau of Reference (BCR). The microwave-assisted continuous-flow extraction provided high correlations in amounts of six heavy metals except Zn in the first step and Cu in the second step extracted from a reference sludge soil, BCR CRM 483, with a conventional batchwise extraction proposed by BCR; continuous-flow extraction assisted by conductive heating provided lower correlations for all the six metals. The proposed method drastically reduced the time required for the sequence extraction to ca. 65 min without losing accuracy and precision of the fractionation analysis of heavy metals in soil, whereas the BCR batchwise method requires ca. 33 h.

  12. Microwave assisted novel MoBi2S5 nanoflowers: Synthesis, characterization, photoelectrochemical performance

    Science.gov (United States)

    Pawar, Nita B.; Mali, Sawanta S.; Kharade, Suvarta D.; Kondalkar, Vijay V.; Ghanwat, Vishvanath B.; Khot, Kishorkumar V.; Patil, Pramod S.; Bhosale, Popatrao N.

    2016-11-01

    In the present article, we have studied the effect of post annealing treatment on microstructural, optical and photoelectrochemical (PEC) properties of MoBi2S5 thin films synthesized by microwave assisted technique. The synthesized thin films are vacuum annealed for 4 h at 473 K temperature. The X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM) and UV-Vis-NIR spectrophotometer techniques were used for characterization of the as deposited and annealed MoBi2S5 thin films. The XRD patterns confirm the synthesized and annealed thin films have nanocrystalline nature with rhombohedral-orthorhombic crystal structure. SEM micrographs indicate that, nanoflowers exhibit sharper end after annealing. The optical absorption study illustrates that the optical band gap energy has been decrease from 2.0 eV to 1.75 eV with annealing. Finally, applicability of synthesized thin films has been checked for PEC property. The J-V curves revealed that synthesized thin film photoanodes are suitable for PEC cell application. As well, used simple, economical method has great potential for synthesis of various thin film materials.

  13. Facile Microwave-Assisted Synthesis of Klockmannite CuSe Nanosheets and Their Exceptional Electrical Properties

    Science.gov (United States)

    Liu, Yong-Qiang; Wang, Feng-Xia; Xiao, Yan; Peng, Hong-Dan; Zhong, Hai-Jian; Liu, Zheng-Hui; Pan, Ge-Bo

    2014-08-01

    Klockmannite copper selenide nanosheets (CuSe NSs) are synthesized by a facile microwave-assisted method and fully characterized. The nanosheets have smooth surface and hexagonal shape. The lateral size is 200-500 nm × 400-800 nm and the thickness is 55 +/- 20 nm. The current-voltage characteristics of CuSe NS films show unique Ohmic and high-conducting behaviors, comparable to the thermally-deposited gold electrode. The high electrical conductivity of CuSe NSs implies their promising applications in printed electronics and nanodevices. Moreover, the local electrical variation is observed, for the first time, within an individual CuSe NS at low bias voltages (0.1 ~ 3 V) by conductive atomic force microscopy (C-AFM). This is ascribed to the quantum size effect of NS and the presence of Schottky barrier. In addition, the influence of the molar ratio of Cu2+/SeO2, reaction temperature, and reaction time on the growth of CuSe NSs is explored. The template effect of oleylamine and the intrinsic crystal nature of CuSe NS are proposed to account for the growth of hexagonal CuSe NSs.

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

    Directory of Open Access Journals (Sweden)

    Guan WW

    2014-10-01

    Full Text Available Weiwei Guan,1,* Wei Gu,2,* Ling Ye,2 Chenyang Guo,1 Su Su,1 Pinxiang Xu,1,3 Ming Xue1,3 1Department of Pharmacology, School of Basic Medical Sciences, Capital Medical University, Beijing, People’s Republic of China; 2Department of Chemical Biology, School of Chemical Biology and Pharmaceutical Sciences, Capital Medical University, Beijing, People’s Republic of China; 3Beijing Laboratory for Biomedical Detection Technology and Instrument, Beijing, People’s Republic of China *These authors contributed equally to this work Abstract: A green, one-step microwave-assisted polyol synthesis was employed to prepare blue luminescent carbon nitride dots (CNDs using folic acid molecules as both carbon and nitrogen sources. The as-prepared CNDs had an average size of around 4.51 nm and could be well dispersed in water. Under excitation at 360 nm, the CNDs exhibited a strong blue luminescence and the quantum yield was estimated to be 18.9%, which is greater than that of other reported CNDs. Moreover, the CNDs showed low cytotoxicity and could efficiently label C6 glioma cells, demonstrating their potential in cell imaging. Keywords: carbon nitride dots (CNDs, folic acid, photoluminescence, cell imaging

  15. Microwave assisted synthesis of ZnO nanoparticles for lighting and dye removal application

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Vijay, E-mail: vijays_phy@rediffmail.com [Department of Physics, University of Free State, P.O. Box 339, Bloemfontein, ZA 9300 (South Africa); Gohain, M. [Department of Chemistry, University of Free State, P.O. Box 339, Bloemfontein, ZA 9300 (South Africa); Som, S.; Kumar, Vinod [Department of Physics, University of Free State, P.O. Box 339, Bloemfontein, ZA 9300 (South Africa); Bezuindenhoudt, B.C.B. [Department of Chemistry, University of Free State, P.O. Box 339, Bloemfontein, ZA 9300 (South Africa); Swart, Hendrik C., E-mail: swarthc@ufs.ac.za [Department of Physics, University of Free State, P.O. Box 339, Bloemfontein, ZA 9300 (South Africa)

    2016-01-01

    In this study, we report on the synthesis of ZnO nanoparticles (NPs) via the microwave-assisted technique. The as-synthesized ZnO nanoparticles were annealed at 500 °C for three hours. The ZnO NPs were characterized by X-ray diffraction (XRD) and scanning electron microscopic techniques. XRD results confirmed the formation of as-synthesized ZnO powder oriented along the (101) direction. The Kubelka–Munk function has been employed to determine the band gap of the ZnO powder. ZnO powder has been studied by photoluminescence (PL) before and after annealing to identify the emission of defects in the visible range. The intensity of the PL emission has decreased after annealing. The synthesized ZnO samples were also studied for methyl orange dye removal from waste water. It has been found that the as-synthesized ZnO shows better adsorption behaviour as compared to the annealed sample.

  16. ZnS nanosheets: Egg albumin and microwave-assisted synthesis and optical properties

    Science.gov (United States)

    Tian, Xiuying; Wen, Jin; Hu, Jilin; Chen, Zhanjun; Wang, Shumei; Peng, Hongxia; Li, Jing

    2016-09-01

    ZnS nanosheets were prepared via egg albumin and microwave-assisted method. The phases, crystalline lattice structures, morphologies, chemical and optical properties were characterized by X-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM), field-emission scanning electron microscope(FE-SEM), selected area electron diffraction (SAED), Fourier transform infrared (FTIR) spectroscopy, ultraviolet-visible (UV-Vis) spectroscopy and fluorescence(FL) spectrometer and growth mechanism of ZnS nanosheets was investigated. The results showed that all samples were pure cubic zinc blende with polycrystalline structure. The width of ZnS nanosheets with a rectangular nanostructure was in the range of 450-750 nm. The chemical interaction existed between egg albumin molecules and ZnS nanoparticles via the amide/carboxylate group. The band gap value calculated was 3.72 eV. The band at around 440 nm was attributed to the sulfur vacancies of the ZnS nanosheets. With increasing volumes of egg albumin, the photoluminescence (PL) intensity of ZnS samples firstly increased and then decreased, attributed to concentration quenching.

  17. Application of ionic liquid-based microwave-assisted extraction of flavonoids from Scutellaria baicalensis Georgi.

    Science.gov (United States)

    Zhang, Qin; Zhao, San-Hu; Chen, Jue; Zhang, Li-Wei

    2015-10-01

    In the present work, a rapid ionic liquid-based microwave-assisted extraction (ILMAE) method was successfully applied to simultaneous extraction of baicalin, wogonoside, baicalein and wogonin from Scutellaria baicalensis Georgi. A series of 1-alkyl-3-methylirnidazolium ionic liquids with different anions and cations were assessed for extraction efficiency, and 1-octyl-3-methylimidazolium bromide was selected as the optimal solvent. In addition, the parameters of ILMAE procedure for the four flavonoids were optimized, and the optimal ILMAE method was validated in the linearity, stability, precision and recovery. Meanwhile, the microstructures of S. baicalensis powders were observed before and after extraction with the help of a scanning electron microscope (SEM) in order to explore the extraction mechanism, and the activity of the crude enzyme solution from S. baicalensis was determined through the hydrolysis of baicalin. Finally, the extraction yields and extraction time of WaterHRE, WaterMAE, ILHRE and Chp were 5.18% (30min), 8.77% (90s), 16.94% (30min) and 18.58% (3h), respectively. The results indicated that compared with the conventional extraction approaches, ILMAE possessed great advantages in extracting flavonoids, such as the highest extraction yield (22.28%), the shortest extraction time (90s), etc.

  18. Photocatalytic perfermance of sandwich-like BiVO4 sheets by microwave assisted synthesis

    Science.gov (United States)

    Liu, Suqin; Tang, Huiling; Zhou, Huan; Dai, Gaopeng; Wang, Wanqiang

    2017-01-01

    Sandwich-like BiVO4 sheets were successfully synthesized in an aqueous solution containing bismuth nitrate, ammonium metavanadate and polyethylene glycol with a molecular weight of 10,000 (PEG-10000) using a facile microwave-assisted method. The as-prepared samples were characterized by scanning electron microscopy, N2 adsorption-desorption, X-ray diffraction, X-ray photoelectron spectroscopy (XPS), and UV-vis diffuse reflectance spectroscopy. The results show that the presence of PEG-10000 plays a critical role in the formation of BiVO4 sheets, and Ostwald ripening is the primary driving force for the formation of sandwich-like structures. The sandwich-like BiVO4 sheets exhibit a high activity for the degradation of methyl orange under visible light irradiation (λ ≥ 420 nm). The enhancement of photocatalytic activity of sandwich-like BiVO4 sheets can be attributed to its large surface area over the irregular BiVO4 particles.

  19. Dissolution of fluoride complexes following microwave-assisted hydrofluoric acid digestion of marine sediments.

    Science.gov (United States)

    Muratli, Jesse M; McManus, James; Mix, Alan; Chase, Zanna

    2012-01-30

    Microwave-assisted, hydrofluoric acid digestion is an increasingly common tool for the preparation of marine sediment samples for analysis by a variety of spectrometric techniques. Here we report that analysis of terrigenous-dominated sediment samples occasionally results in anomalously low values for several elements, including Al, Ba, Ca, Mg, and Sr. Measured concentrations of these elements increased with time between sample preparation and sample analysis, reaching stable values after 8-29 days. This lag is explained by the formation and subsequent dissolution of poorly soluble fluoride phases during digestion. Other elements, such as Fe, Mn, and Ti, showed little or no lag and were quickly measurable at a stable value. Full re-dissolution of the least soluble fluorides, which incorporate Al and Mg, requires up to four weeks at room temperature, and this duration can vary among sedimentary matrices. This waiting time can be reduced to 6 days (or shorter) if the samples are heated to ≈ 60°C for 24h.

  20. Microwave-assisted extraction of polyphenols from Camellia oleifera fruit hull.

    Science.gov (United States)

    Zhang, Liangliang; Wang, Yongmei; Wu, Dongmei; Xu, Man; Chen, Jiahong

    2011-05-27

    The abundant fruit hulls of tea-oil tree (Camellia oleifera) are still underutilized and wastefully discaded to pollute the environment. In order to solve this problem and better utilize the fruit hulls of C. oleifera, a microwave-assisted extraction system was used to extract their polyphenols using water as the extraction solvent. A central composite design (CCD) was used to monitor the effects of three extraction processing parameters--liquid:solid ratio (mL/g), extraction time (min) and extraction temperature (°C)--on the polyphenol yield (%). The results showed that the optimal conditions were liquid:solid ratio of 15.33:1 (mL/g), extraction time of 35 min and extraction temperature of 76 °C. Validation tests indicated that under the optimized conditions the actual yield of polyphenols was 15.05 ± 0.04% with RSD = 0.21% (n = 5), which was in good agreement with the predicted yield. Phenolic compounds in the extracts were analysed by HPLC, and gallic acid was found to be the predominant constituent. The total flavonoid content in the extracts was determined and high total flavonoid content was revealed (140.06 mg/g dry material).

  1. Microwave assisted synthesis of nanocrystalline Fe-phosphates electrode materials and their electrochemical properties.

    Science.gov (United States)

    Kim, D H; Kang, J W; Jung, I O; Im, J S; Kim, E J; Song, S J; Lee, J S; Kim, J

    2008-10-01

    LiFePO4 nanocrystalline particles were synthesized using microwave assisted polyol process within a fast reaction time of 20 minutes without any further heating as a post step. The synthesized LiFePO4 nanocrystalline particles showed mono-dispersed rod and orthorhombic-like shapes with a size of 60 approximately 180 nm. The refined X-ray diffraction pattern of the sample was indexed well to the olivine crystal structure (space group: Pnma) without any impurity phases. The LiFePO4 nanocrystalline particles show a capacity of 161 mAh/g in a voltage range of 2.5-4.2 V with a current density of 0.1 mA/cm2 without any observable capacity fading in extended cycles of 100th. A cyclic voltammetry analysis exhibits distinctly sharp peaks corresponding to the typical LiFePO4/FePO4 redox couples and demonstrates a good reversibility of the sample.

  2. Analysis of Switchable Spin Torque Oscillator for Microwave Assisted Magnetic Recording

    Directory of Open Access Journals (Sweden)

    Mingsheng Zhang

    2015-01-01

    Full Text Available A switchable spin torque oscillator (STO with a negative magnetic anisotropy oscillation layer for microwave assisted magnetic recording is analyzed theoretically and numerically. The equations for finding the STO frequency and oscillation angle are derived from Landau-Lifshitz-Gilbert (LLG equation with the spin torque term in spherical coordinates. The theoretical analysis shows that the STO oscillating frequency remains the same and oscillation direction reverses after the switching of the magnetization of the spin polarization layer under applied alternative magnetic field. Numerical analysis based on the derived equations shows that the oscillation angle increases with the increase of the negative anisotropy energy density (absolute value but decreases with the increase of spin current, the polarization of conduction electrons, the saturation magnetization, and the total applied magnetic field in the z direction. The STO frequency increases with the increase of spin current, the polarization of conduction electrons, and the negative anisotropy energy density (absolute value but decreases with the increase of the saturation magnetization and the total applied magnetic field in the z direction.

  3. Microwave assisted extraction of flavonoids from pomegranate peel and its antioxidant activity

    Directory of Open Access Journals (Sweden)

    Huang Ju

    2017-01-01

    Full Text Available Pomegranate peel, a waste generated from fruit processing industry, which contains maximum amounts of bioactive compounds than the juice, is a potential source of active ingredient such as flavonoids that are known for their antioxidant properties. Microwave-assisted extraction (MAE of flavonoids from pomegranate peel and its antioxidant activity were investigated. Three independent and main variables, including ethanol concentration(%, solvent/solid ratio(mL/g and MAE time(min, which were of significance for the yields of flavonoids were studied. The optimal conditions were determined by the orthogonal design. The maximum extraction yield of 4.260% was achieved at ethanol concentration of 60%, ratio of solvent to material of 40:1 and MAE time of 3min. In vitro antioxidant assays showed that the extract exhibited a strong DPPH radical-scavenging ability with IC50 value of 0.187 mg/mL. Results indicated that MAE was a suitable approach for the extraction of flavonoids from pomegranate peel.

  4. Photocatalytic activity of Eu3+-doped ZnO nanorods synthesized via microwave assisted technique

    Institute of Scientific and Technical Information of China (English)

    P.V. Korake; A.N. Kadam; K.M. Garadkar

    2014-01-01

    The doped ZnO nanorods as a photocatalyst with different Eu contents were prepared by microwave assisted method and they were characterized by means of X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS), UV-Vis spectroscopy, surface area Brunauer-Emmett-Teller (BET), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The average crystallite size and band gap energy of Eu-doped ZnO were varied with the Eu content. The XRD pattern of Eu-doped ZnO indicated hexagonal crystal structure with an average crystallite size of 25 nm. The pres-ence of europium with trivalent state and its doping successfully into the crystal lattice of ZnO matrix were confirmed by XPS tech-nique. The photocatalytic activity of Eu-doped ZnO nanorods was evaluated for methyl orange degradation. The photocatalytic experi-ments showed~91%degradation of methyl orange over 0.2 mol.%Eu doped ZnO sample within 3 h under UV light (365 nm).

  5. Ionic liquids based microwave-assisted extraction of lichen compounds with quantitative spectrophotodensitometry analysis.

    Science.gov (United States)

    Bonny, Sarah; Paquin, Ludovic; Carrié, Daniel; Boustie, Joël; Tomasi, Sophie

    2011-11-30

    Ionic liquids based extraction method has been applied to the effective extraction of norstictic acid, a common depsidone isolated from Pertusaria pseudocorallina, a crustose lichen. Five 1-alkyl-3-methylimidazolium ionic liquids (ILs) differing in composition of alkyl chain and anion were investigated for extraction efficiency. The extraction amount of norstictic acid was determined after recovery on HPTLC with a spectrophotodensitometer. The proposed approaches (IL-MAE and IL-heat extraction (IL-HE)) have been evaluated in comparison with usual solvents such as tetrahydrofuran in heat-reflux extraction and microwave-assisted extraction (MAE). The results indicated that both the characteristics of the alkyl chain and anion influenced the extraction of polyphenolic compounds. The sulfate-based ILs [C(1)mim][MSO(4)] and [C(2)mim][ESO(4)] presented the best extraction efficiency of norstictic acid. The reduction of the extraction times between HE and MAE (2 h-5 min) and a non-negligible ratio of norstictic acid in total extract (28%) supports the suitability of the proposed method. This approach was successfully applied to obtain additional compounds from other crustose lichens (Pertusaria amara and Ochrolechia parella).

  6. Ionic liquids based simultaneous ultrasonic and microwave assisted extraction of phenolic compounds from burdock leaves.

    Science.gov (United States)

    Lou, Zaixiang; Wang, Hongxin; Zhu, Song; Chen, Shangwei; Zhang, Ming; Wang, Zhouping

    2012-02-24

    The ionic liquids based simultaneous ultrasonic and microwave assisted extraction (IL-UMAE) technique was first proposed and applied to isolate compounds. The ionic liquids comprising a range of four anions, five 1-alkyl-3-methylimidazolium derivatives were designed and prepared. The results suggested that varying the anion and cation both had apparent effects on the extraction of phenolics. The results also showed that irradiation power, time and solid-liquid ratio significantly affected the yields. The yields of caffeic acid and quercetin obtained by IL-UMAE were higher than those by regular UMAE. Compared with conventional heat-reflux extraction (HRE), the proposed approach exhibited higher efficiency (8-17% enhanced) and shorter extraction time (from 5h to 30s). The results indicated ILUMAE to be a fast and efficient extraction technique. Moreover, the proposed method was validated by the reproducibility and recovery experiments. The ILUMAE method provided good recoveries (from 96.1% to 105.3%) with RSD lower than 5.2%, which indicated that the proposed method was credible. Based on the designable nature of ionic liquids, and the rapid and highly efficient performance of the proposed approach, ILUMAE provided a new alternative for preparation of various useful substances from solid samples.

  7. Flexible composite via rapid titania coating by microwave-assisted hydrothermal synthesis

    Indian Academy of Sciences (India)

    RICARDO MARQUES E SILVA; ANDERSON THESING; VINICIUS GONÇALVES DEON; ALICE GONÇALVES OSÓRIO; BRUNO DA SILVEIRA NOREMBERG; NATÁLIA HADLER MARINS; MARCELO ORNAGHI ORLANDI; FABIANA VILLELA DA MOTTA; RUBENS MARIBONDO DO NASCIMENTO; NEFTALI LENIN VILLARREAL CARREÑO

    2017-06-01

    The aim of this work was to prepare a flexible nanocomposite from ultra-fine titanium oxide (TiO$_2$) growth on carbon fibre via microwave-assisted hydrothermal synthesis (MHS) and to evaluate its photocatalytic properties. The TiO$_2$ nanoparticles were directly grown on the carbon fibre (CF). Thus, a study comparing the conventional titania coating vs. the MHS were performed. The significant layer interaction as a function of the coating method on the visible and dark dye photodegradation performance was observed. Techniques such as X-ray diffraction, electron microscopy (field-emission scanning electron microscope (FESEM)), Raman spectroscopy, among others were used aiming to characterize the different route samples. This study reports a reproducible and single method to manufacture of nanocomposites through the growth ofTiO$_2$ nanoparticle on CF by MHS that allow controlling the thickness layer. Similar procedure of synthesized nanocomposite could be applied in different chemical compositions to advanced applications, based on the electrochemical nanostructure.

  8. Microwave-Assisted Extraction of Polyphenols from Camellia oleifera Fruit Hull

    Directory of Open Access Journals (Sweden)

    Jiahong Chen

    2011-05-01

    Full Text Available The abundant fruit hulls of tea-oil tree (Camellia oleifera are still underutilized and wastefully discaded to pollute the environment. In order to solve this problem and better utilize the fruit hulls of C. oleifera, a microwave-assisted extraction system was used to extract their polyphenols using water as the extraction solvent. A central composite design (CCD was used to monitor the effects of three extraction processing parameters – liquid:solid ratio (mL/g, extraction time (min and extraction temperature (°C – on the polyphenol yield (%. The results showed that the optimal conditions were liquid:solid ratio of 15.33:1 (mL/g, extraction time of 35 min and extraction temperature of 76 °C. Validation tests indicated that under the optimized conditions the actual yield of polyphenols was 15.05 ± 0.04% with RSD = 0.21% (n = 5, which was in good agreement with the predicted yield. Phenolic compounds in the extracts were analysed by HPLC, and gallic acid was found to be the predominant constituent. The total flavonoid content in the extracts was determined and high total flavonoid content was revealed (140.06 mg/g dry material.

  9. Ionic liquids based simultaneous ultrasonic and microwave assisted extraction of phenolic compounds from burdock leaves

    Energy Technology Data Exchange (ETDEWEB)

    Lou Zaixiang, E-mail: louzaixiang@126.com [State Key Laboratory of Food Science and Technology, School of Food Science and Technology, Jiangnan University, Wuxi 214122 (China); Wang Hongxin, E-mail: whx200720082009@yahoo.cn [State Key Laboratory of Food Science and Technology, School of Food Science and Technology, Jiangnan University, Wuxi 214122 (China); Zhu Song; Chen Shangwei; Zhang Ming; Wang Zhouping [State Key Laboratory of Food Science and Technology, School of Food Science and Technology, Jiangnan University, Wuxi 214122 (China)

    2012-02-24

    The ionic liquids based simultaneous ultrasonic and microwave assisted extraction (IL-UMAE) technique was first proposed and applied to isolate compounds. The ionic liquids comprising a range of four anions, five 1-alkyl-3-methylimidazolium derivatives were designed and prepared. The results suggested that varying the anion and cation both had apparent effects on the extraction of phenolics. The results also showed that irradiation power, time and solid-liquid ratio significantly affected the yields. The yields of caffeic acid and quercetin obtained by IL-UMAE were higher than those by regular UMAE. Compared with conventional heat-reflux extraction (HRE), the proposed approach exhibited higher efficiency (8-17% enhanced) and shorter extraction time (from 5 h to 30 s). The results indicated ILUMAE to be a fast and efficient extraction technique. Moreover, the proposed method was validated by the reproducibility and recovery experiments. The ILUMAE method provided good recoveries (from 96.1% to 105.3%) with RSD lower than 5.2%, which indicated that the proposed method was credible. Based on the designable nature of ionic liquids, and the rapid and highly efficient performance of the proposed approach, ILUMAE provided a new alternative for preparation of various useful substances from solid samples.

  10. Microwave-Assisted Hydrothermal Rapid Synthesis of Calcium Phosphates: Structural Control and Application in Protein Adsorption

    Directory of Open Access Journals (Sweden)

    Zhu-Yun Cai

    2015-07-01

    Full Text Available Synthetic calcium phosphate (CaP-based materials have attracted much attention in the biomedical field. In this study, we have investigated the effect of pH values on CaP nanostructures prepared using a microwave-assisted hydrothermal method. The hierarchical nanosheet-assembled hydroxyapatite (HAP nanostructure was prepared under weak acidic conditions (pH 5, while the HAP nanorod was prepared under neutral (pH 7 and weak alkali (pH 9 condition. However, when the pH value increases to 11, a mixed product of HAP nanorod and tri-calcium phosphate nanoparticle was obtained. The results indicated that the pH value of the initial reaction solution played an important role in the phase and structure of the CaP. Furthermore, the protein adsorption and release performance of the as-prepared CaP nanostructures were investigated by using hemoglobin (Hb as a model protein. The sample that was prepared at pH = 11 and consisted of mixed morphologies of nanorods and nanoprisms showed a higher Hb protein adsorption capacity than the sample prepared at pH 5, which could be explained by its smaller size and dispersed structure. The results revealed the relatively high protein adsorption capacity of the as-prepared CaP nanostructures, which show promise for applications in various biomedical fields such as drug delivery and protein adsorption.

  11. A rapid microwave-assisted solvothermal approach to lower-valent transition metal oxides.

    Science.gov (United States)

    Moorhead-Rosenberg, Zachary; Harrison, Katharine L; Turner, Travis; Manthiram, Arumugam

    2013-11-18

    A green, rapid microwave-assisted solvothermal process using tetraethylene glycol (TEG) as a reducing agent has been explored as a soft-chemistry route for the preparation of various lower-valent transition metal oxides. To demonstrate the feasibility of the approach, lower-valent binary oxides such as V4O9, Mn3O4 or MnO, CoO, and Cu2O have been obtained within a short reaction time of 30 min by reducing, respectively, V2O5, MnO2, Co3O4, and CuO with TEG at LaCoO3, LaNiO3, and La4Ni3O10. The oxidation state of the transition metal ions and the oxygen content in these ternary oxides could be tuned by precisely controlling the reaction temperatures from 160 to 300 °C. The products have been characterized by X-ray powder diffraction and iodometric titration. The versatility of this novel technique is demonstrated by the facile synthesis of V4O9, which has only been produced recently in single-phase form.

  12. The Formation of Nanocrystalline Diamond Coating on WC Deposited by Microwave Assisted Plasma CVD

    Science.gov (United States)

    Toff, M. R. M.; Hamzah, E.; Purniawan, A.

    2010-03-01

    Diamond is one form of carbon structure. The extreme hardness and high chemical resistant of diamond coatings determined that many works on this area relate to coated materials for tribological applications in biomedicine, as mechanical seals or cutting tools for hard machining operations. In the work, nanocrystalline diamond (NCD) coated tungsten carbide (WC) have been deposited by microwave assisted plasma chemical vapor deposition (MAPCVD) from CH4/H2 mixtures. Morphology of NCD was investigated by using Scanning Electron Microscopy (SEM) and Atomic Force Microscopy (AFM). The quality of NCD is defined as ratio between diamond and non diamond and also full width at half maximum (FWHM) was determined using Raman spectra. The result found that the NCD structure can be deposited on WC surface using CH4/H2 gas mixture with grain size ˜20 nm to 100 nm. Increase %CH4 concentration due to increase the nucleation of NCD whereas decrease the quality of diamond. Based on Raman spectra, the quality of NCD is in the range ˜98.82-99.01% and 99.56-99.75% for NCD and microcrystalline (MCD), respectively. In addition, FWHM of NCD is high than MCD in the range of 8.664-62.24 cm-1 and 4.24-5.05 cm-1 for NCD and MCD respectively that indicate the crystallineity of NCD is smaller than MCD.

  13. Rapid microwave-assisted synthesis of dextran-coated iron oxide nanoparticles for magnetic resonance imaging

    Science.gov (United States)

    Osborne, Elizabeth A.; Atkins, Tonya M.; Gilbert, Dustin A.; Kauzlarich, Susan M.; Liu, Kai; Louie, Angelique Y.

    2012-06-01

    Currently, magnetic iron oxide nanoparticles are the only nanosized magnetic resonance imaging (MRI) contrast agents approved for clinical use, yet commercial manufacturing of these agents has been limited or discontinued. Though there is still widespread demand for these particles both for clinical use and research, they are difficult to obtain commercially, and complicated syntheses make in-house preparation unfeasible for most biological research labs or clinics. To make commercial production viable and increase accessibility of these products, it is crucial to develop simple, rapid and reproducible preparations of biocompatible iron oxide nanoparticles. Here, we report a rapid, straightforward microwave-assisted synthesis of superparamagnetic dextran-coated iron oxide nanoparticles. The nanoparticles were produced in two hydrodynamic sizes with differing core morphologies by varying the synthetic method as either a two-step or single-step process. A striking benefit of these methods is the ability to obtain swift and consistent results without the necessity for air-, pH- or temperature-sensitive techniques; therefore, reaction times and complex manufacturing processes are greatly reduced as compared to conventional synthetic methods. This is a great benefit for cost-effective translation to commercial production. The nanoparticles are found to be superparamagnetic and exhibit properties consistent for use in MRI. In addition, the dextran coating imparts the water solubility and biocompatibility necessary for in vivo utilization.

  14. Improving the efficiency of antioxidant extraction from mango peel by using microwave-assisted extraction.

    Science.gov (United States)

    Dorta, Eva; Lobo, M Gloria; González, Mónica

    2013-06-01

    The purpose of this study was to analyze the extraction efficiency of antioxidants from mango peel by comparing two techniques: microwave-assisted (MAE) and traditional solvent (TE) extraction. The number of extraction steps, water content in the extractant, peel weight-to-solvent volume ratio in extractions and extraction time all had an influence on obtaining extracts with high antioxidant capacity, but the extraction technique and the water content in the extractant were the factors with the greatest effect. Using three steps, a water content of 50 % in the ethanol:water extractant, an extraction time of 60 min and a weight-to-volume ratio of 1:10 or 1:50 (w/v) led to the highest antioxidant activity and phytochemicals content in extracts. The extraction time needed to extract phytochemicals from mango peel was similar when MAE and TE were used. However, the antioxidant capacity and phytochemical content were around 1.5-6.0 times higher in the extracts obtained by MAE.

  15. Determination of dieldrin in wool products by gas chromatography with microwave-assisted extraction.

    Science.gov (United States)

    Ohto, Mikiya; Kodama, Shuji; Saito, Yukio; Yamamoto, Atushi

    2006-12-01

    Dieldrin is a moth-proofing agent that was banned by the Stockholm Convention in 2001. The amount of dieldrin in wool products was measured by a microwave-assisted extraction (MAE) method. The optimal conditions were as follows: extraction solvent, acetone/n-hexane (1:1 v/v); extraction temperature, 110 degrees C; extraction time, 10 min; solvent volume, 25 mL. When six samples were used, dieldrin contents determined by GC with the proposed MAE agreed closely with those by the Japanese official method using GC with solvent extraction and cleanup by column chromatography. The proposed MAE has two merits. First, the pretreatment of the MAE needs only 4 h for 11 samples, while that using the Japanese official method needs 2 days for six samples. Second, the volume of organic solvents used for the proposed method was only about one-tenth of that used in the Japanese official method. Our proposed method seems to be easy and useful for daily (routine) tests. Dieldrin contents of 28 used wool products, which were obtained from local clothing shops and ordinary homes, were determined by GC with the proposed MAE, and six products contained dieldrin (0.310-175 ppm). The dry cleaning of the woolen yarn containing 175 ppm dieldrin did not remove a significant amount of dieldrin. Therefore, it seems likely that dieldrin is still distributed slightly but widely throughout the world.

  16. Microwave-Assisted Synthesis of Some 3,5-Arylated 2-Pyrazolines

    Directory of Open Access Journals (Sweden)

    Hassan Ghasemnejad

    2003-07-01

    Full Text Available Condensation of 2-acetylnaphthalene with benzaldehydes under microwave irradiation affords chalcones which undergo facile and clean cyclizations with hydrazines RNHNH2 (R= H, Ph, Ac to afford 3,5-arylated 2-pyrazolines in quantitative yields, also under microwave irradiation and in the presence of dry AcOH as cyclizing agent. The results obtained indicate that, unlike classical heating, microwave irradiation results in higher yields, shorter reaction times (2-12 min. and cleaner reactions.

  17. Thrust Stand Measurements Using Alternative Propellants in the Microwave Assisted Discharge Inductive Plasma Accelerator

    Science.gov (United States)

    Hallock, Ashley K.; Polzin, Kurt A.

    2011-01-01

    Storable propellants (for example water, ammonia, and hydrazine) are attractive for deep space propulsion due to their naturally high density at ambient interplanetary conditions, which obviates the need for a cryogenic/venting system. Water in particular is attractive due to its ease of handling and availability both terrestrially and extra-terrestrially. While many storable propellants are reactive and corrosive, a propulsion scheme where the propellant is insulated from vulnerable (e.g. metallic) sections of the assembly would be well-suited to process these otherwise incompatible propellants. Pulsed inductive plasma thrusters meet this criterion because they can be operated without direct propellant-electrode interaction. During operation of these devices, electrical energy is capacitively stored and then discharged through an inductive coil creating a time-varying current in the coil that interacts with a plasma covering the face of the coil to induce a plasma current. Propellant is accelerated and expelled at a high exhaust velocity (O(10-100 km/s)) by the Lorentz body force arising from the interaction of the magnetic field and the induced plasma current. While this class of thruster mitigates the life-limiting issues associated with electrode erosion, many pulsed inductive plasma thrusters require high pulse energies to inductively ionize propellant. The Microwave Assisted Discharge Inductive Plasma Accelerator (MAD-IPA) is a pulsed inductive plasma thruster that addressees this issue by partially ionizing propellant inside a conical inductive coil before the main current pulse via an electron cyclotron resonance (ECR) discharge. The ECR plasma is produced using microwaves and a static magnetic field from a set of permanent magnets arranged to create a thin resonance region along the inner surface of the coil, restricting plasma formation, and in turn current sheet formation, to a region where the magnetic coupling between the plasma and the theta

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

    Science.gov (United States)

    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.

  19. The effect of microwave-assisted for photo-catalytic degradation of rhodamine B in aqueous nano TiO2 particles dispersions.

    Science.gov (United States)

    Shin, Hyun-Chung; Park, Sung Hoon; Ahn, Ho-Geun; Chung, Minchul; Kim, Byung Whan; Kim, Sun-Jae; Seo, Seong-Gyu; Jung, Sang-Chul

    2011-02-01

    The photo-catalytic decomposition of rhodamine B was examined in aqueous nano TiO2 particles dispersions to assess effects of the microwave radiation assisted photo-catalytic process driven by UV radiation. The results of photo-catalytic degradation of rhodamine B showed that the decomposition rate increased with the microwave intensity, UV intensity, TiO2 particle dosages and the circulating fluid velocity. Addition of oxygen gas in the photo-catalytic degradation of rhodamine B increased the reaction rate. The effect of addition of H2O2 was not significant when photo-catalysis was used without additional microwave radiation or when microwave was irradiated without the use of photo-catalysts. When H2O2 was added under simultaneous use of photo-catalysis and microwave irradiation, however, considerably higher degradation reaction rates were observed. This study demonstrates that the microwave irradiation can play a very important role in photo-catalytic degradation.

  20. Synthesis of whiskers of SiC microwave assisted; Sintesis de whiskers de SiC asistida por microondas

    Energy Technology Data Exchange (ETDEWEB)

    Garza-Mendez, F. J.; Vanegas, A. J.; Vazquez, B. A.; Garza-Paz, J.

    2013-06-01

    We developed a new process for the synthesis of SiC whiskers assisted by microwaves; this is based on the mixture of silica xerogels and graphite powder. As energy source were used microwaves of 2.45 GHz and 1.0 kW of power RMS. On the other hand, mesoporous silica was synthesized via sol-gel, the precursors used were TEOS/H{sub 2}O and ethanol. Through analysis of the BET is determined the value of average pore size (3.0 nm) and the surface area (1090 m2/g).By mean of X-Ray diffraction it was demonstrated that the silica obtained is an amorphous solid and, the powders obtained in the microwave synthesis are {beta}-SiC. Synthesized SiC powders were observed using a SEM in secondary electron mode, it was observed that this powders consists of SiC whiskers. The effect of microwaves on the synthesis of whiskers of SiC is discussed in the present work. (Author) 19 refs.

  1. Preparation of alumina-doped yttria-stabilized zirconia nanopowders by microwave-assisted peroxyl-complex coprecipitation

    Institute of Scientific and Technical Information of China (English)

    QI Liang; XU Ming-xia; TIAN Yu-ming; ZHAO Jin-wei

    2006-01-01

    Alumina-doped yttria-stabilized zirconia (ADYSZ) nanopowders were prepared by microwave-assisted peroxyl-complex coprecipitation (MAPCC) using ZrOCl2·8H2O,Y2O3 and AlCl3·6H2O as starting materials,NH3·H2O as precipitant and H2O2 as complexant. The effects of adding H2O2 and microwave drying on the preparation and properties of ADYSZ were investigated. The precursors and nanopowders were studied by EDX,XRD,SEM and TEM techniques. The results show that the uniformity of component distribution within ADYSZ nanopowders is improved by adding appropriate dosage of H2O2. Complexing reaction between H2O2 and Zr4+ ion restrains the hydrolyzation and precipitation of Zr4+ ion. With the addition of H2O2,Al3+,Y3+ and Zr4+ ions can be precipitated synchronously in a relatively narrow range of pH value. H2O2 also improves the filterability of the wet precipitate. The highly hydrophilic precipitates can be quickly and effectively separated from aqueous solution. During microwave drying process,the moisture of wet precursors is selectively heated. Quick expansion of steam vapor within the wet colloidal particles causes the aggregations burst into numerous tiny lumps. Compared with oven drying,microwave drying can not only shorten drying time but also reduce aggregation intensity of the resultant ADYSZ nanopowders.

  2. Crystal growth behavior of LiFePO4 in microwave-assisted hydrothermal condition: from nanoparticle to nanosheet.

    Science.gov (United States)

    Yang, Gang; Ji, Hongmei; Miao, Xiaowei; Hong, Anqing; Yan, Yuan

    2011-06-01

    By using microwave-assisted hydrothermal crystallization approach, LiFePO4 nanoparticles have been synthesized in several minutes without the use of any organic reducing agent and argon protection. The crystal structure and lattice parameters have been analyzed by using the X-ray diffraction patterns (XRD) and Rietveld refined analysis, and the full width at half-maximum (FWHM) of the characteristic peaks. A preferential orientation of crystal growth occurs upon microwave hydrothermal field. The SEM and TEM images show that the LiFePO4 crystals present a change from nanoparticle to nanosheet with the increasing reaction time from 5 to 20 min. All the samples present a couple of redox peaks in their CV profiles. The peak pair corresponds to the charge/discharge reaction of the Fe3+/Fe2+ redox couple, and evidencing the absence of electroactive iron impurities. Because of the LiFePO4 samples prepared without any carbon, the initial charge/discharge capacities and cycleability of absolutely are affected by the crystal structure which is controlled by the microwave irradiation condition. The relation among the microwave reaction condition, crystal morphology, and the electrochemical properties are presented and discussed in the electrochemical test.

  3. Microwave-assisted extraction of silkworm pupal oil and evaluation of its fatty acid composition, physicochemical properties and antioxidant activities.

    Science.gov (United States)

    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.

  4. Comparison of microwave, ultrasound and accelerated-assisted solvent extraction for recovery of polyphenols from Citrus sinensis peels.

    Science.gov (United States)

    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.

  5. Optimization of microwave-assisted extraction of polyphenols from apple pomace using response surface methodology and HPLC analysis.

    Science.gov (United States)

    Bai, Xue-Lian; Yue, Tian-Li; Yuan, Ya-Hong; Zhang, Hua-Wei

    2010-12-01

    A simple and efficient microwave-assisted extraction of polyphenols from industrial apple pomace was developed and optimized by the maximization of the yield using response surface methodology. A Box-Behnken design was used to monitor the effect of microwave power, extraction time, ethanol concentration and ratio of solvent to raw material (g/mL) on the polyphenols yield. The results showed that the optimal conditions were as follows: microwave power 650.4 W, extraction time 53.7 s, ethanol concentration 62.1% and ratio of solvent to raw material 22.9:1. Validation tests indicated that the actual yield of polyphenols was 62.68±0.35 mg gallic acid equivalents per 100 g dry apple pomace with RSD=0.86% (n=5) under the optimal conditions, which was in good agreement with the predicted yield and higher than those of reflux and ultrasonic-assisted extraction methods. HPLC analysis indicated that the major polyphenols of apple pomace consisted of chlorogenic acid, caffeic acid, syrigin, procyanidin B2, (-)-epicatechin, cinnamic acid, coumaric acid, phlorizin and quercetin, of which procyanidin B2 had the highest content of 219.4 mg/kg.

  6. Microwave-assisted rapid synthesis of birnessite-type MnO{sub 2} nanoparticles for high performance supercapacitor applications

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Xiong; Miao, Wang; Li, Chen; Sun, Xianzhong; Wang, Kai; Ma, Yanwei, E-mail: ywma@mail.iee.ac.cn

    2015-11-15

    Highlights: • Birnessite-type MnO{sub 2} nanoparticles were prepared by the microwave-assisted reflux. • The microwave reaction duration was only 5 min. • A specific capacitance of 329 F g{sup −1} was obtained for birnessite-type MnO{sub 2}. - Abstract: Birnessite-type MnO{sub 2} nanoparticles have been successfully synthesized by the microwave-assisted reflux as short as 5 min. The microstructure and morphology of the products were characterized by X-ray diffraction, N{sub 2} adsorption–desorption isotherms, scanning electron microscopy, transmission electron microscopy. The electrochemical properties of the as-prepared MnO{sub 2} as an electrode material for supercapacitor were investigated by cyclic voltammetry and galvanostatic charge-discharge measurements in 1 M Na{sub 2}SO{sub 4} electrolyte, and a high specific capacitance of 329 F g{sup −1} was achieved at a current density of 0.2 A g{sup −1}. The specific capacitance retention was 92% after 1000 cycles at 2 A g{sup −1}, suggesting that it is a promising electrode material for supercapacitors.

  7. Single-step microwave-assisted hot water extraction of hemicelluloses from selected lignocellulosic materials - A biorefinery approach.

    Science.gov (United States)

    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.

  8. Optimization of microwave-assisted extraction for anthocyanins, polyphenols, and antioxidants from raspberry (Rubus Coreanus Miq.) using response surface methodology.

    Science.gov (United States)

    Teng, Hui; Lee, Won Young; Choi, Yong Hee

    2013-09-01

    Anthocyanins (Acys), polyphenols, and antioxidants were extracted from raspberry (Rubus Coreanus Miq.) using a highly efficient microwave-assisted extraction technique. Different solvents, including methanol, ethanol, and acetone, were tested. The colors of the extracts varied from light yellow to purple red or dark red. SEM and other nutrient analyses verified that ethanol was the most favorable medium for the microwave-assisted extraction of raspberry due to its high output and low toxicity. Effects of process parameters, including microwave power, irradiation time, and solvent concentration, were investigated through response surface methodology. Canonical analysis estimated that the highest total Acys content, total polyphenols content, and antioxidant activity of raspberry were 17.93 mg cyanidin-3-O-glucoside equivalents per gram dry weight, 38.57 mg gallic acid equivalents per gram dry weight, and 81.24%, respectively. The polyphenol compositions of raspberry extract were identified by HPLC with diode array detection, and nine kinds of polyphenols were identified and quantified, revealing that chlorogenic acid, syringic acid, and rutin are the major polyphenols contained in raspberry fruits. Compared with other fruits and vegetables, raspberry contains higher Acy and polyphenol contents with stronger antioxidant activity, suggesting that raspberry fruits are a good source of natural food colorants and antioxidants.

  9. Microwave-assisted facile and rapid Friedel-Crafts benzoylation of arenes catalysed by bismuth trifluoromethanesulfonate

    DEFF Research Database (Denmark)

    Tran, Phoung Hoang; Hansen, Poul Erik; Pham, Thuy Than;

    2014-01-01

    The catalytic activity of metal triflates was investigated in Friedel–Crafts benzoylation under microwave irradiation. Friedel–Crafts benzoylation with benzoyl chloride of a variety of arenes containing electron-rich and electron-poor rings using bismuth triflate under microwave irradiation is de...

  10. Microwave assisted alkaline pretreatment to enhance enzymatic saccharification of catalpa sawdust.

    Science.gov (United States)

    Jin, Shuguang; Zhang, Guangming; Zhang, Panyue; Li, Fan; Wang, Siqi; Fan, Shiyang; Zhou, Shuqiong

    2016-12-01

    Catalpa sawdust, a promising biofuel production biomass, was pretreated by microwave-water, -NaOH, and -Ca(OH)2 to enhance enzymatic digestibility. After 48h enzymatic hydrolysis, microwave-Ca(OH)2 pretreated sample showed the highest reducing sugar yield. The content of hemicellulose and lignin in catalpa sawdust decreased after microwave-alkali pretreatment. SEM observation showed that the catalpa sawdust surface with microwave-Ca(OH)2 pretreatment suffered the most serious erosion. Crystallinity index of catalpa sawdust increased after all three kinds of pretreatment. The optimum conditions of microwave-Ca(OH)2 pretreatment were particle size of 40mesh, Ca(OH)2 dosage of 2.25% (w/v), microwave power of 400W, pretreatment time of 6min, enzyme loading of 175FPU/g, and hydrolysis time of 96h, and the reducing sugar yield of microwave-Ca(OH)2 pretreated catalpa sawdust reached 402.73mg/g, which increased by 682.15% compared with that of raw catalpa sawdust. The catalpa sawdust with microwave-Ca(OH)2 pretreatment is promising for biofuel production with great potential.

  11. Water promoted,microwave-assisted oxidative novel deamination of N-aminoquinazolinones

    Institute of Scientific and Technical Information of China (English)

    M.Arfan; Rasool Khan; Shazia Anjum; Shabir Ahmad; M.Iqbal Choudhary

    2008-01-01

    A novel deamination of 2-alkyl/aryl 3-amino-4(3H)-qninazolinones series using aqueous KMnO4 under thermal condition and microwave irradiation is described.Compared to thermal condition,significantly higher yields in much shorter times were observedfor reactions under microwave irradiation.A plausible mechanism has been proposed for the oxidative water-promoted deamination.

  12. Microwave-assisted Preparation of Temperature Sensitive Poly(N-isopropylacrylamide) Hydrogel with Improved Responsive Properties

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    Poly(N-isopropylacrylamide)-based hydrogel was prepared under microwave irradiation.The hydrogel thus prepared, comparing with that prepared by thermal heating method, exhibits faster swelling and shrinking kinetics. The improved responsive properties are due to the more heterogeneous and porous networks formed under microwave irradiation.

  13. Microwave-assisted Oxidation of Alcohols and Polyarenes with Cetyltrimethylarnmonium Bromochromate

    Institute of Scientific and Technical Information of China (English)

    MOHAMMADI Mohammad Kazem; GHAMMAMY Shahriare; IMANIEH Hossein

    2009-01-01

    An efficient and mild methodology for oxidation of alcohols and polyarenes was described using cetyltrimethylammonium bromochromate (CTMABC) under microwave irradiation.Primary and secondary alcohols and polyarenes could be selectively oxidized under microwave irradiation into the corresponding aldehydes and ketones in high yields and short reaction time,using commercially available and magnetically retrievable oxidative material (CTMABC).

  14. Microwave Assisted Synthesis of N-Arylheterocyclic Substituted-4-aminoquinazoline Derivatives

    Directory of Open Access Journals (Sweden)

    Ping Lu

    2006-04-01

    Full Text Available A simple, efficient, and general method has been developed for the synthesis of various N-aryl heterocylic substituted-4-aminoquinazoline compounds from 4-chloro- quinazoline and aryl heterocyclic amines under microwave irradiation using 2-propanol as solvent. The advantages of the use of microwave irradiation in relation to the classical method were demonstrated.

  15. Detection and characterization of cholesterol-oxidized products using HPLC coupled to dopant assisted atmospheric pressure photoionization tandem mass spectrometry.

    Science.gov (United States)

    Ronsein, Graziella E; Prado, Fernanda M; Mansano, Fernando V; Oliveira, Mauricio C B; Medeiros, Marisa H G; Miyamoto, Sayuri; Di Mascio, Paolo

    2010-09-01

    Oxidation of cholesterol (Ch) by a variety of reactive oxygen species gives rise mainly to hydroperoxides and aldehydes. Despite the growing interest in Ch-oxidized products, the detection and characterization of these products is still a matter of concern. In this work, the main Ch-oxidized products, namely, 3beta-hydroxycholest-5-ene-7alpha-hydroperoxide (7alpha-OOH), 3beta-5alpha-cholest-6-ene-5-hydroperoxide (5alpha-OOH), 3beta-hydroxycholest-4-ene-6alpha-hydroperoxide (6alpha-OOH), 3beta-hydroxycholest-4-ene-6beta-hydroperoxide (6beta-OOH), and 3beta-hydroxy-5beta-hydroxy-B-norcholestane-6beta-carboxaldehyde (ChAld), were detected in the same analysis using high-performance liquid chromatography (HPLC) coupled to dopant assisted atmospheric pressure photoionization tandem mass spectrometry. The use of selected reaction monitoring mode (SRM) allowed a sensitive detection of each oxidized product, while the enhanced product ion mode (EPI) helped to improve the confidence of the analyses. Isotopic labeling experiments enabled one to elucidate mechanistic features during fragmentation processes. The characteristic fragmentation pattern of Ch-oxidized products is the consecutive loss of H(2)O molecules, yielding cationic fragments at m/z 401, 383, and 365. Homolytic scissions of the peroxide bond are also seen. With (18)O-labeling approach, it was possible to establish a fragmentation order for each isomer. The SRM transitions ratio along with EPI and (18)O-labeled experiments give detailed information about differences for water elimination, allowing a proper discrimination between the isomers. This is of special interest considering the emerging role of Ch-oxidized products in the development of diseases.

  16. Microwave assisted hydrothermal synthesis and characterization of ZnO–TNT composites

    Energy Technology Data Exchange (ETDEWEB)

    Cho, Sung Hun; Gyawali, Gobinda; Adhikari, Rajesh [Department of Metallurgy and Materials Engineering, SunMoon University, Asan (Korea, Republic of); Kim, Tae Ho [Department of Environmental Engineering, SunMoon University, Asan (Korea, Republic of); Lee, Soo Wohn, E-mail: swlee@sunmoon.ac.kr [Department of Environmental Engineering, SunMoon University, Asan (Korea, Republic of)

    2014-06-01

    TiO{sub 2} nanotubes with different contents of ZnO (3–40 wt.% ZnO) have been successfully synthesized by microwave assisted hydrothermal process by using commercial TiO{sub 2}-P25 as a precursor. The phase and crystallinity of the obtained ZnO–TNT were analyzed by X-ray Diffraction (XRD). The surface area of the ZnO–TNT was determined by BET method. The effect of the different contents of ZnO on morphology of TiO{sub 2} nanotubes was investigated by SEM and TEM. Optical properties and band gap energy of ZnO–TNT were calculated by using UV–vis DRS spectroscopy and modified Kubelka–Munk equation. Photocatalytic performance of ZnO–TNT was investigated by degradation of rhodamine B (RhB) dye under UV and visible light irradiation. Increasing ZnO content in TNT gradually decreased the diameter and length of nanotubes. Furthermore, addition of 40 wt.% ZnO into the TNT exceeded the saturation limit of ion exchangeability of Zn{sup 2+} and Na{sup +} ions and aggregation of finely dispersed ZnO particles on the surface of TNT were observed. The ZnO–TNT has shown relatively larger band gap energies than that of TiO{sub 2}-P25. However, ZnO–TNT has shown considerable increase in photo-activity for degradation of RhB dye in visible light as compared to UV light irradiation. - Highlights: • ZnO–TNT composites were successfully synthesized. • Investigation of the structural changes in the composites is confirmed. • The photocatalytic activity of the composites was studied. • Composites exhibited better performance under visible light than in UV light.

  17. Supercritical Carbon Dioxide and Microwave-Assisted Extraction of Functional Lipophilic Compounds from Arthrospira platensis

    Directory of Open Access Journals (Sweden)

    Diego A. Esquivel-Hernández

    2016-05-01

    Full Text Available Arthrospira platensis biomass was used in order to obtain functional lipophilic compounds through green extraction technologies such as supercritical carbon dioxide fluid extraction (SFE and microwave-assisted extraction (MAE. The temperature (T factor was evaluated for MAE, while for SFE, pressure (P, temperature (T, and co-solvent (ethanol (CS were evaluated. The maximum extraction yield of the obtained oleoresin was (4.07% ± 0.14% and (4.27% ± 0.10% for SFE and MAE, respectively. Extracts were characterized by gas chromatography mass spectrometry (GC-MS and gas chromatography flame ionization detector (GC-FID. The maximum contents of functional lipophilic compounds in the SFE and MAE extracts were: for carotenoids 283 ± 0.10 μg/g and 629 ± 0.13 μg/g, respectively; for tocopherols 5.01 ± 0.05 μg/g and 2.46 ± 0.09 μg/g, respectively; and for fatty acids 34.76 ± 0.08 mg/g and 15.88 ± 0.06 mg/g, respectively. In conclusion, the SFE process at P 450 bar, T 60 °C and CS 53.33% of CO2 produced the highest yield of tocopherols, carotenoids and fatty acids. The MAE process at 400 W and 50 °C gives the best extracts in terms of tocopherols and carotenoids. For yield and fatty acids, the MAE process at 400 W and 70 °C produced the highest values. Both SFE and MAE showed to be suitable green extraction technologies for obtaining functional lipophilic compounds from Arthrospira platensis.

  18. Supercritical Carbon Dioxide and Microwave-Assisted Extraction of Functional Lipophilic Compounds from Arthrospira platensis

    Science.gov (United States)

    Esquivel-Hernández, Diego A.; López, Víctor H.; Rodríguez-Rodríguez, José; Alemán-Nava, Gibrán S.; Cuéllar-Bermúdez, Sara P.; Rostro-Alanis, Magdalena; Parra-Saldívar, Roberto

    2016-01-01

    Arthrospira platensis biomass was used in order to obtain functional lipophilic compounds through green extraction technologies such as supercritical carbon dioxide fluid extraction (SFE) and microwave-assisted extraction (MAE). The temperature (T) factor was evaluated for MAE, while for SFE, pressure (P), temperature (T), and co-solvent (ethanol) (CS) were evaluated. The maximum extraction yield of the obtained oleoresin was (4.07% ± 0.14%) and (4.27% ± 0.10%) for SFE and MAE, respectively. Extracts were characterized by gas chromatography mass spectrometry (GC-MS) and gas chromatography flame ionization detector (GC-FID). The maximum contents of functional lipophilic compounds in the SFE and MAE extracts were: for carotenoids 283 ± 0.10 μg/g and 629 ± 0.13 μg/g, respectively; for tocopherols 5.01 ± 0.05 μg/g and 2.46 ± 0.09 μg/g, respectively; and for fatty acids 34.76 ± 0.08 mg/g and 15.88 ± 0.06 mg/g, respectively. In conclusion, the SFE process at P 450 bar, T 60 °C and CS 53.33% of CO2 produced the highest yield of tocopherols, carotenoids and fatty acids. The MAE process at 400 W and 50 °C gives the best extracts in terms of tocopherols and carotenoids. For yield and fatty acids, the MAE process at 400 W and 70 °C produced the highest values. Both SFE and MAE showed to be suitable green extraction technologies for obtaining functional lipophilic compounds from Arthrospira platensis. PMID:27164081

  19. Microwave-assisted chemical insertion: a rapid technique for screening cathodes for Mg-ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Kaveevivitchai, Watchareeya; Huq, Ashfia; Manthiram, Arumugam

    2016-12-19

    We report an ultrafast microwave-assisted solvothermal method for chemical insertion of Mg2+ ions into host materials using magnesium acetate [Mg(CH3COO)2] as a metal-ion source and diethylene glycol (DEG) as a reducing agent. For instance, up to 3 Mg ions per formula unit of a microporous host framework Mo2.5+yVO9+z could be inserted in as little as 30 min at 170–195 °C in air. This process is superior to the traditional method which involves the use of organometallic reagents, such as di-n-butylmagnesium [(C4H9)2Mg] and magnesium bis(2,6-di-tert-butylphenoxide) [Mg-(O-2,6-But2C6H3)2], and requires an inert atmosphere with extremely long reaction times. Considering the lack of robust electrolytes for Mg-ion batteries, this facile approach can be readily used as a rapid screening technique to identify potential Mg-ion electrode hosts without the necessity of fabricating electrodes and assembling electrochemical cells. Due to the mild reaction conditions, the overall structure and morphology of the Mg-ion inserted products are maintained and the compounds can be used successfully as a cathode in Mg-ion batteries. The combined synchrotron X-ray and neutron diffraction Rietveld analysis reveals the structure of the Mg-inserted compounds and gives an insight into the interactions between the Mg ions and the open-tunnel host framework.

  20. Accelerated, microwave-assisted, and conventional solvent extraction methods affect anthocyanin composition from colored grains.

    Science.gov (United States)

    Abdel-Aal, El-Sayed M; Akhtar, Humayoun; Rabalski, Iwona; Bryan, Michael

    2014-02-01

    Anthocyanins are important dietary components with diverse positive functions in human health. This study investigates effects of accelerated solvent extraction (ASE) and microwave-assisted extraction (MAE) on anthocyanin composition and extraction efficiency from blue wheat, purple corn, and black rice in comparison with the commonly used solvent extraction (CSE). Factorial experimental design was employed to study effects of ASE and MAE variables, and anthocyanin extracts were analyzed by spectrophotometry, high-performance liquid chromatography-diode array detector (DAD), and liquid chromatography-mass spectrometry chromatography. The extraction efficiency of ASE and MAE was comparable with CSE at the optimal conditions. The greatest extraction by ASE was achieved at 50 °C, 2500 psi, 10 min using 5 cycles, and 100% flush. For MAE, a combination of 70 °C, 300 W, and 10 min in MAE was the most effective in extracting anthocyanins from blue wheat and purple corn compared with 50 °C, 1200 W, and 20 min for black rice. The anthocyanin composition of grain extracts was influenced by the extraction method. The ASE extraction method seems to be more appropriate in extracting anthocyanins from the colored grains as being comparable with the CSE method based on changes in anthocyanin composition. The method caused lower structural changes in anthocaynins compared with the MAE method. Changes in blue wheat anthocyanins were lower in comparison with purple corn or black rice perhaps due to the absence of acylated anthocyanin compounds in blue wheat. The results show significant differences in anthocyanins among the 3 extraction methods, which indicate a need to standardize a method for valid comparisons among studies and for quality assurance purposes.

  1. Shape effect on the antibacterial activity of silver nanoparticles synthesized via a microwave-assisted method.

    Science.gov (United States)

    Hong, Xuesen; Wen, Junjie; Xiong, Xuhua; Hu, Yongyou

    2016-03-01

    Silver nanoparticles (AgNPs) are used as sustained-release bactericidal agents for water treatment. Among the physicochemical characteristics of AgNPs, shape is an important parameter relevant to the antibacterial activity. Three typically shaped AgNPs, nanocubes, nanospheres, and nanowires, were prepared via a microwave-assisted method and characterized by TEM, UV-vis, and XRD. The antibacterial activity of AgNPs was determined by OD growth curves tests, MIC tests, and cell viability assay against Escherichia coli. The interaction between AgNPs and bacterial cells was observed by TEM. The results showed that the three differently shaped AgNPs were nanoscale, 55 ± 10 nm in edge length for nanocubes, 60 ± 15 nm in diameter for nanospheres, 60 ± 10 nm in diameter and 2-4 μm in length for nanowires. At the bacterial concentration of 10(4) CFU/mL, the MIC of nanocubes, nanospheres, and nanowires were 37.5, 75, and 100 μg/mL, respectively. Due to the worst contact with bacteria, silver nanowires exhibited the weakest antibacterial activity compared with silver nanocubes and silver nanospheres. Besides, silver nanocubes mainly covered by {100} facets showed stronger antibacterial activity than silver nanospheres covered by {111} facets. It suggests that the shape effect on the antibacterial activity of AgNPs is attributed to the specific surface areas and facets reactivity; AgNPs with larger effective contact areas and higher reactive facets exhibit stronger antibacterial activity.

  2. Microwave-assisted reactions: Three-component process for the synthesis of 2-amino-2-chromenes under microwave heating

    Institute of Scientific and Technical Information of China (English)

    Ramadan A. Mekheimer; Kamal U. Sadek

    2009-01-01

    2-Amino-2-chromenes are class of heterocycles that posses considerable interest as pigments, cosmetics, potential agro-chemicals and being the main constituents of many natural products. Although, they are generally prepared either under conventional heating, benign reagents or very recently, a three component condensation in poly-ethylene glycol-water in the presence of nanosized magnesium oxide, most of these methods require prolonged reaction time, reagents in stoichiometric amounts and generate moderate yields of products. Microwave technique performs a better yield in a short reaction time (85-94%;5-8 rain). Also, three-component one step reaction is of great interest for cost savings from the point of raw materials, energy and time. A combination between both techniques will be attractive for researchers in that field.

  3. Microwave-assisted synthesis of spheroidal vaterite CaCO 3 in ethylene glycol-water mixed solvents without surfactants

    Science.gov (United States)

    Chen, Yinxia; Ji, Xianbing; Wang, Xiaobo

    2010-10-01

    Spheroidal vaterite CaCO 3 composed of irregular nanoparticals have been synthesized by a fast microwave-assisted method. The structures are fabricated by the reaction of Ca(CH 3COO) 2 with (NH 4) 2CO 3 at 90 °C in ethylene glycol-water mixed solvents without any surfactants. The diameters of the spheroidal vaterite CaCO 3 range from 1 to 2 μm, and the average size of the nanoparticals is about 70 nm. Bundle-shaped aragonite and rhombohedral calcite are also obtained by adjusting the experimental parameters. Our experiments show that the ratio of ethylene glycol to water, microwave power, reaction time, and two sources of ammonium ions and acetate anions are key parameters for the fabrication of spheroidal vaterite CaCO 3. A possible growth mechanism for the spheroidal structures has been proposed, which suggests that the spheroidal vaterite CaCO 3 is formed by an aggregation mechanism.

  4. Microwave-Assisted Improved Synthesis of Oxazolidin-2-ones, Oxazolidine-2-thiones and Thiazolidine-2-thione Chiral Auxiliaries

    Directory of Open Access Journals (Sweden)

    Mario Ordóñez

    2011-10-01

    Full Text Available A microwave assisted method for the synthesis of some typical 4-substituted oxazolidinone chiral auxiliaries used in asymmetric synthesis is reported in this work. Under these conditions, treatment of (S-phenylalaninol, (S-phenylglycinol, (S-valinol and (1S, 2R-norephedrine with ethyl carbonate or carbon disulfide under the appropriate and specific microwave reaction conditions, led to an efficient synthesis of some oxazolidin-2-ones, oxazolidine-2-thiones and thiazolidine-2-thiones. The methodology reported in this paper provides these chiral auxiliaries with improved yields and a remarkable reduction on the reaction times, particularly in the case of thiazolidine-2-thiones, as compared with the conventional methods. All the auxiliaries prepared here show spectroscopic data in full agreement with those previously reported in the literature.

  5. Microwave assisted synthesis of guar gum grafted sodium acrylate/cloisite superabsorbent nanocomposites: reaction parameters and swelling characteristics.

    Science.gov (United States)

    Likhitha, M; Sailaja, R R N; Priyambika, V S; Ravibabu, M V

    2014-04-01

    In this study, superabsorbent nanocomposites of guar gum grafted sodium acrylate have been synthesized via both microwave and conventional techniques. The reaction parameters of both techniques were optimized and the microwave assisted method was proved to have higher grafting yield with lesser time of reaction as compared to the conventional method. X-ray diffraction and scanning electron microscopy analyses revealed that cloisite was exfoliated and uniformly dispersed in guar gum grafted sodium acrylate matrix. The results show that introducing cloisite into the guar gum grafted sodium acrylate network improved the swelling capability and the swelling rate of the superabsorbent nanocomposite was found to be enhanced at an optimal loading of 10% cloisite. The nanocomposites showed high water absorbency within a wide pH range. Preliminary studies on crystal violet dye removal showed promising results.

  6. A microwave-assisted and heteropolyacids-catalysed cyclocondensation reaction for the synthesis of 4(3H)-quinazolinones.

    Science.gov (United States)

    Ighilahriz, Karima; Boutemeur, Baya; Chami, Fariza; Rabia, Cherifa; Hamdi, Maâmar; Hamdi, Safouane M

    2008-04-03

    We have investigated a microwave-assisted synthesis of 4(3H)-quinazolinones by condensation of anthranilic acid, orthoesters (or formic acid) and substituted anilines,using Keggin-type heteropolyacids (H(3)PW(12)O(40).13H(2)O, H(4)SiW(12)O(40).13H(2)O,H(4)SiMo(12)O(40).13H(2)O or H(3)PMo(12)O(40).13H(2)O) as catalysts. We found that the the use of H(3)PW(12)O(40).13H(2)O acid coupled to microwave irradiation allows a solvent-free, rapid (approximately 13min) and high-yielding reaction.

  7. Synthesis of an Isoindoline-Annulated, Tricyclic Sultam Library via Microwave-Assisted, Continuous-Flow Organic Synthesis (MACOS).

    Science.gov (United States)

    Ullah, Farman; Zang, Qin; Javed, Salim; Porubsky, Patrick; Neuenswander, Benjamin; Lushington, Gerald H; Hanson, Paul R; Organ, Michael G

    2012-01-01

    A microwave-assisted, continuous-flow organic synthesis (MACOS) protocol for the synthesis of an isoindoline-annulat-ed, tricyclic sultam library, utilizing a Heck-aza-Michael (HaM) strategy, is reported. This sequence involves a Heck reaction on vi-nylsulfonamides with batch microwave heating followed by a one-pot, sequential intramolecular aza-Michael cyclization/Boc-deprot-ection using MACOS. Subsequent cyclization with either 1,1'-carbonyldiimidazole or chloromethyl pivalate using MACOS provided an array of tricyclic sultams. This efficient three-step protocol requires only a few hours to produce the target sultams starting from simple starting materials. Using this strategy, a 38-member library of isoindoline-annulated sultams was generated in good to excellent overall yields (53-87%).

  8. Synthesis of an Isoindoline-Annulated, Tricyclic Sultam Library via Microwave-Assisted, Continuous-Flow Organic Synthesis (MACOS)

    Science.gov (United States)

    Ullah, Farman; Zang, Qin; Javed, Salim; Porubsky, Patrick; Neuenswander, Benjamin; Lushington, Gerald H.

    2013-01-01

    A microwave-assisted, continuous-flow organic synthesis (MACOS) protocol for the synthesis of an isoindoline-annulat-ed, tricyclic sultam library, utilizing a Heck–aza-Michael (HaM) strategy, is reported. This sequence involves a Heck reaction on vi-nylsulfonamides with batch microwave heating followed by a one-pot, sequential intramolecular aza-Michael cyclization/Boc-deprot-ection using MACOS. Subsequent cyclization with either 1,1′-carbonyldiimidazole or chloromethyl pivalate using MACOS provided an array of tricyclic sultams. This efficient three-step protocol requires only a few hours to produce the target sultams starting from simple starting materials. Using this strategy, a 38-member library of isoindoline-annulated sultams was generated in good to excellent overall yields (53–87%). PMID:24244052

  9. Microwave-Assisted Syntheses of Bioactive Seven-Membered, Macro-Sized Heterocycles and Their Fused Derivatives

    Directory of Open Access Journals (Sweden)

    Mohsine Driowya

    2016-08-01

    Full Text Available This review describes the recent advances in the microwave-assisted synthesis of 7-membered and larger heterocyclic compounds. Several types of reaction for the cyclization step are discussed: Ring Closing Metathesis (RCM, Heck and Sonogashira reactions, Suzuki-Miyaura cross-coupling, dipolar cycloadditions, multi-component reactions (Ugi, Passerini, etc. Green syntheses and solvent-free procedures have been introduced whenever possible. The syntheses discussed herein have been selected to illustrate the huge potential of microwave in the synthesis of highly functionalized molecules with potential therapeutic applications, in high yields, enhanced reaction rates and increased chemoselectivity, compared to conventional methods. More than 100 references from the recent literature are listed in this review.

  10. Microwave assisted sol-gel synthesis of high dielectric constant CCTO and BFN ceramics for MLC applications

    Directory of Open Access Journals (Sweden)

    Sonia

    2017-06-01

    Full Text Available Ba(Fe1/2Nb1/2O3 (BFN and CaCu3Ti4O12 (CCTO ceramic powders were synthesized by microwave assisted sol-gel synthesis technique and sintered at 1100°C and 1000°C, respectively. Calcination and sintering processes were carried out in a microwave furnace. Dielectric constant (εr~2450 and dielectric loss (tan δ~0.5 at frequency of 1 kHz and 20°C were observed for the BFN ceramic samples. Higher value of εr ~ 3600 and lower value of tan δ ~ 0.07 at frequency of 1 kHz and in 20-60°C temperature range for the CCTO ceramic samples suggested its utility for MLC applications. Sharp decrease of εr and sharp increase of tan δ at higher frequencies of BFN ceramic samples indicated the presence of Debye like relaxation.

  11. Microwave-assisted synthesis of poly(3-hexylthiophene) via direct oxidation with FeCl{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Nicho, M.E., E-mail: menicho@uaem.mx [Centro de Investigacion en Ingenieria y Ciencias Aplicadas, Universidad Autonoma del Estado de Morelos (UAEM), Av. Universidad 1001, Col. Chamilpa, C.P. 62210 Cuernavaca, Morelos (Mexico); Garcia-Escobar, C.H.; Hernandez-Martinez, D. [Centro de Investigacion en Ingenieria y Ciencias Aplicadas, Universidad Autonoma del Estado de Morelos (UAEM), Av. Universidad 1001, Col. Chamilpa, C.P. 62210 Cuernavaca, Morelos (Mexico); Linzaga-Elizalde, I. [Centro de Investigaciones Quimicas (CIQ) de la UAEM (Mexico); Cadenas-Pliego, G. [Centro de Investigacion en Quimica Aplicada, Saltillo, Coahuila (Mexico)

    2012-09-20

    In this work, CoolMate microwave synthesis system was employed to synthesize soluble poly(3-hexylthiophene) by direct oxidation of 3-hexylthiophene monomer with FeCl{sub 3} as oxidant. P3HT was synthesized varying reaction time by 2 h, 1 h and 0.5 h. According to the results optimal microwave radiation time for synthesis was 1 h. On the other hand, P3HT was synthesized in two different solvents: chloroform (CHCl{sub 3}) and dichloromethane (CH{sub 2}Cl{sub 2}). The obtained yields depend on the solvent and the reaction time used in the synthesis, microwave-assisted synthesis leads to outstanding increase in yield (with dichloromethane solvent). Homogeneous thin films were prepared by spin-coating technique from toluene. Physicochemical characterization of P3HT polymers was carried out: changes in weight molecular distribution and polydispersity were obtained by HPLC (high-performance liquid chromatography); dyads and triads percent were analyzed by NMR (nuclear magnetic resonance). Surface topographical changes were obtained by atomic force microscopy (AFM). AFM images revealed that the surface morphology depends on synthesis method, reaction time and solvent used. Finally the samples were characterized by thermogravimetric analysis (TGA) and ultraviolet-visible analysis (UV-vis). Compared with the traditional method (without microwave), this method provided considerable decrease in the reaction time, both lower polydispersity and molecular weight, less volume of solvents for the synthesis, as well as more alternatives for solvent choice. The results confirmed the versatility of the procedure by microwave, which yields polymeric materials in 1 h and has no adverse effects on the polymers quality.

  12. Biodiesel and FAME synthesis assisted by microwaves: Homogeneous batch and flow processes

    Energy Technology Data Exchange (ETDEWEB)

    J. Hernando; P. Leton; M.P. Matia; J.L. Novella; J. Alvarez-Builla [Universidad de Alcala, Madrid (Spain). Planta Piloto de Quimica Fina

    2007-07-15

    Fatty acids methyl esters (FAME) have been prepared under microwave irradiation, using homogeneous catalysis, either in batch or in a flow system. The quality of the biodiesel obtained has been confirmed by GC analysis of the isolated product. While the initial experiments have been performed in a small scale laboratory batch reactor, the best experiment has been straightforward converted into a stop-flow process, by the use of a microwave flow system. Compared with conventional heating methods, the process using microwaves irradiation proved to be a faster method for alcoholysis of triglycerides with methanol, leading to high yields of FAME. Short communication. 19 refs., 2 tabs.

  13. Comparison of Conventional Microwave and Focused Microwave-assisted Extraction to Enhance the Efficiency of the Extraction of Antioxidant Flavonols from Jocote Pomace (Spondias purpurea L.).

    Science.gov (United States)

    Reis, Letícia C B; Carneiro, Larissa M; Branco, Carla R C; Branco, Alexsandro

    2015-06-01

    Jocote (Spondias purpurea L.) is rich in phenolic compounds which have antioxidant properties. The focused microwave-assisted extraction (FMAE) was compared with the conventional microwave-assisted extraction (MAE) to obtain flavonols from jocote pomace. The effects of parameters such as the extraction time, the temperature and the composition of the solvent mixture (i.e., the ethanol to water ration) were evaluated and optimized using a statistical experimental design approach. Response surface methodology (RSM) was applied to determine the important effects and interactions of these independent variables on the extractive yield and quantification of some flavonoids. In addition, the antioxidant activity was analyzed. The total phenolic and flavonoid content was determined according to the Folin-Ciocalteu and aluminum chloride methods, respectively. The free radical scavenging activity of the extract was evaluated according to the DPPH assay. The results showed that the optimum extracting parameters used FMAE with extraction time of 20 min, temperature of 68 °C and ethanol composition of 80% in water. Under these conditions, a yield of 3.42% was obtained. Rutin and quercetin were quantified (0.19 mg/mL and 0.024 mg/mL, respectively) through HPLC-DAD. The total phenol and flavonoid contents were found to be 0.897 g GAE/g and 1.271 g QE/g, respectively. In the DPPH scavenging assay, the IC50 value of the extract occurred at 43.10 μg/mL. This study shows that FMAE is suitable as an efficient extraction procedure for the extraction of flavonols from jocote pomace.

  14. Optimization of microwave-assisted extraction for six inorganic and organic arsenic species in chicken tissues using response surface methodology.

    Science.gov (United States)

    Zhang, Wenfeng; Hu, Yuanan; Cheng, Hefa

    2015-09-01

    Response surface methodology was applied to optimize the parameters for microwave-assisted extraction of six major inorganic and organic arsenic species (As(III), As(V), dimethyl arsenic acid, monomethyl arsenic acid, p-arsanilic acid, and roxarsone) from chicken tissues, followed by detection using a high-performance liquid chromatography with inductively coupled mass spectrometry detection method, which allows the simultaneous analysis of both inorganic and organic arsenic species in the extract in a single run. Effects of extraction medium, solution pH, liquid-to-solid ratio, and the temperature and time of microwave-assisted extraction on the extraction of the targeted arsenic species were studied. The optimum microwave-assisted extraction conditions were: 100 mg of chicken tissue, extracted by 5 mL of 22% v/v methanol, 90 mmol/L (NH4 )2 HPO4 , and 0.07% v/v trifluoroacetic acid (with pH adjusted to 10.0 by ammonium hydroxide solution), ramping for 10 min to 71°C, and holding for 11 min. The method has good extraction performance for total arsenic in the spiked and nonspiked chicken tissues (104.0 ± 13.8% and 91.6 ± 7.8%, respectively), except for the ones with arsenic contents close to the quantitation limits. Limits of quantitation (S/N = 10) for As(III), As(V), dimethyl arsenic acid, monomethyl arsenic acid, p-arsanilic acid, and roxarsone in chicken tissues using this method were 0.012, 0.058, 0.039, 0.061, 0.102, and 0.240 mg/kg (dry weight), respectively.

  15. Microwave-Assisted Functionalization of Carbon Nanotubes and Reactive Synthesis of Nanocomposites Project

    Data.gov (United States)

    National Aeronautics and Space Administration — The Offerers will build on their recent innovation of a microwave-induced route to the rapid functionalization, solubilization and reactive synthesis of carbon...

  16. Microwave Assisted Solvent Free Synthesis of Azomethines from Aryl Aldehydes on Melamin Formaldehyde as Solid Support

    Directory of Open Access Journals (Sweden)

    Ramin Rezaei

    2011-01-01

    Full Text Available Various aryl aldehydes underwent prompt one pot conversion into the corresponding azomethines in high yields by reacting with hydroxylamine hydrochloride supported on melamine formaldehyde under microwave irradiation.

  17. Alternative energy input: Mechanochemical, microwave and ultrasound-assisted organic synthesis

    Science.gov (United States)

    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...

  18. Microwave-assisted convenient synthesis of N-arylpyrrolidines in water

    Institute of Scientific and Technical Information of China (English)

    Hong Bo Li; Wu Liang; Lang Liu; Kai Chen; Yi Wu

    2011-01-01

    An efficient and clean synthesis of N-arylpyrrolidines from arylamines and 1,4-dimesyloxybutane was developed using microwave irradiation in an aqueous potassium carbonate medium without any catalyst. The procedure is rapid, simple and convenient.

  19. A Facile Microwave-Assisted Synthesis of Some Fused Pyrimidine Derivatives

    Directory of Open Access Journals (Sweden)

    S. A. Al-Issa

    2014-06-01

    Full Text Available The highly accelerated synthesis of thienopyrimidinones, theino- pyrimidines,thioxotheinopyrimidinones and a thienotriazolopyrimidinone derivatives under microwave irradiation is reported. Compared to conventional conditions, microwaves method offered several advantage likes short time, good yields, simple procedure, mild conditions and easy workup. The structure of synthesized compounds have been characterized on the basis of their elemental analysis and spectral data, and screened for their antimicrobial activity.

  20. Microwave-assisted synthesis of (aminomethylene)bisphosphine oxides and (aminomethylene)bisphosphonates by a three-component condensation

    Science.gov (United States)

    Tajti, Ádám; Dzielak, Anna; Hägele, Gerhard

    2016-01-01

    Summary A practical method was elaborated for the synthesis of (aminomethylene)bisphosphine oxides comprising the catalyst- and solvent-free microwave-assisted three-component condensation of primary amines, triethyl orthoformate and two equivalents of diphenylphosphine oxide. The method is also suitable for the preparation of (aminomethylene)bisphosphonates using (MeO)2P(O)H/(MeO)3CH or (EtO)2P(O)H/(EtO)3CH reactant pairs and even secondary amines. Several intermediates referring to the reaction mechanism together with a few by-products could also be identified. PMID:27559402

  1. Microwave-assisted rapid synthesis of methyl 2,4,5-trimethoxyphenylpropionate, a metabolite of Cordia alliodora.

    Science.gov (United States)

    Sinha, A K; Joshi, B P; Sharma, A; Kumar, J K; Kaul, V K

    2003-12-01

    Microwave assisted condensation of asaronaldehyde (2) with malonic acid in piperidine-AcOH provides 2,4,5-trimethoxycinnamic acid (3) in 87% yield within 4 min, which upon further reduction with PdCl2- HCOOH-aq. NaOH gives 3-(2,4,5-trimethoxy)phenyl propionic acid (4) in 88% yield within 3 min. Esterification of 4 with MeOH-H+ gives methyl 2,4,5-trimethoxyphenylpropionate (1), a metabolite of Cordia alliodora, in 94% yield within 3 min (overall 69% yield).

  2. Microwave-assisted cyclizations promoted by polyphosphoric acid esters: a general method for 1-aryl-2-iminoazacycloalkanes

    Directory of Open Access Journals (Sweden)

    Jimena E. Díaz

    2016-09-01

    Full Text Available The first general procedure for the synthesis of 5 to 7-membered 1-aryl-2-iminoazacycloalkanes is presented, by microwave-assisted ring closure of ω-arylaminonitriles promoted by polyphosphoric acid (PPA esters. 1-Aryl-2-iminopyrrolidines were easily prepared from the acyclic precursors employing a chloroformic solution of ethyl polyphosphate (PPE. The use of trimethylsilyl polyphosphate (PPSE in solvent-free conditions allowed for the synthesis of 1-aryl-2-iminopiperidines and hitherto unreported 1-aryl-2-iminoazepanes. The cyclization reaction involves good to high yields and short reaction times, and represents a novel application of PPA esters in heterocyclic synthesis.

  3. Microwave-assisted synthesis of water-dispersed CdTe/CdSe core/shell type II quantum dots

    OpenAIRE

    Sai Li-Man; Kong Xiang Yang

    2011-01-01

    Abstract A facile synthesis of mercaptanacid-capped CdTe/CdSe (core/shell) type II quantum dots in aqueous solution by means of a microwave-assisted approach is reported. The results of X-ray diffraction and high-resolution transmission electron microscopy revealed that the as-prepared CdTe/CdSe quantum dots had a core/shell structure with high crystallinity. The core/shell quantum dots exhibit tunable fluorescence emissions by controlling the thickness of the CdSe shell. The photoluminescent...

  4. Microwave-assisted synthesis under solvent-free conditions of (E)-2-(Benzo[d]thiazol-2-yl)-3-arylacrylonitriles

    Energy Technology Data Exchange (ETDEWEB)

    Trilleras, Jorge E.; Velasquez, Kelly J.; Pacheco, Dency J., E-mail: jorgetrilleras@mail.uniatlantico.edu.co [Grupo de Investigacion en Compuestos Heterociclicos, Programa de Quimica, Facultad de Ciencias Basicas, Universidad del Atlantico, Barranquilla-Atlantico (Colombia); Quiroga, Jairo; Ortiz, Alejandro [Grupo de Investigacion de Compuestos Heterociclicos, Departamento de Quimica, Universidad del Valle, Cali (Colombia)

    2011-09-15

    A series of (E)-2-(benzo[d]thiazol-2-yl)-3-arylacrylonitriles was synthesized by microwave assisted Knoevenagel condensation under solvent-free conditions from the corresponding 2-(benzo[d]thiazol-2-yl)acetonitrile and aromatic aldehydes with electrondonating/electron withdrawing groups. The reaction times were considerably short and the products obtained in moderate yields (50 to 75%) and good purity. The configuration of the acrylonitrile double bond could not be established by regular NMR methods. However, theoretical studies suggest that the E isomer is more stable than Z, which is in good agreement with some experimental evidences. (author)

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

    Science.gov (United States)

    Gonzalez-Cortes, S; Slocombe, D R; Xiao, T; Aldawsari, A; Yao, B; Kuznetsov, V L; Liberti, E; Kirkland, A I; Alkinani, M S; Al-Megren, H A; Thomas, J M; Edwards, P P

    2016-10-19

    Hydrogen is often described as the fuel of the future, especially for application in hydrogen powered fuel-cell vehicles (HFCV's). However, its widespread implementation in this role has been thwarted by the lack of a lightweight, safe, on-board hydrogen storage material. Here we show that benign, readily-available hydrocarbon wax is capable of rapidly releasing large amounts of hydrogen through microwave-assisted catalytic decomposition. This discovery offers a new material and system for safe and efficient hydrogen storage and could facilitate its application in a HFCV. Importantly, hydrogen storage materials made of wax can be manufactured through completely sustainable processes utilizing biomass or other renewable feedstocks.

  6. Microwave-assisted synthesis of high-loading, highly dispersed Pt/carbon aerogel catalyst for direct methanol fuel cell

    Indian Academy of Sciences (India)

    Zhijun Guo; Hong Zhu; Xinwei Zhang; Fanghui Wang; Yubao Guo; Yongsheng Wei

    2011-06-01

    A Pt supported on carbon aerogel catalyst has been synthesized by the microwave-assisted polyol process. The Pt supported on carbon aerogel catalyst was characterized by high resolution transmission electron microscopy and X-ray diffraction. The results show a uniform dispersion of spherical Pt nanoparticles 2.5–3.0 nm in diameter. Cyclic voltammetry and chronoamperometry were used to evaluate the electrocatalytic activity of the Pt/carbon aerogel catalyst for methanol oxidation at room temperature. The Pt/carbon aerogel catalyst shows higher electrochemical catalytic activity and stability for methanol oxidation than a commercial Pt/C catalyst of the same Pt loading.

  7. Direct Fabrication of Carbon Nanotubes STM Tips by Liquid Catalyst-Assisted Microwave Plasma-Enhanced Chemical Vapor Deposition

    Directory of Open Access Journals (Sweden)

    Fa-Kuei Tung

    2009-01-01

    Full Text Available Direct and facile method to make carbon nanotube (CNT tips for scanning tunneling microscopy (STM is presented. Cobalt (Co particles, as catalysts, are electrochemically deposited on the apex of tungsten (W STM tip for CNT growth. It is found that the quantity of Co particles is well controlled by applied DC voltage, concentration of catalyst solution, and deposition time. Using optimum growth condition, CNTs are successfully synthesized on the tip apex by catalyst-assisted microwave-enhanced chemical vapor deposition (CA-MPECVD. A HOPG surface is clearly observed at an atomic scale using the present CNT-STM tip.

  8. Microwave-assisted cyclizations promoted by polyphosphoric acid esters: a general method for 1-aryl-2-iminoazacycloalkanes

    Science.gov (United States)

    Díaz, Jimena E; Mollo, María C

    2016-01-01

    Summary The first general procedure for the synthesis of 5 to 7-membered 1-aryl-2-iminoazacycloalkanes is presented, by microwave-assisted ring closure of ω-arylaminonitriles promoted by polyphosphoric acid (PPA) esters. 1-Aryl-2-iminopyrrolidines were easily prepared from the acyclic precursors employing a chloroformic solution of ethyl polyphosphate (PPE). The use of trimethylsilyl polyphosphate (PPSE) in solvent-free conditions allowed for the synthesis of 1-aryl-2-iminopiperidines and hitherto unreported 1-aryl-2-iminoazepanes. The cyclization reaction involves good to high yields and short reaction times, and represents a novel application of PPA esters in heterocyclic synthesis. PMID:27829907

  9. Microwave-Assisted Synthesis of (±-Mandelic Acid-d5, Optical Resolution, and Absolute Configuration Determination

    Directory of Open Access Journals (Sweden)

    Claudio Bruno

    2013-01-01

    Full Text Available An efficient microwave-assisted synthesis of (±-mandelic acid-d5 was developed. The racemic mixture was resolved by diastereomeric salt formation using 1-phenylethylamine enantiomers as resolving agents. At each step, the resolution process was checked by determining mandelic acid-d5 enantiomer ee values directly on fractional crystallized diastereomeric salts by chiral capillary electrophoresis analysis. Highly enriched (−- and (+-mandelic acid-d5 (95% and 90% ee, resp. were obtained and their absolute configurations—R and S, respectively—were determined by correlation of the (−-mandelic acid-d5 circular dichroism spectrum to the (R-mandelic acid one.

  10. cis-Apa: a practical linker for the microwave-assisted preparation of cyclic pseudopeptides via RCM cyclative cleavage.

    Science.gov (United States)

    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.

  11. A heterogeneous-catalyst-based, microwave-assisted protocol for the synthesis of 2,2'-bipyridines.

    Science.gov (United States)

    Moore, Lucas R; Vicic, David A

    2008-06-02

    A new method of preparing 2,2'-bipyridines with short reaction times by using microwave assistance and heterogeneous catalysts has been developed. With a Negishi-like protocol, it was found that Ni/Al(2)O(3)-SiO(2) afforded 2,2'-bipyridine products in up to 86% yield in 1 h. Palladium supported on alumina also provided yields of 2,2'-bipyridines comparable to those seen for homogeneous PEPPSI (1,3-diisopropylimidazol-2-ylidene)(3-chloropyridyl)palladium(II)dichloride) and tetrakis(triphenylphosphanyl)palladium complexes.

  12. Microwave assisted synthesis of a novel optical chemosensor for selective Fe{sup 3+} detection

    Energy Technology Data Exchange (ETDEWEB)

    Saleem, Muhammad [Department of Chemistry, Kongju National University, Gongju, Chungnam 314-701 (Korea, Republic of); Kang, Sung Kwon [Department of Chemistry Chungnam National University, Daejeon 305-754 (Korea, Republic of); Lee, Ki Hwan, E-mail: khlee@kongju.ac.kr [Department of Chemistry, Kongju National University, Gongju, Chungnam 314-701 (Korea, Republic of)

    2015-06-15

    Recently, there has been significant interest in the design and development of optical chemosensors for recognition of biologically and environmentally important analytes with high selectivity, sensitivity and low detection-limit because of their fundamental role in medical, environmental and biological applications. Herein, a novel fluorogenic signaling probe 6 for the selective detection of ferric ion in mixed aqueous organic media has been developed through microwave assisted Schiff base formation by reacting 4-amino-3-(2-fluorobenzyl)-1H-1,2,4-triazole-5(4H)-thione 5 with thiophene-2-carbaldehyde. The formation of probe 6 was characterized by FT-IR, {sup 1}H NMR, {sup 13}C NMR, mass spectrometric and single crystal X-ray diffraction analysis. The photophysical results of (Z)-3-(2-fluorobenzyl)-4-[(thiophen-2-ylmethylene) amino]-1H-1,2,4-triazole-5(4H)-thione (6) corroborates its applicability as optical sensing platform for selective Fe{sup 3+} detection in pure organic as well as mixed organic-aqueous media. Through fluorescence titration at 478 nm, we were confirmed that the ligand 6 exhibited remarkable decline in the fluorescence intensity by complexation between 6 and Fe{sup 3+} while it appeared negligible fluorescent quenching in case of the competitive ions in MeOH/water (8:2, v/v, pH 7) at ambient temperature. Meanwhile, the emergence of a new characteristic redshifted signal at 357 nm with gradual increment in the absorption intensity on gentle increase in the ferric ion concentration and continuous shifting in the ligand absorption bands after Fe{sup 3+} addition ascribed the conformational changes in the ligand structure upon Fe{sup 3+} binding. Due to simplicity, low cost, fast response time, considerable sensitivity and robustness, the proposed sensing method might be a practical tool for environmental samples analysis and biological studies. - Highlights: • A novel fluorogenic signaling probe for ferric ion has been developed. • The ligand

  13. Comparison of the Effects of Fluidized-Bed and Fixed-Bed Reactors in Microwave-Assisted Catalytic Decomposition of TCE by Hydrogen

    Directory of Open Access Journals (Sweden)

    Lili Ren

    2012-01-01

    Full Text Available Trichloroethylene (TCE decomposition by hydrogen with microwave heating under different reaction systems was investigated. The activities of a series of catalysts for microwave-assisted TCE hydrodechlorination were tested through the fixed-bed and the fluidized-bed reactor systems. This study found that the different reaction system is suitable for different catalyst type. And there is an interactive relationship between the catalyst type and the reaction bed type.

  14. Decrystallization of Crystals Using Gold "Nano-Bullets" and the Metal-Assisted and Microwave-Accelerated Decrystallization Technique.

    Science.gov (United States)

    Thompson, Nishone; Boone-Kukoyi, Zainab; Shortt, Raquel; Lansiquot, Carisse; Kioko, Bridgit; Bonyi, Enock; Toker, Salih; Ozturk, Birol; Aslan, Kadir

    2016-10-18

    Gout is caused by the overproduction of uric acid and the inefficient metabolism of dietary purines in humans. Current treatments of gout, which include anti-inflammatory drugs, cyclooxygenase-2 inhibitors, and systemic glucocorticoids, have harmful side-effects. Our research laboratory has recently introduced an innovative approach for the decrystallization of biological and chemical crystals using the Metal-Assisted and Microwave-Accelerated Evaporative Decrystallization (MAMAD) technique. In the MAMAD technique, microwave energy is used to heat and activate gold nanoparticles that behave as "nano-bullets" to rapidly disrupt the crystal structure of biological crystals placed on planar surfaces. In this study, crystals of various sizes and compositions were studied as models for tophaceous gout at different stages (i.e., uric acid as small crystals (~10-100 μm) and l-alanine as medium (~300 μm) and large crystals (~4400 μm). Our results showed that the use of the MAMAD technique resulted in the reduction of the size and number of uric acid and l-alanine crystals up to >40% when exposed to intermittent microwave heating (up to 20 W power at 8 GHz) in the presence of 20 nm gold nanoparticles up to 120 s. This study demonstrates that the MAMAD technique can be potentially used as an alternative therapeutic method for the treatment of gout by effective decrystallization of large crystals, similar in size to those that often occur in gout.

  15. Decrystallization of Crystals Using Gold “Nano-Bullets” and the Metal-Assisted and Microwave-Accelerated Decrystallization Technique

    Directory of Open Access Journals (Sweden)

    Nishone Thompson

    2016-10-01

    Full Text Available Gout is caused by the overproduction of uric acid and the inefficient metabolism of dietary purines in humans. Current treatments of gout, which include anti-inflammatory drugs, cyclooxygenase-2 inhibitors, and systemic glucocorticoids, have harmful side-effects. Our research laboratory has recently introduced an innovative approach for the decrystallization of biological and chemical crystals using the Metal-Assisted and Microwave-Accelerated Evaporative Decrystallization (MAMAD technique. In the MAMAD technique, microwave energy is used to heat and activate gold nanoparticles that behave as “nano-bullets” to rapidly disrupt the crystal structure of biological crystals placed on planar surfaces. In this study, crystals of various sizes and compositions were studied as models for tophaceous gout at different stages (i.e., uric acid as small crystals (~10–100 μm and l-alanine as medium (~300 μm and large crystals (~4400 μm. Our results showed that the use of the MAMAD technique resulted in the reduction of the size and number of uric acid and l-alanine crystals up to >40% when exposed to intermittent microwave heating (up to 20 W power at 8 GHz in the presence of 20 nm gold nanoparticles up to 120 s. This study demonstrates that the MAMAD technique can be potentially used as an alternative therapeutic method for the treatment of gout by effective decrystallization of large crystals, similar in size to those that often occur in gout.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

  18. Development of new UV-vis spectroscopic microwave-assisted method for determination of glucose in pharmaceutical samples.

    Science.gov (United States)

    Mabood, Fazal; Hussain, Z; Haq, H; Arian, M B; Boqué, R; Khan, K M; Hussain, K; Jabeen, F; Hussain, J; Ahmed, M; Alharasi, A; Naureen, Z; Hussain, H; Khan, A; Perveen, S

    2016-01-15

    A new UV-Visible spectroscopic method assisted with microwave for the determination of glucose in pharmaceutical formulations was developed. In this study glucose solutions were oxidized by ammonium molybdate in the presence of microwave energy and reacted with aniline to produce a colored solution. Optimum conditions of the reaction including wavelength, temperature, and pH of the medium and relative concentration ratio of the reactants were investigated. It was found that the optimal wavelength for the reaction is 610 nm, the optimal reaction time is 80s, the optimal reaction temperature is 160°C, the optimal reaction pH is 4, and the optimal concentration ratio aniline/ammonium molybdate solution was found to be 1:1. The limits of detection and quantification of the method are 0.82 and 2.75 ppm for glucose solution, respectively. The use of microwaves improved the speed of the method while the use of aniline improved the sensitivity of the method by shifting the wavelength.

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

    Directory of Open Access Journals (Sweden)

    Adam Figiel

    2016-12-01

    Full Text Available 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.

  20. Natural products in Glycyrrhiza glabra (licorice) rhizome imaged at the cellular level by atmospheric pressure matrix-assisted laser desorption/ionization tandem mass spectrometry imaging

    DEFF Research Database (Denmark)

    Li, Bin; Bhandari, Dhaka Ram; Janfelt, Christian

    2014-01-01

    The rhizome of Glycyrrhiza glabra (licorice) was analyzed by high-resolution mass spectrometry imaging and tandem mass spectrometry imaging. An atmospheric pressure matrix-assisted laser desorption/ionization imaging ion source was combined with an orbital trapping mass spectrometer in order...... to obtain high-resolution imaging in mass and space. Sections of the rhizome were imaged with a spatial resolution of 10 μm in the positive ion mode, and a large number of secondary metabolites were localized and identified based on their accurate mass and MS/MS fragmentation patterns. Major tissue...

  1. Immobilization of trypsin on graphene oxide for microwave-assisted on-plate proteolysis combined with MALDI-MS analysis.

    Science.gov (United States)

    Xu, Guobin; Chen, Xiaoyi; Hu, Jianhua; Yang, Pengyuan; Yang, Dong; Wei, Liming

    2012-06-21

    With an ultra-high surface area and abundant functional groups, graphene oxide (GO) provides an ideal substrate for the immobilization of trypsin. We demonstrated that trypsin could be immobilized on GO sheets assisted by polymers as molecular spacers to maintain the activity of the enzyme. And with the trypsin-linked GO as the enzyme immobilization probe, a novel microwave-assisted on-plate digestion method has been developed with subsequent analysis by MALDI-MS. The feasibility and performance of the digestion approach were demonstrated by the proteolysis of standard proteins. The results show that this novel approach substantially accelerated proteolysis and reduced the time required for traditional procedures involving on-plate enzymatic digestion and sample preparation prior to MALDI-MS analysis. The novel digestion approach is simple and efficient, offering great promise for high throughput protein identification.

  2. Synthesis of nanostructured and microstructured ZnO and Zn(OH)2 on activated carbon cloth by hydrothermal and microwave-assisted chemical bath deposition methods

    Science.gov (United States)

    Mosayebi, Elham; Azizian, Saeid; Hajian, Ali

    2015-05-01

    Nanostructured and microstructured ZnO and Zn(OH)2 loaded on activated carbon cloth were synthesized by microwave-assisted chemical bath deposition and hydrothermal methods. By hydrothermal method the deposited sample on carbon fiber is pure ZnO with dandelion-like nanostructures. By microwave-assisted chemical bath method the structure and composition of deposited sample depends on solution pH. At pH = 9.8 the deposited sample on carbon fiber is pure ZnO with flower-like microstructure; but at pH = 10.8 the sample is a mixture of ZnO and Zn(OH)2 with flower-like and rhombic microstructures, respectively. The mechanism of crystal grow by microwave-assisted chemical bath method was investigated by SEM method at both pH.

  3. Analysis of niflumic acid prepared by rapid microwave-assisted evaporation.

    Science.gov (United States)

    Radacsi, Norbert; Stefanidis, Georgios D; Szabó-Révész, Piroska; Ambrus, Rita

    2014-09-01

    Evaporative crystallization is widely applied in several industrial processes, including the pharmaceutical industry. Microwave irradiation can significantly speed up solvent evaporation in these crystallization processes, resulting in reduced particle size due to rapid crystallization. A single-mode microwave setup was used for evaporative crystallization of the model active pharmaceutical ingredient, niflumic acid, and the polymer, polyvinylpirrolidone (PVP). Production of crystals by microwave irradiation offers a modern way for drug formulation, and by reducing the particle size the dissolution rate and bioavailability of the active pharmaceutical ingredient can be enhanced. In this study, a 2.5-fold increase in the dissolution rate of the produced niflumic acid crystals was observed compared to the dissolution rate of the original drug in 120min. When niflumic acid was produced together with the PVP in the microwave system, an amorphous solid dispersion was created with particles in the nano-size range, which showed a 5-fold increase in dissolution rate in 120min compared to the dissolution of the crystalline niflumic acid samples created by the microwave irradiation in the absence of PVP.

  4. Microwaved assisted fast synthesis of n and p-doped Mg{sub 2}Si

    Energy Technology Data Exchange (ETDEWEB)

    Berthebaud, David, E-mail: david.berthebaud@ensicaen.fr; Gascoin, Franck

    2013-06-15

    Magnesium silicide based alloys fast syntheses have been carried out using microwave heating. Precursors were first ball milled powders together under inert gas. Resulting powders were then placed into a glassy carbon crucible before being heated by microwave irradiation. Sintering of the powder was performed by spark plasma method. XRD and SEM/EDS were used to investigate composition, structure and morphology. Thermoelectric performances of the samples were measured in the temperature range of 320–775 K. The doping effect of several elements such as silver, tin, antimony, cobalt and bismuth has been studied. n-Type and p-type Mg{sub 2}Si based materials have been successfully synthesized, with maximum ZT value up to 0.7 and 0.35 at 770 K for a n-type and a p-type sample, respectively. We demonstrate here that the use of microwave irradiation to prepare doped Mg{sub 2}Si is possible, and we discuss here the thermoelectric properties of such samples. - Schematic representation of microwave hybrid heating. - Highlights: • A promising method for fast production of Mg{sub 2}Si in the frame of heat harvesting applications is presented. • A novel technological approaches towards nanostructured materials is proposed. • Thermoelectric properties of Mg{sub 2}Si doped materials prepared under microwave irradiation are discussed.

  5. A novel STM-assisted microwave microscope with capacitance and loss imaging capability.

    Science.gov (United States)

    Imtiaz, Atif; Anlage, Steven M

    2003-04-01

    We report a new technique of scanning capacitance microscopy at microwave frequencies. A near field scanning microwave microscope probe is kept at a constant height of about 1 nm above the sample with the help of scanning tunneling microscope (STM) feedback. The microwaves are incident onto the sample through a coaxial resonator that is terminated at one end with a sharp tip (the same tip is used to conduct STM), and capacitively coupled to a feedback circuit and microwave source at the other end. The feedback circuit keeps the source locked onto the resonance frequency of the resonator and outputs the frequency shift and quality factor change due to property variations of the sample. The spatial resolution due to capacitance variations is congruent with 2.5 nm. The microwave microscope is sensitive to sample sheet resistance, as demonstrated through measurements on a doped silicon sample. We develop a quantitative transmission line model treating the tip to sample interaction as a series combination of capacitance and sheet resistance in the sample.

  6. High yield and facile microwave-assisted synthesis of conductive H{sub 2}SO{sub 4} doped polyanilines

    Energy Technology Data Exchange (ETDEWEB)

    Gizdavic-Nikolaidis, Marija R., E-mail: m.gizdavic@auckland.ac.nz [School of Chemical Sciences, The University of Auckland, Private Bag 92019, Auckland Mail Centre, Auckland, 1142 (New Zealand); Faculty of Physical Chemistry, Studentski Trg 12-16, PO Box 137, 11001, Belgrade (Serbia); Jevremovic, Milutin M. [Public Company Nuclear Facilities of Serbia, 12-14 Mike Petrovica Alasa, Vinca, 11351, Belgrade (Serbia); Milenkovic, Maja [Faculty of Physical Chemistry, Studentski Trg 12-16, PO Box 137, 11001, Belgrade (Serbia); Allison, Morgan C. [School of Chemical Sciences, The University of Auckland, Private Bag 92019, Auckland Mail Centre, Auckland, 1142 (New Zealand); Stanisavljev, Dragomir R. [Faculty of Physical Chemistry, Studentski Trg 12-16, PO Box 137, 11001, Belgrade (Serbia); Bowmaker, Graham A. [School of Chemical Sciences, The University of Auckland, Private Bag 92019, Auckland Mail Centre, Auckland, 1142 (New Zealand); Zujovic, Zoran D. [School of Chemical Sciences, The University of Auckland, Private Bag 92019, Auckland Mail Centre, Auckland, 1142 (New Zealand); MacDiarmid Institute for Advanced Materials and Nanotechnology, Victoria University of Wellington, PO Box 600, Wellington, 6140 (New Zealand); Institute of General and Physical Chemistry, Studentski Trg 12-16, 11001, Belgrade (Serbia)

    2016-04-15

    The microwave-assisted synthesis of polyaniline (PANI) was performed using ammonium persulphate (APS) as oxidizing agent in 0.5 M–2.5 M concentration range of aqueous sulphuric acid (H{sub 2}SO{sub 4}) at 93 W applied microwave power of 10 min duration. The microwave (MW) synthesized PANIs had 3 times higher yield in comparison to PANI samples prepared using a classical method, CS (0 W MW power) at the same temperature for 10 min synthesis duration period. Fourier Transform Infrared (FTIR) and UV–Vis spectroscopies confirmed the formation of PANI structure in all products. The influence of H{sub 2}SO{sub 4} acid dopant on the spin concentration of MW and CS H{sub 2}SO{sub 4} doped PANI samples were examined by EPR spectroscopy, while the morphological characteristics were investigated by using scanning electron microscopy (SEM). XRD results showed amorphous phases in both MW and CS H{sub 2}SO{sub 4} doped PANI samples. Conductivity measurements revealed ∼1.5 times higher conductivity values for MW H{sub 2}SO{sub 4} doped PANI samples in comparison with PANI samples prepared by the CS method under same condition. The influence of sulfate anion in comparison to chloride anion as a dopant on morphological, dopant levels and conductivity properties of MW PANI samples were also investigated. - Highlights: • Nanoporous microwave synthesized doped polyanilines as chemical sensor material. • Morphology and physical properties of polyanilines depend on acid concentration. • Spin concentration is determined by the nature of the polyaniline synthesis.

  7. Microwave-assisted solvothermal synthesis of hierarchical TiO2 microspheres for efficient electro-field-assisted-photocatalytic removal of tributyltin in tannery wastewater.

    Science.gov (United States)

    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 TiO2 microspheres. The synthesis of catalytic materials is based on a self-assembly process induced by microwave-assisted solvothermal reaction. Hierarchical TiO2 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 TiO2 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.

  8. Polarization reversal in BaTiO{sub 3} nanostructures synthesized by microwave-assisted hydrothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Velasco-Davalos, Ivan; Ambriz-Vargas, Fabian [Centre Énergie, Matériaux et Télécommunications, INRS, 1650 Lionel-Boulet, Varennes, Québec J3X1S2 (Canada); Gómez-Yáñez, Carlos [Departamento de Ingeniería en Metalurgia y Materiales, ESIQIE, Instituto Politécnico Nacional, UPALM, Zacatenco, CP 07738 DF, México (Mexico); Thomas, Reji, E-mail: reji.thomas@emt.inrs.ca [Centre Énergie, Matériaux et Télécommunications, INRS, 1650 Lionel-Boulet, Varennes, Québec J3X1S2 (Canada); Ruediger, Andreas, E-mail: ruediger@emt.inrs.ca [Centre Énergie, Matériaux et Télécommunications, INRS, 1650 Lionel-Boulet, Varennes, Québec J3X1S2 (Canada)

    2016-05-15

    Ferroelectric BaTiO{sub 3} nanostructures and thin films were deposited by a microwave assisted hydrothermal process at low temperatures (<250 °C) on metallic Pt/Al{sub 2}O{sub 3}/SiO{sub 2}/Si and Nb:SrTiO{sub 3} (100) substrates. TiO{sub 2} nanoparticles dispersed in the Ba(OH){sub 2} alkaline solution are used as the precursors without any mineralizers. The incorporation of H{sub 2}O{sub 2} into precursor solution served as a strong oxidant and catalyst for the uniform nucleation of BaTiO{sub 3} on the substrate surface. The polycrystalline and epitaxial nature of the films were confirmed by atomic force microscopy and x-ray diffraction studies. We report the ferroelectric behavior of BaTiO{sub 3} films on Nb:SrTiO{sub 3} (100) substrates by piezoresponse force microscopy. - Highlights: • Microwave assisted hydrothermal deposition of highly ordered BaTiO{sub 3} thin films on single crystal substrates. • Fast growth without the needof any mineralizers. • Moderate addition of H{sub 2}O{sub 2} significantly improves the surface coverage. • H{sub 2}O{sub 2} substantially reduces hydrogen incorporation into the film and the associated leakage current. • Out-of-plane polarization reversal demonstrated locally.

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

    Directory of Open Access Journals (Sweden)

    Yuangang Zu

    2012-04-01

    Full Text Available 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.

  10. Microwave assisted synthesis and characterization of Ni/NiO nanoparticles as electrocatalyst for methanol oxidation in alkaline solution

    Science.gov (United States)

    Arunachalam, Prabhakarn; Ghanem, Mohamed A.; Al-Mayouf, Abdullah M.; Al-shalwi, Matar; Hamed Abd-Elkader, Omar

    2017-02-01

    Nickel/Nickel oxide (Ni/NiO) nanoparticles catalyst is prepared by microwave-assisted liquid-phase deposition using ethylene glycol (EG) and water mixture under atmospheric conditions. The physicochemical characterizations of the catalyst carried out by surface area analyzer, x-ray diffraction (XRD), x-ray photoelectron spectroscopy (XPS), electron microscopes measurements suggest the formation of crystalline nanoparticles structure of NiO. The surface area of Ni/NiO prepared using EG/water mixture reaches 70 m2 g-1 which is 2-fold enhsancement in surface area in comparison with NiO prepared in pure EG and an order of magnitude higher than that of bulk nickel prepared in pure water. The methanol electro-oxidation activity of the Ni/NiO nanoparticles obtained in EG/water mixture displayed more than 4-fold increase in oxidation current at 1.7 V versus RHE in comparison with NiO nanoparticles obtained in EG and 20-fold increase compared to bulk nickel catalyst concord with the enhancement of electro-active surface area. The results show the Ni/NiO nanoparticles produced by microwave assisted synthesis has superior activity for methanol oxidation in alkaline solution over the other nickel based catalysts and has potential for mass production.

  11. Optimization of microwave-assisted extraction with saponification (MAES) for the determination of polybrominated flame retardants in aquaculture samples.

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

  13. Microwave-assisted hydrothermal synthesis of CePO{sub 4} nanostructures: Correlation between the structural and optical properties

    Energy Technology Data Exchange (ETDEWEB)

    Palma-Ramírez, D. [Instituto Politécnico Nacional, CICATA-Unidad Altamira, Km 14.5, Carretera Tampico-Puerto Industrial Altamira, C.P. 89600 Altamira, Tamps (Mexico); Domínguez-Crespo, M.A., E-mail: mdominguezc@ipn.mx [Instituto Politécnico Nacional, CICATA-Unidad Altamira, Km 14.5, Carretera Tampico-Puerto Industrial Altamira, C.P. 89600 Altamira, Tamps (Mexico); Torres-Huerta, A.M. [Instituto Politécnico Nacional, CICATA-Unidad Altamira, Km 14.5, Carretera Tampico-Puerto Industrial Altamira, C.P. 89600 Altamira, Tamps (Mexico); Dorantes-Rosales, H. [Instituto Politécnico Nacional, ESIQIE, Departamento de Metalurgia, C.P. 07300 México D.F. (Mexico); Ramírez-Meneses, E. [Universidad Iberoamericana, Departamento de Ingeniería y Ciencias Químicas, Prolongación Paseo de la Reforma 880, Lomas de Santa Fe, C.P. 01219 México D.F. (Mexico); Rodríguez, E. [Instituto Politécnico Nacional, CICATA-Unidad Altamira, Km 14.5, Carretera Tampico-Puerto Industrial Altamira, C.P. 89600 Altamira, Tamps (Mexico)

    2015-09-15

    Highlights: • An enhancement in the hydrothermal synthesis for obtaining of CePO{sub 4} is presented. • Microwave energy can replace the energy by convection for obtaining CePO{sub 4}. • CePO{sub 4} demonstrates to be an option to increase the optical properties of polymers. • Adjusting the pH, the sintering process is not necessary to obtain the desire phase. • CePO{sub 4} morphologies undergo evolution from nanorods to semispherical nanoparticles. - Abstract: In this work, the microwave-assisted hydrothermal method is proposed as an alternative to the synthesis of cerium phosphate (CePO{sub 4}) nanostructures to evaluate the influence of different synthesis parameters on both the structural and optical properties. In order to reach this goal, two different sets of experiments were designed, varying the reaction temperature (130 and 180 °C), synthesis time (15 and 30 min) and sintering temperature (400 and 600 °C), maintaining a constant pH = 3. Thereafter, two experimental conditions were selected to assess changes in the properties of CePO{sub 4} nanopowders with pH (1, 5, 9 and 11). The crystal structure and morphology of the nanostructures were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM), respectively. Diffuse reflectance properties of CePO{sub 4} with different microstructures were studied. The results demonstrated that by using the microwave-assisted hydrothermal method, the shape, size and structural phase of CePO{sub 4} can be modulated by using relatively low synthesis temperatures and short reaction times, and depending on pH, a sintering process is not needed to obtain either a desired phase or size. Under the selected experimental conditions, the materials underwent an evolution from nanorods to semispherical nanoparticles, accompanied by a phase transition from hexagonal to monoclinic.

  14. Microwave-assisted synthesis of the anticancer drug cisplatin, cis-[Pt(NH3)2Cl2].

    Science.gov (United States)

    Petruzzella, Emanuele; Chirosca, Cristian V; Heidenga, Cameron S; Hoeschele, James D

    2015-02-21

    A microwave-assisted synthesis of cisplatin, cis-[Pt(NH3)2Cl2], has been developed and optimized on both a 0.2 and 0.05 millimolar scale. The optimized synthetic procedure was modeled after the Lebedinskii-Golovnya method and is suitable for incorporating the radionuclide, (195m)Pt, into cisplatin for biological studies. Highest yields (47%) and purity are obtained using a K2PtCl4 : NH4OAc : KCl molar ratio of 1 : 4 : 2 at a temperature of 100 °C. The entire synthesis and purification procedure requires approximately 80 min. At a reaction temperature of 150 °C, the trans isomer is the exclusive product, suggesting that complexes of the general form, trans-[Pt(RNH2)2Cl2], can be synthesized directly from K2PtCl4 using [RNH3]OAc (R = alkyl or aryl moieties) via a microwave process. Two novel separation procedures have been developed which efficiently remove the major impurity (1 : 1 Magnus-type salt) from the crude reaction product, yielding a product of purity comparable to that obtained by the Dhara method and suitable for biological studies. These procedures are applicable to both the micro- and macro-scale of synthesis. The question of whether this microwave-assisted synthesis of cisplatin will be a preferred method for incorporating (195m)Pt into cisplatin is yet to be determined.

  15. Decomposition of the mixed rare earth concentrate by microwave-assisted method

    Institute of Scientific and Technical Information of China (English)

    黄宇坤; 张廷安; 刘江; 豆志河; 田俊行

    2016-01-01

    A novel process was proposed to strengthen the decomposition of the mixed rare earth concentrate by utilizing the micro-wave radiation. Mineralogical information on the mechanisms by which microwave heating improved the leaching behavior of rare earth elements (REEs),and an interpretation of the interrelationship between mineralogy, decomposition process, and leaching proc-ess were provided in this study. The influences of the temperature, time of microwave heating and contents of NaOH (mass ratio of NaOH to mixed rare earth concentrate) on the decomposition of mixed rare earth concentrate were investigated. The results revealed that the temperature was the main factor affecting the decomposition process. The recovery of REEs by hydrochloric acid leaching reached 93.28% under the microwave heating conditions: 140 ºC, 30 min and 35.35% NaOH. The BET specific surface area and SEM analysis indicated that the particles of mixed rare earth concentrate were non-hole, while the particles presented a porous structure af-ter heating the concentrate by microwave radiation. For the microwave treated sample after water leaching, the BET specific surface area was 11.04 m2/g, which was higher than the corresponding values (6.94 m2/g) for the mixed rare earth concentrate. This result could be attributed to the phase changes of bastnaesite and monazite, and a number of cracks induced by thermal stress. The increase of BET specific surface area resulted in an increase of the recovery of REEs by promoting interaction within the system of acid leaching.

  16. Microwave-assisted McMurry polymerization utilizing low-valent titanium for the synthesis of poly 2,6-[1,5-bis(dodecyloxy)naphthylene vinylene] (PNV)

    DEFF Research Database (Denmark)

    Thomas, Henrik; Stuhr-Hansen, Nicolai; Westerlund, Fredrik;

    2009-01-01

    Poly 2,6-[1,5-bis(dodecyloxy)naphthylene vinylene] is synthesized by microwave-assisted McMurry polymerization utilizing low-valent titanium generated from titanium tetrachloride and zinc. The obtained polymer is fluorescent with an average molecular weight of approximately 65,000 g/mol and a pol......Poly 2,6-[1,5-bis(dodecyloxy)naphthylene vinylene] is synthesized by microwave-assisted McMurry polymerization utilizing low-valent titanium generated from titanium tetrachloride and zinc. The obtained polymer is fluorescent with an average molecular weight of approximately 65,000 g...

  17. Emergent stent-assisted angioplasty of extracranial internal carotid artery and intracranial stent-based thrombectomy in acute tandem occlusive disease: technical considerations.

    Science.gov (United States)

    Cohen, José E; Gomori, Moshe; Rajz, Gustavo; Moscovici, Samuel; Leker, Ronen R; Rosenberg, Shai; Itshayek, Eyal

    2013-09-01

    Tandem occlusions of the internal carotid artery (ICA) and a major intracranial artery respond poorly to intravenous thrombolytic therapy, and are usually managed by endovascular means. This study describes experience with stent-assisted endovascular ICA revascularization and stent-based thrombectomy. In patients with tandem ICA-middle cerebral artery (MCA)/distal ICA occlusion, the carotid occlusion was recanalized by primary angioplasty and stent implantation, and the distal occlusion by stent-based thrombectomy. Two variant techniques are described. Seven consecutive patients, mean age 64.1 years (range 49-75) and mean admission National Institutes of Health Stroke Scale score of 23, were included. Occlusion sites were tandem proximal ICA and MCA trunk (six patients) and tandem proximal left ICA and ICA terminus (one patient). Complete recanalization with complete perfusion (Thrombolysis in Myocardial Infarction [TIMI] 3, Thrombolysis in Cerebral Infarction [TICI] 3) was achieved in six patients and partial recanalization with partial perfusion (TIMI 2, TICI 2A) in one. Mean time to therapy was 4.9 h (range 3-6.5); mean time to recanalization was 55 min (range 38-65 min). CT performed 1 day after recanalization showed cortical sparing (>90% of the cortex at risk) in seven patients. Five patients (72%) presented with good clinical outcome (modified Rankin Scale (mRS) score 0-2) at 1 month; one patient (patient No 7) reached an mRS score of 3 and one patient died. In selected cases of acute ICA occlusion and concomitant major vessel embolic stroke, angioplasty and stenting of the proximal occlusion and stent-based thrombectomy of the intracranial occlusion may be feasible, effective and safe, and provide early neurological improvement. Further experience and prospective studies are warranted.

  18. Microwave-Assisted Synthesis of Some Quinoxaline-Incorporated Schiff Bases and Their Biological Evaluation

    Directory of Open Access Journals (Sweden)

    L. Achutha

    2013-01-01

    Full Text Available Quinoxaline-incorporated Schiff bases (4a–j were synthesized by the condensation of 2-[(3-methylquinoxalin-2-yloxy]acetohydrazide (3 with indole-3-carbaldehyde, furfuraldehyde, 5-(4-nitrophenyl-2-furfuraldehyde, and substituted benzaldehydes under conventional and microwave irradiation methods. The microwave method was found to be remarkably successful with higher yields, less reaction time, and environmentally friendly compared to conventional heating method. The chemical structures of the synthesized compounds have been confirmed by analytical and spectral data. All the compounds have been evaluated for antitubercular and anti-inflammatory activities.

  19. Mesoporous Silica-Supported Sulfonyldiamine Ligand for Microwave-Assisted Transfer Hydrogenation

    Directory of Open Access Journals (Sweden)

    Shaheen M. Sarkar

    2015-01-01

    Full Text Available N-Sulfonyl-1,2-diamine ligands, derived from 1,2-diaminocyclohexane and 1,2-diaminopropane, were immobilized onto mesoporous SBA-15 silica. The SBA-15-supported sulfonyldiamine-Ru complex was prepared in situ under microwave heating at 60 W for 3 min. The prepared sulfonyldiamine-Ru complex was used as an efficient catalyst for the transfer hydrogenation of ketones to the corresponding secondary alcohols. The heterogeneous complex showed extremely high catalytic activity with 99% conversion rate under microwave heating condition. The complexes were regenerated by simple filtration and reused two times without significant loss of activity.

  20. Microwave-Assisted Fabrication of γ-Fe2O3 Nanoparticles from

    Directory of Open Access Journals (Sweden)

    Mohammad Kooti

    2011-01-01

    Full Text Available Maghemite (γ-Fe2O3 nanoparticles which have a wide range of applications were fabricated by microwave heating of acetylacetonato iron (III precursor. The precursor is very easy to make, and on irradiation by microwave decomposes to maghemite nanoparticles. The as-prepared γ-Fe2O3 nanostructured has been characterized by X-ray powder diffraction, energy dispersive X-ray spectroscopy (EDX, scanning electron microscope (SEM and transmission electron microscopy (TEM techniques. The maghemite nanoparticles were obtained in high yield and purity and the average size of the particles was estimated to be about 13 nm.

  1. Microwave-Assisted Synthesis of Bioactive Six-Membered Heterocycles and Their Fused Analogues

    Directory of Open Access Journals (Sweden)

    Mohsine Driowya

    2016-04-01

    Full Text Available This review describes the formation of six-membered heterocyclic compounds and their fused analogues under microwave activation using modern organic transformations including cyclocondensation, cycloaddition, multicomponents and other modular reactions. The review is divided according to the main heterocycle types in order of increasing complexity, starting with heterocyclic systems containing one, two and three heteroatoms and their fused analogues. Recent microwave applications are reviewed, with special focus on the chemistry of bioactive compounds. Selected examples from the 2006 to 2015 literature are discussed.

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

    Science.gov (United States)

    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.

  3. Microwave-Assisted Esterification: A Discovery-Based Microscale Laboratory Experiment

    Science.gov (United States)

    Reilly, Maureen K.; King, Ryan P.; Wagner, Alexander J.; King, Susan M.

    2014-01-01

    An undergraduate organic chemistry laboratory experiment has been developed that features a discovery-based microscale Fischer esterification utilizing a microwave reactor. Students individually synthesize a unique ester from known sets of alcohols and carboxylic acids. Each student identifies the best reaction conditions given their particular…

  4. Field emission characteristics of SnO2/CNT composite prepared by microwave assisted wet impregnation

    CSIR Research Space (South Africa)

    Kesavan Pillai, Sreejarani

    2012-01-01

    Full Text Available nanoparticles on CNTs, which was consistent with the results from X-ray diffraction. Enhanced field emission performance was observed for SnO2/CNT composite prepared by a microwave method when compared to pure CNTs and SnO2/CNT prepared by conventional wet...

  5. Microwave-assisted pretreatment of woody biomass with ammonium molybdate activated by H2O2.

    Science.gov (United States)

    Verma, Pradeep; Watanabe, Takahito; Honda, Yoichi; Watanabe, Takashi

    2011-02-01

    Pretreatments for enzymatic saccharification are crucial for the establishment of lignocellulosic biorefineries. In this study, we focused on ammonium ions and peroxometal complexes as potential delignifying agents. We first examined the pretreatment of beech wood with nine different ammonium salts in the presence of H(2)O(2). Significant pretreatment effects were found only for ammonium molybdate, which is transformed to a peroxometal complex on reacting with H(2)O(2). Since microwave sensitizer effects are expected for (peroxo)molybdate, beech wood was pretreated using external heating and microwave irradiation. As a result, a maximum sugar yield of 59.5% was obtained by microwave irradiation at 140°C for 30 min, while external heating in an autoclave gave a sugar yield of 41.8%. We also found that an ammonium ion is the key counterion accelerating the pretreatment with molybdate. These results highlight the powerful selective delignifying capability of the H(2)O(2)-activated ammonium molybdate system energized by microwave radiation.

  6. Student-Driven Design of Peptide Mimetics: Microwave-Assisted Synthesis of Peptoid Oligomers

    Science.gov (United States)

    Pohl, Nicola L. B.; Kirshenbaum, Kent; Yoo, Barney; Schulz, Nathan; Zea, Corbin J.; Streff, Jennifer M.; Schwarz, Kimberly L.

    2011-01-01

    An experiment for the undergraduate organic laboratory is described in which peptide mimetic oligomers called "peptoids" are built stepwise on a solid-phase resin. Students employ two modern strategies to facilitate rapid multistep syntheses: solid-phase techniques to obviate the need for intermediate purifications and microwave irradiation to…

  7. Microwave-Assisted Synthesis of Poly(Aspartic Acid-Itaconic Acid) Copolymer and Its Characterization

    Institute of Scientific and Technical Information of China (English)

    Zhang Yuling; Jiang Yijian; Hu Zhiguang; Wei Hanxiao; Guo Jun; Wang Jilong

    2016-01-01

    Poly(aspartic acid-itaconic acid) copolymer was synthesized from aspartic acid (Asp) and itaconic acid (Ita) un-der microwave irradiation. The effects of microwave power, microwave irradiation time, molar ratio of itaconic acid and aspartic acid, catalyst type, catalyst and organic solvent content on copolymer yield, and the performance for inhibition of CaCO3 fouling were investigated. It was found that the product yield achieved a highest record of 95% when the amount of catalyst NaH2PO4was 0.012 mol, the amount of organic solvent propylene carbonate was 16 mL, the molar ratio of Asp/Ita was 3:1, the microwave output power was 1200 W and the irradiation time was 5.5 min. And the product performance for inhibition of calcium carbonate also reached a highest value of 94.38%. Structural characterization of the product showed that the product was the aspartic acid-itaconic acid copolymer.

  8. Microwave-assisted base-free synthesis of trans-cinnamic acids using hypervalent iodonium salts

    Institute of Scientific and Technical Information of China (English)

    Min Zhu; Chao Shentu; Zhong Shi Zhou

    2007-01-01

    A fast and convenient base-free Heck reaction of acrylic acid with hypervalent iodonium salts was achieved under microwave irradiation in water, providing a simple method for the synthesis of trans-cinnamic acids in good yields in short time.

  9. Microwave-assisted synthesis of bio-active heterocycles in aqueous media

    KAUST Repository

    Polshettiwar, Vivek

    2010-01-01

    Synthesis of bio-active heterocycles and fine chemicals in aqueous media are one of the best solutions for the development of green and sustainable protocols. To illustrate the advantages of aqueous MW chemistry in heterocycle synthesis, in this chapter, various synthetic pathways developed in recent years in aqueous reaction media using microwave irradiation are described.

  10. Microwave-assisted Bohlmann–Rahtz synthesis of highly-substituted 2-aminonicotinates

    OpenAIRE

    Bagley, Mark C; Alnomsy, Ayed; Temple, Scott J

    2016-01-01

    Microwave irradiation of 2-carbethoxyacetamidine and an ethynyl ketone under acidic or basic conditions in ethanol at 150 °C for 1.5 h facilitated Bohlmann-Rahtz pyridine synthesis to give highly-substituted ethyl 2 aminonicotinates with total regiocontrol and in reasonable to excellent yield, following purification by immobiliza tion upon an acidic resin.

  11. Microwave-assisted silica-promoted solvent-free synthesis of triazoloquinazolinone and benzimidazoquinazolinones

    Indian Academy of Sciences (India)

    G Krishnamurthy; K V Jagannath

    2013-07-01

    The derivative of triazolo/benzimidazoquinazolinones is prepared via silica-promoted solvent-free method using microwave irradiation with an excellent yield. The newly synthesized compounds were characterized by various techniques like IR, NMR and Mass spectroscopy. The compound with 1a was crystallized and analysed by single crystal X-ray diffraction studies.

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

    Science.gov (United States)

    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.

  13. Microwave-assisted headspace single-drop microextration of chlorobenzenes from water samples.

    Science.gov (United States)

    Vidal, Lorena; Domini, Claudia E; Grané, Nuria; Psillakis, Elefteria; Canals, Antonio

    2007-05-29

    A one-step and in-situ sample preparation method used for quantifying chlorobenzene compounds in water samples has been developed, coupling microwave and headspace single-drop microextraction (MW-HS-SDME). The chlorobenzenes in water samples were extracted directly onto an ionic liquid single-drop in headspace mode under the aid of microwave radiation. For optimization, a Plackett-Burman screening design was initially used, followed by a mixed-level factorial design. The factors considered were: drop volume, aqueous sample volume, stirring speed, ionic strength, extraction time, ionic liquid type, microwave power and length of the Y-shaped glass-tube. The optimum experimental conditions found from this statistical evaluation were: a 5 microL microdrop of 1-hexyl-3-methylimidazolium hexafluorophosphate exposed for 20 min to the headspace of a 30 mL aqueous sample, irradiated by microwaves at 200 W and placed in a 50 mL spherical flask connected to a 25 cm Y-shaped glass-tube. Under the optimised experimental conditions, the response of a high performance liquid chromatographic system was found to be linear over the range studied and with correlation coefficients ranging between 0.9995 and 0.9999. The method showed a good level of repeatability, with relative standard deviations varying between 2.3 and 8.3% (n=5). Detection limits were found in the low microg L(-1) range varying between 0.016 and 0.039 microg L(-1). Overall, the performance of the proposed method demonstrated the favourable effect of microwave sample irradiation upon HS-SDME. Finally, recovery studies from different types of environmental water samples revealed that matrix had little effect upon extraction.

  14. Microwave-assisted headspace single-drop microextration of chlorobenzenes from water samples

    Energy Technology Data Exchange (ETDEWEB)

    Vidal, Lorena [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain); Domini, Claudia E. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain); Grane, Nuria [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain); Psillakis, Elefteria [Department of Environmental Engineering, Technical University of Crete, Polytechneioupolis, GR-73100 Chania, Crete (Greece); Canals, Antonio [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain)]. E-mail: a.canals@ua.es

    2007-05-29

    A one-step and in-situ sample preparation method used for quantifying chlorobenzene compounds in water samples has been developed, coupling microwave and headspace single-drop microextraction (MW-HS-SDME). The chlorobenzenes in water samples were extracted directly onto an ionic liquid single-drop in headspace mode under the aid of microwave radiation. For optimization, a Plackett-Burman screening design was initially used, followed by a mixed-level factorial design. The factors considered were: drop volume, aqueous sample volume, stirring speed, ionic strength, extraction time, ionic liquid type, microwave power and length of the Y-shaped glass-tube. The optimum experimental conditions found from this statistical evaluation were: a 5 {mu}L microdrop of 1-hexyl-3-methylimidazolium hexafluorophosphate exposed for 20 min to the headspace of a 30 mL aqueous sample, irradiated by microwaves at 200 W and placed in a 50 mL spherical flask connected to a 25 cm Y-shaped glass-tube. Under the optimised experimental conditions, the response of a high performance liquid chromatographic system was found to be linear over the range studied and with correlation coefficients ranging between 0.9995 and 0.9999. The method showed a good level of repeatability, with relative standard deviations varying between 2.3 and 8.3% (n = 5). Detection limits were found in the low {mu}g L{sup -1} range varying between 0.016 and 0.039 {mu}g L{sup -1}. Overall, the performance of the proposed method demonstrated the favourable effect of microwave sample irradiation upon HS-SDME. Finally, recovery studies from different types of environmental water samples revealed that matrix had little effect upon extraction.

  15. Development, comparison and application of sorbent-assisted accelerated solvent extraction, microwave-assisted extraction and ultrasonic-assisted extraction for the determination of polybrominated diphenyl ethers in sediments.

    Science.gov (United States)

    Song, Shanjun; Shao, Mingwu; Tang, Hua; He, Yajuan; Wang, Weihua; Liu, Liliang; Wu, Jiajia

    2016-12-02

    Fast and selective analytical methods were developed based on sorbent-assisted mechanism and microwave-assisted extraction (SA-MAE), accelerate solvent extraction (SA-ASE) and ultrasonic-assisted extraction (SA-UAE) for the determination of polybrominated diphenyl ethers (PBDEs) in sediments. The experimental parameters, such as extraction conditions and sorbent amounts, were optimized according to Taguchi Orthogonal Arrays. The accuracy of developed SA-methods was a satisfactory ranging from 71% to 118%. The inter/intra-day RSDs were extraction intensity may produce various matrix effects. In addition, the developed SA-ASE method was successfully applied on real environmental samples collected from a typical polluted area. The data and calculation suggested local environmental contamination pattern and potential pollution source.

  16. A MICROWAVE-ASSISTED LIQUEFACTION AS A PRETREATMENT FOR THE BIOETHANOL PRODUCTION BY THE SIMULTANEOUS SACCHARIFICATION AND FERMENTATION OF CORN MEAL

    Directory of Open Access Journals (Sweden)

    Svetlana Nikolić

    2008-11-01

    Full Text Available A microwave-assisted liquefaction as a pretreatment for the bioethanol production by the simultaneous saccharification and fer entation (SSF of corn meal using Saccharomyces cerevisiae var. ellipsoideus yeast in a batch system was studied. An optimal power of microwaves of 80 W and the 5-min duration of the microwave treatment were selected by following the concentration of glucose released from the corn meal suspensions at hidromodul of 1:3 (corn meal to water ratio in the liquefaction step. The results indicated that the microwave pretreatment could increase the maximum ethanol concentration produced in the SSF process for 13.4 %. Consequently, a significant increase of the ethanol productivity on substrate (YP/S, as well as the volumetric ethanol productivity (P in this process, could be achieved

  17. Comparison of heat and mass transfer of different microwave-assisted extraction methods of essential oil from Citrus limon (Lisbon variety) peel.

    Science.gov (United States)

    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.

  18. Microwave assisted synthesis of sheet-like Cu/BiVO{sub 4} and its activities of various photocatalytic conditions

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Xi [College of Materials Science and Engineering, Qiqihar University, Qiqihar 161006 (China); College of Chemistry and Chemical Engineering, Qiqihar University, Qiqihar 161006 (China); Li, Li, E-mail: qqhrll@163.com [College of Materials Science and Engineering, Qiqihar University, Qiqihar 161006 (China); College of Chemistry and Chemical Engineering, Qiqihar University, Qiqihar 161006 (China); College of Heilongjang Province Key Laboratory of Fine Chemicals, Qiqihar University, Qiqihar 161006 (China); Yi, Tingting [College of Chemistry and Chemical Engineering, Qiqihar University, Qiqihar 161006 (China); Zhang, WenZhi [College of Materials Science and Engineering, Qiqihar University, Qiqihar 161006 (China); College of Chemistry and Chemical Engineering, Qiqihar University, Qiqihar 161006 (China); Zhang, Xiuli; Wang, Lili [College of Chemistry and Chemical Engineering, Qiqihar University, Qiqihar 161006 (China)

    2015-09-15

    The Cu/BiVO{sub 4} photocatalyst with visible-light responsivity was prepared by the microwave-assisted hydrothermal method. The phase structures, chemical composition and surface physicochemical properties were well-characterized via X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV–vis diffuse reflectance absorption (UV–vis/DRS), scanning electron microscopy (SEM), and N{sub 2} adsorption–desorption tests. Results indicate that the crystal structure of synthetic composite materials is mainly monoclinic scheelite BiVO{sub 4}, which is not changed with the increasing doping amount of Cu. In addition, the presence of Cu not only enlarges the range of the composite materials under the visible-light response, but also increases the BET value significantly. Compared to pure BiVO{sub 4}, 1% Cu/BiVO{sub 4}-160 performs the highest photocatalytic activity to degrade methylene blue under the irradiation of ultraviolet, visible and simulated sunlight. In addition, the capture experiments prove that the main active species was superoxide radicals during photocatalytic reaction. Moreover, the 1% Cu/BiVO{sub 4}-160 composite shows good photocatalytic stability after three times of recycling. - Graphical abstract: A series of BiVO{sub 4} with different amounts of Cu doping were prepared by the microwave-assisted method, moreover, which performed the high photocatalytic activities to degrade methylene blue under multi-mode. - Highlights: • A series of Cu/BiVO{sub 4} with different amounts of Cu doping were prepared by microwave-assisted synthesis. • The morphologies of as-samples were different with the amount of Cu doping increased. • Compared with pure BiVO{sub 4}, as-Cu/BiVO{sub 4} showed stronger absorption in the visible light region obviously. • 1% Cu/BiVO{sub 4}-160 performed the high photocatalytic activities to degrade methylene blue under multi-mode. • OH{sup •} and h{sup +} both play important roles in the photocatalytic reaction.

  19. 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.

    Science.gov (United States)

    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(NH(3))(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 degrees 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(NH(3))(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 approximately 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).

  20. 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

    Science.gov (United States)

    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).